U.S. patent application number 09/280614 was filed with the patent office on 2001-07-12 for aerosol hair cosmetic compositions containing non-ionically derivatized starches.
Invention is credited to ALTIERI, PAUL A., COTTRELL, IAN W., HENLEY, MATTHEW J., PAUL, CHARLES W., SOLAREK, DANIEL B., TOLCHINSKY, MARIA, VITALE, MELISSA J..
Application Number | 20010007655 09/280614 |
Document ID | / |
Family ID | 22012327 |
Filed Date | 2001-07-12 |
United States Patent
Application |
20010007655 |
Kind Code |
A1 |
PAUL, CHARLES W. ; et
al. |
July 12, 2001 |
AEROSOL HAIR COSMETIC COMPOSITIONS CONTAINING NON-IONICALLY
DERIVATIZED STARCHES
Abstract
The present invention is directed to low volatile organic
compound aerosol hair cosmetic compositions which contain
nonionically derivatized starches optionally hydrolyzed and/or
ionically modified. Such compositions provide a clear solution with
a low viscosity, good spray characteristics, a clear, non-tacky
film, good stiffness, and improved humidity resistance.
Inventors: |
PAUL, CHARLES W.; (MADISON,
NJ) ; HENLEY, MATTHEW J.; (GREENWOOD, IN) ;
ALTIERI, PAUL A.; (BELLE MEAD, NJ) ; VITALE, MELISSA
J.; (PLAINSBORO, NJ) ; TOLCHINSKY, MARIA;
(MONMOUTH JUNCTION, NJ) ; SOLAREK, DANIEL B.;
(BELLE MEAD, NJ) ; COTTRELL, IAN W.; (PRINCETON,
NJ) |
Correspondence
Address: |
LAURELEE A. DUNCAN
NATIONAL STARCH AND CHEMICAL COMPANY
PO BOX 6500
BRIDGEWATER
NJ
08807-0500
US
|
Family ID: |
22012327 |
Appl. No.: |
09/280614 |
Filed: |
March 29, 1999 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
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09280614 |
Mar 29, 1999 |
|
|
|
09057717 |
Apr 9, 1998 |
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Current U.S.
Class: |
424/70.11 ;
424/45; 424/47; 424/70.13; 424/70.15; 424/70.16 |
Current CPC
Class: |
A61K 8/046 20130101;
A61K 8/732 20130101; A61Q 5/06 20130101; Y10S 424/02 20130101; Y10S
424/01 20130101 |
Class at
Publication: |
424/70.11 ;
424/70.13; 424/70.15; 424/45; 424/47; 424/70.16 |
International
Class: |
A61L 009/04; A61K
007/00; A61K 009/00; A61K 007/06; A61K 007/11 |
Claims
We claim:
1. A hair cosmetic composition comprising: a) a fixative effective
amount of a nonionically derivatized starch; b) from about 5 to
about 55% of a propellant; c) up to about 50% of a solvent; and d)
water.
2. The composition of claim 1, wherein the starch is present in an
amount of from about 0.5 to 15% by weight of the composition.
3. The composition of claim 1, wherein the starch is present in an
amount of about 2 to 10% by weight of the composition.
4. The composition of claim 1, wherein the starch is a waxy
starch.
5. The composition of claim 1, wherein the starch is a high amylose
starch.
6. The composition of claim 1, wherein the starch is nonionically
derivatized using from about 1 to about 50% of a nonionic modifying
reagent.
7. The composition of claim 6, wherein the starch is nonionically
derivatized using from about 5 to about 25% of a nonionic modifying
reagent.
8. The composition of claim 1, wherein the starch is nonionically
derivatized using a reagent selected from the group consisting of
alkylene oxide, acetic anhydride, and butyl ketene dimer.
9. The composition of claim 8, wherein the starch is nonionically
derivatized using an alkylene oxide.
10. The composition of claim 9, wherein the starch is nonionically
derivatized using propylene oxide.
11. The composition of claim 1, wherein the starch is further at
least partially hydrolyzed.
12. The composition of claim 1, wherein the starch is further
anionically or zwitterionically modified.
13. The composition of claim 1, wherein the starch is further
cationically modified at a level of less than about 0.03
equivalents per 100 grams starch.
14. The composition of claim 12, wherein the starch is anionically
modified using a reagent selected from the group consisting of
alkenyl succinic anhydrides, inorganic phosphates, sulfates,
phosphonates, sulfonates, and sodium chloroacetic acids.
15. The composition of claim 14, wherein the starch is anionically
modified using the reagent octenyl succinic anhydride.
16. The composition of claim 12, wherein the starch is
zwitterionically modified using a reagent selected from the group
consisting of N-(2-chloroethyl)-iminobis(methylene) diphosphonic
acid and 2-chloroethylaminodipropionic acid.
17. The composition of claim 13, wherein the starch is cationically
modified using a reagent containing a group selected from the group
consisting amino, imino, ammonium, sulfonium, and phosphonium.
18. The composition of claim 17, wherein the starch is cationically
modified using a reagent selected from the group consisting of
3-chloro-2-hydroxypropyltrimethly ammonium chloride,
2-diethylaminoethyl chloride, epoxypropyltrimethylammonium chloride
and 4-chloro-2-butenyltrimethylammonium chloride.
19. The composition of claim 1, further comprising a fixative or
conditioning polymer.
20. The composition of claim 1, further comprising a polymer
selected from the group consisting of vinyl
acetate/crotonates/vinyl neodecanoate copolymer,
octylacrylamide/acrylates/butylaminoethyl methacrylate copolymer,
vinyl acetate/crotonates, polyvinylpyrrolidone (PVP),
polyvinylpyrrolidone/vinyl acetate copolymer, PVP acrylates
copolymer, vinyl acetate/crotonic acid/vinyl proprionate,
acrylates/acrylamide, acrylates/octylacrylamide, acrylates
copolymer, acrylates/hydroxyacrylate- s copolymer, and alkyl esters
of polyvinylmethylether/maleic anhydride,
diglycol/cyclohexanedimethanol/isophthalates/sulfoisophthalates
copolymer, vinyl acetate/butyl maleate and isobornyl acrylate
copolymer, vinylcaprolactam/PVP/dimethylaminoethyl methacrylate,
vinyl acetate/alkylmaleate half ester/N-substituted acrylamide
terpolymers, vinyl
caprolactam/vinylpyrrolidone/methacryloamidopropyl
trimethylammonium chloride terpolymer, methacrylates/acrylates
copolymer/amine salt, polyvinylcaprolactam, polyurethanes,
polyquaternium-4, polyquaternium-10, polyquaternium-11,
polyquaternium-46, hydroxypropyl guar, hydroxypropyl guar
hydroxypropyl trimmonium chloride, polyvinyl formamide,
polyquarternium-7, and hydroxypropyl trimmonium chloride guar.
21. The composition of claim 20, wherein the polymer is polyvinyl
pyrrolidone.
22. The composition of claim 20, wherein the starch and polymer are
slurried together, cooked, and dried.
23. A hair cosmetic composition comprising: a) a fixative effective
amount of a propylene oxide modified high amylose starch/polyvinyl
pyrrolidone (PVP) mixture prepared by slurrying the modified starch
with the PVP, jet cooking, and spray drying; b) from about 5 to
about 55% of a propellant; c) up to about 50% of a solvent; and d)
water.
24. The composition of claim 1, wherein the composition is
substantially solvent-free.
25. The composition of claim 23, wherein the composition is
substantially solvent-free.
26. The composition of claim 1, further comprising at least one
additional modified or unmodified starch.
27. The composition of claim 26, wherein the additional starch is
selected from the group consisting of hydroxypropylated starches,
octenyl succinate derivates, and 2-chloroethylamino dipropionic
acid derivatives.
28. The composition of claim 23, further comprising at least one
additional modified or unmodified starch.
29. The composition of claim 28, wherein the additional starch is
selected from the group consisting of hydroxypropylated starches,
octenyl succinate derivates, and 2-chloroethylamino dipropionic
acid derivatives.
30. A method of styling hair comprising applying to the hair the
composition of claim 1.
31. A method of styling hair comprising applying to the hair the
composition of claim 23.
32. A method of styling hair comprising applying to the hair the
composition of claim 24.
33. A method of styling hair comprising applying to the hair the
composition of claim 25.
Description
BACKGROUND OF THE INVENTION
[0001] This application is a continuation-in-part of U.S. Ser. No.
09/057,717 filed Apr. 9, 1998.
[0002] The present invention relates to novel aerosol hair cosmetic
compositions, particularly hair fixative compositions, which
contain nonionically derivatized starches and to a process for
setting hair utilizing such compositions.
[0003] In their most basic form, hair cosmetic compositions contain
a film-forming polymer, which acts as the cosmetic, and a delivery
system, which is usually one or more alcohols, a mixture of alcohol
and water, or water. In the case of aerosol delivery, the delivery
system will also contain a propellant, typically a volatile
hydrocarbon.
[0004] The hair setting or styling process ordinarily involves the
application of an aqueous solution or dispersion of one or more
film-forming materials to combed hair which has previously been
wettened or dampened whereupon the treated hair is wound on curlers
or otherwise styled and dried. In the alternative, application of
this solution or dispersion may be to hair which has already been
styled and dried. Once the aqueous solution or dispersion has
dried, the individual hairs will have a film deposited thereon
which presence will prolong the retention of curls or other desired
configurations in the user's hair. Furthermore, the presence of
such films will impart such desirable properties as body and
smoothness.
[0005] To be effective, the film-forming ingredients of a hair
cosmetic composition preferably meet a number of requirements. The
film derived from these ingredients should be flexible, yet possess
strength and elasticity. The ingredients should display good
adhesion to hair so as to avoid dusting or flaking off with the
passage of time or when the hair is subjected to stress; should not
interfere with the combing and brushing of the hair; should remain
free of tack or gumminess under humid conditions; should be clear,
transparent, and glossy, and should maintain clarity upon aging.
Further, the ingredients should maintain good anti-static
properties and should be easily removable by washing with water and
either a soap or shampoo.
[0006] Many film-forming agents have been used in hair cosmetic
compositions including, for example, a colloidal solution
containing a gum such as tragacanth or a resin such as shellac. The
films formed of these materials are, however, quite brittle and the
form holding the setting is easily broken if the hair is disturbed.
This not only reduces the hair holding power of the material, but
also leads to undesirable flaking. Further, some of these
film-formers, particularly the resins, are water insoluble and
therefore not easily removed with water and soap or shampoo.
[0007] Starches are often preferred over resins as they are more
cost effective and natural. Hair cosmetic compositions which
contain starches are also known in the art. For example, GB
1,285,547 discloses a hair setting composition containing a highly
substituted cationic starch having an amylose content of more than
50% by weight. EP 487 000 discloses cosmetic compositions which
contain enzymatically degraded optionally crosslinked starches.
However, such derivatives are not significantly soluble in
water.
[0008] Due to environmental regulations controlling the emission of
volatile organic compounds (VOCs) into the atmosphere, VOC
emissions have been restricted to 80% in some states, and will soon
be restricted to 55% in California. VOC is measured as a wt/wt %
based upon the hair cosmetic formulation. As used herein, a
volatile organic compound containing from 1 to 10 carbon atoms,
which has a vapor pressure of at least 0.1 mm Hg at 20.degree. C.,
and is photochemically active. Water is generally substituted for
at least a portion of the volatile organic compounds and so has
become a greater component in hair cosmetic compositions.
[0009] Many fixatives, particularly starches, are incompatible with
water in that they are not fully soluble, resulting in starch
precipitates which may clog aerosol valves and produce poor spray
aesthetics. Further, many starch fixatives are also incompatible
with propellant. Surprisingly, it has now been discovered that
nonionically derivatized starches are useful in aerosol hair
cosmetic compositions with low volatile organic compounds in that
they provide a clear solution with a low viscosity, good spray
aesthetics, improved humidity resistance, and good fixative
properties.
SUMMARY OF THE INVENTION
[0010] The present invention is directed to low volatile organic
compound aerosol hair cosmetic compositions which contain
nonionically derivatized, particularly propylene oxide derivatized,
starches. The nonionically derivatized starch may be further
hydrolyzed, particularly enzymatically hydrolyzed by at least one
endo-enzyme. In addition, the nonionically derivatized starch may
be ionically modified, particularly by octenyl succinic anhydride
(OSA). Use of such starches is novel and advantageous in that they
provide a clear solution with a low viscosity, and good spray
characteristics. Further, the resultant composition provides a
clear film which is not tacky, has good hold, and improved humidity
resistance.
[0011] The present hair cosmetic composition contains by weight
from about 0.5 to about 15% of the instant starch, from about 5 to
about 55% of a propellant, from zero to about 50% of a solvent, and
sufficient water to bring the composition up to 100%.
[0012] An object of this invention is to provide a novel hair
cosmetic composition which contains nonionically derivatized
starches and low volatile organic compounds.
[0013] Another object of this invention is to provide a novel hair
cosmetic composition which contains nonionically derivatized
starches which have been hydrolyzed.
[0014] Still another object of this invention is to provide a novel
hair cosmetic composition which contains starches which have been
derivatized with propylene oxide and enzymatically hydrolyzed.
[0015] Yet another object of this invention is to provide a novel
hair cosmetic composition which contains starches which have been
nonionically derivatized, hydrolyzed, and ionically modified.
[0016] A further object of this invention is to provide a novel
hair cosmetic composition which contains starches which have been
derivatized with propylene oxide, enzymatically hydrolyzed and
modified with octenyl succinic anhydride.
[0017] A still further object of this invention is to provide a
novel hair cosmetic composition which has improved humidity
resistance, superior stability and contains low volatile organic
compounds.
[0018] A yet further object of this invention is to provide a novel
hair cosmetic composition which contains starch which has been
derivatized and coprocessed with polyvinyl pyrrolidone.
[0019] These and other objects of the present invention will become
apparent to one skilled in the art from the following detailed
description and examples below.
DETAILED DESCRIPTION OF THE INVENTION
[0020] The present invention is directed to aerosol hair cosmetic
compositions, i.e., hair sprays, which contain nonionically
derivatized starches, particularly propylene oxide derivatized
starches, in a low or no volatile organic compound (hereinafter
VOC) solution, particularly less than 55% VOC, most particularly
less than 35% VOC, by weight of the hair setting composition. The
starch may be additionally hydrolyzed, particularly enzymatically
hydrolyzed. Further, the starch may be modified using ionic
substituents. Use of such starches is novel and advantageous in
that they provide a clear solution with a low viscosity, and good
spray characteristics. Further, the resultant composition provides
a clear film which is not tacky and good curl retention.
[0021] The hair cosmetic composition of the instant invention
contains a fixative effective amount of a nonionically derivatized
starch, particularly from about 0.5 to about 15% starch, more
particularly from about 2 to about 10% by weight; from about 5 to
about 55% of a propellant, particularly from about 5 to about 40%,
from zero to about 50% of a solvent, particularly from about 5 to
about 35% by weight; and sufficient water to bring the composition
to 100%.
[0022] All starches and flours (hereinafter "starch") are suitable
for use herein and may be derived from any native source. A native
starch or flour as used herein, is one as it is found in nature.
Also suitable are starches and flours derived from a plant obtained
by standard breeding techniques including crossbreeding,
translocation, inversion, transformation or any other method of
gene or chromosome engineering to include variations thereof. In
addition, starch or flours derived from a plant grown from
artificial mutations and variations of the above generic
composition which may be produced by known standard methods of
mutation breeding are also suitable herein. Typical sources for the
starches and flours are cereals, tubers, roots, legumes and fruits.
The native source can be corn, pea, potato, sweet potato, banana,
barley, wheat, rice, sago, amaranth, tapioca, arrowroot, canna,
sorghum, and waxy or high amylose varieties thereof. As used
herein, the term "waxy" is intended to include a starch or flour
containing at least about 95% by weight amylopectin and the term
"high amylose" is intended to include a starch or flour containing
at least about 45% by weight amylose.
[0023] The starch is first nonionically derivatized using an ester
or ether which is compatible with the system, particularly with the
solvent and the propellant. Methods of nonionic derivatization are
well known in the art and may be found for example in Starch
Chemistry and Technology, 2nd ed., Edited by Whistler, et al.,
Academic Press, Inc., Orlando (1984) or Modified Starches:
Properties and Uses, Wurzburg, O.B., CRC Press, Inc., Florida,
(1986).
[0024] Nonionic reagents include, but are not limited to alkylene
oxides such as ethylene oxide, propylene oxide, and butylene oxide,
acetic anhydride, and butyl ketene dimer. Particularly suitable
nonionic reagents are the alkylene oxides, more particularly
propylene oxide. The nonionic reagent is added in an amount of from
about 1 to 50%, particularly from about 5 to 25%, more particularly
from about 7.5 to 18%.
[0025] For example, the starch may be derivatized using propylene
oxide as follows. An aqueous starch slurry containing from about 5
to about 40%, particularly 30 to 40%, solids is prepared. From
about 20 to about 30% percent sodium sulfate based on the weight of
the starch is added. The pH is then adjusted to about 11 to about
13 by addition of a 3% sodium hydroxide solution in an amount of
from about 40 to about 60% based upon the weight of the starch. The
desired amount of propylene oxide is added. The temperature is
brought to the range of about 35 to 50.degree. C., particularly
about 40.degree. C., and the process is allowed to continue for
about 18 to about 24 hours.
[0026] The starch is generally at least partially gelatinized. If
conversion is to be accomplished enzymatically, the gelatinization
is conventionally conducted prior to conversion. Gelatinization may
be accomplished using any technique known in the art, particularly
steam cooking, more particularly jet-cooking, and then converted
(hydrolyzed). The conversion is important if a reduced molecular
weight starch and a reduced viscosity of the starch solution or
dispersion is desired, such as when the starch is to be used in a
hair spray. The conversion may be accomplished by any method known
in the art, such as by enzymes, acid, dextrinization, man-ox, or
oxidation, particularly by enzymes. If conversion is conducted
using acid or oxidation methods, then it may be done prior to or
after derivatization of the starch.
[0027] The enzymatic hydrolysis of the starch is carried out using
techniques known in the art. Any enzyme or combination of enzymes,
known to degrade starch may be used, particularly endo-enzymes.
Enzymes useful in the present application include, but are not
limited to, .alpha.-amylase, .beta.-amylase, maltogenase,
glucoamylase, pullulanase, particularly .alpha.-amylase and
pullulanase. The amount of enzyme used is dependent upon the enzyme
source and activity, base material used, and the amount of
hydrolysis desired. Typically, the enzyme is used in an amount of
from about 0.01 to about 1.0%, particularly from about 0.01 to
0.3%, by weight of the starch.
[0028] The optimum parameters for enzyme activity will vary
depending upon the enzyme used. The rate of enzyme degradation
depends upon factors known in the art, including the enzyme
concentration, substrate concentration, pH, temperature, the
presence or absence of inhibitors, and the degree and type of
modification. These parameters may be adjusted to optimize the
digestion rate of the starch base.
[0029] Generally the enzyme treatment is carried out in an aqueous
or buffered slurry at a starch solids level of about 10 to about
40%, depending upon the base starch being treated. A solids level
of from about 15 to 35% is particularly useful, from about 18 to
25% more particularly useful, in the instant invention. In the
alternative, the process may utilize an enzyme immobilized on a
solid support.
[0030] Typically, enzyme digestion is carried out at the highest
solids content feasible without reducing reaction rates in order to
facilitate any desired subsequent drying of the starch composition.
Reaction rates may be reduced by high solids content as agitation
becomes difficult or ineffective and the starch dispersion becomes
more difficult to handle.
[0031] The pH and temperature of the slurry should be adjusted to
provide effective enzyme hydrolysis. These parameters are dependent
upon the enzyme to be used and are known in the art. In general, a
temperature of about 22 to about 65.degree. C. is used,
particularly from about 50 to about 62.degree. C. In general, the
pH is adjusted to about 3.5 to about 7.5, particularly from about
4.0 to about 6.0, using techniques known in the art.
[0032] In general, the enzyme reaction will take from about 0.5 to
about 24 hours, particularly about 0.5 to about 4 hours. The time
of the reaction is dependent upon the type of starch used, the
amount of enzyme used, and the reaction parameters of solids
percent, pH, and temperature.
[0033] The enzyme degradation is then terminated by any technique
known in the art such as acid or base deactivation, heat
deactivation, ion exchange, and solvent extraction. For example,
acid deactivation may be accomplished by adjusting the pH to lower
than 2.0 for at least 30 minutes or heat deactivation may be
accomplished by raising the temperature to about 85 to about
95.degree. C. and maintaining it at that temperature for at least
about 10 minutes to fully deactivate the enzyme. Heat deactivation
is not suitable if a granular product is desired as the heat
necessary to deactivate the enzyme will generally also gelatinize
the starch.
[0034] The conversion reaction is continued until the starch is
sufficiently degraded to provide proper spray characteristics,
particularly to a viscosity of from about 7 to about 80 seconds,
more particularly from about 10 to about 60 seconds, measured at
19% w/w solid concentration at room temperature using a standard
funnel method. The resultant product may be further characterized
by a dextrose equivalent (DE) of from about 2 to about 40 and/or a
water fluidity of from about 60 to 80.
[0035] Funnel viscosity, as used herein, is defined by the
following procedure. The starch dispersion to be tested is adjusted
to 19% (w/w) measured by refractometer. The temperature of the
dispersion is controlled at 22.degree. C. A total of 100 ml of the
starch dispersion is measured into a graduated cylinder. It is then
poured into a calibrated funnel while using a finger to close the
orifice. A small amount is allowed to flow into the graduate to
remove any trapped air and the balance is poured back into the
funnel. The graduated cylinder in then inverted over the funnel so
that the contents draw (flow) into the funnel while the sample is
running. Using a timer, the time required for the 100 ml sample to
flow through the apex of the funnel is recorded.
[0036] The glass portion of the funnel is a standard 58.degree.,
thick-wall, resistance glass funnel whose top diameter is about 9
to about 10 cm with the inside diameter of the stem being about
0.381 cm. The glass stem of the funnel is cut to an approximate
length of 2.86 cm from the apex, carefully fire-polished, and
refitted with a long stainless steel tip which is about 5.08 cm
long with an outside diameter of about 0.9525 cm. The interior
diameter of the steel tip is about 0.5952 cm at the upper end where
is attached to the glass stem and about 0.4445 cm at the outflow
end with the restriction in the width occurring at about 2.54 cm
from the ends. The steel tip is attached to the glass funnel by
means of a Teflon tube. The funnel is calibrated so as to allow 100
ml of water to go through in six seconds using the above
procedure.
[0037] Finally, the starch may be ionically modified, either
anionically, cationically, or zwitterionically. Starch modification
techniques are known in the art and may be found, for example, in
Starch Chemistry and Technology, 2nd ed., Edited by Whistler, et
al., Academic Press, Inc., Orlando (1984) or Modified Starches:
Properties and Uses, Wurzburg, O.B., CRC Press, Inc., Florida,
(1986).
[0038] Anionic modification may be accomplished by any reagent
known in the art, such as alkenyl succinic anhydrides, inorganic
phosphates, sulfates, phosphonates, sulfonates, and sodium
chloroacetic acids. Particularly suitable anionic reagents are
alkyenyl succinic anhydrides and sodium chloroacetic acids, more
particularly octenyl succinic anhydride.
[0039] Modification of starch using octenyl succinic anhydride may
be accomplished by reacting the selected starch with sufficient
octenyl succinic anhydride reagent such that the resulting starch
is sufficiently soluble or dispersible in the water or water
solvent delivery system. In particular, the starch will be modified
to have a degree of substitution from about 0.2 to about 3.0,
preferably from about 0.3 to about 1.6. The degree of substitution
(DS) is used herein to describe the number of ester substituted
groups per anhydroglucose unit of the starch molecule.
[0040] Cationic modification must be to a low degree of
substitution, particularly less than about 0.3 equivalents per 100
grams starch. The cationic modification may be accomplished by any
reagent known in the art including those containing amino, imino,
ammonium, sulfonium, or phosphonium groups. Such cationic
derivatives include those with nitrogen containing groups
comprising primary, secondary, tertiary and quaternary amines and
sulfonium and phosphonium groups attached through either ether or
ester linkages. Cationic modification, particularly tertiary amino
or quaternary ammonium etherification of starch, typically prepared
by treatment with 3-chloro-2-hydroxypropyltrimethyl ammonium
chloride, 2-diethylaminoethyl chloride, epoxypropyl
trimethylammonium chloride, 3-chloro-2-hydroxypropyldimethyl
dodecyl ammonium chloride, and 4-chloro-2-butenyltrimethylammonium
chloride.
[0041] Zwitterionic modification may be accomplished using any
reagents known in the art, such as
N-(2-chloroethyl)-iminobis(methylene)diphosphon- ic acid and
2-chloroethylaminodipropionic acid (CEPA).
[0042] In general, the degree of nonionic derivatization desired
will be greater when the starch is not ionically jonically modified
than when the starch is ionically modified.
[0043] Optionally, the starch may then be neutralized by raising
the pH of the solution to from about 5 to about 9. This may be done
by any method known in the art, particularly by the addition of
amino methyl propanol sodium hydroxide, potassium hydroxide, or
other bases know in the art.
[0044] The starch solution is generally filtered to remove
impurities, particularly fragmented starch. Filtration may be
accomplished by any technique known in the art, particularly by
filtration through diatomaceous earth.
[0045] The starch may be used as a solution or may be recovered in
powdered form by conventional techniques, such as drum-drying or
spray-drying.
[0046] The modified starch may further be blended or coprocessed
with other fixative or conditioning polymers. Such polymer may be
selected from polymers known in the art, such as vinyl
acetate/crotonates/vinyl neodecanoate copolymer,
octylacrylamide/acrylates/butylaminoethyl methacrylate copolymer,
vinyl acetate/crotonates, polyvinylpyrrolidone (PVP),
polyvinylpyrrolidone/vinyl acetate copolymer, PVP acrylates
copolymer, vinyl acetate/crotonic acid/vinyl proprionate,
acrylates/acrylamide, acrylates/octylacrylamide, acrylates
copolymer, acrylates/hydroxyacrylates copolymer, and alkyl esters
of polyvinylmethylether/maleic anhydride,
diglycol/cyclohexanedimethanol/iso- phthalates/sulfoisophthalates
copolymer, vinyl acetate/butyl maleate and isobornyl acrylate
copolymer, vinylcaprolactam/PVP/dimethylaminoethyl methacrylate,
vinyl acetate/alkylmaleate half ester/N-substituted acrylamide
terpolymers, vinyl caprolactam/vinylpyrrolidone/methacryloamid-
opropyl trimethylammonium chloride terpolymer,
methacrylates/acrylates copolymer/amine salt, polyvinylcaprolactam,
polyurethanes, polyquaternium-4, polyquaternium-10,
polyquaternium-11, polyquaternium-46, hydroxypropyl guar,
hydroxypropyl guar hydroxypropyl trimmonium chloride, polyvinyl
formamide, polyquaternium-7, and hydroxypropyl trimmonium chloride
guar particularly polyvinyl pyrrolidone.
[0047] To coprocess the starch and the polymer, the polymer is
dissolved in water. The modified starch is then slurried into the
dispersed polymer and the slurry is processed. Processing includes
cooking and drying, particularly jet cooking and spray drying, and
includes the methods disclosed in U.S. Pat. Nos. 5,149,799;
4,280,851; 5,188,674 and 5,571,552 incorporated herein by
reference.
[0048] The delivery system in most cases will be a blend of water
and one or more volatile organic compounds acting as solvents. The
amount of solvent will be present in an amount of from zero to
about 50%, particularly from about 5 to about 35% by weight of the
composition. However, it is possible to prepare hair cosmetic
compositions containing the present starches in which the delivery
system comprises primarily water or even essentially no
solvent.
[0049] Typically, the organic solvent will be a lower alcohol
(herein defined as an alcohol having from 1 to 7 carbon atoms),
particularly methanol, ethanol, propanol, isopropanol, or butanol.
Also suitable are acetals, esters, and ketones, particularly
dimethoxymethane and acetone.
[0050] A propellant is added to formulate the aerosol hair cosmetic
composition. Propellants useful in the instant invention include,
but are not limited to, ethers, such as dimethyl ether; one or more
lower boiling hydrocarbons such as C.sub.3-C.sub.6 straight and
branched chain hydrocarbons, for example, propane, butane, and
isobutane; halogenated hydrocarbons, such as, hydrofluorocarbons,
for example, 1,1-difluoroethane and 1,1,1,2-tetrafluoroethane,
present as a liquefied gas; and the compressed gases, for example,
nitrogen, air and carbon dioxide.
[0051] The amount of propellant used in the hair cosmetic
compositions of this invention may vary from about 5 to about 55%,
particularly from about 5 to about 40% by weight of the hair
cosmetic composition. It should be noted that the above propellants
are volatile organic compounds. However, the emission of
halogenated hydrocarbons such as hydrofluorocarbons, and the
compressed gases are not at this time subject to environmental
regulations; therefore, these compounds may be formulated into the
hair sprays of this invention without inclusion in the total VOC
content.
[0052] Optional conventional additives may also be incorporated
into the hair spray compositions of this invention to provide
certain modifying properties to the composition. Included among
these additives are plasticizers, such as glycerine, glycol and
phthalate esters; emollients, lubricants and penetrants, such as
lanolin compounds; fragrances and perfumes; UV absorbers; dyes and
other colorants; thickeners; anticorrosion agents; detackifying
agents; combing aids and conditioning agents; antistatic agents;
neutralizers; glossifiers; preservatives; foam stabilizers;
emulsifiers; and surfactants. Such additives are commonly used in
hair cosmetic compositions known heretofore. These additives are
present in small, effective amounts to accomplish their function,
and generally will comprise from about 0.1 to 10% by weight each,
and from about 0.1 to 20% by weight total, based on the weight of
the composition.
[0053] The instant starch-containing hair care compositions may
also be combined with other modified or unmodified starches that
provide added functional benefits. For example, formulations with
2-chloroethylamino dipropionic acid derivatives of potato starch or
hydroxypropyl starch phosphate may be incorporated for thickening
or rheology modification in hair styling lotions and creams, and
starches such as tapioca starch, corn starch, aluminum starch
octenyl succinate, or corn starch modified may be used in the hair
care compositions as aesthetic enhancers to provide silkier,
smoother formulations. Modified starches, as used herein, is
intended to include without limitation, converted starches,
cross-linked starches, acetylated and organically esterified
starches, hydroxypropylated and hydroxyethylated starches,
phosphorylated and inorganically esterified starches, cationically,
anionically or zwitterionically modified starches, and succinated
and substituted succinated starches. Such modified starches are
known in the art for example in Modified Starches: Properties and
Uses by Wurzburg. Particularly suitable modified starches include
hydroxypropylated starches, octenyl succinate derivatives, and
2-chloroethylamino dipropionic acid derivatives.
[0054] To prepare the aerosol hair cosmetic composition, a solution
of the starch in the water or water/solvent mixture is prepared.
Then any optional additives may be added.
[0055] The mixture is then pressurized with propellant according to
conventional standards known in the art to form the aerosol hair
cosmetic composition. Pressures utilized are those conventionally
used to prepare aerosol sprays, such as from about 30 psi to about
110 psi.
[0056] Hair cosmetic compositions include, but are not limited to,
hair fixative compositions and styling aids, such as hair sprays
and mousses.
[0057] One advantage of the instant starch-containing hair care
compositions is that the starches are substantially soluble in
water and compatible with the propellant. This allows a reduced
solvent or a substantially solvent-free composition to be
formulated. Solubility is important in that the presence of
particulate matter (i.e., undissolved starch) may clog the valve
actuators, interfering with delivery of the composition by
aerosol.
[0058] Another advantage of the instant compositions is that they
are of relatively low viscosity. This helps to eliminate the
undesirable stickiness and heaviness associated with many
conventional hair cosmetic compositions.
[0059] A further advantage of the instant hair cosmetic
compositions is that they do not become tacky at high relative
humidity (RH), unlike many conventional water-based
starch-containing hair cosmetic compositions.
[0060] The present starches may also be used in skin, oral, and
other hair care applications, such as lotions, creams, sun screens,
lip balms, tanning products, oral rinses, antiperspirants,
shampoos, and conditioners.
[0061] The following examples are presented to further illustrate
and explain the present invention and should not be taken as
limiting in any regard.
EXAMPLES
[0062] All percentages in the examples are calculated on a wt/wt
basis. The following test procedures are used throughout the
examples.
[0063] A. Determination of the High Humidity Curl Retention of Hair
Sprays
[0064] The curl retention properties of the hair spray starches are
measured at 72.degree. F./90% Relative Humidity over a period of 24
hours.
[0065] Equipment:
[0066] 8" Remi Blue String European Brown hair
[0067] Barber shears
[0068] Nylon comb
[0069] White Cotton thread (size #8)
[0070] 3".times.1/2" Teflon mandrels
[0071] Forced air oven @120.degree. F.
[0072] Plexiglass retention board
[0073] Environmental chamber (precision to .+-.2 R.H. @72.degree.
F.)
[0074] Prell Shampoo
[0075] Procedure:
[0076] Preparation of Curl Swatches
[0077] 1. Separate hair into small swatches of approximately 2
grams in weight.
[0078] 2. Secure hair sample 3/4" from root end by winding with
cotton thread.
[0079] 3. Fold over at root end and secure the hair into a small
loop with thread. Leave approximately 6" of loose thread to secure
identification tag.
[0080] 4. In order to prevent loss of individual hair shafts during
combing, glue the root end at the thread windings with epoxy
cement. Allow cement to harden.
[0081] 5. Wash hair swatch in a 10% solution of shampoo. Then rinse
thoroughly with warm tap water.
[0082] 6. Comb to untangle the hair shafts.
[0083] 7. Cut the hair swatch to measure 6" in length from the
looped root end. Dry @120.degree. F.
[0084] Preparation and Exposure of Test Samples
[0085] 1. Wet hair and comb through to remove snarls.
[0086] 2. Squeeze-out excess water by running the swatch between
thumb and index finger.
[0087] 3. Curl hair into a coil configuration by rolling it on a
1/2" diameter Teflon mandrel. Secure hair on mandrel with plastic
clips.
[0088] 4. Dry hair, mandrel and clip 120.degree. F.
[0089] 5. When hair is dry and cool, carefully remove clips and
hair curl from the mandrel.
[0090] 6. Suspend the hair curl from the bound end. Apply a
controlled amount of hair spray in a controlled manner. In
evaluating an aerosol hair spray, a 2 second "burst" is evenly
applied to both the from and back of the curl from a distance of
6".
[0091] 7. Lay the freshly sprayed curl on a horizontal surface and
allow to air dry for 1 hour.
[0092] 8. Suspend the dry curls in random fashion from graduated,
clear, transparent, plexiglass curl retention boards.
[0093] 9. Take initial curl height reading (L.sub.o) and set curl
retention boards into the environmental chamber.
[0094] 10. Record curl length (L.sub.t) at the 15, 30, 60 and 90
minute, 2, 3, 4, 5 and 24 hour intervals.
[0095] Calculations
[0096] Calculate percentage curl retention by:
Curl Retention %=L-L.sub.t/L-L.sub.o.times.100
[0097] Where:
[0098] L=length of hair fully extended
[0099] L.sub.o=length of hair before exposure
[0100] L.sub.t=length of hair after exposure
[0101] B. Initial Curl Droop
[0102] Scope
[0103] Initial curl droop (ICD) is defined as the immediate loss of
curl integrity upon spraying a suspended, dry curl with a
water-containing formulation.
[0104] Equipment
[0105] 6" Brown hair (9 rolled swatches per sample)
[0106] Plexiglass retention board
[0107] Digital timers or stop watches
[0108] Procedure
[0109] 1. Determine both spray rate and polymer deposition of each
aerosol sample prior to testing.
[0110] 2. Roll swatches onto white Teflon mandrels.
[0111] 3. Let rolled hair cool and equilibrate at 50% RH,
72.degree. F. for at least three hours before removing from the
mandrel.
[0112] 4. Suspend the hair curl from the bound end onto the
retention board using the attached clip. Make sure that the bottom
of the curl is lined up with the "0" mark on the board.
[0113] 5. Spray the first side of the curled hair from left to
right for the time period specified to maintain uniform polymer
deposition by tracking total spray time. Pivot the curl 180 degrees
using the clip and complete the spraying cycle on the other side
before rotating back to the original position. All spraying should
be done from a distance of six inches (nozzle to hair).
[0114] 6. Record the curl length after 30, 60 and 90 seconds, as
well as 2, 4, and 6 minutes following initial spraying, using
markings on board.
[0115] 7. In order to run more than one curl at a time, begin to
spray a second curl after the first curl has been tracked for 2-4
minutes. Using another timer, repeat the procedure as described
above. Be careful not to allow over spray to contact initial curl.
Repeat this process once initial curl has been tracked for 6
minutes.
[0116] Results
[0117] Calculate percent curl retention for each time interval.
[0118] C. Taber Stiffness Test Procedure
[0119] Aerosol hair spray formulations are tested for stiffness on
three 41/4" swatches of brown European virgin hair and the results
pooled and averaged. The swatches are first dried in an oven at
110.degree. F. for 30 minutes to remove moisture and then dried in
a desiccator for 15 minutes. The swatches are weighed and the
weight recorded as W.sub.1. Each swatch is sprayed with a hair
spray formulation for one second and then clipped to a retention
board and dried in a 110.degree. F. oven for 15 minutes. The
swatches are cooled in the desiccator and reweighed. This weight
was recorded as W.sub.2. The swatches are then placed to
equilibrate overnight at 50% relative humidity and 23.degree.
C.
[0120] Stiffness is tested using a Taber V-5 Stiffness Tester from
Taber Industries of North Tonawanda, N.Y., designed for evaluating
stiffness and resilience of paper, cardboard, and other flexible
materials. The following procedure and calculation are used with
hair samples.
[0121] When the machine is first turned on, the optical encoder
inside the unit is oriented and the pendulum balanced according to
manufacture's instructions.
[0122] The hair swatch is inserted between the clamp jaws, with the
lower edge resting lightly on the bottom gauge. The clamp jaws are
tightened by turning the screws on either side of the clamp.
[0123] The swatch is centered between the bottom rollers. With one
finger, apply light pressure to the control lever switch and
deflect the driving disc to the left until the line on the pendulum
is under the 15.degree. deflection mark. Use a smooth, continuous
motion without abrupt starts and stops.
[0124] Record the stiffness reading on the outer scale that falls
opposite to the zero line on the driving disc (LS). Now deflect the
same swatch to the right by 15.degree. and take that stiffness
reading (RS). Average the left and right readings and multiply by
five. The product is the stiffness value for that swatch.
[0125] D. Removability Test Procedure
[0126] Using aerosol formulas, spray eight hair swatches with
experimental formulation and eight with control formulation and
allow to dry at ambient conditions for one hour. For each swatch,
rinse under tap water for 1 minute while working fingers into hair.
Put wet swatches in 110.degree. F. oven until dry. Pair off
experimental swatches vs. control swatches, and evaluate
subjectively for residual stiffness, flake, and feel
properties.
[0127] E. Tack and Drying Time Test Procedure
[0128] Suspend eight sets of two untreated hair swatches, each
separately. Spray one swatch of each set with experimental
formulation and other swatch with control formulation
simultaneously. Immediately feel swatches for tack and drying
times. Record time that tack starts, tack ends, and when each
swatch feels dry. Subtract tack start time from tack end time to
obtain total tack time.
Example 1
Preparation of Starch Modified with Propylene Oxide
[0129] a. A 40% aqueous solution of waxy starch was prepared and
25% sodium sulfate was added. The pH was then adjusted to about
11.5 uses a 3% sodium hydroxide solution. The starch was treated
with 7.5% propylene oxide. The pH was then adjusted to 5.5 using
dilute sulfuric acid.
[0130] b. Example 1a was repeated using a propylene oxide level of
15%.
[0131] c. Example 1a was repeated using a propylene oxide level of
3%.
[0132] d. Example 1a was repeated using a 50% amylose corn
starch.
[0133] e. Example 1a was repeated using a 70% amylose corn
starch.
[0134] f. Example 1b was repeated using tapioca starch.
[0135] g. Example 1b was repeated using potato starch.
Example 2
Preparation of Hydrolyzed Starch Modified with Propylene Oxide
[0136] a. The slurried starch of Example 1a was adjusted to a pH of
5.5 using sulfuric acid and cooked until fully gelatinized. The
starch was then hydrolyzed using .alpha.-amylase to a funnel
viscosity of about 30 seconds.
[0137] b. Example 2a was repeated using a 70% amylose starch.
[0138] c. Example 2a was repeated hydrolyzing to a funnel viscosity
of 10 seconds.
[0139] d. Example 2a was repeated hydrolyzing to a funnel viscosity
of 60 seconds.
Example 3
Preparation of Hydrolyzed Starch Modified with Propylene Oxide and
Octenyl Succinic Anhydride
[0140] a. A 40% aqueous slurry of Amioca.TM. starch was prepared.
25% sodium sulfate was added. The pH was then adjusted to about
11.50 by addition of a 3% sodium hydroxide solution. The starch was
then treated with propylene oxide at a level of 7.5%. After
reaction the pH was adjusted to 3.5 using sulfuric acid. The
solution was allowed to stir for one hour and the pH was then
adjusted to 5.5 with 3% sodium hydroxide. Next the starch was
cooked until fully gelatinized and hydrolyzed with alpha-amylase to
a funnel viscosity of 30 seconds. The starch cook was cooled to
room temperature. Octenyl succinic anhydride was then added at a
level of 6% while maintaining the pH at 7.5 using 25% sodium
hydroxide solution. The starch was allowed to react until caustic
consumption stopped. The pH was then adjusted to 5.5 using dilute
hydrochloric acid solution. The starch was then filtered through
Celite (Celite 512 is a diatomaceous earth commercially available
from Celite Corporation).
[0141] b. Example 3a was repeated using propylene oxide at a level
of 15%.
[0142] c. Example 3a was repeated using propylene oxide at a level
of 3%.
[0143] d. Example 3a was repeated hydrolyzing the starch to a
funnel viscosity of less than 10 seconds.
[0144] e. Example 3a was repeated hydrolyzing the starch to a
funnel viscosity of 15 seconds.
[0145] f. Example 3a was repeated hydrolyzing the starch to a
funnel viscosity of 60 seconds.
[0146] g. Example 3a was repeated hydrolyzing the starch using
concentrated hydrochloric acid for sixteen hours and then
neutralizing by addition of sodium carbonate and sodium
hydroxide.
[0147] h. Example 3a was repeated hydrolyzing the starch by using
sodium hypochlorite solution for sixteen hours. 10% sodium
bisulfite solution was added to remove residual hypochlorite and
neutralized using dilute hydrochloric acid.
[0148] i. Example 3a was repeated using potato starch in place of
Amioca.
Example 4
Preparation of Other Modified Hydrolyzed Starches
[0149] a. A 40% aqueous slurry of Amioca.TM. starch was prepared.
The pH was adjusted to about 11.5 using 3% NaOH. The slurry was
treated with 5% 3-chloro-2-hydroxypropyltrimethyl ammonium
chloride. The slurry was allowed to react for 10-12 hours while
maintaining pH=11.5 using 3% NaOH. The starch was then adjusted to
pH=5.5 using dilute hydrochloric acid solution, filtered and
washed. Next the starch was cooked until fully gelatinized and
hydrolyzed with alpha-amylase to a funnel viscosity of 30 seconds.
The starch cook was cooled to room temperature. Octenyl succinic
anhydride was then added at a level of 6%. The pH was maintained at
7.5 using 25% sodium hydroxide solution. The starch was allowed to
react until caustic consumption stopped. The pH was then adjusted
to 5.5 using dilute hydrochloric acid solution. The starch was then
filtered through Celite (Celite 512 is a diatomaceous earth
commercially available from Celite Corporation).
[0150] b. Example 4a was repeated using
3-chloro-2-hydroxypropyltrimethyl ammonium chloride at a level of
10%.
[0151] c. Example 4a was repeated substituting the use of
2-chloroethylaminodiproprionic acid at a level of 5% for the use of
3-chloro-2-hydroxypropyltrimethyl.
[0152] d. A 40% aqueous slurry of Amioca.TM. starch was prepared.
25% sodium sulfate was added. The pH was then adjusted to about
11.50 by addition of a 3% sodium hydroxide solution. The starch was
then treated with propylene oxide at a level of 7.5%. After
reaction the pH was adjusted to 3.5 using sulfuric acid. The
solution was allowed to stir for one hour and the pH was then
adjusted to 5.5 with 3% sodium hydroxide. Next the starch was
cooked until fully gelatinized and hydrolyzed with alpha-amylase to
a funnel viscosity of 30 seconds. The starch cook was cooled to
room temperature. Acetic anhydride was added at a level of 7.5%,
while maintaining the slurry pH=7.5 with 25% NaOH. The starch was
allowed to react until caustic consumption stopped. The pH was then
adjusted to 5.5 using dilute hydrochloric acid solution. The starch
was then filtered through Celite (Celite 512 is a diatomaceous
earth commercially available from Celite Corporation).
[0153] e. A 40% aqueous slurry of Amioca.TM. starch was prepared.
25% sodium sulfate was added. The pH was then adjusted to about
11.50 by addition of a 3% sodium hydroxide solution. The starch was
then treated with propylene oxide at a level of 7.5%. After
reaction the pH was adjusted to 3.5 using sulfuric acid. The
solution was allowed to stir for one hour and the pH was adjusted
to 5.5 with 3% sodium hydroxide. Next the starch was cooked until
fully gelatinized and hydrolyzed with alpha-amylase to a funnel
viscosity of 30 seconds. The starch cook was cooled to room
temperature. Acetic anhydride was added at a level of 7.5%, while
maintaining the slurry pH=7.5 with 25% NaOH. Octenyl succinic
anhydride was then added at a level of 6%, maintaining pH=7.5 using
25% NaOH. The starch was allowed to react until caustic consumption
stopped. The pH was then adjusted to 5.5 using dilute hydrochloric
acid solution. The starch was then filtered through Celite (Celite
512 is a diatomaceous earth commercially available from Celite
Corporation).
Example 5
Coprocessing of Starch with a Polymer
[0154] 5 g of polyvinyl pyrrolidone (PVP) were dissolved in 900
grams of water. 100 g of the starch of example 1e is then slurried
into the polymer solution. The slurry was jet cooked at
150-155.degree. C. and then conveyed under pressure directly to the
spray drier to prevent retrogradation. The cooked slurry was spray
dried with an inlet temperature of 230.degree. C. and an outlet
temperature of 120.degree. C.
Example 6
Neutralization of the Starch
[0155] The starches of examples 1-5 were neutralized by the
addition of 2-amino 2-methyl 1-propanol.
Example 7
Preparation of Hair Spray Solution
[0156] a) The starches of examples 1-6 were each made into a hair
spray solution using the following method. The starch was diluted
with water to a 7.5% solids solution. Dimethyl ether propellant was
added to made the final concentration 5% starch, 33% propellant,
and 62% water.
Example 8
Performance of Starches in an Aerosol Hair Spray
[0157] The starches from Examples 3a and 3b were formulated into
low VOC aerosol hair spray systems according to the following
formulations. All values reported are parts by weight, based on the
total weight of the hair spray composition.
1 Parts by Weight (dry basis) Ingredient Alcohol-free (33% VOC)
starch polymer 5.0 deionized water 62.0 dimethyl ether 33.0
[0158] With agitation, the starch polymer is sifted into deionized
water until homogeneous. Solutions were filtered and filled into
aerosol containers. Cans were charged with dimethyl ether
propellant. Hair spray formulations were tested for spray
characteristics on 2 gram swatches of European brown hair. The
sprays were delivered with a Seaquist NS-34 valve (0.013" vapor
tap.times.0.013" stem orifice.times.0.040" dip tube diameter)
having an Excel 200 Misty (0.016" orifice) actuator in a 2 second
burst from a distance of six inches. Formulas were compared to:
[0159] Control A (diglycol/CHDM/isophthalates/SIP copolymer in a 5%
solids, 33% VOC aerosol, commercially available from Eastman
Chemical Company, Kingsport, Tenn.);
[0160] Control B (VA/crotonates/vinyl neodecanoate copolymer in a
5% solids, anhydrous aerosol commercially available from National
Starch and Chemical Company, Bridgewater, N.J.);
[0161] Control C (acrylates/octylacrylamide copolymer in a 5%
solids, anhydrous aerosol commercially available from National
Starch and Chemical Company, Bridgewater, N.J.); and/or
[0162] Control D (octylacrylamide/acrylates/butylaminoethyl
methacrylate copolymer in a 5% solids anhydrous aerosol
commercially available from National Starch and Chemical Company,
Bridgewater, N.J.).
2 Anhydrous Formulations Ingredient Parts by Weight (dry basis)
polymer 5.0 2-amino-2-methyl-1-propanol (AMP).sup.a 1.0 anhydrous
ethanol 69.0 A-46 hydrocarbon.sup.b 25.0 .sup.acommercially
available from Angus Chemical Company .sup.bisobutane/propane
[0163] Aerosol Solubility
[0164] The solubility of the starches in the hair spray composition
are determined by checking clarity immediately after formulation
and after 12 hours. The results are shown in Table I below.
3 TABLE I Starch Initial After 12 hours Example 3a clear slightly
hazy Example 3b clear clear
[0165] Spray Characteristics
[0166] The spray characteristics of the alcohol-free aerosols were
rated on a scale from A to F, with A being the best spray. An "A"
rating indicates a wide spray cone, fine spray, small particle
size, and no foam on the hair or actuator. An "F" rating indicates
a narrow spray cone, spitting at the actuator, large particle size,
and obvious foaming on the hair or actuator. Mean particle size of
the sprays were measured by a Malvern Series 2600 Droplet and
Particle Size Analyzer from Malvern Instruments Inc. of
Southborough, Mass. The results are listed in Table II.
4TABLE II Polymer % VOC Aerosol Mean Particle Size (.mu.) Spray
Rating Example 3a 33 33.92 B Example 3b 33 30.97 B
[0167] High Humidity (90%) Curl Retention
[0168] Mean retention values of nine samples are listed in Table
III, below.
5TABLE III 15 30 60 90 Polymer min. min. min. min. 2 hr. 3 hr. 4
hr. 5 hr. 24 hr. Exam- 95.5 91.8 89.5 88.8 86.6 85.0 84.3 84.3 80.5
ple 3a Exam- 94.0 90.8 89.2 86.2 83.9 82.2 78.4 78.4 67.9 ple 3b
Con- 95.6 92.0 89.0 87.6 84.0 80.4 80.4 80.4 70.4 trol A Con- 90.7
85.4 78.1 73.3 73.0 70.2 69.1 65.7 53.9 trol B Con- 97.9 96.6 93.1
93.1 92.5 91.2 91.2 91.2 90.5 trol D
[0169] All of the starch examples are comparable in humidity
resistance with the controls.
[0170] Shampoo Removability Evaluations
[0171] Shampoo removability compared to Control C is listed in
Table IV, below.
6 TABLE IV Polymer Stiffness Flake Example 3a = =
[0172] Results are statistically equivalent to the control.
[0173] Taber Stiffness
7 TABLE V Polymer % of Control D Stiffness Example 3a 65% Control A
72%
[0174] Tack and Drying Time
[0175] Tack and drying time was compared to Control D.
8TABLE VI Polymer Total Tack Time Drying Time Example 3a + +
[0176] Example 3a is statistically superior (less tack, quicker
drying time) than the control.
[0177] Initial Curl Droop
[0178] The compositions were tested at 50% relative humidity (RH).
Mean % curl retention values of nine values per sample are shown in
Table X below.
9TABLE VII Starch .dwnarw. 30 sec 60 sec 90 sec 2 min 4 min 6 min
Example 3a 93.46 91.98 91.98 88.42 86.99 84.76
Example 9
Evaluation of Starch/Polymer in Mousse
[0179]
10 Ingredient Amount (g) Polymer 3.00 Tergitol NP-9
Surfactant.sup.a 0.60 Dowicil 200.sup.b 0.20 Water 88.20 Propellant
A-46.sup.c 8.00 .sup.aNonoxynol-9 commercially available from Union
Carbide .sup.bQuaternium-15 commercially available from Dow
Chemical Co. .sup.cIsobutane/Propane
[0180] The polymer was slowly dispersed into the water with
agitation. The Tergitol and Dowicil were added with continued
agitation. The resultant solution was filtered and used to fill
aerosol cans. The cans were charged with the propellant.
[0181] Polymers
[0182] Starch of Example 5
[0183] Luviskol VA 64 (PVP/VA 60/40), commercially available from
BASF Gafquat, commercially available from International Specialty
Products 50:50 blend of Example 5:Gafquat
[0184] Wet combability and feel
[0185] The mousse was dispensed onto a wet swatch of hair and
combed. Both the wet combability and feel of the formulation using
the starch of example 5 were equivalent to that of the
Luviskol.
[0186] Both the wet combability and feel of the formulation using
the 50:50 blend example 5: Gafquat were equivalent to that of the
Gafquat alone.
[0187] Subjective Stiffness
[0188] The starch of example 5 provided more stiffness than that of
Luviskol. The mousse was then reformulated using 2.25% and 1.5%
starch of example 5, using water to substitute for the removed
starch. The comparison with Luviskol (at 3%) is shown below.
11 3% Example 5 stiffer than Luviskol 2.25% Example 5 equivalent
stiffness to Luviskol 1.5% Example 5 less stiff than Luviskol
[0189] The stiffness of the 50:50 blend, Example 5:Gufquat was
equal to that of the Gafquat.
12 High Humidity Curl Retention Polymer Mean Retention (%) Example
5 43.49 Gafquat 36.84 Luviskol 15.57
Example 10
Preparation of All-Natural Texturizing Fixative Lotion
[0190]
13 Ingredients % By Weight Phase A: Deionized Water 55.85 (1)
Potato Starch Modified 1.75 (2) Brij 78 2.00 Phase B: (3) DC 345
7.50 (4) DC 200 2.50 Phase C: (5) Lanette O 1.40 (6) Germall II
1.00 Phase D: Propylene Glycol 5.00 Example 1e 3.00 Phase E:
Deionized Water 20.00 100.00 INCI Designations: (1) Potato Starch
Modified (National Starch and Chemical) (2) Steareth-20 (ICI
Surfactants) (3) Cyclomethicone (Dow Corning) (4) Dimethicone (Dow
Corning) (5) Cetearyl Alcohol (Henkel) (6) Diazolidinyl Urea
(Sutton Labs)
[0191] Procedure:
[0192] Potato starch modified was added to cold water and mixed for
2 minutes. The starch solution as heated to 80.degree. C. with
mixing at moderate speed. Mixing was continued for 25 minutes at
80.degree. C. Brij 78 was added and mixed until dissolved. Phase B
was premixed and added to Phase A under high speed (8,000-10,000
RPM). Lanette O was then added at 80.degree. C. and mixed, followed
by addition of Germall II. Phase D was premixed and then Phase E
was added to Phase D and mixed well. Phase DE was added to Phase
ABC and mixing was continued for approximately 10-15 minutes.
* * * * *