U.S. patent application number 14/452478 was filed with the patent office on 2014-12-11 for material release system.
This patent application is currently assigned to Haviland Products Company. The applicant listed for this patent is Haviland Products Company. Invention is credited to Kenneth E. DeLine, Jeffrey W. Putt, John E. Walls.
Application Number | 20140364352 14/452478 |
Document ID | / |
Family ID | 32869569 |
Filed Date | 2014-12-11 |
United States Patent
Application |
20140364352 |
Kind Code |
A1 |
Walls; John E. ; et
al. |
December 11, 2014 |
Material Release System
Abstract
A material encapsulation and release system having a first zone
(1) containing a first amount of material (2) bound by a first
capsule wall (3) and, if desired, a second zone (4) containing a
second amount of material (5) bound by a second capsule wall (6),
each capsule wall responsive to similar or dissimilar activation
means (7) to release the first amount of material (2) in the first
zone (1) and the second amount of material (5) in the second zone
(4).
Inventors: |
Walls; John E.; (Kentwood,
MI) ; Putt; Jeffrey W.; (Denver, CO) ; DeLine;
Kenneth E.; (Avon, CO) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
Haviland Products Company |
Grand Rapids |
MI |
US |
|
|
Assignee: |
Haviland Products Company
Grand Rapids
MI
|
Family ID: |
32869569 |
Appl. No.: |
14/452478 |
Filed: |
August 5, 2014 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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10544586 |
Aug 4, 2005 |
8834934 |
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PCT/US04/03834 |
Feb 11, 2004 |
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14452478 |
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60446908 |
Feb 11, 2003 |
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Current U.S.
Class: |
510/100 |
Current CPC
Class: |
A61K 8/24 20130101; A61K
8/37 20130101; A61K 2800/26 20130101; A61K 8/33 20130101; A61Q
19/10 20130101; A61K 9/5057 20130101; A61K 8/11 20130101; A61K
8/365 20130101; A61K 2800/45 20130101; A61K 9/5073 20130101; A61K
9/5084 20130101; A61K 2800/28 20130101 |
Class at
Publication: |
510/100 |
International
Class: |
A61K 8/11 20060101
A61K008/11; A61K 8/37 20060101 A61K008/37; A61K 8/33 20060101
A61K008/33; A61Q 19/10 20060101 A61Q019/10 |
Claims
1-130. (canceled)
131. A material release system, comprising: an amount of material;
a capsule having a capsule wall which bounds said amount of
material, wherein said capsule releases said amount of material in
response to an activation element; a liquid carrier having a pH,
said liquid carrier including a plurality of said capsules which do
not degrade in said liquid carrier; and an amount of indicator
material mixed into said liquid carrier, wherein release of said
amount of material in response to an activation element alters said
pH of said liquid carrier, and wherein said amount of indicator
material mixed into said liquid carrier changes color in response
to altered said pH.
132. A material release system as described in claim 131, wherein
said activation element comprises an activation material applied to
said capsule.
133. A material release system as described in claim 131, wherein
said activation element comprises an amount of force applied to
said capsule.
134. A material release system as described in claim 131, wherein
said amount of material comprises a base or an acid.
135. A material release system as described in claim 134, wherein
said base is selected from the group consisting of: sodium acetate,
sodium carbonate, sodium bicarbonate, sodium borate, sodium
citrate, sodium folate, sodium hydroxide, sodium phosphate dibasic,
sodium phosphate tribasic, sodium polymetaphosphate, sodium
pyrophosphate, sodium folate, sodium glycerophosphate, sodium ortho
silicate, sodium meta silicate, sodium hypochlorite, sodium
metaborate, sodium perborate, sodium tartrate, trisodium phosphate,
potassium salts thereof, lithium salts thereof, and combinations
thereof.
136. A material release system as described in claim 134, wherein
said acid is selected from the group consisting of: methanoic acid,
ethanoic acid, propanoic acid, butanoic acid, valeric acid, caproic
acid, caprylic acid, capric acid, lauric acid, myristic acid,
palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic
acid, cyclohexanecarboxylic acid, phenylacetic acid, benzoic acid,
oxalic acid, malonic acid, succinic acid, glutaric acid, adipic
acid, pimelic acid, suberic acid, maleic acid, fumaric acid,
phthalic acid, isophthalic acid, terephthalic acid, hemimellitic
acid, trimellitic acid, trimesic acid, succinic anhydride, maleic
anhydride, phthalic anhydride, glycolic acid, lactic acid,
hydroxybutyric acid, mandelic acid, glyceric acid, malic acid,
tartaric acid, citric acid, ascorbic acid, and combinations
thereof.
137. A material release system as described in claim 134, wherein
said capsule comprises a material selected from the group
consisting of: polyvinyl alcohol, polyvinyl alcohol/ethylene
copolymer, polyvinyl pyrolidone, polyvinyl pyrrolidone/acetate
copolymer, polyvinyl methyl ether, polyvinyl methyl ether/maleic
anhydride copolymer, polyvinyl methyl ether/maleic acid half ester
copolymer, polyacrylamide, poly (acrylamide/acrylic acid)
copolymer, polyacrylic acid, polyallylamine, poly(4-ammonium
styrenesulfonic acid), poly(diallyldimethylammonium chloride),
poly(ethylene/acrylic acid) copolymer,
poly(ethylene/1,2-butylene)diol, polyethylene glycol mw>6000,
poly(ethylene glycol) methyl ether, poly(ethylene glycol) dimethyl
ether, poly(ethylene glycol/propylene glycol) monobutyl ether,
poly(2-ethyl-2-oxazoline), poly(hexamethylene adipate) diol,
poly(hexamethylene carbonate) diol, poly(neopentyl adipate),
poly(neopentyl sebacate), poly(polytetrahydrofuran carbonate) diol,
poly(sodium 4-styrene sulfonate), poly styrene sulfonic acid,
polyvinyl phosphonic acid, poly(4-vinylpyridine), tapioca dextrin,
maize dextrin, waxy dextrin, starch, methyl cellulose, ethyl
cellulos, hydroxy ethyl cellulose, isopropyl cellulose, hydroxy
isopropyl cellulose, agar-agar, carrageenan,
carboxymethylcellulose, polyasparatate, acacia, gum tragacanth, or
combinations thereof.
138. A material release system as described in claim 134, wherein
said base or said acid comprises a particle.
139. A material release system as described in claim 138, wherein
said particle has a size between about 10 microns and 300
microns.
140. A material release system as described in claim 139, wherein
said particle has a size selected from the group consisting of:
between about 10 microns and about 30 microns, between about 20
microns and about 40 microns, between about 30 microns and about 50
microns, between about 40 microns and about 60 microns, between
about 50 microns and about 70 microns, between about 60 microns and
about 80 microns, between about 70 microns and about 90 microns,
between about 80 microns and about 100 microns, between about 90
microns and about 110 microns, between about 100 microns and about
120 microns, between about 110 microns to about 130 microns,
between about 120 microns to about 140 microns, between about 130
microns and about 150 microns, between about 140 microns to about
160 microns, between about 150 microns and about 170 microns,
between about 160 microns to about 180 microns, between about 170
microns to about 190 microns, between about 180 microns to about
200 microns, between about 190 microns and about 210 microns,
between about 200 microns and about 220 microns, between about 210
microns and about 230 microns, between about 220 microns and about
240 microns, between about 230 microns and about 250 microns,
between about 240 microns to about 260 microns, between about 250
microns to about 270 microns, between about 260 microns and about
280 microns, between about 270 microns to about 290 microns,
between about 280 microns and about 300 microns.
141. A material release system as described in claim 139, wherein
said capsule wall which bounds said amount of material comprises a
coat on said particle.
142. A material release system as described in claim 141, wherein
said coat has a thickness of between about 2 microns and about 45
microns.
143. A material release system as described in claim 142, wherein
said coat has a thickness selected from the group consisting of:
between about 2 microns to about 6 microns, between about 4 microns
to about 8 microns, between about 6 microns to about 10 microns,
between about 8 microns and about 12 microns, between about 10
microns and about 14 microns, between about 12 microns and about 16
microns, between about 14 microns and about 18 microns, between
about 16 microns and about 20 microns, between about 18 microns to
about 22 microns, between about 20 microns to about 24 microns,
between about 22 microns to about 26 microns, between about 24
microns and about 28 microns, between about 26 microns and about 30
microns, between about 28 microns and about 32 microns, between
about 30 microns and about 34 microns, between about 32 microns and
about 36 microns, between about 34 microns and about 38 microns,
between about 36 microns and about 40 microns, between about 38
microns and about 42 microns, between about 40 microns and about 44
microns, and about 42 microns and about 46 microns.
144. A material release system as described in claim 134, wherein
said capsule has a size of between about 10 microns and about 300
microns.
145. A material release system as described in claim 144, wherein
said capsule has a size selected from the group consisting of:
between about 15 microns to about 30 microns, between about 20
microns to about 40 microns, between about 30 microns to about 50
microns, between about 40 microns to about 60 microns, between
about 500 microns to about 70 microns, between about 60 microns to
about 80 microns, between about 70 microns to about 90 microns,
between about 80 microns to about 100 microns, between about 90
microns to about 110 microns, between about 100 microns to about
120 microns, between about 110 microns to about 130 microns,
between about 120 microns to about 140 microns, between about 130
microns to about 150 microns, between about 140 microns to about
160 microns, between about 150 microns to about 170 microns,
between about 160 microns to about 180 microns, between about 170
microns to about 190 microns, between about 180 microns to about
200 microns, between about 190 microns to about 210 microns,
between about 200 microns to about 220 microns, between about 210
microns to about 230 microns, between about 220 microns to about
240 microns, between about 230 microns to about 250 microns,
between about 240 microns to about 260 microns, between about 250
microns to about 270 microns, between about 260 microns to about
280 microns, between about 270 microns to about 290 microns, and
between about 280 microns to about 300 microns
146. A material release system as described in claim 134, wherein
said amount of indicator material changes color in response to an
increase in pH of said carrier.
147. A material release system as described in claim 134, wherein
said amount of indicator material changes color in response to a
decrease in pH of said carrier.
148. A material release system as described in claim 131, wherein
said carrier has an initial pH of between 4-8.
149. A material release system as described in claim 148, wherein
said carrier has an initial pH of between about 5.0 and about
7.0.
150. A material release system as described in claim 149, wherein
said carrier has an initial pH of between 6.0-7.5.
151. A material release system as described in claim 149, wherein
said amount of indicator is selected from the group consisting of:
brilliant yellow, bromthylmol blue, m-nitrophenol, neutral red,
phenophtalein.
152. A material release system as described in claim 151, wherein
said carrier has a final pH of between about 7.0 and about 9.4.
153. A material release system as described in claim 152, wherein
said carrier has a final pH of between 7.0 and 8.0.
154. A material release system as described in claim 146, wherein
said carrier has an initial pH of greater than about 7.0 and a
final pH of greater than about 7.0.
155. A material release system as described in claim 134, wherein
said carrier has an initial pH of less or equal to 7.0 and a final
pH of greater than 7.0.
156. A material release system as described in claim 134, wherein
said carrier has an initial pH of greater than or equal to 7.0 and
a final pH of less than 6.5
157. A material release system as described in claim 134, wherein
said carrier has an initial pH of less than or equal to 7.0 and a
final pH of greater than 7.5.
158. A material release system as described in claim 154, wherein
said amount of indicator is selected from the group consisting of:
alizarin red S, alkali blue, clayton yellow, cresol red, curcumin,
m-cresol purple, o-cresophthalein, phenol violet,
p-naphtholbenzein, thymol violet, thymolphtalein, titan yellow.
159. A material release system as described in claim 146, wherein
said carrier has an initial pH of about 7.0 or less and a final pH
of about 7.0 or less.
160. A material release system as described in claim 159, wherein
said amount of indicator is selected from the group consisting of:
alzarin red, bromcresol green, bromcresol purple, bromcresol blue,
congo red, crystal violet, dimethyl yellow, ethyl violet, malachite
green, m-cresol purple, ntanil yellow, methyl orange, methyl
purple, methyl red, methyl violet, phenol red, resorcin blue, and
thymol blue.
161. A material release system as described in claim 131, wherein
said capsule comprises a first capsule wall enclosed by a second
capsule wall, said amount of material disposed between said first
and second capsule wall.
162. A material release system as described in claim 131, wherein
said capsule comprises a first capsule wall enclosed by a second
capsule wall, said material bound by said first capsule wall, said
indicator material disposed between said first capsule wall and
said second capsule wall.
163. A material release system as described in claim 162, wherein
said activation element acts on said second capsule wall to release
said indicator material, said activation element acts upon said
first capsule wall to release said amount of material.
164. A material release system as described in claim 163, wherein
said activation element comprises a first activation element and a
second activation element, said second activation element acts on
said second capsule wall to release said indicator material, said
second activation element comprising an amount of force applied to
said second capsule wall, said first activation element acts upon
said first capsule wall to release said amount of material, said
first activation element comprises an activation material.
165. A material release system as described in claim 163, wherein
said activation element comprises a first activation element and a
second activation element, said second activation element acts on
said second capsule wall to release said indicator material, said
second activation element comprises an activation material applied
to said second capsule wall, said first activation element acts
upon said first capsule wall to release said amount of material,
said first activation element comprises an amount of force.
166. A material release system as described in claim 131, wherein
said carrier comprises a composition suitable as a hand wash
agent.
167. A material release system, comprising: an amount of material
comprising at least one of a base and an acid; a capsule having a
capsule wall which bounds said amount of material, wherein said
capsule releases said amount of material in response to an
activation element; a liquid carrier having a pH between 4 and 8,
said liquid carrier including a plurality of said capsules which do
not degrade in said liquid carrier; and an amount of indicator
material mixed into said liquid carrier, wherein release of said
amount of material in response to an activation element alters said
pH of said liquid carrier to be between either 4-7 or 7-8, and
wherein said amount of indicator material mixed into said liquid
carrier changes color in response to altered said pH.
Description
[0001] This United States patent application is a continuation of
U.S. patent application Ser. No. 10/544,586, filed Aug. 4, 2005,
which is a United States National Stage of International Patent
Cooperation Treaty Patent Application No. PCT/US04/03834, filed
Feb. 11, 2004, which claims the benefit of U.S. Provisional Patent
Application 60/446,908, filed Feb. 11, 2003, each hereby
incorporated by reference herein.
I. TECHNICAL FIELD
[0002] A material encapsulation and release system having a first
zone containing a first amount of material bound by a first capsule
wall and, if desired, a second zone containing a second amount of
material bound by a second capsule wall, each capsule wall
responsive to similar or dissimilar activation means to release the
first amount of material in the first zone and the second amount of
material in the second zone.
II. BACKGROUND
[0003] Conventional microcapsules may provide a material within a
capsule for use in controlled delivery systems. Conventional
encapsulation technology may provide a capsule wall made of a first
capsule layer adjoined directly with a second layer as described by
U.S. Pat. Nos. 6,511,749; 5,985,354; 5,912,017; and 4,861,627,
issued to Mathiowitz. Similarly, a single capsule may provide an
intermixture of two polymeric layers as described by U.S. Pat. No.
3,627,693 issued to Scarpelli, hereby incorporated by reference
herein.
[0004] While these conventional encapsulation technologies may in
certain circumstances provide a single capsule wall having an
interior capsule surface and an exterior capsule surface which
exhibit different chemical properties allowing for encapsulation of
a wider variety of materials, many problems with regard to the
encapsulation and delivery of materials remain yet unresolved.
[0005] A significant problem with conventional encapsulation
technology can be that the interior of a single capsule does not
allow for the discrete separation of different amounts or kinds of
material(s). As such, conventional capsules have an undivided
interior volume which contains one kind of material.
[0006] Another significant problem with conventional encapsulation
technology can be that the material contained within a single
capsule cannot be released in discrete amounts in response to
different discrete environmental circumstances. Conventional
capsule walls rupture either because they degrade in response to
exposure to a chemical environment or in response to the change in
application of force on the capsule wall. Upon rupture the entire
contents of the capsule are released. As such, while an amount of
material may be released in response to a first discrete
environmental circumstance, there is no mechanism by which
conventional capsule technology can hold the release of a second
discrete amount of material in abeyance until exposed to a second
different discrete environmental circumstance.
[0007] Another problem with conventional encapsulation technology
can be that separate capsules or mixtures of separate capsules may
not deliver proportioned amounts of two different materials. Where
different types of capsules each containing a different material
are mixed, differential settling of the mixture or differential
rupture of the two types of capsule mixes the contained materials
in different proportions.
[0008] Another problem with conventional encapsulation technology
can be failure to provide perceivable sensorial indicia of material
release other than the perceivable sensorial indicia of the
material itself, such as flavor, fragrance or color. In those
instances of an encapsulated material having no sensorial indicia
there may be no manner of ascertaining release of such material
from a capsule.
[0009] Another problem with conventional encapsulation technology
can be that release of encapsulated material does not further
provide indicia coupled to discrete event occurrence.
[0010] Material release from conventional capsule technology may
provide pleasing sensorial attributes such as flavor, color, or
fragrance. However, conventional encapsulation and delivery
technology may not release flavor, color, or fragrance for the
purpose of informing the user that a separate discrete event has
occurred, such as therapeutic efficacy or the elapse of a
pre-determined length of time.
[0011] Another problem with conventional encapsulation technology
can be the failure to further provide a carrier suitable for both
conveyance of encapsulated material without rupture of the capsule
walls and for washing hands. Specifically, as to conventional
carriers suitable for washing hands, the carrier may not provide an
encapsulated material released to indicate that a duration of hand
washing has occurred, or achievement of efficacious hand washing
with the carrier.
[0012] The instant invention addresses each of these concerns with
respect to conventional encapsulation technology.
III. DISCLOSURE OF INVENTION
[0013] Accordingly, a broad object of the invention can be to
provide a single capsule having a first zone containing a first
material released in response to a first activation means which
provides perceivable sensorial indicia of material release other
than then the perceivable sensorial indicia inherent to the
material itself, even if the released material itself does not
provide perceivable sensorial indicia at all.
[0014] Another broad object of the invention can be to provide a
single capsule having a first zone containing a first material
released in response to a first activation means which provides
perceivable sensorial indicia coupled to discrete event
occurrence.
[0015] Another broad object of the invention can be to provide a
single capsule having a first zone containing a first material
released in response to a first activation means which acts upon a
carrier to provide perceivable sensorial indicia of material
release.
[0016] Another broad object of the invention can be to provide a
single capsule having at least two zones which separate into
discrete amounts at least two amounts of material.
[0017] Another significant object of the invention can be to
provide a single capsule having a first zone which provides a first
amount of material and at least one additional zone which provides
a second amount of material released in response to an activation
means.
[0018] Another significant object of the invention can be to
provide a single capsule having a first zone containing a first
amount of material released in response to first activation means
and at least one additional zone containing a second amount of
material released in response to second activation means, whether
instant or disparate in time.
[0019] Another significant object of the invention can be to
provide a capsule which can deliver in proportion a first amount of
material and a second amount of material regardless of the number
or rate at which capsules rupture.
[0020] Another significant object of the invention can be to
deliver and release different materials from a single capsule
obviating the need to mix different types of conventional capsules
together.
[0021] Another significant object of the invention can be to
release an amount of a first material and an amount of a second
material in substantially contemporaneous, overlapped, or serial in
time.
[0022] Another broad object of the invention can be to provide a
single capsule having a first zone containing a first material
released in response to a first activation means and a second zone
containing a second material released in response to such first
activation means or a second activation means which provides at
least one perceivable sensorial indicia coupled to discrete event
occurrence.
[0023] Naturally, further objects of the invention are disclosed
throughout the specification and drawings.
IV. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] FIG. 1 provides a cross section view of a particular
embodiment of the invention which provides a capsule having first
zone containing a first amount of material bound by a first capsule
wall.
[0025] FIG. 2 provides a cross section view of a particular
embodiment of the invention which provides a capsule having a first
zone containing a first amount of material bound by a first capsule
wall conveyed by a carrier.
[0026] FIG. 3 provides a cross section view of a particular
embodiment of the invention which provides a capsule having a first
zone containing a first amount of material bound by a first capsule
wall and a second zone containing a second amount of material bound
by a second capsule wall.
[0027] FIG. 4 provides a cross section view of a particular
embodiment of the invention which provides a capsule having a first
zone containing a first amount of material bound by a first capsule
wall and a second zone containing a second amount of material bound
by a second capsule wall conveyed in a carrier.
V. MODE(S) FOR CARRYING OUT THE INVENTION
[0028] Generically, a material encapsulation and release system
having a first zone (1) containing a first amount of material (2)
bound by a first capsule wall (3) and, if desired, a second zone
(4) containing a second amount of material (5) bound by a second
capsule wall (6), each capsule wall responsive to similar or
dissimilar activation means (7) to release the first amount of
material (2) in the first zone (1) and the second amount of
material (5) in the second zone (4).
[0029] Now referring primarily to FIG. 1, that shows a generic
embodiment of the material encapsulation and release system having
a first zone (1) containing a first amount of material (2) bound by
a first capsule wall (3).
[0030] The first zone (1) defined by the inside surface of the
first capsule wall (3) can be, but is not limited to, a
substantially spherical, ovoid, or lozenge shaped volume. The
configuration of the first capsule wall (3) to adjust volume of the
first zone (1) to allow containment of the first amount of material
(2), whether a solid or a liquid. As to certain embodiments of the
invention, the first zone (1) can have a volume in the range of
about one hundred nanoliters to about one microliter; however, the
invention does not necessarily limit the first zone (1) to these
relatively small volumes, and the first zone (1) can have a volume
in excess of one microliter.
[0031] The first amount of material (2) contained within the first
zone (1) can be any manner of useful material, substance,
composition, mixture, colloidal suspension, or the like. The
material can be either a liquid or a solid. The solids or liquids
contained by the capsules may be aqueous soluble or non-aqueous
soluble depending on the application, such as: surfactants,
enzymes, flavors, fragrances, bleach or bleaching agents, pH change
indicators, dyes, anti-statics, fabric softener, lubricants,
emollients, insecticides, disinfectants, perfume, dentifrice,
vaccines, drugs, medications, amino acids, nucleic acids, microbes,
hormones, antiviral proteins, antiviral peptides, industrial
chemicals (which includes a wide variety of materials such as
oxidizing agents, reducing agents, free radical initiators, or the
like), bioactive agents, lotions, gels, colloidal dispersions, or
the like. These numerous solids or liquids may be further combined
to impart or enhance moisturizing, lubricity, color, fragrance,
texture, viscosity, or sound.
[0032] With respect to certain embodiments of the invention, the
first amount of material (2) contained in the first zone (1) can be
a base. The base can be one of the following non-limiting examples:
sodium acetate, sodium carbonate, sodium bicarbonate, sodium
borate, sodium citrate, sodium folate, sodium hydroxide, sodium
phosphate dibasic, sodium phosphate tribasic, sodium
polymetaphosphate, sodium pyrophosphate, sodium folate, sodium
glycerophosphate, sodium ortho silicate, sodium meta silicate,
sodium hypochlorite, sodium metaborate, sodium perborate, sodium
tartrate, trisodium phosphate, potassium salts thereof, lithium
salts thereof, individually or in various combinations.
[0033] Certain bases, such as trisodium phosphate, are available as
anhydrous trisodium phosphate, and are available with various
amounts of associated water such as five (5) moles, nine (9) moles,
or twelve (12) moles of water, or the like, and any hydrated form
of a base may be used as the first amount of material (2) in
accordance with the invention.
[0034] With respect to other embodiments of the invention, the
first amount of material (2) contained in the first zone (1) can be
an acid. The acid can be one of the following non-limiting
examples: methanoic acid, ethanoic acid, propanoic acid, butanoic
acid, valeric acid, caproic acid, caprylic acid, capric acid,
lauric acid, myristic acid, palmitic acid, stearic acid, oleic
acid, linoleic acid, linolenic acid, cyclohexanecarboxylic acid,
phenylacetic acid, benzoic acid, oxalic acid, malonic acid,
succinic acid, glutaric acid, adipic acid, pimelic acid, suberic
acid, maleic acid, fumaric acid, phthalic acid, isophthalic acid,
terephthalic acid, hemimellitic acid, trimellitic acid, trimesic
acid, succinic anhydride, maleic anhydride, phthalic anhydride,
glycolic acid, lactic acid, hydroxybutyric acid, mandelic acid,
glyceric acid, malic acid, tartaric acid, citric acid, and ascorbic
acid.
[0035] With respect to further embodiments of the invention, the
first amount of material (1) contained in the first zone (1) can be
a dye. The dye can be one of the following non-limiting examples:
azo dye, disazo dye, diazonium salts, azoxy dye, hydrazo dye,
benzidine dye, anthraquinone dye, triphenylmethane dye, aniline
dye, aquonium dye, cationic dye, chrome dye, fluorescent dye, leuco
dye, nitro dye, naphthol dye, toluidine dye, acridine dye,
tetrakisazo dye, thiazole dye, fluorine dye, oxazin dye,
tetraazolium salt dye, thiazin dye, pyronin dye, rhodamine dye,
safranin dye, phthalocyanin dye, acid dye, base dye, and
substituted analogs thereof.
[0036] The first amount of material (2) contained in the first zone
(1) can comprise a particle. Whether the first amount of material
(2) comprises a base particle, an acid particle, or a dye particle,
a plurality of particles can be established between about 10
microns and 300 microns. By sieving the base particles, acid
particles, or dye particles with different mesh (United States
standard mesh, or otherwise) particle size between about 10 microns
and about 30 microns, between about 20 microns and about 40
microns, between about 30 microns and about 50 microns, between
about 40 microns and about 60 microns, between about 50 microns and
about 70 microns, between about 60 microns and about 80 microns,
between about 70 microns and about 90 microns, between about 80
microns and about 100 microns, between about 90 microns and about
110 microns, between about 100 microns and about 120 microns,
between about 110 microns to about 130 microns, between about 120
microns to about 140 microns, between about 130 microns and about
150 microns, between about 140 microns to about 160 microns,
between about 150 microns and about 170 microns, between about 160
microns to about 180 microns, between about 170 microns to about
190 microns, between about 180 microns to about 200 microns,
between about 190 microns and about 210 microns, between about 200
microns and about 220 microns, between about 210 microns and about
230 microns, between about 220 microns and about 240 microns,
between about 230 microns and about 250 microns, between about 240
microns to about 260 microns, between about 250 microns to about
270 microns, between about 260 microns and about 280 microns,
between about 270 microns to about 290 microns, or between about
280 microns and about 300 microns, can be obtained.
[0037] As a non-limiting example, trisodium phosphate can be
crushed and sieved to obtain a plurality of trisodium phosphate
particles of between about 30 micron and about 250 micron. By
selection of different sieves a plurality of trisodium phosphate
particles of between about 40 micron and about 100 micron, or
between about 50 micron and about 80 micron. A particular
embodiment of the invention utilizes trisodium phosphate particles
sieved through a first United States standard mesh 200 and then
sieved through a second United States standard mesh 270.
[0038] Each particle of the base, acid, or dye as described above
can comprise as to some embodiments of the invention, the first
amount of material (2) contained in the first zone (1). As to these
embodiments of the invention in which the first amount of material
(2) comprises a particle, the particle can be bounded by a capsule
wall (3) or coat applied by fluid bed process (also known as
Wurster Process). Particles to be coated are placed in a chamber
where air is injected from below, whereby particles are suspend in
the circulating air. Depending on the composition of the capsule
wall or coat material it is dissolved in either water or a solvent.
The capsule wall or coat material can then be sprayed into the
chamber where it is adsorbed onto the surface of the particles.
Warm air can facilitate removal of excess water or solvent from the
capsule wall or coat material applied to the particle.
[0039] A wide variety of capsule wall or coat materials can be
applied by fluid bed process including, individually or as
mixtures: polyvinyl alcohol, polyvinyl alcohol/ethylene copolymer,
polyvinyl pyrolidone, polyvinyl pyrrolidone/acetate copolymer,
polyvinyl methyl ether, polyvinyl methyl ether/maleic anhydride
copolymer, polyvinyl methyl ether/maleic acid half ester copolymer,
polyacrylamide, poly (acrylamide/acrylic acid) copolymer,
polyacrylic acid, polyallylamine, poly(4-ammonium styrenesulfonic
acid), poly(diallyldimethylammonium chloride),
poly(ethylene/acrylic acid) copolymer,
poly(ethylene/1,2-butylene)diol, polyethylene glycol mw>6000,
poly(ethylene glycol) methyl ether, poly(ethylene glycol) dimethyl
ether, poly(ethylene glycol/propylene glycol) monobutyl ether,
poly(2-ethyl-2-oxazoline), poly(hexamethylene adipate) diol,
poly(hexamethylene carbonate) diol, poly(neopentyl adipate),
poly(neopentyl sebacate), poly(polytetrahydrofuran carbonate) diol,
poly(sodium 4-styrene sulfonate), poly styrene sulfonic acid,
polyvinyl phosphonic acid, poly(4-vinylpyridine), tapioca dextrin,
maize dextrin, waxy dextrin, starch, methyl cellulose, ethyl
cellulos, hydroxy ethyl cellulose, isopropyl cellulose, hydroxy
isopropyl cellulose, agar-agar, carrageenan,
carboxymethylcellulose, polyasparatate, acacia, and gum
tragacanth.
[0040] The fluid bed process can continue until the desired level
of coating is achieved. Typically, the level of coating is
described as percent increase of the original particle size. As a
non-limiting example, the trisodium phosphate particles described
above of between about 50 micron and 80 micron can be coated with
fully hydrolyzed polyvinyl alcohol (molecular weight of about 4000)
(commercially available under the brand name Celvol 107) to
increase the size of the trisodium phosphate particle between about
five percent and about thirty percent. The fluid bed process can be
adjusted to obtain a percent increase in particle size using fully
hydrolyzed polyvinyl alcohol or other capsule wall or coat material
of between about 3% and about 5%, about 5%, between about 5% and
about 7%, between about 7% and about 9%, about 10%, between about
9% and about 11%, between 11% and about 13%, between about 13% and
about 15%, about 15%, between 15% and about 17%, between about 17%
and about 19%, between about 19% and about 21%, about 20%, about
21% and about 23%, about 23% and about 25%, about 25%, about 25%
and about 27%, about 27% to 29%, about 29% to about 31%, or about
30%.
[0041] With respect to a wide variety of embodiments of the
invention prepared utilizing the fluid bed process, the first
capsule wall (3) can have a thickness selected between about 2
microns and about 45 microns. Narrow ranges in capsule wall
thickness can be achieved with the above-described capsule wall or
coat materials such that the first capsule wall (3) or coat can
have a thickness selected from between about 2 microns to about 6
microns, between about 4 microns to about 8 microns, between about
6 microns to about 10 microns, between about 8 microns and about 12
microns, between about 10 microns and about 14 microns, between
about 12 microns and about 16 microns, between about 14 microns and
about 18 microns, between about 16 microns and about 20 microns,
between about 18 microns to about 22 microns, between about 20
microns to about 24 microns, between about 22 microns to about 26
microns, between about 24 microns and about 28 microns, between
about 26 microns and about 30 microns, between about 28 microns and
about 32 microns, between about 30 microns and about 34 microns,
between about 32 microns and about 36 microns, between about 34
microns and about 38 microns, between about 36 microns and about 40
microns, between about 38 microns and about 42 microns, between
about 40 microns and about 44 microns, and about 42 microns and
about 46 microns.
[0042] The resulting capsule can have a size between about 10
microns and about 300 microns from which narrow ranges of capsule
size can be used for particular applications. Capsules can be
obtained within narrow size ranges including without limitation
between about 15 microns to about 30 microns, between about 20
microns to about 40 microns, between about 30 microns to about 50
microns, between about 40 microns to about 60 microns, between
about 500 microns to about 70 microns, between about 60 microns to
about 80 microns, between about 70 microns to about 90 microns,
between about 80 microns to about 100 microns, between about 90
microns to about 110 microns, between about 100 microns to about
120 microns, between about 110 microns to about 130 microns,
between about 120 microns to about 140 microns, between about 130
microns to about 150 microns, between about 140 microns to about
160 microns, between about 150 microns to about 170 microns,
between about 160 microns to about 180 microns, between about 170
microns to about 190 microns, between about 180 microns to about
200 microns, between about 190 microns to about 210 microns, and so
forth up to about 300 microns.
[0043] Adjustment of the capsule size and the thickness of the
capsule wall can yield a controllable spectrum of material release
rates from the capsules. Now referring to Table 1 and Table 2
below, with respect to a capsule wall (3) comprised of polyvinyl
alcohol, the larger the capsule the more rapid the release of
material from the capsule when exposed to an activation element (7)
comprising water (even though the capsule wall remains the same
thickness). Also, the thinner the capsule wall (3) the more rapid
the release of material from the capsule when exposed to an
activation (7) comprising water.
[0044] Table 1 and Table 2 plot Percent Density of water into which
material has been released (greater amount of released material the
greater the density) from capsules have a capsule wall having a
thickness represented as a percent increase over the size of the
particle which the capsule wall coats (5%, 10%, 15%, 20%, 25%, 30%)
versus time.
[0045] Again referring primarily to FIG. 1, the first amount of
material (2) can comprise an amount of liquid, such as a solution
of base, a solution of acid, or a solution of dye, or an oil such
as: lemon oil, lime oil, vanilla oil, wintergreen oil, spearamint
oil, sandalwood oil, musk oil, jojoba oil, bergamot oil, casis oil,
lavender oil, chamomile oil, valerian oil, peony oil, rose oil, St.
John's wort oil, cypress oil, rosemary oil, ylang ylang oil,
passionflower oil, neroli oil, cedarwood oil, Frankincense oil,
lemongrass oil, orange oil, mandarin oil, witch hazel, cucumber
oil, aloe oil, juniper oil, sage oil, pomegranate oil, mint oil,
gardenia oil, jasmine oil, narcissus oil, lilac oil, magnolia oil,
honeysuckle oil, apricot oil, blackberry oil, papaya oil,
huckleberry oil, kiwi oil, mango oil, bayberry oil, clove oil,
eucalyptus oil, amaretto oil, cinnamon oil, and sesame oil.
[0046] Particles and liquids not miscible in water, or materials
soluble in liquids not miscible in water, may be encapsulated using
coacervation process. The two immiscible liquids are mixed together
under high speed shear mixing. As the shear is increased, the
liquid not water miscible is broken into tiny droplets. A water
soluble capsule wall material, such as gelatin, can be provided in
the aqueous portion of the mixture. When the droplets are of the
desired size, the water soluble capsule material can be salted out
of solution by the addition of materials that reduce the solubility
of the capsule material. A variety of materials that are water
soluble can be added to the mixture which reduces the solubility of
the gelatin. As the capsule wall material is pushed out of
solution, it is adsorbed onto the droplets. When gelatin is used it
may re-dissolve if the equilibrium is disturbed. Therefore, as to
those embodiments utilizing gelatin as a capsule wall material a
cross-linking agent can be used to harden the gelatin, such as an
aldehyde. A most useful aldehyde is glutaraldehyde. The aldehyde
will harden the gelatin so that when mixing is complete, it may be
filtered, washed and remain in tact.
[0047] Used to a lesser degree is a coacervation method where a
capsule wall material soluble in solvent may be used by saturating
the solvent and force the coating substance out of solution to be
adsorbed onto a particle or droplet. Typically another solvent that
is miscible with the first solvent, but is not a solvent for the
substance being coated is preferred.
[0048] Now referring primarily to FIG. 2, the capsules described
above can be mixed into a carrier (10). The carrier can be selected
to avoid or limit degradation of the first capsule wall (3) to
prevent the first amount of material (2) from release into the
carrier (10). As such, a capsule wall material can be selected
which avoids release of the first amount of material into one or
more carriers, without limitation ethylene glycol, propylene
glycol, polyethylene glycol, polypropylene glycol, poly(ethylene
glycol/propylene glycol), 1,3-propanediol, 1,2-butanediol,
2,3-butanediol, 1,4-butanediol, 1,6-hexanediol, pinacol, glycerol,
neopentylglycol, pentaerythritol, meso-hydrobenzoin,
1,2-cyclopentanediol, 1,2-cyclohexanediol, methanol, ethanol,
isopropanol, n-propanol, n-butanol, isobutanol, sec-butanol,
tert-butanol, n-pentanol, isopentanol, amyl alcohol, tert-pentanol,
cyclopentanol, cyclohexanol, n-hexanol, n-heptanol, n-octanol,
n-nonanol. n-decanol, n-dodecanol n-tetradecanol, n-hexadecanol,
n-octadecanol, phenoxyethanol, benzyl alcohol, diphenyl carbinol,
tetraphenylcarbinol, methoxyethanol, ethoxyethanol, propoxyethanol,
butoxyethanol, hexoxyethanol, methoxypropanol, ethoxypropanol,
propoxypropanol, butoxyepropanol, hexoxypropanol, ethoxyethoxy
methanol, ethoxyethoxy ethanol, ethoxyethoxy propanol, ethoxyethoxy
butanol, ethoxyethoxy hexanol, propoxypropoxy methanol,
propoxypropoxy ethanol, propoxypropoxy propanol, propoxypropoxy
butanol, propoxypropoxy hexanol.
[0049] The carrier (10) can further include an amount of indicator
material (11). The indicator material can be a color change
material which as a non-limiting example can be responsive to
altered pH of the carrier (10). As to some embodiments of the
invention the indicator material may have a first color in a first
pH range of about 5.0 pH and about 7.0 pH, such as brilliant
yellow, bromthylmol blue, m-nitrophenol, neutral red,
phenophtalein. The indicator material may have a second color in a
second pH range of about 7.0 and about 9.4. As such, the indicator
material (11) can provide the carrier (10) with a first color in
the first pH range and a second color in the second pH range.
[0050] Other embodiments of the invention can utilize indicator
materials that have a first pH range and a second pH range above
about 7.0 pH. As to these embodiments a first color and a second
color can be obtained for the same carrier (10) at alkaline pH
utilizing as a non-limiting examples: alizarin red S, alkali blue,
clayton yellow, cresol red, curcumin, m-cresol purple,
o-cresophthalein, phenol violet, p-naphtholbenzein, thymol violet,
thymolphtalein, or titan yellow.
[0051] Similarly other embodiments of the invention can utilize
indicator materials that have a first pH range and a second pH
range at about or below 7.0 pH. As to these embodiments a first
color and a second color can be obtained for the same carrier (10)
at acid pH utilizing as a non-limiting examples: alzarin red,
bromcresol green, bromcresol purple, bromcresol blue, congo red,
crystal violet, dimethyl yellow, ethyl violet, malachite green,
m-cresol purple, ntanil yellow, methyl orange, methyl purple,
methyl red, methyl violet, phenol red, resorcin blue, and thymol
blue.
[0052] Numerous and varied compositions can be achieved by varying
the first amount of material (2), the first capsule wall or coat
(3), the carrier (10) and the indicator material (11). The
following non-limiting examples provide wash agents with a color
changing carrier include:
[0053] A first amount of material (2) comprising an amount of
citric acid, and wherein the capsule wall (3) or coat comprises
polyvinyl alcohol, and wherein the carrier (10) comprises a mixture
of:
[0054] a. an amount of polypropelene glycol (2000);
[0055] b. an amount of Miracare MP35;
[0056] c. an amount of Tegosoft PSE 141G; and
[0057] d. an amount of sodium phosphate monobasic;
[0058] and wherein the amount of indicator material (11) comprises
an amount of methyl orange in the carrier (10).
[0059] A first amount of material (2) comprising trisodium
phosphate, and wherein the capsule wall (3) or coat comprises
polyvinyl alcohol, and wherein the carrier (10) comprises a mixture
of:
[0060] a. an amount of polypropelene glycol (2000);
[0061] b. an amount of Miracare MP35; and
[0062] c. an amount of Tegosoft PSE 141G; and wherein the amount of
indicator material (11) comprises an amount of phenolphthalein in
the carrier (10).
[0063] A first amount of material (2) comprising trisodium
phosphate, and wherein the capsule wall (3) or coat comprises
polyvinyl alcohol, and wherein said carrier (10) comprises a
mixture of:
[0064] a. an amount of polypropelene glycol (2000);
[0065] b. an amount of Miracare MP35;
[0066] c. an amount of Tegosoft PSE 141G; and
[0067] d. an amount of sodium bicarbonate;
[0068] and wherein the amount of indicator material (11) comprises
an amount of methyl orange.
[0069] A first amount of material (2) comprising trisodium
phosphate, and wherein the capsule wall (3) or coat comprises
polyvinyl alcohol, and wherein the carrier (10) comprises a mixture
of:
[0070] a. an amount of polypropelene glycol (2000);
[0071] b. an amount of Miracare MP35;
[0072] c. an amount of Tegosoft PSE 141G; and
[0073] d. an amount of sodium bicarbonate;
[0074] and wherein the amount of indicator material (11) comprises
an amount of phenol violet.
[0075] A first amount of material (2) comprises citric acid, and
wherein the capsule wall (3) or coat comprises said polyvinyl
acetate-paraffin wax, and wherein the carrier (10) comprises a
mixture of:
[0076] a. an amount of water;
[0077] b. an amount of ammonium lauryl sulfate;
[0078] c. an amount of Silwet L-7220;
[0079] d. an amount of Tegosoft PSE 141G; and
[0080] e. an amount of sodium phosphate monobasic;
[0081] and wherein the amount of indicator material (11) comprises
an amount of said methyl orange.
[0082] A first amount of material (2) comprises said amount of
sodium triphosphate, and
[0083] wherein the capsule wall (3) or coat comprises said
polyvinyl acetate-paraffin wax, and wherein the carrier (10)
comprises a mixture of:
[0084] a. an amount of water;
[0085] b. an amount of ammonium lauryl sulfate;
[0086] c. an amount of Silwet L-7220;
[0087] d. an amount of Tegosoft PSE 141G; and
[0088] e. an amount of sodium phosphate monobasic;
[0089] and wherein the amount of indicator material (11) comprises
and amount of said phenolphtalein.
[0090] The following non-limiting examples provide wash agents with
a indicator material (11) comprising either copious amounts of foam
generated by the carrier or sound generated by rupture of the
bubbles comprising the foam:
[0091] A first amount of material (2) comprising citric acid, and
wherein the capsule wall (3) or coat comprises polyvinyl
acetate-paraffin wax, and wherein said carrier comprises a mixture
of:
[0092] a. an amount of polypropelene glycol (2000);
[0093] b. an amount of Miracare MP35;
[0094] c. an amount of Tegosoft PSE 141G; and
[0095] d. an amount of sodium bicarbonate.
[0096] A first amount of material (2) comprising citric acid, and
wherein the capsule wall (3) or coat comprises polyvinyl alcohol
(Cevol 107), and wherein the carrier (10) comprises a mixture
of:
[0097] a. an amount of polypropelene glycol (2000);
[0098] b. an amount of Miracare MP35;
[0099] c. an amount of Tegosoft PSE 141G; and
[0100] d. an amount of sodium bicarbonate.
[0101] Now again referring to FIG. 2, each of the preceding
non-limiting examples provides a first capsule wall (3) which
remains substantially dormant in the carrier (11) until presented
to a first activation element (7). The first activation element (7)
acts upon the first capsule wall (3) to release the first amount of
material (2) contained in the first zone (1).
[0102] With respect to certain capsule wall or coat materials, the
first activation element (7) can comprise an activation material
(8) which without limitation can be an alcohol, an ether, a glycol
ether, a dihydric alcohol, a polyol, a lactone, or water. With
respect to various embodiments of the invention, the first
activation element corresponds to the chemical environment at a
particular step in a process. As a non-limiting example, the
application of an amount of water during hand washing.
[0103] With respect to other embodiments of the invention, the
capsule wall or coat materials can be made responsive to a first
activation element (7) comprising an amount of force (9) caused by
change in motion, change in pressure, or the like. As a
non-limiting example, the capsule wall material can be selected and
configured to be responsive to the forces generated during
efficacious hand washing.
[0104] With respect to the embodiments of the invention
above-described having a capsule wall (3) of polyvinyl alcohol the
first activation element (7)(8) comprises an amount of water. When
presented with water the capsule wall (3) degrades and ruptures
releasing the first amount of material (2) into the carrier (10).
As to those carriers having an indicator material (11) comprising a
color change material responsive to change of pH, if the capsule
releases base or acid the carrier (10) can change color. As to
those carriers having an amount of base, release of acid from the
capsule can generate copious amounts of foam or sound.
[0105] With respect to the embodiments of the invention
above-described having a capsule wall (3) of polyvinyl
acetate-paraffin wax the first activation element (7)(9) comprises
an amount of force. When presented with sufficient force from
within or from without the capsule wall (3) degrades or ruptures to
release said first amount of material (2). Again, as to those
carriers having an indicator material (11) comprising a color
change material responsive to change of pH, if the capsule releases
base or acid the carrier (10) can change color. As to those
carriers having an amount of base, release of acid from the capsule
can generate copious amounts of foam or sound.
[0106] Understandably, the composition or thickness, or both the
composition and thickness, of the capsule can be adjusted as
above-described to delay release of the first amount of material
(2) from the time presented with the first activation element (7).
As such, perceivable sensorial indicia (color, color change,
fragrance, sound, foam generation, and the like) can occur
substantially coincident with or be coupled to discrete event
occurrence.
[0107] Now referring primarily to FIG. 3, the invention can further
include a second zone (4) containing a second amount of material
(5) bound by a second capsule wall (6) or coat. The second zone (4)
can also have various boundary configurations which may include,
but are not limited to, substantially spherical, ovoid, lozenge, or
the like which define the volume of the second zone (4).
[0108] The second amount of material (5) contained in the second
zone (4) can be the same as the first amount of material (2) or a
different material, including, but not limited to, any of the
above-described materials use as the first amount of material (2),
such as a base, an acid, a dye, an indicator material, a color
change material, or pH color change material. The second amount of
material (5) can engage a portion or all of the exterior surface of
the first capsule wall (3). As such, the second amount of material
must not degrade, solubilize, or act upon the first capsule wall
(3) to release the first amount of material (2). Embodiments of the
invention provide solutions to this problem in at least three ways.
First, the first amount of material (2) contained in the first zone
(1), the first capsule wall (2), and the second amount of material
(5) in the second zone (4) can be chemically coordinated such that
the first capsule wall (3) is selected to resist degradation by the
first amount of material (2) contained in the first zone (1) and
the second amount of material (5) contained in the second zone (4).
Second, the first amount of material (2) and the second amount of
material (5) can both be selected to avoid degradation of the first
capsule wall (3). Third, the first capsule wall (3) can comprise
two layers--an inside layer of the first capsule wall (3) to
resistant degradation by the first amount of material (2) contained
in the first zone (1) and an outside layer of the first capsule
wall (3) to resistant degradation by the second amount of material
(5) contained in the second zone (4).
[0109] The second amount of material can be deposited on the
exterior surface of the first capsule wall (3) by fluid bed
process, vapor phase process (the material to be applied is
vaporized under low vacuum and high temperature and injected toward
the first capsule wall (3) to be coated), prilling (spraying the
capsules into a solution of the second amount of material),
evaporative coating (dipping the capsules in a solution of the
second amount of material and drying).
[0110] The invention can further include a second capsule wall (6)
configured to the boundary of the second zone (4). The second
capsule wall (6) can be selected from the capsule wall materials as
above-described. As such, the second capsule wall can be selected
to resist degradation by the second amount of material (5)
contained by the second zone (4) and by the carrier (11) into which
the multiple zone capsules are mixed. Again, as for the first
capsule wall, embodiments of the invention may utilize two layers
to present capsule wall material which resist the second amount of
material (5) and the carrier (10) which may be one or a combination
of the carrier materials above-described.
[0111] Again, the multiple zone capsule provides a second capsule
wall (3) which remains substantially dormant in the carrier (11)
until presented to a second activation element ( ). The second
activation element (7) acts upon the second capsule wall (3) to
release the second amount of material (2) contained in the second
zone (1).
[0112] With respect to certain second capsule wall or coat
materials, the second activation element (12) can comprise an
activation material (13) which without limitation can be an
alcohol, an ether, a glycol ether, a dihydric alcohol, a polyol, a
lactone, or water.
[0113] The second activation element (12) can alternately comprise
an amount of force (14) caused by change in motion, change in
pressure, or the like. As a non-limiting example, the capsule wall
material can be selected and configured to be responsive to the
forces generated during efficacious hand washing.
[0114] The second activation element (12) can be coupled to a
single step in a process into which both the second amount of
material and the first amount of material are released
substantially coincidentally, staggered, serially, or serially
separated by an elapse of time. The release of the second amount of
material (5) or the release of the first amount of material (2) can
provide perceivable sensorial indicia which can be coupled to the
occurrence of a discrete event or provide a reinforcer to induce
the user to continue use of the composition until the discrete
event, or used in various combinations or permutations of both.
[0115] The first activation element (7) and the second activation
element (12) can alternately be coupled to two discrete steps, or
where the second activation element mixed with the second amount of
material creates the first activation element for release of the
first amount of material (2).
[0116] Additional numerous and varied compositions can be achieved
by varying the first amount of material (2), the first capsule wall
or coat (3), the second amount of material (5), the second capsule
wall (6) or coat the carrier (10). The following non-limiting
examples provide wash agents with a color changing carrier
include:
[0117] The first amount of material (2) comprises citric acid, and
wherein the first capsule wall (3) or coat comprises polyvinyl
alcohol (Cevol 107), and wherein the second amount of material ( )
comprises bromophenol blue; and wherein the second capsule wall ( )
or coat comprises polyvinyl alcohol (Cevol 107), and wherein the
carrier comprises a mixture of:
[0118] a. an amount of polypropelene glycol (2000);
[0119] b. an amount of Miracare MP35; and
[0120] c. an amount of Tegosoft PSE 141G.
[0121] In this non-limiting example, the multiple zone capsule
remains dormant until the addition of an amount of water and the
second capsule wall degrades to release the indicator material (11)
into the carrier (10) and the first capsule wall degrades to
release the acid into the carrier (11). The acid acts to reduce pH
of the carrier and the indicator material changes color.
[0122] The first amount of material (2) comprises citric acid, and
wherein the first capsule wall (3) or coat comprises polyvinyl
alcohol (Cevol 107), and wherein the second amount of material
comprises bromophenol blue; and wherein the second capsule wall (6)
or coat comprises polyvinyl alcohol (Cevol 107), and wherein the
carrier (10) comprises a mixture of:
[0123] a. an amount of polypropelene glycol (2000);
[0124] b. an amount of Miracare MP35;
[0125] c. an amount of Tegosoft PSE 141G; and
[0126] d. an amount of sodium phosphate monobasic.
[0127] In this non-limiting example, the multiple zone capsule
remains dormant until the addition of an amount of water and the
second capsule wall degrades to release the indicator material (11)
into the carrier (10) and the first capsule wall degrades to
release the acid into the carrier (11). The acid acts to reduce pH
of the carrier and the indicator material changes color and
generates copious amounts of foam.
[0128] The first amount of material (2) comprises trisodium
phosphate, and wherein the first coat comprises polyvinyl alcohol
(Cevol 107), and wherein the second amount of material (5)
comprises cresol red; and wherein the second capsule wall (6)
comprises polyvinyl alcohol (Cevol 107), and wherein said carrier
comprises a mixture of:
[0129] a. an amount of polypropelene glycol (2000);
[0130] b. an amount of Miracare MP35; and
[0131] c. an amount of Tegosoft PSE 141G.
[0132] In this non-limiting example, the multiple zone capsule
remains dormant until the addition of an amount of water and the
second capsule wall degrades to release the indicator material (11)
into the carrier (10) and the first capsule wall degrades to
release the base into the carrier (11). The base acts to increase
pH of the carrier and the indicator material changes color.
[0133] The first amount of material (3) comprises citric acid, and
wherein the first capsule wall (3) or coat comprises polyvinyl
alcohol (Cevol 107), wherein said second amount of material (5)
comprises bromophenol blue; and wherein the second capsule wall (6)
or coat comprises polyvinyl acetate-paraffin wax, and wherein the
carrier comprises a mixture of:
[0134] a. an amount of water;
[0135] b. an amount of ammonium lauryl sulfate;
[0136] c. an amount of Silwet L-7220;
[0137] d. an amount of Tegosoft PSE 141G; and
[0138] e. an amount of sodium phosphate monobasic.
[0139] In this non-limiting example, the multiple zone capsule
remains dormant until application of a sufficient amount of force
ruptures the second capsule wall (6) to release the indicator
material (11) into the carrier (10) and the first capsule wall
degrades in response to water added to carrier to release the base
into the carrier (11). The base acts to increase pH of the carrier
and the indicator material changes color.
[0140] Each of the numerous and varied embodiments of the multiple
zone material encapsulation and release system can be assigned to
one of four broad categories. The first broad category and the
second broad category comprises those embodiments of the multiple
zone encapsulation and release system which comprise a first
capsule wall (3) and a second capsule wall (6) which degrade in
response to a second activation element and a first activation
element which are the same (either the same chemical activation
element or the same force application activation element) to
release the second amount of material (5) and the first amount of
material (2).
[0141] The third broad category of the multiple zone material
encapsulation and release system invention comprises those
embodiments having a second capsule wall (6) which releases the
second amount of material in response to a second activation
element comprising a chemical activation element and a first
capsule wall (3) which releases the first amount of material (1) in
response to a first activating element comprising a change in force
upon the capsule.
[0142] The fourth broad category of the multiple zone material
encapsulation and release system invention comprises those
embodiments having the second capsule wall (6) which releases the
second amount of material (6) in response to a second activating
element comprising a change in force upon the second capsule wall
(6) and having a first capsule wall (3) which releases the first
amount of material (2) in response to a first activation element
comprising a chemical activation element.
[0143] The following description of particular embodiments of the
invention provide a sufficient number of examples of each of the
single zone material encapsulation and release system and the
multiple zone material encapsulation and release system to allow
the manufacture and use of a numerous and varied embodiments of the
invention encompassed by the generic descriptions above-provided
and are not intended to be limiting with respect to the scope or
breadth of the invention.
EXAMPLE 1
[0144] An amount of water soluble blue dye (although other colors
can be used) can be encapsulated in the first zone by the use of
vapor phase disposition. A dimer of para-xylene is vaporized by
heating to about 175.degree. C. at -1 torr. The vapor phase can
then be pyrolyzed at about 660.degree. C. and at about -0.5 torr to
break the dimer into a pair reactive radicals. The pair of radicals
are then applied to the surface of the dye where they react to form
a poly (para-xylene) polymer thereby establishing a first capsule
wall which bounds the first zone containing the amount of water
soluble dye.
[0145] The resulting encapsulated dye is then added to alcohol. 1
gram of capsules is added to 2 grams of isopropanol. To this is
added 0.5 grams of a water soluble yellow dye. When the dye is
solubilized the solution is heated to 50.degree. C. so that all the
alcohol is removed. The resulting product is the original capsule
containing the blue dye with the yellow dye absorbed or engaging
the entirety of the outside surface of the first wall encapsulating
the blue dye. The second zone of yellow dye can be similarly vapor
phase coated, as described above.
[0146] 0.1 grams of this particular embodiment of the multiple zone
encapsulation system can be added to about 50 grams of an ethylene
glycol carrier containing 1.5 grams dodecylether polyoxyethylene
ethanol (12 moles) and 0.5 grams of disodium cocoamphodiacelate. A
small portion of solution can be transferred to the surface of the
hands for washing. When water is applied to the hands, foaming
increases and after about 5-10 seconds the foam turns a light
yellow. After about another 5-10 seconds, the foam turns green as a
result of the blue dye being released and combining with the yellow
dye.
EXAMPLE 2
[0147] First, 200 grams of a 10% solution (w/w) of gelatin are
heated to about 40.degree. C. and vigorously stirred. To this can
be added about 2.0 grams of methylsalicylate. 110 grams of a 20%
solution (w/w) of sodium sulfate are added to induce coacervation.
The mixture can be cooled to 50.degree. C. and 3 grams of
glutaraldeyde are added to harden the gelatin. The pH is adjusted
to 3.8. The procedure results in a first zone of methylsalicylate
encapsulated by a first capsule wall which ruptures upon
application of sufficient pressure.
[0148] Subsequently, 200 grams of a 10% solution (w/w) of gelatin
are heated to 40.degree. C. and vigorously stirred. About 1 gram of
the microcapsules prepared as described above are added. 1.0 gram
of 3-hydroxy-4-methoxybenzaldehyde can be added followed by 110
grams of a 20% solution of sodium sulfate to induce coacervation.
The mixture is cooled to 50.degree. C. 3 grams of glutaraldehyde
are added to harden the gelatin. The pH is adjusted to 4.0. The
procedure results in a second zone of
3-hydroxy-4-methoxybenzaldehyde encapsulated by a second capsule
wall which ruptures in response to application of a sufficient
amount of pressure.
[0149] 0.1 gram of the multiple zone encapsulation system invention
described above can be added to 50 grams of water containing 1.3
grams of sodium lauryl sulfate, 0.5 grams of
disodiumcocoamphodiacetate. After gentle mixing, a portion of the
composition can be transferred to the surface of the hands. Washing
of the hands generates sufficient forces to rupture the second
capsule wall releasing from the second zone
3-hydroxy-4-methoxybenzaldehyde after about 7 seconds generating a
first fragrance of vanilla. After the elapse of about another 8
seconds, washing of the hands generates sufficient forces to
rupture the first capsule wall releasing methylsalicylate contained
in the first zone to provide a second fragrance of winter
green.
EXAMPLE 3
[0150] In a manner similar to that described in Example 2,
methylsalicylate encapsulated with a gelatin yields a first zone of
material having a first capsule wall which ruptures in response to
application of sufficient force. 1.0 gram of the capsules prepared
as such can be added to 2 grams of isopropanol. To this 0.5 grams
of a water soluble yellow dye can be added. The dye can be
solubilized and the solution heated to about 50.degree. C. until
all alcohol is removed. The resulting material is encapsulated
using vapor phase deposition as described in Example 1.
[0151] 0.1 gram of the above-described capsule can be added to
about 50 grams of ethylene glycol containing 1.5 grams of
dodecylether polyoxyethylene ethanol (12 moles EO) and 0.5 grams of
disodium cocoamphodiacetate to provide a carrier. A small portion
of the composition can be transferred onto the surface of the hands
for handwashing. When water is applied an almost immediate color
change to yellow occurs. After an elapse of time of about 10
seconds and with continued rubbing, the light smell of wintergreen
is generated.
EXAMPLE 4
[0152] In a manner similar to Example 1, a water soluble blue dye
provides a first material containged in a first zone encapsulated
using vapor phase deposition to provide a first capsule wall. 0.5
grams of the prepared capsules can be added to 100 grams of a 10%
solution (w/w) of gelatin and are mixed gently so as not to rupture
the capsules. 1.0 gram of methylsalicylate is added. 55 grams of a
20% (w/w) solution of sodium sulfate are added to induce
coacervation. The mixture is cooled to 50.degree. C.; 1.5 grams of
glutaraldehyde are added to harden the gelatin. The pH is adjusted
to 3.8. The resulting multiple zone capsule invention can be
filtered, washed and dried.
[0153] About 0.1 gram of the above described multiple zone capsules
are added to 50 grams of ethylene glycol containing 1.5 grams of
dodecyletherpolyoxyethylene ethanol (12 moles EO) and 0.5 grams of
disodium cocoamphodiacetate to provide a carrier. A small portion
of the composition can be transferred to the surface of the hands
for handwashing. Application of the forces generated during
handwashing releases the methylsalicylate from the second zone
providing a first fragrance of wintergreen. About 8 seconds after
the addition of water (second activating environment) the
composition on the surface of the hands turns a light blue due to
the release of the dye from the first zone.
[0154] A large number of permutations and combinations of the
multiple zone encapsulation invention can be made and used for
handwashing compositions some of which are set out in Table 3
below.
TABLE-US-00001 TABLE 3 Zone 1 Wall 1 Zone 2 Wall 2 1 Color Soluble
Color Friable 2 Color Soluble Scent Friable 3 Color Friable Color
Soluble 4 Color Friable Scent Soluble 5 Scent Soluble Scent Friable
6 Scent Soluble Color Friable 7 Scent Friable Scent Soluble 8 Scent
Friable Color Soluble
EXAMPLE 5
[0155] A particle can be obtained by sizing citric acid crystals
using a 200 mesh sieve. The particles collected after sizing are
about .ltoreq.75.mu.. These particles can again be sieved through a
270 mesh sieve. That which passes through is discarded and those
crystals remaining are now .gtoreq.53.mu. but .ltoreq.75.mu.. These
crystals are placed in a Wuerster coating unit, or as is otherwise
known as a fluid bed coater. Air rising from the bottom causes the
crystals to be suspended and circulate in the chamber.
Concurrently, volatilized polyvinyl alcohol previously dissolved in
a water/alcohol solution is introduced. The polyvinyl alcohol can
be a low molecular weight polymer (Mw=4000), which can be fully
hydrolyzed. Such a polymer is commercially available from Celanese
Corporation as Celvol 107. The coating process continues until the
beads increase in size to about 70.mu. to 90.mu.. The beads are
then removed from the coater as finished product.
[0156] A non-aqueous cleaning composition is prepared by mixing 50
grams of polypropylene glycol (2000), 5.0 grams of Miracare MP35,
available from Rhodia, Inc., 1.0 gram of Tegosoft PSE141G,
available from Goldschmidt Chemical Corp., 0.2 gram sodium
phosphate monobasic, 0.02 gram of methyl orange, and 0.3 gram of
the above described beads. The composition is gently blended so as
not to rupture or otherwise disturb the beads. The composition has
a very light yellow color due to the poor solubility of the sodium
phosphate in a non-aqueous environment.
[0157] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam becomes yellow immediately as the sodium
phosphate dissolves. As the rubbing continues, capsule walls are
slowly dissolved by the solvating action of the water. The carrier
and other addenda lack sufficient polarity and solvating strength
to dissolve the capsule walls in situ, thereby allowing for
suitable shelf-life. When the citric acid crystals are exposed,
they begin to dissolve. Prior to this event, the pH of the medium
is about 4.5, which allows the methyl yellow to remain yellow. With
the release of the acid, the pH drops to 3.1. This shift causes the
methyl orange to change from yellow to red, due to the protonation
of the dye molecule. The time required for the color change is
about 35 seconds.
[0158] The wall thickness of the bead may be increased to adjust
the time required for release of the citric acid into the carrier.
Alternately, sodium phosphate monobasic can be encapsulated to mix
with the citric acid into the carrier so as to create a change from
red to yellow.
EXAMPLE 6
[0159] In like manner as described in Example 5, a bead can be
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated. The carrier used can be the same with the
exception of the elimination of sodium phosphate monobasic and the
methyl orange being replaced with phenolphthalein. The pH of the
carrier can be established as slightly acid at 6.5.
[0160] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam remains clear. As the rubbing continues, the
walls of the beads are slowly dissolved by the solvating action of
the water. When the trisodium phosphate is exposed, it begins to
dissolve. Prior to this event, the pH of the medium is about 6.5,
which allows the phenolphthalein to remain clear. With the release
of the basic trisodium phosphate, the pH increases to 10.1. This
shift causes the phenolphthalein to change from clear to a vibrant
red, due to the protonation of the dye molecule. The time required
for the color change is about 30 seconds.
[0161] The capsule wall thickness of the bead may be increased to
accordingly change the time required for release. Alternately, an
acid such as citric, tartaric or ascorbic acid can be encapsulated
to mix with trisodium phosphate, or other basic substance, in the
carrier so as to create a change from red to clear.
EXAMPLE 7
[0162] In like manner as described in Example 5, a capsule is
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated. The composition used can be the same with
the exception of the addition of the same amount of sodium
bicarbonate in lieu sodium phosphate monobasic and the methyl
orange being replaced with phenol violet. The pH of the carrier can
be established as slightly acid at 6.5 and the addition of the
sodium bicarbonate makes the carrier a very light yellow.
[0163] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam turns a stronger yellow as the sodium
bicarbonate is dissolved. As the rubbing continues, the capsule
walls slowly dissolve by the solvating action of the water. When
the trisodium phosphate is exposed, it begins to dissolve. Prior to
this event, the pH of the medium is about 8.2, which allows the
phenol violet to impart an intense yellow color. With the release
of the basic trisodium phosphate, the pH increases to 10.6. This
shift causes the phenol violet to change from yellow to a violet,
due to the protonation of the dye molecule. The time required for
the color change is about 38 seconds.
[0164] Again, the capsule wall thickness of the bead may be
increased to accordingly change the time required for release.
Alternately, a weak base such as the sodium bicarbonate can be
encapsulated to mix with the trisodium phosphate, or a stronger
base, into the composition so as to create a change from violet to
yellow.
EXAMPLE 8
[0165] A capsule can be prepared by sizing citric acid crystals
using a 200 mesh sieve. The particles collected after sizing are
all .ltoreq.75.mu.. This material is again sieved through a 270
mesh sieve. That which passes through is discarded and those
crystals remaining are now .gtoreq.53.mu. but .ltoreq.75.mu.. These
crystals are placed in a Wuerster coating unit, or as is otherwise
known as a fluid bed coater. Air rising from the bottom causes the
crystals to be suspended and circulate in the chamber.
Concurrently, volatilized polyvinyl acetate/paraffin wax previously
dissolved in a xylene/methoxy ethanol solution is introduced. The
polyvinyl acetate is a medium molecular weight polymer (Mw=83,000)
and has a Ford No. 4 viscosity @ 25.degree. C. of 13-14.5 sec. The
paraffin wax has a melt range of 73.degree.-80.degree. C. The
coating process continues until the beads increase in size to about
75 to 100.mu.. The beads are then removed from the coater as
finished product.
[0166] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.7 grams of ammonium lauryl sulfate
(70%), Silwet L-7220, available from Rhodia, Inc., 1.0 gram of
Tegosoft PSE141G, available from Osi Specialties, 0.2 gram sodium
phosphate monobasic, 0.02 gram of methyl orange, and 0.3 gram of
the above described beads. The composition is gently blended so as
not to rupture or otherwise disturb the beads. The composition has
a very distinct yellow color. This is in contrast to Example 1
wherein the sodium phosphate was not dissolved but dispersed. In an
aqueous medium, the dissolution of the phosphate salt permits the
pH indicator to become a strong yellow.
[0167] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is yellow. As the rubbing continues, the walls
of the beads are slowly ruptured by the mechanical action of
washing. Prior to this event, the pH of the medium is about 4.5,
which allows the methyl yellow to remain yellow. With the release
of the citric acid, the pH drops to 3.1. This shift causes the
methyl orange to change from yellow to red, due to the protonation
of the dye molecule. The time required for the color change is
about 24 seconds.
EXAMPLE 9
[0168] In like manner as described in Example 8, a capsule can be
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated. The composition used is the same with the
exception of the methyl orange being replaced with phenolphthalein.
The pH of the carrier is slightly acid at 4.5 due to the complete
dissolution of the sodium phosphate monobasic.
[0169] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam remains clear due to the acid nature of the
composition. As the rubbing continues, the walls of the beads are
ruptured by the mechanical action of washing. When the trisodium
phosphate is exposed, it begins to dissolve. Prior to this event,
the pH of the medium is about 4.5, which allows the phenolphthalein
to remain clear. With the release of the basic trisodium phosphate,
the pH increases to 9.7. This shift causes the phenolphthalein to
change from clear to a vibrant red, due to the protonation of the
dye molecule. The time required for the color change is about 32
seconds.
[0170] The capsule wall thickness of the capsule may be increased
to accordingly change the time required for release. Alternately,
an acid such as citric, tartaric, ascorbic acid, or the salt of an
acid can be encapsulted to mix the trisodium phosphate, or other
basic substance, in the aqueous carrier so as to create a change
from red to clear.
EXAMPLE 10
[0171] In like manner as described in Example 5, a capsule can be
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated. The composition used is the same with the
exception of the addition of the same amount of sodium bicarbonate
in lieu sodium phosphate monobasic and the methyl orange being
replaced with phenol violet. The pH of the carrier is slightly
alkaline at 8.2 and the addition of the sodium bicarbonate makes
the solution an intense yellow.
[0172] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is immediately a bright yellow. As the rubbing
continues, the walls of the beads are ruptured through the
mechanical action of washing. When the trisodium phosphate is
exposed, it begins to dissolve. Prior to this event, the pH of the
medium is about 8.2, which allows the phenol violet to impart an
intense yellow color. With the release of the basic trisodium
phosphate, the pH increases to 10.6. This shift causes the phenol
violet to change from yellow to a violet, due to the protonation of
the dye molecule. The time required for the color change is about
29 seconds.
[0173] The capsule wall thickness can be increased to accordingly
change the time required for release. Alternately, a weak base such
as the sodium bicarbonate can be encapsuled to mix the trisodium
phosphate, or a stronger base, in the carrier so as to create a
change from violet to yellow.
EXAMPLE 11
[0174] Capsules can be prepared wherein methyl salicylate is
encapsulated. This is accomplished using a process known as
coacervation. Coacervation takes advantage of the immiscibility of
various substances in water. In the present instance, methyl
salicylate, or as it is also known, oil of wintergreen, is added to
water. With high speed shear mixing, the methyl salicylate is
broken into smaller droplets, but yet is never emulsified. Gelatin
is added to the mixing dispersion wherein the gelatin dissolves in
water and is then adsorbed onto the surface of the methyl
salicylate droplets by saturating the solution with a spectator
salt, and pushing the gelatin out of solution. While still mixing,
glutaraldehyde is added to harden or cross-link the gelatin since
it would lack sufficient integrity to remain in tact otherwise.
With the addition of the aldehyde complete, the mixing is stopped
and the beads are removed, filtered and washed.
[0175] A non-aqueous cleaning composition is prepared by mixing 50
grams of polyethylene glycol (600), 7.0 grams of Igepal CO-880,
available from Rhodia, Inc., 2.0 grams of Surfonic DDA-12,
available from Huntsman Corp., and 0.5 gram of the above described
beads. The composition is gently blended so as not to rupture or
otherwise disturb the beads. The composition is clear and has no
discernable odor.
[0176] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. Foam is generated immediately with no other noticeable
result. As the rubbing continues, the walls of the beads are
ruptured due to the mechanical action of washing. After
approximately 25 seconds, there is a detectable odor of oil of
wintergreen.
EXAMPLE 12
[0177] In like manner as described in Example 7, beads are prepared
except that methyl salicylate is substituted with
3-methoxy-4-hydroxy benzaldehyde (vanillin). This is similarly
accomplished using coacervation with gelatin and hardening with
glutaraldehyde.
[0178] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.0 grams of sodium octyl sulfate, 0.6
gram of sodium dodecyl benzene sulfonate, and 0.7 gram of the above
described beads. The composition is gently blended so as not to
rupture or otherwise disturb the beads. The composition is clear
and has no discernable odor.
[0179] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. Foam is generated immediately with no other noticeable
result. As the rubbing continues, the walls of the beads are
ruptured due to the mechanical action of washing. After
approximately 22 seconds, there is a detectable odor of
vanilla.
EXAMPLE 13
[0180] A capsule can be prepared by sizing sugar crystals using a
170 mesh sieve. The particles collected after sizing are all
.ltoreq.90.mu.. This material is again sieved through a 230 mesh
sieve. That which passes through is discarded and those crystals
remaining are now .gtoreq.63.mu. but .ltoreq.90.mu.. These crystals
are placed in a Wuerster coating unit, or as is otherwise known as
a fluid bed coater. Air rising from the bottom causes the crystals
to be suspended and circulate in the chamber. Concurrently,
volatilized blue dye, previously dissolved in a water solution is
introduced. The dye is water soluble blue dye #7. The coating
process continues until the beads increase in size to about 100 to
130.mu.. At this point the dye solution is removed and replace with
the same polyvinyl alcohol solution as described in Example 5. The
dye coated beads are then further coated with the polyvinyl alcohol
to provide a protective layer. The coating process continues until
the beads increase in size to about 125 to 160.mu.. The beads are
then removed from the coater as finished product.
[0181] A non-aqueous cleaning composition is prepared by mixing 50
grams of polypropylene glycol (2000), 5.0 grams of Miracare MP35,
available from Rhodia, Inc., 1.0 gram of Tegosoft PSE141G,
available from Goldschmidt Chemical Corp., and 0.6 gram of the
above described beads. The composition is gently blended so as not
to rupture or otherwise disturb the beads. The composition is clear
and has no color.
[0182] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The composition foams but remains as white foam. As the
rubbing continues, the walls of the beads are slowly dissolved by
the solvating action of the water. As the polyvinyl alcohol is
removed and exposes the dye, the dye immediately dissolves and
imparts a distinct color shift from white to blue. The time
required for the color change is about 38 seconds.
[0183] Capsule wall thickness can be increased to accordingly
change the time required for release.
EXAMPLE 14
[0184] A capsule can be prepared by sizing sugar crystals using a
170 mesh sieve. The particles collected after sizing are
.ltoreq.90.mu.. This material is again sieved through a 230 mesh
sieve. That which passes through is discarded and those crystals
remaining are now .gtoreq.63.mu. but .ltoreq.90.mu.. These crystals
are placed in a Wuerster coating unit, or as is otherwise known as
a fluid bed coater. Air rising from the bottom causes the crystals
to be suspended and circulate in the chamber. Concurrently,
volatilized blue dye, previously dissolved in a water solution is
introduced. The dye is water soluble blue dye #7. The coating
process continues until the beads increase in size to about 100 to
130.mu.. At this point the dye solution is removed and replace with
the same polyvinyl acetate/paraffin wax solution as described in
Example 4. The dye coated beads are then further coated with the
polyvinyl acetate/wax combination to provide a protective layer.
The coating process continues until the beads increase in size to
about 125 to 160.mu.. The beads are then removed from the coater as
finished product.
[0185] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.7 grams of ammonium lauryl sulfate
(70%), Silwet L-7220, available from Rhodia, Inc., 1.0 gram of
Tegosoft PSE141G, available from OSi Specialties, and 0.6 gram of
the above described beads. The composition is gently blended so as
not to rupture or otherwise disturb the beads. The composition has
a very distinct yellow color.
[0186] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is initially white. As the rubbing continues,
the walls of the beads are slowly ruptured by the mechanical action
of washing. The foam changes quickly from clear to blue. The time
required for the color change is about 32 seconds.
EXAMPLE 15
[0187] A capsule can be prepared by sizing citric acid crystals
using a 200 mesh sieve. The particles collected after sizing are
all .ltoreq.75.mu.. This material is again sieved through a 270
mesh sieve. That which passes through is discarded and those
crystals remaining are now .gtoreq.53.mu. but .ltoreq.75.mu.. These
crystals are placed in a Wuerster coating unit, or as is otherwise
known as a fluid bed coater. Air rising from the bottom causes the
crystals to be suspended and circulate in the chamber.
Concurrently, volatilized polyvinyl alcohol previously dissolved in
a water/alcohol solution is introduced. The polyvinyl alcohol is a
low molecular weight polymer (Mw=4000), which is fully hydrolyzed.
Such a polymer is commercially available from Celanese Corporation
as Celvol 107. The coating process continues until the beads
increase in size to about 70.mu. to 90.mu.. The beads are then
removed from the coater as finished product.
[0188] A non-aqueous cleaning composition is prepared by mixing 50
grams of polypropylene glycol (2000), 5.0 grams of Miracare MP35,
available from Rhodia, Inc., 1.0 gram of Tegosoft PSE141G,
available from Goldschmidt Chemical Corp., 0.2 gram sodium
bicarbonate, and 0.3 gram of the above described beads. The
composition is gently blended so as not to rupture or otherwise
disturb the beads.
[0189] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. As the rubbing continues, the walls of the beads are
slowly dissolved by the solvating action of the water. When the
citric acid crystals are exposed, they begin to dissolve. Prior to
this event, the pH of the medium is about 8.2. With the release of
the acid, the pH drops to 3.1. This shift causes the sodium
bicarbonate to react with the citric acid. The double displacement
reaction liberates carbon dioxide. The rapid release of CO.sub.2
causes the foam to effervesce, which is both visible and audible.
The time required for the effect to occur is about 24 seconds.
[0190] Capsule wall thickness can be increased to accordingly
change the time required for release.
EXAMPLE 16
[0191] A capsule can be prepared by sizing citric acid crystals
using a 200 mesh sieve. The particles collected after sizing are
all .ltoreq.75.mu.. This material is again sieved through a 270
mesh sieve. That which passes through is discarded and those
crystals remaining are now .gtoreq.53.mu. but .ltoreq.75.mu.. These
crystals are placed in a Wuerster coating unit, or as is otherwise
known as a fluid bed coater. Air rising from the bottom causes the
crystals to be suspended and circulate in the chamber.
Concurrently, volatilized polyvinyl acetate/paraffin wax previously
dissolved in a xylene/methoxy ethanol solution is introduced. The
polyvinyl acetate is a medium molecular weight polymer (Mw=83,000)
and has a Ford No. 4 viscosity @ 25.degree. C. of 13-14.5 sec. The
paraffin wax has a melt range of 73.degree.-80.degree. C. The
coating process continues until the beads increase in size to about
75 to 100.mu.. The beads are then removed from the coater as
finished product.
[0192] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.7 grams of ammonium lauryl sulfate
(70%), Silwet L-7220, available from Rhodia, Inc., 1.0 gram of
Tegosoft PSE141G, available from Osi Specialties, 0.2 gram sodium
bicarbonate, and 0.3 gram of the above described beads. The
composition is gently blended so as not to rupture or otherwise
disturb the beads.
[0193] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is white. As the rubbing continues, the walls
of the beads are slowly ruptured by the mechanical action of
washing. Prior to this event, the pH of the medium is about 8.2.
With the release of the citric acid, the pH drops to 3.1. This
shift causes the sodium bicarbonate to react with the citric acid.
The double displacement reaction liberates carbon dioxide. The
rapid release of CO.sub.2 causes the foam to effervesce, which is
both visible and audible. The time required for the effect to occur
is about 22 seconds.
EXAMPLE 17
[0194] A capsule can be prepared by sizing citric acid crystals
using a 200 mesh sieve. The particles collected after sizing are
all .ltoreq.75.mu.. This material is again sieved through a 270
mesh sieve. That which passes through is discarded and those
crystals remaining are now .gtoreq.53.mu. but .ltoreq.75.mu.. These
crystals are placed in a Wuerster coating unit, or as is otherwise
known as a fluid bed coater. Air rising from the bottom causes the
crystals to be suspended and circulate in the chamber.
Concurrently, volatilized polyvinyl alcohol previously dissolved in
a water/alcohol solution is introduced. The polyvinyl alcohol is a
low molecular weight polymer (Mw=4000), which is fully hydrolyzed.
Such a polymer is commercially available from Celanese Corporation
as Celvol 107. The coating process continues until the beads
increase in size to about 70 to 90.mu.. The polyvinyl alcohol
solution is removed and replaced with a 30% aqueous solution of
bromphenol blue. The same beads are coated again with the pH dye
indicator until reaching a bead size of 75.mu. to 95.mu.. Finally,
the bromphenol blue solution is removed and replaced with the same
polyvinyl alcohol solution described above. The coating process
continues until the beads are coated to an increased and final size
of 90.mu. to 115.mu.. The beads are then removed from the
coater.
[0195] In like manner as described in Example 5, a non-aqueous
cleaning composition is prepared by mixing 50 grams of
polypropylene glycol (2000), 5.0 grams of Miracare MP35, available
from Rhodia, Inc., 1.0 gram of Tegosoft PSE141G, available from
Goldschmidt Chemical Corp., 0.2 gram sodium phosphate monobasic,
and 0.7 gram of the above described beads. The composition is
gently blended so as not to rupture or otherwise disturb the beads.
The composition is completely clear since there is no dye in the
carrier, but rather encapsulated in the heretofore described
bead.
[0196] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is initially white. The sodium phosphate
monobasic dissolves. As the rubbing continues, the walls of the
beads are slowly dissolved by the solvating action of the water.
The carrier and other addenda lack sufficient polarity and
solvating strength to do so in situ, thereby allowing for suitable
shelf-life. The bromphenol blue is released initially thereby
causing the foam to turn blue. This requires about 8 seconds. As
the rubbing continues, the second layer of polyvinyl alcohol is
dissolved. When the citric acid crystal are exposed, they begin to
dissolve. Prior to this event, the pH of the medium is about 4.4,
which allows the bromphenol blue to remain blue. With the release
of the acid, the pH drops to 3.2. This shift causes the bromphenol
blue to change from blue to yellow, due to the protonation of the
dye molecule. The time required for the color change is about 38
seconds.
[0197] Capsule wall thickness of the bead may be increased to
accordingly change the time required for release. Alternately,
sodium phosphate monobasic can be encapsuled to mix with citric
acid in the carrier so as to create a change from yellow to
blue.
EXAMPLE 18
[0198] In like manner as described in Example 17, a capsule can be
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated in lieu of the citric acid. Similarly, the
bead is coated with cresol red in place of phenolphthalein. This is
likewise coated with polyvinyl alcohol. The pH of the carrier is
slightly acid at 6.5 and therefore needs no agent to create an acid
environment.
[0199] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam remains clear. As the rubbing continues, the
walls of the beads are slowly dissolved by the solvating action of
the water. When the cresol red is exposed, it immediately turns the
foam yellow. The time required is about 6 seconds. The second layer
of polyvinyl alcohol begins to dissolve. When the trisodium
phosphate is exposed, it is solubilized. Prior to this event, the
pH of the medium is about 6.5, which allows the cresol red to
remain yellow. With the release of the basic trisodium phosphate,
the pH increases to 10.1. This shift causes the cresol red to
change from yellow to purple, due to the protonation of the dye
molecule. The time required for the second color change is about 34
seconds.
[0200] Capsule wall thickness can be increased to accordingly
change the time required for release. It is also evident that one
may encapsulate an acid such as citric, tartaric or ascorbic acid
and mix the trisodium phosphate, or other basic substance, into the
composition so as to create a change from purple to yellow. This
example demonstrates a color change using and acid-to-base shift in
pH.
EXAMPLE 19
[0201] In like manner as described in Example 18, a capsule can be
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated. The capsules thus formed are then coated
with a 30% aqueous solution of thymolphthalein such that the beads
are about 75.mu. to 95.mu. in diameter. The beads are finally
coated with the original polyvinyl alcohol solution so that the
average size is in the range of 90.mu. to 115.mu.. The composition
used is the same with the exception of the addition of the same
amount of sodium bicarbonate in lieu sodium phosphate monobasic.
The pH of the carrier is slightly basic at 8.2.
[0202] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is initially white. As the rubbing continues,
the walls of the beads are slowly dissolved by the solvating action
of the water. When the thymolphthalein is released, the solution
continues to remain white since at a pH of 8.2, thymolphthalein is
colorless. When the trisodium phosphate is exposed as the rubbing
action continues, it begins to dissolve. Prior to this event, the
pH of the medium is about 8.2, which again favors the
thymolphthalein to remain clear. With the release of the basic
trisodium phosphate, the pH increases to 10.6. This shift causes
the thymolphthalein to change from clear to blue, due to the
protonation of the dye molecule. The time required for the color
change is about 29 seconds.
[0203] The capsule wall thickness can be increased to accordingly
change the time required for release. Alternately, a weak base such
as the sodium bicarbonate can be encapsulated to mix trisodium
phosphate, or a stronger base, in the carrier so as to create a
change from blue to clear. This example demonstrates a color change
using and base-to-base shift in pH.
EXAMPLE 20
[0204] In like manner as described in Example 17, a capsule can be
prepared with the sole exception being that the second application
of poly vinyl alcohol is replaced with the solvent based mixture of
polyvinyl acetate and paraffin wax. The resulting bead is therefore
citric acid coated with polyvinyl alcohol. This is then coated with
bromphenol blue and finally with the heretofore described mixture
of polyvinyl acetate and paraffin wax.
[0205] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.7 grams of ammonium lauryl sulfate
(70%), Silwet L-7220, available from Rhodia, Inc., 1.0 gram of
Tegosoft PSE141G, available from Osi Specialties, 0.2 gram sodium
phosphate monobasic, and 0.7 gram of the above described beads. The
composition is gently blended so as not to rupture or otherwise
disturb the beads. The composition is colorless. Since the pH
indicator dye is encapsulated, and although the sodium phosphate is
fully dissolved, there is no color imparted.
[0206] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is initially white. The sodium phosphate
monobasic dissolves. As the rubbing continues, the walls of the
beads are slowly ruptured by the mechanical action of washing. The
bromphenol blue is released initially thereby causing the foam to
turn blue. This requires about 7 seconds. As the rubbing continues,
the second layer of polyvinyl alcohol is dissolved. When the citric
acid crystal are exposed, they begin to dissolve. Prior to this
event, the pH of the medium is about 4.4, which allows the
bromphenol blue to remain blue. With the release of the acid, the
pH drops to 3.2. This shift causes the bromphenol blue to change
from blue to yellow, due to the protonation of the dye molecule.
The time required for the color change is about 38 seconds.
[0207] Capsule wall thickness can be increased to accordingly
change the time required for release. Alternately, the sodium
phosphate monobasic can be encapsulated to mix with the citric acid
in the carrier so as to create a change from yellow to blue.
EXAMPLE 21
[0208] In like manner as described in Example 20, a capsule can be
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated in lieu of the citric acid. Similarly, the
bead is coated with cresol red in place of phenolphthalein. The
difference is that the bead is then coated with a solvent based
mixture of polyvinyl acetate and paraffin wax. The pH of the
carrier is slightly acid at 6.5 and therefore needs no agent to
create an acid environment.
[0209] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam remains clear. As the rubbing continues, the
walls of the beads are slowly ruptured by the mechanical action of
washing. When the cresol red is exposed, it immediately turns the
foam yellow. The time required is about 6 seconds. The second layer
of polyvinyl alcohol begins to dissolve. When the trisodium
phosphate is exposed, it is solubilized. Prior to this event, the
pH of the medium is about 6.5, which allows the cresol red to
remain yellow. With the release of the basic trisodium phosphate,
the pH increases to 10.1. This shift causes the cresol red to
change from yellow to purple, due to the protonation of the dye
molecule. The time required for the second color change is about 34
seconds.
[0210] Capsule wall thickness of the bead may be increased to
accordingly change the time required for release. Alternately, an
acid such as citric, tartaric or ascorbic acid an be encapsulated
and mix the trisodium phosphate, or other basic substance, into the
composition so as to create a change from purple to yellow.
EXAMPLE 22
[0211] In like manner as described in Example 19, a capsule can be
prepared except that sodium triphosphate (12 moles of water) is
similarly encapsulated. The capsule thus formed are then coated
with a 30% aqueous solution of thymolphthalein such that the beads
are about 75 to 95.mu. in diameter. The difference is now that the
capsules are coated with the heretofore described solvent solution
of polyvinyl acetate and paraffin wax so that the average size is
in the range of 90.mu. to 115.mu.. The composition used is the same
with the exception of the addition of the same amount of sodium
bicarbonate in lieu sodium phosphate monobasic. The pH of the
carrier is slightly basic at 8.2.
[0212] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is initially white. As the rubbing continues,
the walls of the beads are slowly ruptured by the mechanical action
of washing. When the thymolphthalein is released, the solution
continues to remain white since at a pH of 8.2, thymolphthalein is
colorless. When the trisodium phosphate is exposed as the rubbing
action continues, it begins to dissolve. Prior to this event, the
pH of the medium is about 8.2, which again favors the
thymolphthalein to remain clear. With the release of the basic
trisodium phosphate, the pH increases to 10.6. This shift causes
the thymolphthalein to change from clear to blue, due to the
protonation of the dye molecule. The time required for the color
change is about 29 seconds.
[0213] Capsule wall thickness can be increased to accordingly
change the time required for release. Alternately, a weak base such
as the sodium bicarbonate can be encapsulated to mix with the
trisodium phosphate, or a stronger base, in the carrier so as to
create a change from blue to clear. This example demonstrates a
color change using and base-to-base shift in pH.
EXAMPLE 23
[0214] In like manner as described in Example 11, capsules are
prepared with methyl salicylate encapsulated. The prepared capsules
are then placed in a fluid bead coater and coated with a 30%
aqueous solution of blue dye. These coated beads are then
subsequently coated with polyvinyl alcohol as described in Example
5. This results in a multi-walled bead wherein the outside is
polyvinyl alcohol with a dye underneath. Then there is a hard
gelatin layer containing methyl salicylate.
[0215] A non-aqueous cleaning composition is prepared by mixing 50
grams of polypropylene glycol (2000), 5.0 grams of Miracare MP35,
available from Rhodia, Inc., 1.0 gram of Tegosoft PSE141G,
available from Goldschmidt Chemical Corp., and 1.0 gram of the
above described beads. The composition is gently blended so as not
to rupture or otherwise disturb the beads. The composition is
completely clear since there is no dye in the carrier, but rather
encapsulated in the heretofore described bead.
[0216] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is initially white. As the rubbing continues,
the walls of the beads are slowly dissolved by the solvating action
of the water. The blue dye is released thereby causing the foam to
turn blue. This requires about 5 seconds. As the rubbing continues,
the second layer of gelatin is ruptured through the mechanical
action of rubbing. When the methyl salicylate is released, the
distinct smell of oil of wintergreen is detected. The time required
for the color change is about 32 seconds.
EXAMPLE 24
[0217] A capsule can be prepared by sizing sugar crystals using a
170 mesh sieve. The particles collected after sizing are all
.ltoreq.90.mu.. This material is again sieved through a 230 mesh
sieve. That which passes through is discarded and those crystals
remaining are now .gtoreq.63.mu. but .ltoreq.90.mu.. These crystals
are placed in a Wuerster coating unit, or as is otherwise known as
a fluid bed coater. Air rising from the bottom causes the crystals
to be suspended and circulate in the chamber. Concurrently,
volatilized blue dye, previously dissolved in a water solution is
introduced. The dye is water soluble blue dye #7. The coating
process continues until the capsules or beads increase in size to
about 100 to 130.mu.. At this point the dye solution is removed and
replace with the same polyvinyl alcohol solution as described in
Example 1. The dye coated capsules or beads are then further coated
with the polyvinyl alcohol to provide a protective layer. The
coating process continues until the capsules increase in size to
about 125 to 160.mu.. A 30% solution of a yellow dye is then coated
onto the beads already formed so that the size range is between
about 140 and 180.mu.. Finally, these beads are again coated with
polyvinyl alcohol as described above to a finished size range of
about 165 and 200.mu.. Therefore, a multi-walled bead is realized
that is coated on the outside with polyvinyl alcohol protecting a
yellow dye underneath. Below this is another layer of polyvinyl
alcohol protecting a blue dye underneath. The beads are then
removed from the coating unit.
[0218] A non-aqueous cleaning composition is prepared by mixing 50
grams of polypropylene glycol (2000), 5.0 grams of Miracare MP35,
available from Rhodia, Inc., 1.0 gram of Tegosoft PSE141G,
available from Goldschmidt Chemical Corp., and 1.2 grams of the
above described beads. The composition is gently blended so as not
to rupture or otherwise disturb the beads. The composition is clear
and has no color.
[0219] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The composition foams but remains as white foam. As the
rubbing continues, the walls of the beads are slowly dissolved by
the solvating action of the water. As the polyvinyl alcohol is
removed and exposes the dye, the dye immediately dissolves and
imparts a distinct color shift from white to yellow. The time
required for the initial color change is about 7 seconds. As the
rubbing continues, the next layer of polyvinyl alcohol dissolves
thereby releasing the blue dye. The foam changes from yellow to
green when the two dyes interact. The time required for the second
color change is about 33 seconds.
[0220] Capsule wall thickness can be increased to accordingly
change the time required for release.
EXAMPLE 25
[0221] A capsule can be prepared by sizing sugar crystals using a
170 mesh sieve. The particles collected after sizing are all
.ltoreq.90.mu.. This material is again sieved through a 230 mesh
sieve. That which passes through is discarded and those crystals
remaining are now .gtoreq.63.mu. but .ltoreq.90.mu.. These crystals
are placed in a Wuerster coating unit, or as is otherwise known as
a fluid bed coater. Air rising from the bottom causes the crystals
to be suspended and circulate in the chamber. Concurrently,
volatilized blue dye, previously dissolved in a water solution is
introduced. The dye is water soluble blue dye #7. The coating
process continues until the beads increase in size to about 100 to
130.mu.. At this point the dye solution is removed and replaced
with the same polyvinyl alcohol solution as described in Example 1.
The dye coated beads are then further coated with the polyvinyl
alcohol to provide a protective layer. The coating process
continues until the beads increase in size to about 125 to 160.mu..
A 25% solution of sodium acetate is then coated onto the beads
already formed so that the size range is between about 140 and
180.mu.. Finally, these beads are again coated with polyvinyl
alcohol as heretofore described to a finished size range of about
165 and 200.mu.. Therefore, a multi-walled bead is realized that is
coated on the outside with polyvinyl alcohol protecting sodium
acetate underneath. Below this is layer of polyvinyl alcohol
protecting a blue dye underneath. The beads are then removed from
the coating unit.
[0222] A non-aqueous cleaning composition is prepared by mixing 50
grams of polypropylene glycol (2000), 5.0 grams of Miracare MP35,
available from Rhodia, Inc., 1.0 gram of Tegosoft PSE141G,
available from Goldschmidt Chemical Corp., 0.6 gram sodium
carbonate, and 1.2 grams of the above described beads. The
composition is gently blended so as not to rupture or otherwise
disturb the beads. The composition is clear and has no color.
[0223] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The composition foams but remains as white foam. As the
rubbing continues, the protective layer of polyvinyl alcohol
dissolves thereby exposing the sodium acetate. When the sodium
acetate interacts with the already dissolved sodium carbonate,
there is a double displacement reaction resulting in the release of
carbon dioxide gas. This effervescence causes the foam to lather
even more. The time for this release is about 7 seconds. As the
rubbing continues, the second layer of polyvinyl alcohol dissolves
thereby releasing the dye. It immediately turns the foam blue. The
time required for this action is about 29 seconds.
EXAMPLE 26
[0224] In like manner as described in Example 11, capsules can be
prepared with methyl salicylate encapsulated. The prepared beads
are then placed in a fluid bead coater and coated with a 30%
aqueous solution of blue dye. These coated beads are then
subsequently coated with polyvinyl acetate/paraffin wax as
described in Example 4. This results in a multi-walled bead wherein
the outside is polyvinyl alcohol with a dye underneath. Then there
is a hard gelatin layer containing methyl salicylate.
[0225] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.7 grams of ammonium lauryl sulfate
(70%), Silwet L-7220, available from Rhodia, Inc., 1.0 gram of
Tegosoft PSE141G, available from Osi Specialties, and 1.2 grams of
the above described beads. The composition is gently blended so as
not to rupture or otherwise disturb the beads. The composition is
colorless and odorless.
[0226] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The foam is initially white. As the rubbing continues,
the walls of the beads are slowly dissolved by the solvating action
of the water. The blue dye is released initially thereby causing
the foam to turn blue. This requires about 5 seconds. As the
rubbing continues, the second layer of gelatin is ruptured through
the mechanical action of rubbing. When the methyl salicylate is
released, the distinct smell of oil of wintergreen is detected. The
time required for the color change is about 32 seconds.
EXAMPLE 27
[0227] A capsule can be prepared by sizing sugar crystals using a
170 mesh sieve. The particles collected after sizing are all
.ltoreq.90.mu.. This material is again sieved through a 230 mesh
sieve. That which passes through is discarded and those crystals
remaining are now .gtoreq.63.mu. but .ltoreq.90.mu.. These crystals
are placed in a Wuerster coating unit, or as is otherwise known as
a fluid bed coater. Air rising from the bottom causes the crystals
to be suspended and circulate in the chamber. Concurrently,
volatilized blue dye, previously dissolved in a water solution is
introduced. The dye is water soluble blue dye #7. The coating
process continues until the beads increase in size to about 100 to
130.mu.. At this point the dye solution is removed and replace with
the same polyvinyl alcohol solution as described in Example 5. The
dye coated beads are then further coated with the polyvinyl alcohol
to provide a protective layer. The coating process continues until
the beads increase in size to about 125 to 160.mu.. A 30% solution
of a yellow dye is then coated onto the beads already formed so
that the size range is between about 140 and 180.mu.. Finally,
these beads are again coated with polyvinyl acetate/paraffin wax
composition as described in Example 4 to a finished size range of
about 165 and 200.mu.. Therefore, a multi-walled bead is realized
that is coated on the outside with polyvinyl acetate and paraffin
wax protecting a yellow dye underneath. Below this is layer of
polyvinyl alcohol protecting a blue dye underneath. The beads are
then removed from the coating unit.
[0228] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.7 grams of ammonium lauryl sulfate
(70%), Silwet L-7220, available from Rhodia, Inc., 1.0 gram of
Tegosoft PSE141G, available from Osi Specialties, and 1.2 grams of
the above described beads.
[0229] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The composition foams but remains as white foam. As the
rubbing continues, the walls of the beads are ruptured by the
mechanical action of washing. As the polyvinyl acetate/wax layer is
removed, the dye immediately dissolves and imparts a distinct color
shift from white to yellow. The time required for the initial color
change is about 9 seconds. As the rubbing continues, the next layer
of polyvinyl alcohol dissolves thereby releasing the blue dye. The
foam changes from yellow to green when the two dyes interact. The
time required for the second color change is about 36 seconds.
[0230] Capsule wall thickness of the bead may be increased to
accordingly change the time required for release.
EXAMPLE 28
[0231] A capsule can be prepared by sizing sugar crystals using a
170 mesh sieve. The particles collected after sizing are all
.ltoreq.90.mu.. This material is again sieved through a 230 mesh
sieve. That which passes through is discarded and those crystals
remaining are now .gtoreq.63.mu. but .ltoreq.90.mu.. These crystals
are placed in a Wuerster coating unit, or as is otherwise known as
a fluid bed coater. Air rising from the bottom causes the crystals
to be suspended and circulate in the chamber. Concurrently,
volatilized blue dye, previously dissolved in a water solution is
introduced. The dye is water soluble blue dye #7. The coating
process continues until the beads increase in size to about 100 to
130.mu.. At this point the dye solution is removed and replaced
with the same polyvinyl alcohol solution as described in Example 1.
The dye coated beads are then further coated with the polyvinyl
alcohol to provide a protective layer. The coating process
continues until the beads increase in size to about 125 to 160.mu..
A 25% solution of sodium acetate is then coated onto the beads
already formed so that the size range is between about 140 and
180.mu.. Finally, these beads are again coated with polyvinyl
acetate/paraffin wax composition as described in Example 8 to a
finished size range of about 165 and 200.mu.. Therefore, a
multi-walled bead is realized that is coated on the outside with
polyvinyl acetate and paraffin wax protecting a yellow dye
underneath. Below this is layer of polyvinyl alcohol protecting a
blue dye underneath. The beads are then removed from the coating
unit.
[0232] An aqueous cleaning composition is prepared by mixing 50
grams of deionized water, 5.7 grams of ammonium lauryl sulfate
(70%), Silwet L-7220, available from Rhodia, Inc., 1.0 gram of
Tegosoft PSE141G, available from Osi Specialties, and 1.2 grams of
the above described beads.
[0233] An effective amount of this composition is poured onto the
hands. Rubbing begins along with the addition of a small amount of
warm water. The composition foams but remains as white foam. As the
rubbing continues, the protective layer of polyvinyl acetate/wax
ruptures thereby exposing the sodium acetate. When the sodium
acetate interacts with the already dissolved sodium carbonate,
there is a double displacement reaction resulting in the release of
carbon dioxide gas. This effervescence causes the foam to lather
even more. The time for this release is about 5 seconds. As the
rubbing continues, the second layer of polyvinyl alcohol dissolves
thereby releasing the dye. It immediately turns the foam blue. The
time required for this action is about 30 seconds.
[0234] These numerous examples along with some of the various
permutations and combinations of the multiple zone encapsulation
system set out in Table 1 used to generate handwashing compositions
is not intended to limit the invention to only those permutations
and combinations of the multiple zone encapsulation system describe
or only to those methods of use described, or solely to handwashing
applications, but is intended to be illustrative of the wide
variety of single and multiple zone capsules that can be made and
the wide variety of applications in which the invention can be
used, such as formulations that comprise, individually or in
combination, elements, substances, compositions, components, or
materials, that are suitable for application to the human skin,
hair, or nails such as soaps, shampoos, conditioners, moisturizers,
masks, depilatories, lotions, creams, toothpastes, teeth whiteners,
make up removers, cuticle oil; or can be useful with respect to:
cleaning formulations; pharmaceutical formulations; surface
preparation or finishing formulations such as automotive finish
cleaners and waxes; upholstery cleaners; carpet cleaners; or the
like.
[0235] Importantly, it should be understood that the multiple zone
encapsulation system can further include a third capsule wall
defining a third zone containing a third amount of material, a
fourth capsule wall defining a fourth zone, and so forth, each of
which can respond to a third activation element or a fourth
activation element, if desired.
[0236] Also, it should be understood that the materials contained
within the zones can further include materials that individually or
in combination with the materials of other zone can generate
perceivable tactile indicia, auditory indicia, additional visual
indicia, or additional fragrance indicia in response to the
activation elements selected.
[0237] The basic concepts of the invention may be embodied and
claimed in a variety of ways. The invention involves a material
encapsulation and delivery system; capsules providing one or more
zones containing materials; carriers in which such capsules can be
conveyed and into which such materials can be released; cosmetics,
hand wash agents, and other useful compositions conveying such
capsules; and methods of making and using embodiments of the
invention.
[0238] While specific illustrative examples of the invention are
disclosed in the description and drawings, it should be understood
that these illustrative examples are not intended to be limiting
with respect to the generic nature of the invention which
encompasses numerous and varied embodiments; many alternatives are
implicit or inherent. Each feature or element of the invention is
to be understood to be representative of a broader function or of a
great variety of alternative or equivalent elements. Where the
feature or element is described in device-oriented terminology,
each element of the device is to be understood to perform a
function. Neither the description nor the terminology is intended
to limit the scope of the claims herein included solely to an
apparatus or to a method.
[0239] Particularly, it should be understood that as the disclosure
relates to elements of the invention, the words for each element
may be expressed by equivalent apparatus terms or method
terms--even if only the function or result is the same. Such
equivalent, broader, or even more generic terms should be
considered to be encompassed in the description of each element or
action. Such terms can be substituted where desired to make
explicit the implicitly broad coverage to which this invention is
entitled. As but one example, it should be understood that all
actions may be expressed as a means for taking that action or as an
element which causes that action. Similarly, each physical element
disclosed should be understood to encompass a disclosure of the
action which that physical element facilitates. Regarding this last
aspect, as but one example, the disclosure of a "capsule" should be
understood to encompass disclosure of the act of
"encapsulating"--whether explicitly discussed or not--and,
conversely, were there effectively disclosure of the act of
"encapsulating", such a disclosure should be understood to
encompass disclosure of a "capsule" and even a "means for
encapsulating". Such changes and alternative terms are to be
understood to be explicitly included in the description.
[0240] As such, it should be understood that a variety of changes
may be made to the invention as described without departing from
the essence of the invention. The disclosure encompassing both the
explicit embodiment(s) shown, the great variety of implicit
alternative embodiments, and the methods or processes are relied
upon to support the claims of this application.
[0241] Any patents, publications, or other references mentioned in
this application for patent are hereby incorporated by reference.
In addition, as to each term used it should be understood that
unless its utilization is inconsistent with such interpretation,
common dictionary definitions should be understood as incorporated
by reference for each term and all definitions, alternative terms,
and synonyms such as contained in the Random House Webster's
Unabridged Dictionary, second edition.
[0242] Thus, the applicant(s) should be understood to claim at
least: i) each of the material encapsulation systems as herein
disclosed and described, ii) the related methods disclosed and
described, iii) similar, equivalent, and even implicit variations
of each of these devices and methods, iv) those alternative designs
which accomplish each of the functions shown as are disclosed and
described, v) those alternative designs and methods which
accomplish each of the functions shown as are implicit to
accomplish that which is disclosed and described, vi) each feature,
component, and step shown as separate and independent inventions,
vii) the applications enhanced by the various systems or components
disclosed, viii) the resulting products produced by such systems or
components, ix) methods and apparatuses substantially as described
hereinbefore and with reference to any of the accompanying
examples, x) the related methods disclosed and described, xi)
similar, equivalent, and even implicit variations of each of these
systems and methods, xii) those alternative designs which
accomplish each of the functions shown as are disclosed and
described, xiii) those alternative devices and methods which
accomplish each of the functions shown as are implicit to
accomplish that which is disclosed and described, ivx) each
feature, component, and step shown as separate and independent
inventions, xv) the various combinations and permutations of each
of the above, and xvi) each potentially dependent claim or concept
as a dependency on each and every one of the independent claims or
concepts presented.
[0243] It should be understood for practical reasons, the applicant
may initially present only apparatus or method claims and then only
with initial dependencies. The applicant does not waive any right
to present additional independent or dependent claims which are
supported by the description during the prosecution of this
application. The applicant specifically reserves all rights to file
continuation, division, continuation-in-part, or other continuing
applications to claim the various inventions described without
limitation by any claim made in a prior application to the generic
nature of the invention or the breadth of any claim made in a
subsequent application.
[0244] Further, the use of the transitional phrase "comprising" is
used to maintain "open-end" claims herein, according to traditional
claim interpretation. Thus, unless the context requires otherwise,
it should be understood that the term "comprise" or variations such
as "comprises" or "comprising", are intended to imply the inclusion
of a stated element or step or group of elements or steps but not
the exclusion of any other element or step or group of elements or
steps. Such terms should be interpreted in their most expansive
form so as to afford the applicant the broadest coverage legally
permissible.
[0245] The claims set forth in this specification are hereby
incorporated by reference as part of this description of the
invention, and the applicant expressly reserves the right to use
all of or a portion of such incorporated content of such claims as
additional description to support any of or all of the claims or
any element or component thereof, and the applicant further
expressly reserves the right to move any portion of or all of the
incorporated content of such claims or any element or component
thereof from the description into the claims or vice-versa as
necessary to define the matter for which protection is sought by
this application or by any subsequent continuation, division, or
continuation-in-part application thereof, or to obtain any benefit
of, reduction in fees pursuant to, or to comply with the patent
laws, rules, or regulations of any country or treaty, and such
content incorporated by reference shall survive during the entire
pendency of this application including any subsequent continuation,
division, or continuation-in-part application thereof or any
reissue or extension thereon.
* * * * *