U.S. patent number RE45,538 [Application Number 13/891,411] was granted by the patent office on 2015-06-02 for benefit agent containing delivery particle.
This patent grant is currently assigned to The Procter & Gamble Company. The grantee listed for this patent is Jiten Odhavji Dihora, Sandra Jacqueline Guinebretiere, An Pintens, Peggy Dorothy Sands, Johan Smets. Invention is credited to Jiten Odhavji Dihora, Sandra Jacqueline Guinebretiere, An Pintens, Peggy Dorothy Sands, Johan Smets.
United States Patent |
RE45,538 |
Smets , et al. |
June 2, 2015 |
Benefit agent containing delivery particle
Abstract
The present invention relates to benefit agent containing
delivery particles, compositions comprising said particles, and
processes for making and using the aforementioned particles and
compositions. When employed in compositions, for example,
compositions for cleaning, fabric care, or coating onto various
substrates, textiles or surfaces, such particles increase the
efficiency of benefit agent delivery, thereby allowing reduced
amounts of benefit agents to be employed. In addition to allowing
the amount of benefit agent to be reduced, such particles allow a
broad range of benefit agents to be employed.
Inventors: |
Smets; Johan (Lubbeek,
BE), Sands; Peggy Dorothy (Appleton, WI),
Guinebretiere; Sandra Jacqueline (Appleton, WI), Pintens;
An (Merksem, BE), Dihora; Jiten Odhavji
(Hamilton, OH) |
Applicant: |
Name |
City |
State |
Country |
Type |
Smets; Johan
Sands; Peggy Dorothy
Guinebretiere; Sandra Jacqueline
Pintens; An
Dihora; Jiten Odhavji |
Lubbeek
Appleton
Appleton
Merksem
Hamilton |
N/A
WI
WI
N/A
OH |
BE
US
US
BE
US |
|
|
Assignee: |
The Procter & Gamble
Company (Cincinnati, OH)
|
Family
ID: |
39325228 |
Appl.
No.: |
13/891,411 |
Filed: |
May 10, 2013 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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60861996 |
Nov 30, 2006 |
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60860645 |
Nov 22, 2006 |
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Reissue of: |
11986094 |
Nov 20, 2007 |
7968510 |
Jun 28, 2011 |
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Current U.S.
Class: |
1/1 |
Current CPC
Class: |
A23P
10/30 (20160801); A61K 8/11 (20130101); A61P
43/00 (20180101); A23L 33/15 (20160801); A61Q
13/00 (20130101); C11D 3/505 (20130101); A61K
8/8152 (20130101); C11D 17/0039 (20130101); A61K
8/84 (20130101); A23L 27/72 (20160801); A61K
2800/56 (20130101); Y10T 428/2984 (20150115); A61K
2800/412 (20130101); A23V 2002/00 (20130101); Y10T
428/2985 (20150115); A23V 2002/00 (20130101); A23V
2200/332 (20130101); A23V 2250/21 (20130101) |
Current International
Class: |
A61K
8/11 (20060101) |
Field of
Search: |
;512/1-4
;428/402.2,402.21 |
References Cited
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Other References
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Primary Examiner: Choi; Ling
Assistant Examiner: Reuther; Lanee
Attorney, Agent or Firm: McBride; James F. Miller; Steven
W.
Parent Case Text
CROSS-REFERENCES TO RELATED APPLICATIONS
This application claims priority under 35 U.S.C. .sctn.119(e) to
U.S. Provisional Application Ser. No. 60/861,996 filed Nov. 30,
2006, and U.S. Provisional Application Ser. No. 60/860,645 filed
Nov. 22, 2006.
Claims
What is claimed is:
1. A composition comprising a particle composition comprising one
or more particles comprising a core material and a wall material
that at least partially surrounds said core material, said
particles being selected from the group consisting of Type 1
particles having a Volume Weighted Fracture Strength of less than
.[.about.]. 0.8 MPa, Type 2 particles having a Volume Weighted
Fracture Strength of from .[.about 0.5.]. .Iadd.0.8 .Iaddend.MPa to
.[.about.]. .Iadd.less than .Iaddend.2 MPa, Type 3 particles having
a Volume Weighted Fracture Strength of from .[.about 1.5.]. .Iadd.2
.Iaddend.MPa to .[.about.]. .Iadd.less than .Iaddend.5 MPa, Type 4
particles having a Volume Weighted Fracture Strength of from
.[.about.]. 5 MPa to about 16 MPa.Iadd., .Iaddend.and mixtures
thereof, wherein the volume weight of each type of particle in said
particle composition is as follows: Type 1 Particles: from about 5%
to about 50%; Type 2 Particles: from about 5% to about 50%; Type 3
Particles: from about 5% to about .[.90.]. .Iadd.25.Iaddend.%; and
Type 4 Particles: from about 5% to about 50%; wherein said
composition is a consumer product.
2. The composition of claim 1, wherein said particles' core
material comprises a material selected from the group consisting of
perfume raw materials, silicone oils, waxes, hydrocarbons, higher
fatty acids, essential oils, lipids, skin coolants, vitamins,
sunscreens, antioxidants, glycerine, catalysts, bleach particles,
silicon dioxide particles, malodor reducing agents,
odor-controlling materials, chelating agents, anti-static agents,
softening agents, insect and moth repelling agents, colorants,
antioxidants, chelants, bodying agents, drape and form control
agents, smoothness agents, wrinkle control agents, sanitization
agents, disinfecting agents, germ control agents, mold control
agents, mildew control agents, antiviral agents, drying agents,
stain resistance agents, soil release agents, fabric refreshing
agents and freshness extending agents, chlorine bleach odor control
agents, dye fixatives, dye transfer inhibitors, color maintenance
agents, optical brighteners, color restoration/rejuvenation agents,
anti-fading agents, whiteness enhancers, anti-abrasion agents, wear
resistance agents, fabric integrity agents, anti-wear agents,
anti-pilling agents, defoamers, anti-foaming agents, UV protection
agents, sun fade inhibitors, anti-allergenic agents, enzymes, water
proofing agents, fabric comfort agents, shrinkage resistance
agents, stretch resistance agents, stretch recovery agents, skin
care agents, glycerin, and natural actives, antibacterial actives,
antiperspirant actives, cationic polymers, dyes and mixtures
thereof.
3. The composition of claim 1 wherein said particles' wall material
comprises a material selected from the group consisting of
polyamine, polyurea, polyurethane polysaccharides and modified
polysaccharides, gel forming proteins, modified celluloses,
carboxylic acid containing acrylic polymers, gelatin, gum arabic,
urea crosslinked with formaldehyde, urea crosslinked with
gluteraldehyde, melamine crosslinked with formaldehyde, chitin and
chitosan and modified chitin and modified chitosan, sodium
alginate, latexes, silicon dioxide, sodium silicates and mixtures
thereof.
4. The composition of claim 1 wherein said particle comprises at
least 1 weight % of a benefit agent.
5. The composition of claim 1 wherein said particles' core material
comprises, based on total core material weight, at least about 20
wt % benefit agent.
6. The composition of claim 5 said benefit agent comprises a
perfume composition, said particles comprising, based on total
particle weight, from about 20 weight % to about 95 weight %, of
said perfume composition.
7. The composition of claim 6, wherein said perfume composition
comprises a Quadrant III perfume raw material.
8. The composition of claim 1 wherein said particles' comprise a
core material comprising: a.) a perfume composition having a Clog P
of less than 4.5; b.) a perfume composition comprising, based on
total perfume composition weight, 60% perfume materials having a
Clog P of less than 4.0; c.) a perfume composition comprising,
based on total perfume composition weight, 35% perfume materials
having a Clog P of less than 3.5; d.) a perfume composition
comprising, based on total perfume composition weight, 40% perfume
materials having a Clog P of less than 4.0 and at least 1% perfume
materials having a Clog P of less than 2.0; e.) a perfume
composition comprising, based on total perfume composition weight,
40% perfume materials having a Clog P of less than 4.0 and at least
15% perfume materials having a Clog P of less than 3.0; f.) a
perfume composition comprising, based on total perfume composition
weight, at least 1% butanoate esters and at least 1% of pentanoate
esters; g.) a perfume composition comprising, based on total
perfume composition weight, at least 2% of an ester comprising an
allyl moiety and at least 10% of another perfume comprising an
ester moiety; h.) a perfume composition comprising, based on total
perfume composition weight, at least 1% of an aldehyde comprising
an alkyl chain moiety; i.) a perfume composition comprising, based
on total perfume composition weight, at least 2% of a butanoate
ester; j.) a perfume composition comprising, based on total perfume
composition weight, at least 1% of a pentanoate ester; k.) a
perfume composition comprising, based on total perfume composition
weight, at least 3% of an ester comprising an allyl moiety and 1%
of an aldehyde comprising an alkyl chain moiety; l.) a perfume
composition comprising, based on total perfume composition weight,
at least 25% of a perfume comprising an ester moiety and 1% of an
aldehyde comprising an alkyl chain moiety; m.) a perfume
compositions comprising, based on total perfume composition weight,
at least 2% of a material selected from
4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one,
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one and
3-buten-2-one,3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)- and
mixtures thereof; n.) a perfume composition comprising, based on
total perfume composition weight, at least 0.1% of
tridec-2-enonitrile, and mandaril, and mixtures thereof; o.) a
perfume composition comprising, based on total perfume composition
weight, at least 2% of a material selected from
3,7-dimethyl-6-octene nitrile,
2-cyclohexylidene-2-phenylacetonitrile and mixtures thereof; p.) a
perfume composition comprising, based on total perfume composition
weight, at least 80% of one or more perfumes comprising a moiety
selected from the group consisting of esters, aldehydes, ionones,
nitriles, ketones and combinations thereof; q.) a perfume
composition comprising, based on total perfume composition weight,
at least 3% of an ester comprising an allyl moiety; a perfume
composition comprising, based on total perfume composition weight,
at least 20% of a material selected from the group consisting of:
1-methylethyl-2-methylbutanoate; ethyl-2-methyl pentanoate;
1,5-dimethyl-1-ethenylhexyl-4-enyl acetate; p-metnh-1-en-8-yl
acetate; 4-(2,6,6-trimethyl-2-cyclo-hexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic
acid,3-(1-methylethyl)-ethyl ester; bycyclo [2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enylacetate;
hexyl 2-methyl propanoate; ethyl-2-methylbutanoate; 4-undecanone;
5-heptyldihydro-2(3h)-furanone;1,6-nonadien-3-ol,3,7-dimethyl-;
3,7-dimethylocta-1,6-dien-3-o;
3-cyclohexene-1-carboxaldehyde,dimethyl-;3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl tricycle
[5.2.1.0]decan-2-carboxylate; 2,2-dimethyl-cyclohexanepropanol;
hexyl ethanoate,
7-acetyl,1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl naphtalene;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde; 1-spiro
[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro;
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol;
3-buten-2-one,3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-;
hexanoic acid, 2-propenyl ester; (z)-non-6-en-1-al;1-decyl
aldehyde; 1-octanal; 4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
alpha-hexylcinnamaldehyde; ethyl-2,4-hexadienoate; 2-propenyl
3-cyclohexanepropanoate; and mixtures thereof; r.) a perfume
composition comprising, based on total perfume composition weight,
at least 20% of a material selected from the group consisting of:
1-methylethyl-2-methylbutanoate; ethyl-2-methyl pentanoate;
1,5-dimethyl-1-ethenylhex-4-enyl acetate; p-menth-1-en-8-yl
acetate; 4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic
acid,3-(1-methylethyl)-ethyl ester; bycyclo [2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enyl
acetate; hexyl 2-methyl propanoate;
ethyl-2-methylbutanoate,4-undecanolide;
5-heptyldihydro-2(3h)-furanone; 5-hydroxydodecanoic acid;
decalactones; undecalactones, 1,6-nonadien-3-ol,3,7-dimethyl-;
3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl tricycle
[5.2.1.0]decan-2-carboxylate; 2,2-dimethyl-cyclohexanepropanol;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde; 1-spiro
[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro,
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;1-(2,6,6-trimethyl-2-cyc-
lohexenyl)-2-buten-1-one; 3,7-dimethyloctan-3-ol;
3-buten-2-one,3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-;
hexanoic acid, 2-propenyl ester; (z)-non-6-en-1-al; 1-decyl
aldehyde; 1-octanal; 4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
ethyl-2,4-hexadienoate; 2-propenyl 3-cyclohexanepropanoate; and
mixtures thereof; s.) a perfume composition comprising, based on
total perfume composition weight, at least 5% of a material
selected from the group consisting of
3-cyclohexene-1-carboxaldehyde,dimethyl-;
3-buten-2-one,3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-;
patchouli oil; Hexanoic acid, 2-propenyl ester; 1-Octanal; 1-decyl
aldehyde; (z)-non-6-en-1-al; methyl nonyl acetic aldehyde;
ethyl-2-methylbutanoate; 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 4-hydroxy-3-ethoxybenzaldehyde;
4-hydroxy-3-methoxybenzaldehyde; 3-hydroxy-2-methyl-4-pyrone;
3-hydroxy-2-ethyl-4-pyrone and mixtures thereof; t.) a perfume
composition comprising, based on total perfume composition weight,
less than 10% perfumes having a Clog P greater than 5.0; u.) a
perfume composition comprising geranyl palmitate; or v.) a perfume
composition comprising a first and an optional second material,
said first material having: (i) a Clog P of at least 2; (ii) a
boiling point of less than about 280.degree. C.; and second
optional second material, when present, having (i) a Clog P of less
than 2.5; and (ii) a ODT of less than about 100 ppb.
9. A method of treating and/or cleaning a situs, said method
comprising a.) optionally washing and/or rinsing said situs; b.)
contacting said situs with a composition according to claim 1 and
c.) optionally washing and/or rinsing said situs.
10. A situs treated with a composition according to claim 1.
11. A composition according to claim 1 said composition comprising
a formaldehyde scavenger.
12. The composition of claim 1, wherein said Type 1 particles have
a Volume Weighted Fracture Strength of from about 0.1 MPa to
.[.about.]. .Iadd.less than .Iaddend.0.8 MPa, said Type 2 particles
have a Volume Weighted Fracture Strength of from .[.about.]. 0.8
MPa to about 1.8 MPa, said Type 3 particles have a Volume Weighted
Fracture Strength of from about 2 MPa to about 4 MPa, and said Type
4 particles have a Volume Weighted Fracture Strength of from about
5 MPa to about 9 MPa.
13. The composition of claim 1, wherein said Type 1 particles have
a Volume Weighted Fracture Strength of from about 0.25 MPa to about
0.75 MPa, said Type 2 particles have a Volume Weighted Fracture
Strength of from about 1 MPa to about 1.7 MPa, said Type 3
particles have a Volume Weighted Fracture Strength of from about 2
MPa to about 3 MPa, and said Type 4 particles have a Volume
Weighted Fracture Strength of from about 6 MPa to about 8 MPa.
14. The composition of claim 1 wherein the volume weight of each
type of particle is follows: Type 1 Particles, from about 5% to
about 25%; Type 2 Particles: from about 5% to about 50%; Type 3
Particles: from about 5% to about 25%; and Type 4 Particles: from
about 5% to about 25%.
.Iadd.15. A composition comprising a particle composition
comprising one or more particles comprising a core material and a
wall material that at least partially surrounds said core material,
said particles being selected from the group consisting of Type 1
particles having a Volume Weighted Fracture Strength of less than
0.8 MPa, Type 2 particles having a Volume Weighted Fracture
Strength of from 0.8 MPa to less than 2 MPa, Type 3 particles
having a Volume Weighted Fracture Strength of from 2 MPa to less
than 5 MPa, Type 4 particles having a Volume Weighted Fracture
Strength of from 5 MPa to about 16 MPa, and mixtures thereof,
wherein the volume weight of each type of particle in said particle
composition is as follows: Type 1 particles: from about 5% to about
50%; Type 2 particles: from about 5% to about 50%; Type 3
particles: from about 5% to about 90%; and Type 4 particles: from
about 5% to about 50%; with the proviso that the sum of the
percentages of the Type 1, Type 2, Type 3 and Type 4 particles in
the particle composition is always 100%; wherein said composition
is a consumer product..Iaddend.
.Iadd.16. A composition comprising a particle composition
comprising one or more particles comprising a core material and a
wall material that at least partially surrounds said core material,
said particles being selected from the group consisting of Type 1
particles having a Volume Weighted Fracture Strength of from about
0.1 MPa to less than 0.8 MPa, Type 2 particles having a Volume
Weighted Fracture Strength of from 0.8 MPa to about 1.8 MPa, Type 3
particles having a Volume Weighted Fracture Strength of from about
2 MPa to about 4 MPa, Type 4 particles having a Volume Weighted
Fracture Strength of from about 5 MPa to about 9 MPa, and mixtures
thereof, wherein the volume weight of each type of particle in said
particle composition is as follows: Type 1 particles: from about 5%
to about 50%; Type 2 particles: from about 5% to about 50%; Type 3
particles: from about 5% to about 90%; and Type 4 particles: from
about 5% to about 50%; with the proviso that the sum of the
percentages of the Type 1, Type 2, Type 3 and Type 4 particles in
the particle composition is always 100%; wherein said composition
is a consumer product..Iaddend.
.Iadd.17. A composition comprising a particle composition
comprising one or more particles comprising a core material and a
wall material that at least partially surrounds said core material,
said particles being selected from the group consisting of Type 1
particles having a Volume Weighted Fracture Strength of from about
0.25 MPa to about 0.75 MPa, Type 2 particles having a Volume
Weighted Fracture Strength of from about 1 MPa to about 1.7 MPa,
Type 3 particles having a Volume Weighted Fracture Strength of from
about 2 MPa to about 3 MPa, Type 4 particles having a Volume
Weighted Fracture Strength of from about 6 MPa to about 8 MPa, and
mixtures thereof, wherein the volume weight of each type of
particle in said particle composition is as follows: Type 1
particles: from about 5% to about 50%; Type 2 particles: from about
5% to about 50%; Type 3 particles: from about 5% to about 90%; and
Type 4 particles: from about 5% to about 50%; with the proviso that
the sum of the percentages of the Type 1, Type 2, Type 3 and Type 4
particles in the particle composition is always 100%; wherein said
composition is a consumer product..Iaddend.
.Iadd.18. A composition comprising a particle composition
comprising one or more particles comprising a core material and a
wall material that at least partially surrounds said core material,
said particles being selected from the group consisting of Type 1
particles having a Volume Weighted Fracture Strength of from about
0.1 MPa to less than 0.8 MPa, Type 2 particles having a Volume
Weighted Fracture Strength of from 0.8 MPa to about 1.8 MPa, Type 3
particles having a Volume Weighted Fracture Strength of from about
2 MPa to about 4 MPa, Type 4 particles having a Volume Weighted
Fracture Strength of from about 5 MPa to about 9 MPa, and mixtures
thereof, wherein the volume weight of each type of particle in said
particle composition is as follows: Type 1 particles: from about 5%
to about 25%; Type 2 particles: from about 5% to about 50%; Type 3
particles: from about 5% to about 25%; and Type 4 particles: from
about 5% to about 25%; wherein said composition is a consumer
product..Iaddend.
.Iadd.19. A composition comprising a particle composition
comprising one or more particles comprising a core material and a
wall material that at least partially surrounds said core material,
said particles being selected from the group consisting of Type 1
particles having a Volume Weighted Fracture Strength of from about
0.25 MPa to about 0.75 MPa, Type 2 particles having a Volume
Weighted Fracture Strength of from about 1 MPa to about 1.7 MPa,
Type 3 particles having a Volume Weighted Fracture Strength of from
about 2 MPa to about 3 MPa, Type 4 particles having a Volume
Weighted Fracture Strength of from about 6 MPa to about 8 MPa, and
mixtures thereof, wherein the volume weight of each type of
particle in said particle composition is as follows: Type 1
particles: from about 5% to about 25%; Type 2 particles: from about
5% to about 50%; Type 3 particles: from about 5% to about 25%; and
Type 4 particles: from about 5% to about 25%; wherein said
composition is a consumer product..Iaddend.
Description
FIELD OF INVENTION
The present application relates to benefit agent containing
delivery particles, compositions comprising such particles, and
processes for making and using such particles and compositions.
BACKGROUND OF THE INVENTION
Benefit agents, such as perfumes, silicones, waxes, flavors,
vitamins and fabric softening agents, are expensive and generally
less effective when employed at high levels in personal care
compositions, cleaning compositions, and fabric care compositions.
As a result, there is a desire to maximize the effectiveness of
such benefit agents. One method of achieving such objective is to
improve the delivery efficiencies of such benefit agents.
Unfortunately, it is difficult to improve the delivery efficiencies
of benefit agents as such agents may be lost do to the agents'
physical or chemical characteristics, or such agents may be
incompatible with other compositional components or the situs that
is treated.
Accordingly, there is a need for a benefit agent containing
delivery particle that provides improved benefit agent delivery
efficiency.
SUMMARY OF THE INVENTION
The present invention relates to benefit agent containing delivery
particles comprising a core material and a wall material that at
least partially surrounds the core material. The present invention
also relates to compositions comprising said particles, and
processes for making and using such particles and compositions.
DETAILED DESCRIPTION OF THE INVENTION
Definitions
As used herein "consumer product" means baby care, beauty care,
fabric & home care, family care, feminine care, health care,
snack and/or beverage products or devices intended to be used or
consumed in the form in which it is sold, and not intended for
subsequent commercial manufacture or modification. Such products
include but are not limited to diapers, bibs, wipes; products for
and/or methods relating to treating hair (human, dog, and/or cat),
including, bleaching, coloring, dyeing, conditioning, shampooing,
styling; deodorants and antiperspirants; personal cleansing;
cosmetics; skin care including application of creams, lotions, and
other topically applied products for consumer use; and shaving
products, products for and/or methods relating to treating fabrics,
hard surfaces and any other surfaces in the area of fabric and home
care, including: air care, car care, dishwashing, fabric
conditioning (including softening), laundry detergency, laundry and
rinse additive and/or care, hard surface cleaning and/or treatment,
and other cleaning for consumer or institutional use; products
and/or methods relating to bath tissue, facial tissue, paper
handkerchiefs, and/or paper towels; tampons, feminine napkins;
products and/or methods relating to oral care including
toothpastes, tooth gels, tooth rinses, denture adhesives, tooth
whitening; over-the-counter health care including cough and cold
remedies, pain relievers, RX pharmaceuticals, pet health and
nutrition, and water purification; processed food products intended
primarily for consumption between customary meals or as a meal
accompaniment (non-limiting examples include potato chips, tortilla
chips, popcorn, pretzels, corn chips, cereal bars, vegetable chips
or crisps, snack mixes, party mixes, multigrain chips, snack
crackers, cheese snacks, pork rinds, corn snacks, pellet snacks,
extruded snacks and bagel chips); and coffee.
As used herein, the term "cleaning composition" includes, unless
otherwise indicated, granular or powder-form all-purpose or
"heavy-duty" washing agents, especially cleaning detergents;
liquid, gel or paste-form all-purpose washing agents, especially
the so-called heavy-duty liquid types; liquid fine-fabric
detergents; hand dishwashing agents or light duty dishwashing
agents, especially those of the high-foaming type; machine
dishwashing agents, including the various tablet, granular, liquid
and rinse-aid types for household and institutional use; liquid
cleaning and disinfecting agents, including antibacterial hand-wash
types, cleaning bars, mouthwashes, denture cleaners, dentifrice,
car or carpet shampoos, bathroom cleaners; hair shampoos and
hair-rinses; shower gels and foam baths and metal cleaners; as well
as cleaning auxiliaries such as bleach additives and "stain-stick"
or pre-treat types, substrate-laden products such as dryer added
sheets, dry and wetted wipes and pads, nonwoven substrates, and
sponges; as well as sprays and mists.
As used herein, the term "fabric care composition" includes, unless
otherwise indicated, fabric softening compositions, fabric
enhancing compositions, fabric freshening compositions and
combinations there of.
As used herein, the phrase "benefit agent containing delivery
particle" encompasses microcapsules including perfume
microcapsules.
As used herein, the terms "particle", "benefit agent containing
delivery particle", "capsule" and "microcapsule" are
synonymous.
As used herein, the articles including "a" and "an" when used in a
claim, are understood to mean one or more of what is claimed or
described.
As used herein, the terms "include", "includes" and "including" are
meant to be non-limiting.
The test methods disclosed in the Test Methods Section of the
present application should be used to determine the respective
values of the parameters of Applicants' inventions.
Unless otherwise noted, all component or composition levels are in
reference to the active portion of that component or composition,
and are exclusive of impurities, for example, residual solvents or
by-products, which may be present in commercially available sources
of such components or compositions.
All percentages and ratios are calculated by weight unless
otherwise indicated. All percentages and ratios are calculated
based on the total composition unless otherwise indicated.
It should be understood that every maximum numerical limitation
given throughout this specification includes every lower numerical
limitation, as if such lower numerical limitations were expressly
written herein. Every minimum numerical limitation given throughout
this specification will include every higher numerical limitation,
as if such higher numerical limitations were expressly written
herein. Every numerical range given throughout this specification
will include every narrower numerical range that falls within such
broader numerical range, as if such narrower numerical ranges were
all expressly written herein.
Benefit Agent Containing Delivery Particle
Applicants discovered that the problem of achieving effective and
efficient benefit agent delivery can be solved in an economical
manner when a benefit agent containing delivery particle, having
comprising a core material and a wall material that at least
partially surrounds said core material and a certain combination of
physical and chemical characteristics is employed. Such physical
and chemical characteristics are defined by the Volume Weighted
Fracture Strength. The delivery effectiveness and efficiency can be
further tailored by selecting particles having the following Volume
Weighted Fracture Strengths as listed for each application: 1.)
Type 1 Benefit Agent Containing Delivery Particles (Type 1
Particles). Such particles may be employed when a benefit, for
example, odor is desired in/from a wash solution. Such particles
may have a Volume Weighted Fracture Strength less than about 0.8
MPa, from about 0.8 MPa to about 0.1 MPa, or even from about 0.75
MPa to about 0.25 MPa. 2.) Type 2 Benefit Agent Containing Delivery
Particles (Type 2 Particles). Such particles may be employed when a
benefit, for example, odor is desired from a wet situs. Such
particles may have a Volume Weighted Fracture Strength from about
0.5 MPa to about 2 MPa, from about 0.8 MPa to about 1.8 MPa, or
even from about 1 MPa to about 1.7 MPa. 3.) Type 3 Benefit Agent
Containing Delivery Particles (Type 3 Particles). Such particles
may be employed when a benefit, for example, odor is desired from a
dry situs dried after being contacted with such particles. Such
particles may have a Volume Weighted Fracture Strength from about
1.5 MPa or even 2 MPa to about 5 MPa, from about 1.5 MPa or even 2
MPa to about 4 MPa, or from about 1.5 MPa or even 2 MPa to about 3
MPa. 4.) Type 4 Benefit Agent Containing Delivery Particles (Type 4
Particles). Such particles may be employed when a benefit, for
example, odor is desired from a situs during wear/use after such
situs is contacted with such particles. Such particle may have a
Volume Weighted Fracture Strength from about 5 MPa to about 16 MPa,
from about 5 MPa to about 9 MPa, or even from about 6 MPa to about
8 MPa.
In short, the level of benefit at any one point may be tailored by
selecting the desired amount type of each class of benefit agent
containing delivery particle.
In one aspect, Applicants disclose a particle composition wherein
the total volume weight of the particles is 100% and the volume
weight of each type of particle may be as follows: Type 1
Particles. From about 0% to about 100%, from about 5% to about 50%,
or even from about 5% to about 25%; Type 2 Particles: From about 0%
to about 100%, from about 5% to about 50%, or even from about 5% to
about 25%; Type 3 Particles: From about 0% to 100%, from about 5%
to about 90%, or even from about 5% to about 25%; and Type 4
Particles: From about 0% to about 100%, from about 5% to about 50%,
or even from about 5% to about 25%. With the proviso that the sum
of the percentage of the Type 1, 2, 3 and 4 Benefit Agent
Containing Delivery Particles is always 100%--such sum cannot
exceed or be less than 100%.
In one aspect, a consumer product comprising from about 0.001% to
about 25%, from about 0.001% to about 10%, or from about 0.01% to
about 3%, based on total consumer product mass weight, of the
aforementioned particle composition is disclosed.
In one aspect, a cleaning composition comprising from about 0.005%
to about 10%, from about 0.01% to about 3%, or from about 0.1% to
about 1% based on total cleaning composition mass weight of the
aforementioned particle composition is disclosed.
In one aspect, a fabric care composition comprising from about
0.005% to about 10%, from about 0.01% to about 3%, or from about
0.1% to about 1% based on total fabric care mass weight of the
aforementioned particle composition is disclosed.
In one aspect, when the aforementioned particle composition is
employed in a consumer product, for example a liquid consumer
product, the particle composition may have a deposition of at least
10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or even 100%.
In one aspect, when the aforementioned particle composition is
employed in a consumer product, for example a liquid consumer
product, the particle composition may have less than 50%, 40%, 30%,
20%, 10% or even 0% leakage of the encapsulated benefit agent from
the microcapsules of said particle composition into said consumer
product.
Useful wall materials include materials selected from the group
consisting of polyethylenes, polyamides, polystyrenes,
polyisoprenes, polycarbonates, polyesters, polyacrylates,
polyureas, polyurethanes, polyolefins, polysaccharides, epoxy
resins, vinyl polymers, and mixtures thereof. In one aspect, useful
wall materials include materials that are sufficiently impervious
to the core material and the materials in the environment in which
the benefit agent containing delivery particle will be employed, to
permit the delivery benefit to be obtained. Suitable impervious
wall materials include materials selected from the group consisting
of reaction products of one or more amines with one or more
aldehydes, such as urea cross-linked with formaldehyde or
gluteraldehyde, melamine cross-linked with formaldehyde;
gelatin-polyphosphate coacervates optionally cross-linked with
gluteraldehyde; gelatin-gum Arabic coacervates; cross-linked
silicone fluids; polyamine reacted with polyisocyanates and
mixtures thereof. In one aspect, the wall material comprises
melamine cross-linked with formaldehyde.
Useful core materials include perfume raw materials, silicone oils,
waxes, hydrocarbons, higher fatty acids, essential oils, lipids,
skin coolants, vitamins, sunscreens, antioxidants, glycerine,
catalysts, bleach particles, silicon dioxide particles, malodor
reducing agents, odor-controlling materials, chelating agents,
antistatic agents, softening agents, insect and moth repelling
agents, colorants, antioxidants, chelants, bodying agents, drape
and form control agents, smoothness agents, wrinkle control agents,
sanitization agents, disinfecting agents, germ control agents, mold
control agents, mildew control agents, antiviral agents, drying
agents, stain resistance agents, soil release agents, fabric
refreshing agents and freshness extending agents, chlorine bleach
odor control agents, dye fixatives, dye transfer inhibitors, color
maintenance agents, optical brighteners, color
restoration/rejuvenation agents, anti-fading agents, whiteness
enhancers, anti-abrasion agents, wear resistance agents, fabric
integrity agents, anti-wear agents, anti-pilling agents, defoamers
and anti-foaming agents, UV protection agents for fabrics and skin,
sun fade inhibitors, anti-allergenic agents, enzymes, water
proofing agents, fabric comfort agents, shrinkage resistance
agents, stretch resistance agents, stretch recovery agents, skin
care agents, glycerin, and natural actives such as aloe vera,
vitamin E, shea butter, cocoa butter, and the like, brighteners,
antibacterial actives, antiperspirant actives, cationic polymers,
dyes and mixtures thereof. In one aspect, said perfume raw material
is selected from the group consisting of alcohols, ketones,
aldehydes, esters, ethers, nitrites alkenes. In one aspect the core
material comprises a perfume. In one aspect, said perfume comprises
perfume raw materials selected from the group consisting of
alcohols, ketones, aldehydes, esters, ethers, nitrites alkenes and
mixtures thereof. In one aspect, said perfume may comprise a
perfume raw material selected from the group consisting of perfume
raw materials having a boiling point (B.P.) lower than about
250.degree. C. and a ClogP lower than about 3, perfume raw
materials having a B.P. of greater than about 250.degree. C. and a
ClogP of greater than about 3, perfume raw materials having a B.P.
of greater than about 250.degree. C. and a ClogP lower than about
3, perfume raw materials having a B.P. lower than about 250.degree.
C. and a ClogP greater than about 3 and mixtures thereof. Perfume
raw materials having a boiling point B.P. lower than about
250.degree. C. and a ClogP lower than about 3 are known as Quadrant
I perfume raw materials, perfume raw materials having a B.P. of
greater than about 250.degree. C. and a ClogP of greater than about
3 are known as Quadrant IV perfume raw materials, perfume raw
materials having a B.P. of greater than about 250.degree. C. and a
ClogP lower than about 3 are known as Quadrant II perfume raw
materials, perfume raw materials having a B.P. lower than about
250.degree. C. and a ClogP greater than about 3 are known as a
Quadrant III perfume raw materials. In one aspect, said perfume
comprises a perfume raw material having B.P. of lower than about
250.degree. C. In one aspect, said perfume comprises a perfume raw
material selected from the group consisting of Quadrant I, II, III
perfume raw materials and mixtures thereof. In one aspect, said
perfume comprises a Quadrant III perfume raw material. Suitable
Quadrant I, II, III and IV perfume raw materials are disclosed in
U.S. Pat. No. 6,869,923 B1.
In one aspect, said perfume comprises a Quadrant IV perfume raw
material. While not being bound by theory, it is believed that such
Quadrant IV perfume raw materials can improve perfume odor
"balance". Said perfume may comprise, based on total perfume
weight, less than about 30%, less than about 20%, or even less than
about 15% of said Quadrant IV perfume raw material.
In one aspect, said benefit agent delivery particles' core material
comprises: a.) a perfume composition having a Clog P of less than
4.5; b.) a perfume composition comprising, based on total perfume
composition weight, 60% perfume materials having a Clog P of less
than 4.0; c.) a perfume composition comprising, based on total
perfume composition weight, 35% perfume materials having a Clog P
of less than 3.5; d.) a perfume composition comprising, based on
total perfume composition weight, 40% perfume materials having a
Clog P of less than 4.0 and at least 1% perfume materials having a
Clog P of less than 2.0; e.) a perfume composition comprising,
based on total perfume composition weight, 40% perfume materials
having a Clog P of less than 4.0 and at least 15% perfume materials
having a Clog P of less than 3.0; f.) a perfume composition
comprising, based on total perfume composition weight, at least 1%
butanoate esters and at least 1% of pentanoate esters; g.) a
perfume composition comprising, based on total perfume composition
weight, at least 2% of an ester comprising an allyl moiety and at
least 10% of another perfume comprising an ester moiety; h.) a
perfume composition comprising, based on total perfume composition
weight, at least 1% of an aldehyde comprising an alkyl chain
moiety; i.) a perfume composition comprising, based on total
perfume composition weight, at least 2% of a butanoate ester; j.) a
perfume composition comprising, based on total perfume composition
weight, at least 1% of a pentanoate ester; k.) a perfume
composition comprising, based on total perfume composition weight,
at least 3% of an ester comprising an allyl moiety and 1% of an
aldehyde comprising an alkyl chain moiety; l.) a perfume
composition comprising, based on total perfume composition weight,
at least 25% of a perfume comprising an ester moiety and 1% of an
aldehyde comprising an alkyl chain moiety; m.) a perfume
compositions comprising, based on total perfume composition weight,
at least 2% of a material selected from
4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one,
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one and 3-buten-2-one,
3-methyl-4-(2,6,6-tri-methyl-1-cyclohexen-2-yl)- and mixtures
thereof; n.) a perfume composition comprising, based on total
perfume composition weight, at least 0.1% of tridec-2-enonitrile,
and mandaril, and mixtures thereof; o.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
of a material selected from 3,7-dimethyl-6-octene nitrile,
2-cyclo-hexylidene-2-phenylacetonitrile and mixtures thereof; p.) a
perfume composition comprising, based on total perfume composition
weight, at least 80% of one or more perfumes comprising a moiety
selected from the group consisting of esters, aldehydes, ionones,
nitrites, ketones and combinations thereof; q.) a perfume
composition comprising, based on total perfume composition weight,
at least 3% of an ester comprising an allyl moiety; a perfume
composition comprising, based on total perfume composition weight,
at least 20% of a material selected from the group consisting of:
1-methylethyl-2-methylbutanoate; ethyl-2-methyl pentanoate;
1,5-dimethyl-1-ethenylhexyl-4-enyl acetate; p-metnh-1-en-8-yl
acetate; 4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate 1,5-dimethyl-1-ethenylhex-4-enylacetate;
hexyl 2-methyl propanoate; ethyl-2-methylbutanoate; 4-undecanone;
5-heptyldihydro-2(3h)-furanone; 1,6-nonadien-3-ol, 3,7dimethyl-;
3,7-dimethylocta-1,6-dien-3-o; 3-cyclohexene-1-carboxaldehyde,
dimethyl-; 3,7-dimethyl-6-octene nitrile;
4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl tricycle
[5.2.1.0]decan-2-carboxylate; 2,2-dimethyl-cyclohexanepropanol;
hexyl ethanoate, 7-acetyl,
1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl naphtalene;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one; 7-octen-2-ol,
2-methyl-6-methylene-, dihydro; cyclohexanol,
2-(1,1-dimethylethyl)-, acetate; hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal ;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
alpha-hexylcinnamaldehyde; ethyl-2,4-hexadienoate; 2-propenyl
3-cyclohexanepropanoate; and mixtures thereof; r.) a perfume
composition comprising, based on total perfume composition weight,
at least 20% of a material selected from the group consisting of:
1-methylethyl-2-methylbutanoate; ethyl-2-methyl pentanoate;
1,5-dimethyl-1-ethenylhex-4-enyl acetate; p-menth-1-en-8-yl
acetate; 4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enyl
acetate; hexyl 2-methyl propanoate; ethyl-2-methylbutanoate,
4-undecanolide; 5-heptyldihydro-2(3h)-furanone; 5-hydroxydodecanoic
acid; decalactones; undecalactones, 1,6-nonadien-3-ol,
3,7dimethyl-; 3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde, dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl tricycle
[5.2.1.0]decan-2-carboxylate; 2,2-dimethyl-cyclohexanepropanol;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde; 1-spiro
[4,5]dec-7-en-7-yl-4-pentenen-1-one; 7-octen-2-ol,
2-methyl-6-methylene-, dihydro, cyclohexanol,
2-(1,1-dimethylethyl)-, acetate; hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
ethyl-2,4-hexadienoate; 2-propenyl 3-cyclohexanepropanoate; and
mixtures thereof; s.) a perfume composition comprising, based on
total perfume composition weight, at least 5% of a material
selected from the group consisting of
3-cyclohexene-1-carboxaldehyde, dimethyl-; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; patchouli oil;
Hexanoic acid, 2-propenyl ester; 1-Octanal; 1-decyl aldehyde;
(z)-non-6-en-1-al; methyl nonyl acetic aldehyde;
ethyl-2-methylbutanoate; 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 4-hydroxy-3-ethoxybenzaldehyde;
4-hydroxy-3-methoxybenzaldehyde; 3-hydroxy-2-methyl-4-pyrone;
3-hydroxy-2-ethyl-4-pyrone and mixtures thereof; t.) a perfume
composition comprising, based on total perfume composition weight,
less than 10% perfumes having a Clog P greater than 5.0; u.) a
perfume composition comprising geranyl palmitate; or v.) a perfume
composition comprising a first and an optional second material,
said first material having: (i) a Clog P of at least 2; (ii) a
boiling point of less than about 280.degree. C.; and second
optional second material, when present, having (i) a Clog P of less
than 2.5; and (ii) a ODT of less than about 100 ppb.
The perfume raw materials and accords may be obtained from one or
more of the following companies Firmenich (Geneva, Switzerland),
Givaudan (Argenteuil, France), IFF (Hazlet, N.J.), Quest (Mount
Olive, N.J.), Bedoukian (Danbury, Conn.), Sigma Aldrich (St. Louis,
Mo.), Millennium Specialty Chemicals (Olympia Fields, Ill.),
Polarone International (Jersey City, N.J.), Fragrance Resources
(Keyport, N.J.), and Aroma & Flavor Specialties (Danbury,
Conn.).
Process of Making Benefit Agent Containing Delivery Particles
The particle disclosed in the present application may be made via
the teachings of U.S. Pat. No. 6,592,990 B2 and/or U.S. Pat. No.
6,544,926 B1 and the examples disclosed herein.
Anionic emulsifiers are typically used during the particle making
process to emulsify the benefit agent prior to microcapsule
formation. While not being bound by theory, it is believed that the
anionic materials adversely interact with the cationic surfactant
actives that are often found in compositions such as fabric care
compositions--this may yield an aesthetically unpleasing
aggregation of particles that are employed in said composition. In
addition to the unacceptable aesthetics, such aggregates may result
in rapid phase separation of the particles from the bulk phase.
Applicants discovered that such aggregates can be prevented by the
addition of certain aggregate inhibiting materials including
materials selected from the group consisting of salts, polymers and
mixtures thereof. Useful aggregate inhibiting materials include,
divalent salts such as magnesium salts, for example, magnesium
chloride, magnesium acetate, magnesium phosphate, magnesium
formate, magnesium boride, magnesium titanate, magnesium sulfate
heptahydrate; calcium salts, for example, calcium chloride, calcium
formate, calcium acetate, calcium bromide; trivalent salts, such as
aluminum salts, for example, aluminum sulfate, aluminum phosphate,
aluminum chloride n-hydrate and polymers that have the ability to
suspend anionic particles such as soil suspension polymers, for
example, (polyethylene imines, alkoxylated polyethylene imines,
polyquaternium-6 and polyquatemium-7.
In one aspect of the invention, benefit agent containing delivery
particles are manufactured and are subsequently coated with a
material to reduce the rate of leakage of the benefit agent from
the particles when the particles are subjected to a bulk
environment containing, for example, surfactants, polymers, and
solvents. Non-limiting examples of coating materials that can serve
as barrier materials include materials selected from the group
consisting of polyvinyl pyrrolidone homopolymer, and its various
copolymers with styrene, vinyl acetate, imidazole, primary and
secondary amine containing monomers, methyl acrylate, polyvinyl
acetal, maleic anhydride; polyvinyl alcohol homopolymer, and its
various copolymers with vinyl acetate, 2-acrylamide-2-methylpropane
sulfonate, primary and secondary amine containing monomers,
imidazoles, methyl acrylate; polyacrylamides; polyacrylic acids;
microcrystalline waxes; paraffin waxes; modified polysaccharides
such as waxy maize or dent corn starch, octenyl succinated
starches, derivatized starches such as hydroxyethylated or
hydroxypropylated starches, carrageenan, guar gum, pectin, xanthan
gum; modified celluloses such as hydrolyzed cellulose acetate,
hydroxy propyl cellulose, methyl cellulose, and the like; modified
proteins such as gelatin; hydrogenated and non-hydrogenated
polyalkenes; fatty acids; hardened shells such as urea crosslinked
with formaldehyde, gelatin-polyphosphate, melamine-formaldehyde,
polyvinyl alcohol cross-linked with sodium tetraborate or
gluteraldehyde; latexes of styrene-butadiene, ethyl cellulose,
inorganic materials such as clays including magnesium silicates,
aluminosilicates; sodium silicates, and the like; and mixtures
thereof. Such materials can be obtained from CP Kelco Corp. of San
Diego, Calif., USA; Degussa AG or Dusseldorf, Germany; BASF AG of
Ludwigshafen, Germany; Rhodia Corp. of Cranbury, N.J., USA; Baker
Hughes Corp. of Houston, Tex., USA; Hercules Corp. of Wilmington,
Del., USA; Agrium Inc. of Calgary, Alberta, Canada, ISP of New
Jersey U.S.A. In one aspect wherein the particle is employed in a
fabric conditioning composition, the coating material comprises
sodium silicate. While not being bound by theory, it is believed
that sodium silicate's solubility at high pH, but poor solubility
at low pH makes it an ideal material for use on particles that may
be used in compositions that are formulated at pH below 7 but used
in an environment wherein the pH is greater or equal to 7. The
benefit agent containing delivery particles made be made by
following the procedure described in U.S. Pat. No. 6,592,990.
However, the coating aspect of the present invention is not limited
to the benefit agent containing delivery particles of the present
invention as any benefit agent containing delivery particle may
benefit from the coatings and coating processes disclosed
herein.
Suitable equipment for use in the processes disclosed herein may
include continuous stirred tank reactors, homogenizers, turbine
agitators, recirculating pumps, paddle mixers, plough shear mixers,
ribbon blenders, vertical axis granulators and drum mixers, both in
batch and, where available, in continuous process configurations,
spray dryers, and extruders. Such equipment can be obtained from
Lodige GmbH (Paderborn, Germany), Littleford Day, Inc. (Florence,
Ky., U.S.A.), Forberg AS (Larvik, Norway), Glatt Ingenieurtechnik
GmbH (Weimar, Germany), Niro (Soeborg, Denmark), Hosokawa Bepex
Corp. (Minneapolis, Minn., USA), Arde Barinco (New Jersey,
USA).
Formaldehyde Scavenging
In one aspect, benefit agent containing delivery particles may be
combined with a formaldehyde scavenger. In one aspect, such benefit
agent containing delivery particles may comprise the benefit agent
containing delivery particles of the present invention. Suitable
formaldehyde scavengers include materials selected from the group
consisting of sodium bisulfite, urea, ethylene urea, cysteine,
cysteamine, lysine, glycine, serine, carnosine, histidine,
glutathione, 3,4-diaminobenzoic acid, allantoin, glycouril,
anthranilic acid, methyl anthranilate, methyl 4-aminobenzoate,
ethyl acetoacetate, acetoacetamide, malonamide, ascorbic acid,
1,3-dihydroxyacetone dimer, biuret, oxamide, benzoguanamine,
pyroglutamic acid, pyrogallol, methyl gallate, ethyl gallate,
propyl gallate, triethanol amine, succinamide, thiabendazole,
benzotriazol, triazole, indoline, sulfanilic acid, oxamide,
sorbitol, glucose, cellulose, poly(vinyl alcohol), partially
hydrolyzed poly(vinylformamide), poly(vinyl amine), poly(ethylene
imine), poly(oxyalkyleneamine), poly(vinyl alcohol)-co-poly(vinyl
amine), poly(4-aminostyrene), poly(1-lysine), chitosan, hexane
diol, ethylenediamine-N,N'-bisacetoacetamide,
N-(2-ethylhexyl)acetoacetamide, 2-benzoylacetoacetamide,
N-(3-phenylpropyl)acetoacetamide, lilial, helional, melonal,
triplal, 5,5-dimethyl-1,3-cyclohexanedione,
2,4-dimethyl-3-cyclohexenecarboxaldehyde,
2,2-dimethyl-1,3-dioxan-4,6-dione, 2-pentanone, dibutyl amine,
triethylene-tetramine, ammonium hydroxide, benzylamine,
hydroxycitronellol, cyclohexanone, 2-butanone, pentane dione,
dehydroacetic acid, or a mixture thereof. These formaldehyde
scavengers may be obtained from Sigma/Aldrich/Fluka of St. Louis,
Mo. U.S.A. or PolySciences, Inc. of Warrington, Pa. U.S.A.
Such formaldehyde scavengers are typically combined with a slurry
containing said benefit agent containing delivery particle, at a
level, based on total slurry weight, of from about 2 wt. % to about
18 wt. %, from about 3.5 wt. % to about 14 wt. % or even from about
5 wt. % to about 13 wt. %.
In one aspect, such formaldehyde scavengers may be combined with a
product containing a benefit agent containing delivery particle,
said scavengers being combined with said product at a level, based
on total product weight, of from about 0.005% to about 0.8%,
alternatively from about 0.03% to about 0.5%, alternatively from
about 0.065% to about 0.25% of the product formulation.
In another aspect, such formaldehyde scavengers may be combined
with a slurry containing said benefit agent containing delivery
particle, at a level, based on total slurry weight, of from about 2
wt. % to about 14 wt. %, from about 3.5 wt. % to about 14 wt. % or
even from about 5 wt. % to about 14 wt. % and said slurry may be
added to a product matrix to which addition an identical or
different scavenger may be added at a level, based on total product
weight, of from about 0.005% to about 0.5%, alternatively from
about 0.01% to about 0.25%, alternatively from about 0.05% to about
0.15% of the product formulation.
In one aspect, one or more of the aforementioned formaldehyde
scavengers may be combined with a liquid fabric enhancing product
containing a benefit agent containing delivery particle at a level,
based on total liquid fabric enhancing product weight, of from
0.005% to about 0.8%, alternatively from about 0.03% to about 0.4%,
alternatively from about 0.06% to about 0.25% of the product
formulation.
In one aspect, such formaldehyde scavengers may be combined with a
liquid laundry detergent product containing a benefit agent
containing delivery particle, said scavengers being selected from
the group consisting of sodium bisulfite, urea, ethylene urea,
cysteine, cysteamine, lysine, glycine, serine, carnosine,
histidine, glutathione, 3,4-diaminobenzoic acid, allantoin,
glycouril, anthranilic acid, methyl anthranilate, methyl
4-aminobenzoate, ethyl acetoacetate, acetoacetamide, malonamide,
ascorbic acid, 1,3-dihydroxyacetone dimer, biuret, oxamide,
benzoguanamine, pyroglutamic acid, pyrogallol, methyl gallate,
ethyl gallate, propyl gallate, tri-ethanol amine, succinamide,
thiabendazole, benzotriazol, triazole, indoline, sulfanilic acid,
oxamide, sorbitol, glucose, cellulose, poly(vinyl alcohol),
partially hydrolyzed poly(vinylformamide), poly(vinyl amine),
poly(ethylene imine), poly(oxyalkyleneamine), poly(vinyl
alcohol)-co-poly(vinyl amine), poly(4-aminostyrene),
poly(1-lysine), chitosan, hexane diol,
ethylenediamine-N,N'-bisacetoacetamide,
N-(2-ethylhexyl)acetoacetamide, 2-benzoylacetoacetamide,
N-(3-phenylpropyl)acetoacetamide, lilial, helional, melonal,
triplal, 5,5-dimethyl-1,3-cyclohexanedione,
2,4-dimethyl-3-cyclohexenecarboxaldehyde,
2,2-dimethyl-1,3-dioxan-4,6-dione, 2-pentanone, dibutyl amine,
triethylenetetramine, ammonium hydroxide, benzylamine,
hydroxycitronellol, cyclohexanone, 2-butanone, pentane dione,
dehydroacetic acid and mixtures thereof, and combined with said
liquid laundry detergent product at a level, based on total liquid
laundry detergent product weight, of from about 0.003 wt. % to
about 0.20 wt. %, from about 0.03 wt. % to about 0.20 wt. % or even
from about 0.06 wt. % to about 0.14 wt. %.
In one aspect, such formaldehyde scavengers may be combined with a
hair conditioning product containing a benefit agent containing
delivery particle, at a level, based on total hair conditioning
product weight, of from about 0.003 wt. % to about 0.30 wt. %, from
about 0.03 wt. % to about 0.20 wt. % or even from about 0.06 wt. %
to about 0.14 wt. %., said selection of scavengers being identical
to the list of scavengers in the previous paragraph relating to a
liquid laundry detergent product.
Compositions Comprising Benefit Agent Containing Delivery
Particles
Applicants' compositions comprise an embodiment of the particle
disclosed in the present application. In one aspect, said
composition is a consumer product. While the precise level of
particle that is employed depends on the type and end use of the
composition, a composition may comprise from about 0.01 to about
10, from about 0.1 to about 10, or even from about 0.2 to about 5
weight % of said particle based on total composition weight. In one
aspect, a cleaning composition may comprise, from about 0.1 to
about 1 weight % of such particle based on total cleaning
composition weight of such particle. In one aspect, a fabric
treatment composition may comprise, based on total fabric treatment
composition weight, form about 0.01 to about 10% of such
particle.
Aspects of the invention include the use of the particles of the
present invention in laundry detergent compositions (e.g.,
TIDE.TM.), hard surface cleaners (e.g., MR CLEAN.TM.), automatic
dishwashing liquids (e.g., CASCADE.TM.), dishwashing liquids (e.g.,
DAWN.TM.), and floor cleaners (e.g., SWIFFER.TM.). Non-limiting
examples of cleaning compositions may include those described in
U.S. Pat. Nos. 4,515,705; 4,537,706; 4,537,707; 4,550,862;
4,561,998; 4,597,898; 4,968,451; 5,565,145; 5,929,022; 6,294,514;
and 6,376,445. The cleaning compositions disclosed herein are
typically formulated such that, during use in aqueous cleaning
operations, the wash water will have a pH of between about 6.5 and
about 12, or between about 7.5 and 10.5. Liquid dishwashing product
formulations typically have a pH between about 6.8 and about 9.0.
Cleaning products are typically formulated to have a pH of from
about 7 to about 12. Techniques for controlling pH at recommended
usage levels include the use of buffers, alkalis, acids, etc., and
are well known to those skilled in the art.
Fabric treatment compositions disclosed herein typically comprise a
fabric softening active ("FSA"). Suitable fabric softening actives,
include, but are not limited to, materials selected from the group
consisting of quats, amines, fatty esters, sucrose esters,
silicones, dispersible polyolefins, clays, polysaccharides, fatty
oils, polymer latexes and mixtures thereof.
Adjunct Materials
While not essential for the purposes of the present invention, the
non-limiting list of adjuncts illustrated hereinafter are suitable
for use in the instant compositions and may be desirably
incorporated in certain embodiments of the invention, for example
to assist or enhance performance, for treatment of the substrate to
be cleaned, or to modify the aesthetics of the composition as is
the case with perfumes, colorants, dyes or the like. It is
understood that such adjuncts are in addition to the components
that are supplied via Applicants' delivery particles and FSAs. The
precise nature of these additional components, and levels of
incorporation thereof, will depend on the physical form of the
composition and the nature of the operation for which it is to be
used. Suitable adjunct materials include, but are not limited to,
polymers, for example cationic polymers, surfactants, builders,
chelating agents, dye transfer inhibiting agents, dispersants,
enzymes, and enzyme stabilizers, catalytic materials, bleach
activators, polymeric dispersing agents, clay soil
removal/anti-redeposition agents, brighteners, suds suppressors,
dyes, additional perfume and perfume delivery systems, structure
elasticizing agents, fabric softeners, carriers, hydrotropes,
processing aids and/or pigments. In addition to the disclosure
below, suitable examples of such other adjuncts and levels of use
are found in U.S. Pat. Nos. 5,576,282, 6,306,812 B1 and 6,326,348
B1 that are incorporated by reference.
As stated, the adjunct ingredients are not essential to Applicants'
cleaning and fabric care compositions. Thus, certain embodiments of
Applicants' compositions do not contain one or more of the
following adjuncts materials: bleach activators, surfactants,
builders, chelating agents, dye transfer inhibiting agents,
dispersants, enzymes, and enzyme stabilizers, catalytic metal
complexes, polymeric dispersing agents, clay and soil
removal/anti-redeposition agents, brighteners, suds suppressors,
dyes, additional perfumes and perfume delivery systems, structure
elasticizing agents, fabric softeners, carriers, hydrotropes,
processing aids and/or pigments. However, when one or more adjuncts
are present, such one or more adjuncts may be present as detailed
below:
Surfactants--The compositions according to the present invention
can comprise a surfactant or surfactant system wherein the
surfactant can be selected from nonionic and/or anionic and/or
cationic surfactants and/or ampholytic and/or zwitterionic and/or
semi-polar nonionic surfactants. The surfactant is typically
present at a level of from about 0.1%, from about 1%, or even from
about 5% by weight of the cleaning compositions to about 99.9%, to
about 80%, to about 35%, or even to about 30% by weight of the
cleaning compositions.
Builders--The compositions of the present invention can comprise
one or more detergent builders or builder systems. When present,
the compositions will typically comprise at least about 1% builder,
or from about 5% or 10% to about 80%, 50%, or even 30% by weight,
of said builder. Builders include, but are not limited to, the
alkali metal, ammonium and alkanolammonium salts of polyphosphates,
alkali metal silicates, alkaline earth and alkali metal carbonates,
aluminosilicate builders polycarboxylate compounds. ether
hydroxypolycarboxylates, copolymers of maleic anhydride with
ethylene or vinyl methyl ether,
1,3,5-trihydroxybenzene-2,4,6-trisulphonic acid, and
carboxymethyl-oxysuccinic acid, the various alkali metal, ammonium
and substituted ammonium salts of polyacetic acids such as
ethylenediamine tetraacetic acid and nitrilotriacetic acid, as well
as polycarboxylates such as mellitic acid, succinic acid,
oxydisuccinic acid, polymaleic acid, benzene 1,3,5-tricarboxylic
acid, carboxymethyloxysuccinic acid, and soluble salts thereof.
Chelating Agents--The compositions herein may also optionally
contain one or more copper, iron and/or manganese chelating agents.
If utilized, chelating agents will generally comprise from about
0.1% by weight of the compositions herein to about 15%, or even
from about 3.0% to about 15% by weight of the compositions
herein.
Dye Transfer Inhibiting Agents--The compositions of the present
invention may also include one or more dye transfer inhibiting
agents. Suitable polymeric dye transfer inhibiting agents include,
but are not limited to, polyvinylpyrrolidone polymers, polyamine
N-oxide polymers, copolymers of N-vinylpyrrolidone and
N-vinylimidazole, polyvinyloxazolidones and polyvinylimidazoles or
mixtures thereof. When present in the compositions herein, the dye
transfer inhibiting agents are present at levels from about
0.0001%, from about 0.01%, from about 0.05% by weight of the
cleaning compositions to about 10%, about 2%, or even about 1% by
weight of the cleaning compositions.
Dispersants--The compositions of the present invention can also
contain dispersants. Suitable water-soluble organic materials are
the homo- or co-polymeric acids or their salts, in which the
polycarboxylic acid may comprise at least two carboxyl radicals
separated from each other by not more than two carbon atoms.
Enzymes--The compositions can comprise one or more detergent
enzymes which provide cleaning performance and/or fabric care
benefits. Examples of suitable enzymes include, but are not limited
to, hemicellulases, peroxidases, proteases, cellulases, xylanases,
lipases, phospholipases, esterases, cutinases, pectinases,
keratanases, reductases, oxidases, phenoloxidases, lipoxygenases,
ligninases, pullulanases, tannases, pentosanases, malanases,
.beta.-glucanases, arabinosidases, hyaluronidase, chondroitinase,
laccase, and amylases, or mixtures thereof. A typical combination
is a cocktail of conventional applicable enzymes like protease,
lipase, cutinase and/or cellulase in conjunction with amylase.
Enzyme Stabilizers--Enzymes for use in compositions, for example,
detergents can be stabilized by various techniques. The enzymes
employed herein can be stabilized by the presence of water-soluble
sources of calcium and/or magnesium ions in the finished
compositions that provide such ions to the enzymes.
Catalytic Metal Complexes--Applicants' compositions may include
catalytic metal complexes. One type of metal-containing bleach
catalyst is a catalyst system comprising a transition metal cation
of defined bleach catalytic activity, such as copper, iron,
titanium, ruthenium, tungsten, molybdenum, or manganese cations, an
auxiliary metal cation having little or no bleach catalytic
activity, such as zinc or aluminum cations, and a sequestrate
having defined stability constants for the catalytic and auxiliary
metal cations, particularly ethylenediaminetetraacetic acid,
ethylenediamine-tetra (methyl-enephosphonic acid) and water-soluble
salts thereof. Such catalysts are disclosed in U.S. Pat. No.
4,430,243.
If desired, the compositions herein can be catalyzed by means of a
manganese compound. Such compounds and levels of use are well known
in the art and include, for example, the manganese-based catalysts
disclosed in U.S. Pat. No. 5,576,282.
Cobalt bleach catalysts useful herein are known, and are described,
for example, in U.S. Pat. Nos. 5,597,936 and 5,595,967. Such cobalt
catalysts are readily prepared by known procedures, such as taught
for example in U.S. Pat. Nos. 5,597,936, and 5,595,967.
Compositions herein may also suitably include a transition metal
complex of a macropolycyclic rigid ligand--abbreviated as "MRL". As
a practical matter, and not by way of limitation, the compositions
and cleaning processes herein can be adjusted to provide on the
order of at least one part per hundred million of the benefit agent
MRL species in the aqueous washing medium, and may provide from
about 0.005 ppm to about 25 ppm, from about 0.05 ppm to about 10
ppm, or even from about 0.1 ppm to about 5 ppm, of the MRL in the
wash liquor.
Preferred transition-metals in the instant transition-metal bleach
catalyst include manganese, iron and chromium. Preferred MRL's
herein are a special type of ultra-rigid ligand that is
cross-bridged such as
5,12-diethyl-1,5,8,12-tetraazabicyclo[6.6.2]hexa-decane.
Suitable transition metal MRLs are readily prepared by known
procedures, such as taught for example in WO 00/32601, and U.S.
Pat. No. 6,225,464.
Processes of Making and Using Compositions
The compositions of the present invention can be formulated into
any suitable form and prepared by any process chosen by the
formulator, non-limiting examples of which are described in U.S.
Pat. No. 5,879,584; U.S. Pat. No. 5,691,297; U.S. Pat. No.
5,574,005; U.S. Pat. No. 5,569,645; U.S. Pat. No. 5,565,422; U.S.
Pat. No. 5,516,448; U.S. Pat. No. 5,489,392; U.S. Pat. No.
5,486,303 all of which are incorporated herein by reference.
Method of Use
Compositions containing the benefit agent delivery particle
disclosed herein can be used to clean or treat a situs inter alia a
surface or fabric. Typically at least a portion of the situs is
contacted with an embodiment of Applicants' composition, in neat
form or diluted in a liquor or dispersed in a binder material, for
example, a wash liquor, or a dispersed particle composition and
binder. The situs may be optionally washed and/or rinsed before
and/or after contact. In one aspect, a situs is optionally washed
and/or rinsed, contacted with a particle according to the present
invention or composition comprising said particle and then
optionally washed and/or rinsed. For purposes of the present
invention, washing includes but is not limited to, scrubbing, and
mechanical agitation. The fabric may comprise most any fabric
capable of being laundered or treated in normal consumer use
conditions. Liquors that may comprise the disclosed compositions
may have a pH of from about 3 to about 11.5. Such compositions are
typically employed at concentrations of from about 500 ppm to about
15,000 ppm in solution. When the wash solvent is water, the water
temperature typically ranges from about 5.degree. C. to about
90.degree. C. and, when the situs comprises a fabric, the water to
fabric ratio is typically from about 1:1 to about 30:1.
When the particle composition comprises particles dispersed in
binder, the dispersed particle composition and binder can be dried
or cured on the situs. A releasing force such as pressure,
friction, heat, actinic radiation, laser light, electromagnetic
radiation, chemical degradation, or ultrasonics can be used to
release the core contents from the particles.
Some applications employ parts per million of particles to binder
where trace amounts of core are sufficient for the application. In
other applications such compositions are employed at concentration
of from 0.001% by weight of the composition to 90% by weight
capsules in a slurry of capsules and binder. Binder can be used at
a ratio of particles to binder at from 3:1 to about 0.0001 to 1 by
weight depending on the intended application. When the situs
comprises a polymeric substrate the capsules are used at a ratio of
from 1.5:1 and preferably a range from 0.001:1 to 1.2:1. With a
heavier paper surface, the particles and binder can be applied at a
coat rate of from 2.5 to 12 grams per square meter, preferably 3 to
9 gsm. with the particles being at from 0.001 to 75% of the coating
by weight.
Test Methods
It is understood that the test methods that are disclosed in the
Test Methods Section of the present application should be used to
determine the respective values of the parameters of Applicants'
invention as such invention is described and claimed herein.
(1) Fracture Strength a.) Place 1 gram of particles in 1 liter of
distilled deionized (DI) water. b.) Permit the particles to remain
in the DI water for 10 minutes and then recover the particles by
filtration. c.) Determine the average rupture force of the
particles by averaging the rupture force of 50 individual
particles. The rupture force of a particle is determined using the
procedure given in Zhang, Z.; Sun, G; "Mechanical Properties of
Melamine-Formaldehyde microcapsules," J. Microencapsulation, vol
18, no. 5, pages 593-602, 2001. Then calculate the average fracture
strength by dividing the average rupture force (in Newtons) by the
average cross-sectional area of the spherical particle
(.pi.r.sup.2, where r is the radius of the particle before
compression), said average cross-sectional area being determined as
follows: (i) Place 1 gram of particles in 1 liter of distilled
deionized (DI) water. (ii) Permit the particles to remain in the DI
water for 10 minutes and then recover the particles by filtration.
(iii) Determine the particle size distribution of the particle
sample by measuring the particle size of 50 individual particles
using the experimental apparatus and method of Zhang, Z.; Sun, G;
"Mechanical Properties of Melamine-Formaldehyde microcapsules," J.
Microencapsulation, vol 18, no. 5, pages 593-602, 2001. (iv)
Average the 50 independent particle diameter measurements to obtain
an average particle diameter. d) For a capsule slurry the sample is
divided into three particle size fractions covering the particle
size distribution. Per particle size fraction about 30 fracture
strengths are determined.
(2) ClogP The "calculated logP" (ClogP) is determined by the
fragment approach of Hansch and Leo (cf., A. Leo, in Comprehensive
Medicinal Chemistry, Vol. 4, C. Hansch, P. G. Sammens, J. B.
Taylor, and C. A. Ramsden, Eds. P. 295, Pergamon Press, 1990,
incorporated herein by reference). ClogP values may be calculated
by using the "CLOGP" program available from Daylight Chemical
Information Systems Inc. of Irvine, Calif. U.S.A.
(3) Boiling Point Boiling point is measured by ASTM method
D2887-04a, "Standard Test Method for Boiling Range Distribution of
Petroleum Fractions by Gas Chromatography," ASTM International.
(4) Volume Weight Fractions Volume weight fractions are determined
via the method of single-particle optical sensing (SPOS), also
called optical particle counting (OPC). Volume weight fractions are
determined via a AccuSizer 780/AD supplied by Particle Sizing
Systems of Santa Barbara Calif., U.S.A.
Procedure: 1) put the sensor in a cold state by flushing water
through the sensor 2) confirm background counts are less than 100
(if got more than 100, continue the flush) 3) prepare particle
standard: pipette approx. 1 ml of shaken particles into blender
filled with approx. 2 cups of DI water. Blend it. Pipette approx. 1
ml of diluted blended particles into 50 ml DI water. 4) measure
particle standard: pipette approx. 1 ml of double diluted standard
into Accusizer bulb. Press the start measurement-Autodilution
button. Confirm particles counts are more than 9200 by looking in
the status bar. If counts are less than 9200, press stop and inject
more sample. 5) immediately after measurement, inject one full
pipette of soap (5% Micro 90) into bulb and press the Start
Automatic Flush Cycles button.
(5) Volume Weighted Fracture Strength (VWFS) VWFS=(fracture
strength.sub.1.times.volume fraction.sub.1)+(fracture
strength.sub.2.times.volume fraction.sub.2)+(fracture
strength.sub.3.times.volume fraction.sub.3) Fracture
strength.sub.1=average fracture strength measured from a pool of 10
microcapsules (with similar particle size) Volume
fraction.sub.1=volume fraction determined via Accusizer of particle
distribution corresponding to fracture strength.sub.1 The spread
around the fracture strength to determine the volume fraction is
determined as follows: For particle batches with a mean particle
sizes of about 15 um a spread of about 10 um is used, for particle
batches with a mean particle sizes of about 30 um and above, a
spread of about 10 to 15 um is used
Examples
TABLE-US-00001 Fracture Strength Volume Particle Mean Determination
at Volume Fracture batch Particle Size 3 particle sizes Fractions
Strength Melamine 31 micron 21 micron: 1 to 1.5 based 1.8 MPa 25
micron MPa polyurea 31 micron: 1.6 MPa 30% 41 micron: 1.2 MPa 25 to
36 micron 40% 36 to 50 micron 30%
(6) Benefit Agent Leakage Test a.) Obtain 2, one gram samples of
benefit agent particle composition. b.) Add 1 gram (Sample 1) of
particle composition to 99 grams of product matrix that the
particle will be employed in and with the second sample immediately
proceed to Step d below. c.) Age the particle containing product
matrix (Sample 1) of a.) above for 2 weeks at 35.degree. C. in a
sealed, glass jar. d.) Recover the particle composition's particles
from the product matrix of c.) (Sample 1 in product matrix) and
from particle composition (Sample 2) above by filtration. e.) Treat
each particle sample from d.) above with a solvent that will
extract all the benefit agent from each samples' particles. f.)
Inject the benefit agent containing solvent from each sample from
e.) above into a Gas Chromatograph and integrate the peak areas to
determine the total quantity of benefit agent extracted from each
sample. g.) The benefit agent leakage is defined as: Value from f.)
above for Sample 2-Value from f.) above for Sample 1.
EXAMPLES
While particular embodiments of the present invention have been
illustrated and described, it would be obvious to those skilled in
the art that various other changes and modifications can be made
without departing from the spirit and scope of the invention. It is
therefore intended to cover in the appended claims all such changes
and modifications that are within the scope of this invention.
Example 1
80 Wt % Core/20 Wt % Wall Urea Based Polyurea Capsule
2 grams of Urea (Sigma Aldrich of Milwaukee, Wis.) is dissolved in
20 g deionized water. 1 gram of resorcinol (Sigma Aldrich of
Milwaukee, Wis.) is added to the homogeneous urea solution. 20 g of
37 wt % formaldehyde solution (Sigma Aldrich of Milwaukee, Wis.) is
added to the solution, and the pH of the slurry is adjusted to 8.0
using 1M sodium hydroxide solution (Sigma Aldrich of Milwaukee,
Wis.). The reactants are allowed to sit at 35.degree. C. for 2
hours. In a separate beaker, 80 grams of fragrance oil is added
slowly to the urea-formaldehyde solution. The mixture is agitated
using a Janke & Kunkel Laboretechnik mixer using a pitched,
3-blade agitator to achieve a 31 micron mean oil droplet size
distribution. The pH of the slurry is adjusted to 3.0 using 1M
Hydrochloric Acid to initiate the condensation reaction. The
solution is heated to 65.degree. C. and allowed to react in a
constant temperature water bath, while slowly agitating the
contents of the mixture. The contents are allowed to react for 4
hours at 65.degree. C.
The Volume Average Fracture Strength Fracture is determined to be
1.5 MPa.
Example 2
85% Core/15 Wt % Wall Melamine Based Polyurea Capsule
A first mixture is prepared by combining 208 grams of water and 5
grams of alkyl acrylate-acrylic acid copolymer (Polysciences, Inc.
of Warrington, Pa., USA). This first mixture is adjusted to pH 5.0
using acetic acid.
178 grams of the capsule core material which comprise a fragrance
oil is added to the first mixture at a temperature of 45.degree. C.
to form an emulsion. The ingredients to form the capsule wall
material are prepared as follows: 9 grams of a corresponding
capsule wall material copolymer pre-polymer (butylacrylate-acrylic
acid copolymer) and 90 grams of water are combined and adjusted to
pH 5.0. To this mixture is added 28 grams of a partially methylated
methylol melamine resin solution ("Cymel 385", 80% solids, Cytec).
This mixture is added to the above described fragrance oil-in-water
emulsion with stirring at a temperature of 45 degrees Centigrade.
High speed blending is used to achieve a volume-mean particle size
of 16 micron. The temperature of the mixture is gradually raised to
65 degrees Centigrade, and is maintained at this temperature
overnight with continuous stirring to initiate and complete
encapsulation.
To form the acrylic acid-alkyl acrylate copolymer capsule wall, the
alkyl group can be selected from ethyl, propyl, butyl, amyl, hexyl,
cyclohexyl, 2-ethylhexyl, or other alkyl groups having from one to
about sixteen carbons, preferably one to eight carbons.
The Volume Average Fracture Strength Fracture is determined to be
3.3 MPa.
Example 3
90% Core/10 Wt % Wall Melamine Based Polyurea Capsule
A first mixture is prepared by combining 208 grams of water and 5
grams of alkyl acrylate-acrylic acid copolymer (Polysciences, Inc.
of Warrington, Pa., USA). This first mixture is adjusted to pH 5.0
using acetic acid.
280 grams of the capsule core material which comprise a fragrance
oil is added to the first mixture at a temperature of 45.degree. C.
to form an emulsion. The ingredients to form the capsule wall
material are prepared as follows: 9 grams of a corresponding
capsule wall material copolymer pre-polymer (butylacrylate-acrylic
acid copolymer) and 90 grams of water are combined and adjusted to
pH 5.0. To this mixture is added 28 grams of a partially methylated
methylol melamine resin solution ("Cymel 385", 80% solids, Cytec).
This mixture is added to the above described fragrance oil-in-water
emulsion with stirring at a temperature of 45 degrees Centigrade.
High speed blending is used to achieve a volume-mean particle size
of 18 micron. The temperature of the mixture is gradually raised to
65 degrees Centigrade, and is maintained at this temperature
overnight with continuous stirring to initiate and complete
encapsulation.
To form the acrylic acid-alkyl acrylate copolymer capsule wall, the
alkyl group can be selected from ethyl, propyl, butyl, amyl, hexyl,
cyclohexyl, 2-ethylhexyl, or other alkyl groups having from one to
about sixteen carbons, preferably one to eight carbons.
The Volume Average Fracture Strength Fracture is determined to be
0.5 MPa.
Example 4
80% Core/20 Wt % Wall Melamine Based Polyurea Capsule
A first mixture is prepared by combining 208 grams of water and 5
grams of alkyl acrylate-acrylic acid copolymer (Polysciences, Inc.
of Warrington, Pa., USA). This first mixture is adjusted to pH 5.0
using acetic acid.
125 grams of the capsule core material which comprises a fragrance
oil is added to the first mixture at a temperature of 45.degree. C.
to form an emulsion. The ingredients to form the capsule wall
material are prepared as follows: 9 grams of a corresponding
capsule wall material copolymer pre-polymer (butylacrylate-acrylic
acid copolymer) and 90 grams of water are combined and adjusted to
pH 5.0. To this mixture is added 28 grams of a partially methylated
methylol melamine resin solution ("Cymel 385", 80% solids, Cytec).
This mixture is added to the above described fragrance oil-in-water
emulsion with stirring at a temperature of 45 degrees Centigrade.
High speed blending is used to achieve a volume-mean particle size
of 15 micron. The temperature of the mixture is gradually raised to
65 degrees Centigrade, and is maintained at this temperature
overnight with continuous stirring to initiate and complete
encapsulation.
To form the acrylic acid-alkyl acrylate copolymer capsule wall, the
alkyl group can be selected from ethyl, propyl, butyl, amyl, hexyl,
cyclohexyl, 2-ethylhexyl, or other alkyl groups having from one to
about sixteen carbons, preferably one to eight carbons.
The Volume Average Fracture Strength Fracture is determined to be
9.5 MPa.
Example 5
85% Core/15 Wt % Wall Melamine Based Polyurea Capsule
A first mixture is prepared by combining 208 grams of water and 5
grams of alkyl acrylate-acrylic acid copolymer (Polysciences, Inc.
of Warrington, Pa., USA). This first mixture is adjusted to pH 5.0
using acetic acid.
178 grams of the capsule core material which comprise a fragrance
oil is added to the first mixture at a temperature of 45.degree. C.
to form an emulsion. The ingredients to form the capsule wall
material are prepared as follows: 9 grams of a corresponding
capsule wall material copolymer pre-polymer (butylacrylate-acrylic
acid copolymer) and 90 grams of water are combined and adjusted to
pH 5.0. To this mixture is added 28 grams of a partially methylated
methylol melamine resin solution ("Cymel 385", 80% solids, Cytec).
This mixture is added to the above described fragrance oil-in-water
emulsion with stirring at a temperature of 45 degrees Centigrade.
High speed blending is used to achieve a volume-mean particle size
of 15 microns. The temperature of the mixture is gradually raised
to 65 degrees Centigrade, and is maintained at this temperature
overnight with continuous stirring to initiate and complete
encapsulation.
To form the acrylic acid-alkyl acrylate copolymer capsule wall, the
alkyl group can be selected from ethyl, propyl, butyl, amyl, hexyl,
cyclohexyl, 2-ethylhexyl, or other alkyl groups having from one to
about sixteen carbons, preferably one to eight carbons.
The Volume Average Fracture Strength Fracture is determined to be
15.1 MPa.
Example 6
80 Wt % Core/20 Wt % Wall Melamine Formaldehyde Capsule
18 grams of a blend of 50% butyl acrylate-acrylic acid copolymer
emulsifier (Colloid C351, 25% solids, pka 4.5-4.7, Kemira) and 50%
polyacrylic acid (35% solids, pKa 1.5-2.5, Aldrich) is dissolved
and mixed in 200 grams deionized water. The pH of the solution is
adjusted to pH of 3.5 with sodium hydroxide solution. 6.5 grams of
partially methylated methylol melamine resin (Cymel 385, 80% solids
Cytec) is added to the emulsifier solution. 200 grams of perfume
oil is added to the previous mixture under mechanical agitation and
the temperature is raised to 60.degree. C. After mixing at higher
speed until a stable emulsion is obtained, the second solution and
3.5 grams of sodium sulfate salt are poured into the emulsion. This
second solution contains 10 grams of butyl acrylate-acrylic acid
copolymer emulsifier (Colloid C351, 25% solids, pka 4.5-4.7,
Kemira), 120 grams of distilled water, sodium hydroxide solution to
adjust pH to 4.6, 30 grams of partially methylated methylol
melamine resin (Cymel 385, 80% Cytec). This mixture is heated to
75.degree. C. and maintained 6 hours with continuous stirring to
complete the encapsulation process. 23 grams of acetoacetamide
(Sigma-Aldrich, Saint Louis, Mo., U.S.A.) is added to the
suspension.
Example 7
80 Wt % Core/20 Wt % Wall Melamine Formaldehyde Capsule
20 grams of butyl acrylate-acrylic acid copolymer emulsifier
(Colloid C351, 25% solids, pKa 4.5-4.7, Kemira) is dissolved and
mixed in 200 grams deionized water. The pH of the solution is
adjusted to pH of 5.5 with sodium hydroxide solution. 6 grams of
partially methylated methylol melamine resin (Cymel 385, 80%
solids, Cytec) is added to the emulsifier solution. 200 grams of
perfume oil is added to the previous mixture under mechanical
agitation and the temperature is raised to 55.degree. C. After
mixing at higher speed until a stable emulsion is obtained, the
second solution and 9 grams of sodium sulfate salt is added to the
emulsion. This second solution contains 8 grams of polyacrylic acid
(35% solids, pka 1.5-2.5, Aldrich), 120 grams of distilled water,
sodium hydroxide solution to adjust pH to 4.4, 35 grams of
partially methylated methylol melamine resin (Cymel 385, 80%
solids, Cytec). This mixture is heated to 80.degree. C. and
maintained 4 hours with continuous stirring to complete the
encapsulation process. 23 grams of acetoacetamide (Sigma-Aldrich,
Saint Louis, Mo., U.S.A.) is added to the suspension.
Example 8
Non-limiting examples of product formulations containing
microcapsules summarized in the following table.
TABLE-US-00002 EXAMPLES (% wt) XI XII XIII XIV XV XVI XVII XVIII
XIX XX FSA.sup.a 14 16.47 14 12 12 16.47 -- -- 5 5 FSA.sup.b --
3.00 -- -- -- FSA.sup.c -- -- 6.5 -- -- Ethanol 2.18 2.57 2.18 1.95
1.95 2.57 -- -- 0.81 0.81 Isopropyl -- -- -- -- -- -- 0.33 1.22 --
-- Alcohol Starch.sup.d 1.25 1.47 2.00 1.25 -- 2.30 0.5 0.70 0.71
0.42 Microcapsule 0.6 0.75 0.6 0.75 0.37 0.60 0.37 0.6 0.37 0.37 (%
active)* Formaldehyde 0.40 0.13 0.065 0.25 0.03 0.030 0.030 0.065
0.03 0.03 Scavenger.sup.e Phase 0.21 0.25 0.21 0.21 0.14 -- -- 0.14
-- -- Stabilizing Polymer.sup.f Suds -- -- -- -- -- -- -- 0.1 -- --
Suppressor.sup.g Calcium 0.15 0.176 0.15 0.15 0.30 0.176 --
0.1-0.15 -- -- Chloride DTPA.sup.h 0.017 0.017 0.017 0.017 0.007
0.007 0.20 -- 0.002 0.002 Preservative 5 5 5 5 5 5 -- 250.sup.j 5 5
(ppm).sup.i,j Antifoam.sup.k 0.015 0.018 0.015 0.015 0.015 0.015 --
-- 0.015 0.015 Dye (ppm) 40 40 40 40 40 40 11 30-300 30 30 Ammonium
0.100 0.118 0.100 0.100 0.115 0.115 -- -- -- -- Chloride HCl 0.012
0.014 0.012 0.012 0.028 0.028 0.016 0.025 0.011 0.011
Structurant.sup.l 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01
Neat 0.8 0.7 0.9 0.5 1.2 0.5 1.1 0.6 1.0 0.9 Unencapsulated Perfume
Deionized Balance Balance Balance Balance Balance Balance Balance
Balance - Balance Balance Water
.sup.aN,N-di(tallowoyloxyethyl)-N,N-dimethylammonium chloride.
.sup.bMethyl bis(tallow amidoethyl)2-hydroxyethyl ammonium methyl
sulfate. .sup.cReaction product of Fatty acid with
Methyldiethanolamine in a molar ratio 1.5:1, quaternized with
Methylchloride, resulting in a 1:1 molar mixture of
N,N-bis(stearoyl-oxy-ethyl) N,N-dimethyl ammonium chloride and
N-(stearoyl-oxy-ethyl) N,-hydroxyethyl N,N dimethyl ammonium
chloride. .sup.dCationic high amylose maize starch available from
National Starch under the trade name CATO .RTM.. .sup.eThe
formaldehyde scavenger is acetoacetamide available from Aldrich.
.sup.fCopolymer of ethylene oxide and terephthalate having the
formula described in U.S. Pat. No. 5,574,179 at col. 15, lines 1-5,
wherein each X is methyl, each n is 40, u is 4, each R1 is
essentially 1,4-phenylene moieties, each R2 is essentially
ethylene, 1,2-propylene moieties, or mixtures thereof. .sup.gSE39
from Wacker .sup.hDiethylenetriaminepentaacetic acid. .sup.iKATHON
.RTM. CG available from Rohm and Haas Co. "PPM" is "parts per
million." .sup.jGluteraldehyde .sup.kSilicone antifoam agent
available from Dow Corning Corp. under the trade name DC2310.
.sup.lHydrophobically-modified ethoxylated urethane available from
Rohm and Haas under the tradename Aculan 44. *Suitable combinations
of the microcapsules provided in Examples 1 through 7.
Example 9
Microcapsules in Dry Laundry Formulations
TABLE-US-00003 % w/w granular laundry detergent composition
Component A B C D E F G Brightener 0.1 0.1 0.1 0.2 0.1 0.2 0.1 Soap
0.6 0.6 0.6 0.6 0.6 0.6 0.6 Ethylenediamine 0.1 0.1 0.1 0.1 0.1 0.1
0.1 disuccinic acid Acrylate/maleate 1.5 1.5 1.5 1.5 1.5 1.5 1.5
copolymer Hydroxyethane 0.4 0.4 0.4 0.4 0.4 0.4 0.4 di(methylene
phosphonic acid) Mono-C.sub.12-14 alkyl, di- 0.5 0.5 0.5 0.5 0.5
0.5 0.5 methyl, mono-hydroyethyl quaternary ammonium chloride
Linear alkyl benzene 0.1 0.1 0.2 0.1 0.1 0.2 0.1 Linear alkyl
benzene 10.3 10.1 19.9 14.7 10.3 17 10.5 sulphonate Magnesium
sulphate 0.4 0.4 0.4 0.4 0.4 0.4 0.4 Sodium carbonate 19.5 19.2
10.1 18.5 29.9 10.1 16.8 Sodium sulphate 29.6 29.8 38.8 15.1 24.4
19.7 19.1 Sodium Chloride 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Zeolite 9.6
9.4 8.1 18 10 13.2 17.3 Photobleach particle 0.1 0.1 0.2 0.1 0.2
0.1 0.2 Blue and red carbonate 1.8 1.8 1.8 1.8 1.8 1.8 1.8 speckles
Ethoxylated Alcohol AE7 1 1 1 1 1 1 1 Tetraacetyl ethylene 0.9 0.9
0.9 0.9 0.9 0.9 0.9 diamine agglomerate (92 wt % active) Citric
acid 1.4 1.4 1.4 1.4 1.4 1.4 1.4 PDMS/clay agglomerates 10.5 10.3 5
15 5.1 7.3 10.2 (9.5% wt % active PDMS) Polyethylene oxide 0.2 0.2
0.2 0.2 0.2 0.2 0.2 Enzymes e.g. Protease (84 0.2 0.3 0.2 0.1 0.2
0.1 0.2 mg/g active), Amylase (22 mg/g active) Suds suppressor 0.2
0.2 0.2 0.2 0.2 0.2 0.2 agglomerate (12.4 wt % active) Sodium
percarbonate 7.2 7.1 4.9 5.4 6.9 19.3 13.1 (having from 12% to 15%
active AvOx) Perfume oil 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Solid perfume
particles 0.4 0 0.4 0.4 0.4 0.4 0.6 Perfume microcapsules* 1.3 2.4
1 1.3 1.3 1.3 0.7 Water 1.4 1.4 1.4 1.4 1.4 1.4 1.4 Misc 0.1 0.1
0.1 0.1 0.1 0.1 0.1 Total Parts 100 100 100 100 100 100 100
*Microcapsule added as 35% active slurry. Core/wall ratio can range
from 80/20 up to 90/10 and average particle diameter can range from
5 .mu.m to 50 .mu.m
Example 10
Liquid Laundry Formulations (HDLs)
TABLE-US-00004 Ingredient HDL 1 HDL 2 HDL 3 HDL 4 HDL 5 HDL 6 Alkyl
Ether Sulphate 0.00 0.50 12.0 12.0 6.0 7.0 Dodecyl Benzene 8.0 8.0
1.0 1.0 2.0 3.0 Sulphonic Acid Ethoxylated Alcohol 8.0 6.0 5.0 7.0
5.0 3.0 Citric Acid 5.0 3.0 3.0 5.0 2.0 3.0 Fatty Acid 3.0 5.0 5.0
3.0 6.0 5.0 Ethoxysulfated 1.9 1.2 1.5 2.0 1.0 1.0 hexamethylene
diamine quaternized Diethylene triamine penta 0.3 0.2 0.2 0.3 0.1
0.2 methylene phosphonic acid Enzymes 1.20 0.80 0 1.2 0 0.8
Brightener (disulphonated 0.14 0.09 0 0.14 0.01 0.09 diamino
stilbene based FWA) Cationic hydroxyethyl 0 0 0.10 0 0.200 0.30
cellulose Poly(acrylamide-co- 0 0 0 0.50 0.10 0
diallyldimethylammonium chloride) Hydrogenated Castor Oil 0.50 0.44
0.2 0.2 0.3 0.3 Structurant Boric acid 2.4 1.5 1.0 2.4 1.0 1.5
Ethanol 0.50 1.0 2.0 2.0 1.0 1.0 1,2 propanediol 2.0 3.0 1.0 1.0
0.01 0.01 Glutaraldehyde 0 0 19 ppm 0 13 ppm 0 Diethyleneglycol
(DEG) 1.6 0 0 0 0 0 2,3-Methyl-1,3- 1.0 1.0 0 0 0 0 propanediol (M
pdiol) Mono Ethanol Amine 1.0 0.5 0 0 0 0 NaOH Sufficient To pH 8
pH 8 pH 8 pH 8 pH 8 pH 8 Provide Formulation pH of: Sodium Cumene
2.00 0 0 0 0 0 Sulphonate (NaCS) Silicone (PDMS) emulsion 0.003
0.003 0.003 0.003 0.003 0.003 Perfume 0.7 0.5 0.8 0.8 0.6 0.6
Polyethyleneimine 0.01 0.10 0.00 0.10 0.20 0.05 Perfume
Microcapsules* 1.00 5.00 1.00 2.00 0.10 0.80 Water Balance Balance
Balance Balance Balance Balance to to to to to to 100% 100% 100%
100% 100% 100% *Perfume Microcapsules in accordance with the
teaching of the present specification.
The dimensions and values disclosed herein are not to be understood
as being strictly limited to the exact numerical values recited.
Instead, unless otherwise specified, each such dimension is
intended to mean both the recited value and a functionally
equivalent range surrounding that value. For example, a dimension
disclosed as "40 mm" is intended to mean "about 40 mm".
All documents cited in the Detailed Description of the Invention
are, in relevant part, incorporated herein by reference; the
citation of any document is not to be construed as an admission
that it is prior art with respect to the present invention. To the
extent that any meaning or definition of a term in this document
conflicts with any meaning or definition of the same term in a
document incorporated by reference, the meaning or definition
assigned to that term in this document shall govern.
While particular embodiments of the present invention have been
illustrated and described, it would be obvious to those skilled in
the art that various other changes and modifications can be made
without departing from the spirit and scope of the invention. It is
therefore intended to cover in the appended claims all such changes
and modifications that are within the scope of this invention.
* * * * *
References