U.S. patent application number 09/932435 was filed with the patent office on 2003-06-12 for use of xanthan gum as a hair fixative.
Invention is credited to Cao, Hongjie, Martino, Gary T., Richardson, Paul H..
Application Number | 20030108505 09/932435 |
Document ID | / |
Family ID | 25462308 |
Filed Date | 2003-06-12 |
United States Patent
Application |
20030108505 |
Kind Code |
A1 |
Cao, Hongjie ; et
al. |
June 12, 2003 |
Use of xanthan gum as a hair fixative
Abstract
The present invention is directed to the use of xanthan gum,
particularly heat treated xanthan gum, as a fixative in hair
cosmetic compositions. Xanthan gum is advantageous in that it may
be used with other hair fixatives and provides rheology modifying
and other properties including excellent stiffness, gloss, dry
comb, wet comb, non-flake, anti-static, feel and high humidity curl
retention.
Inventors: |
Cao, Hongjie; (Hillsborough,
NJ) ; Martino, Gary T.; (Monmouth Junction, NJ)
; Richardson, Paul H.; (Vernon, NJ) |
Correspondence
Address: |
Karen G. Kaiser
NATIONAL STARCH AND CHEMICAL COMPANY
10 Finderne Avenue
Bridgewater
NJ
08807-0500
US
|
Family ID: |
25462308 |
Appl. No.: |
09/932435 |
Filed: |
August 17, 2001 |
Current U.S.
Class: |
424/70.13 |
Current CPC
Class: |
A61K 8/73 20130101; A61Q
5/06 20130101 |
Class at
Publication: |
424/70.13 |
International
Class: |
A61K 007/06; A61K
007/11 |
Claims
We claim:
1. A hair cosmetic composition comprising a fixative effective
amount of xanthan gum.
2. The composition of claim 1, wherein the xanthan gum has been
heat treated at a moisture content of less than about 25%, a
temperature of at least about 60.degree. C. for at least about 30
minutes.
3. The composition of claim 2, wherein the temperature is at least
100.degree. C.
4. The composition of claim 3, wherein the temperature is at least
105.degree. C.
5. The composition of claim 2, wherein the moisture content is less
than about 8%.
6. The composition of claim 3, wherein the moisture content is less
than about 1%.
7. The composition of claim 2, wherein the heat treatment is for at
least about one hour.
8. The composition of claim 3, wherein the heat treatment is for at
least about 2.5 hours.
9. The composition of claim 2, wherein the heat treatment is at a
moisture of less than about 1% and the temperature is at least
about 105.degree. C. for at least about 2.5 hours.
10. The composition of claim 1, wherein the composition is selected
from the group consisting of a spray, a mousse, a hair lotion, a
cream, a pomade, and a gel.
11. The composition of claim 10, wherein the composition is a
gel.
12. The composition of claim 13 characterized by a viscosity of at
least about 8000 cps, a high humidity curl retention of at least
about (80%) and a turbidity of no more than about 100 NTU.
13. The composition of claim 1, further comprising a second
fixative polymer.
14. The composition of claim 13 wherein the second fixative polymer
is selected from the group comprising acrylates copolymer,
octylacrylamide/acrylates/butylaminoethyl methacrylate copolymer,
acrylates/octylacrylamide copolymer, VA/crotonates/vinyl
Neodeanoate copolymer, poly(N-vinyl acetamide), poly(N-vinyl
formamide), polyurethane, corn starch modified, sodium polystyrene
sulfonate, polyquaternium-4, polyquaternium-10 and
polurethane/acrylates copolymer.
15. The composition of claim 2, wherein the composition is a
gel.
16. The composition of claim 16 further comprising a second
fixative polymer.
17. The composition of claim 17 wherein the second fixative polymer
is selected from the group comprising acrylates copolymer,
octylacrylamide/acrylates/butylaminoethyl methacrylate copolymer,
acrylates/octylacrylamide copolymer, VA/crotonates/vinyl
Neodeanoate copolymer, poly(N-vinyl acetamide), poly(N-vinyl
formamide), polyurethane, corn starch modified, sodium polystyrene
sulfonate, polyquaternium-4, polyquaternium-10 and
polyurethane/acrylates copolymer.
18. A method of preparing the composition of claim 1, comprising
dispersing the xanthan gum in water; and mixing in other hair
cosmetic components.
19. A method of preparing the composition of claim 2, comprising
dispersing the xanthan gum in water; and mixing in other hair
cosmetic components.
20. A method of preparing the composition of claim 17 comprising
dispersing the xanthan gum in water; and mixing in other hair
cosmetic components.
21. A method of providing fixative properties to the hair
comprising applying the composition of claim 1.
22. A method of providing curl retention under high humidity
conditions comprising applying the composition of claim 1.
Description
BACKGROUND OF THE INVENTION
[0001] The present invention relates to the use of xanthan gum,
particularly heat treated xanthan gum, as a fixative in hair
cosmetic compositions and hair fixative compositions comprising
xanthan gum.
[0002] Xanthan gum is a polysaccharide gum derived from the
bacterium Xanthomonas and is well known in the art. It is composed
of a main chain comprising .beta.-(1,4) D-glucose units.
Trisaccharide side chains on alternating anhydroglucose units are
composed of a glucuronic acid residue between two mannose units. At
most of the terminal mannose units is a pyruvate moiety and the
non-terminal mannose carries an acetyl group. It has pseudoplastic
or shear-thinning behavior characterized by a decrease in apparent
viscosity in response to an increase in shear rate.
[0003] Xanthan gum is typically used in many industrial
applications as a rheology modifier; thickening, viscosifying and
gelling when combined with other polymers. It has also been used to
impart stability to emulsions and prevent the settling out of
solids. Its limited ability to disperse in either hot or cold water
allows xanthan gum to be formulated into a broad variety of
applications including pharmaceuticals, household products, foods,
and personal care products.
[0004] Xanthan gum with an apparent average molecular weight of
greater than 16,000,000 has been used to stabilize and improve the
feel of emulsified cosmetics such as toilet water, creams and
cleansing gels (JP Application No. 10-140503).
[0005] Xanthan gum which has been heat-treated is also known in the
art. For example, EP 321 216 enhances the viscosity profile of
xanthan gum by thermally treating it in the dry state (15% moisture
or less). Heat treatment of xanthan gum is also known in JP
Application No. 8-193055 which heat treats xanthan gum in the
powdered form.
[0006] Surprisingly, it has now been discovered that xanthan gum,
particularly heat treated xanthan gum, is a suitable fixative for
hair cosmetic compositions.
SUMMARY OF THE INVENTION
[0007] The present invention is directed to the use of xanthan gum,
particularly heat treated xanthan gum, as a fixative in hair
cosmetic compositions. Xanthan gum is advantageous in that it may
be used with other hair fixatives and provides rheology modifying
and other properties including excellent stiffness, gloss, dry
comb, wet comb, non-flake, anti-static, feel and high humidity curl
retention.
DETAILED DESCRIPTION OF THE INVENTION
[0008] The present invention is directed to the use of xanthan gum,
particularly heat treated xanthan gum, as a fixative in hair
cosmetic compositions.
[0009] The xanthan gum may be used in a purified form or may be
heat treated. Heat treatment of xanthan gum is typically done at
low moisture, particularly less than about 25%, more particularly
less than about 8%, most particularly less than about 1%, at a
temperature of at least about 60.degree. C., more particularly at
least 100.degree. C., and most particularly at least about
105.degree. C. for a period of time of about 30 minutes,
particularly at least one hour, more particularly at least 2.5
hours.
[0010] The moisture content, pH, temperature and time of heat
treatment may be adjusted by one skilled in the art to achieve the
viscosity, dispersibility, gel texture, solution clarity, and other
properties desired. It will further be dependent upon the starting
material used (grade, viscosity, molecular weight, and particle
size). Typically, low moisture is used to improve the impact of
heat-treatment. However, at any given moisture, increasing the
temperature or time generally increases viscosity to a maximum and
further heating decreases the viscosity of the xanthan gum at the
concentrations used in this invention. Acidic pH are typically more
suitable; a pH of 2-4 is most suitable.
[0011] Heat treatment of xanthan gum may be accomplished by a
variety of methods known in the art including without limitation
oven, fluidized bed, infrared and microwave heat treatments. The
particle size of the resultant heat-treated xanthan gum may be
adjusted using methods known in the art such as milling.
[0012] The xanthan gum may further be modified either before or
after heat treatment. The xanthan gum may be converted by
oxidation, enzyme conversion, acid hydrolysis, heat and/or acid
dextrinization, or shear. The xanthan gum may also be chemically,
enzymatically or physically modified. Suitable chemical derivatives
include esters, such as the acetate, and half esters, such as the
succinate, octenyl succinate and tetradecenyl succinate; phosphate
derivatives; ethers such as hydroxyalkyl ethers and cationic
ethers; or any other derivatives or combinations thereof.
Modification may also be by chemical crosslinking. Crosslinking
agents suitable for use herein include phosphorus oxychloride,
epichlorohydrin, sodium trimetaphosphate and adipic-acetic mixed
acid anyhrides. Such processes are also known in the art.
Typically, the xanthan gum will not be modified other than by
crosslinking or heat treatment.
[0013] The xanthan gum may also be purified by any method known in
the art to remove off flavors and colors that are native to the
xanthan gum or are created during the modification or heat
treatment processes as long as the heat treatment is not
substantially impacted.
[0014] The resultant heat-treated xanthan gum has improved
dispersibility, such that under given conditions of temperature and
agitation, the time to fully disperse the resultant gum is
typically reduced by 25%, more particularly 50%, most particularly
70% compared to non-heat treated xanthan.
[0015] Xanthan gum, native or heat treated, provides fixative
properties to hair cosmetic compositions including hair sprays,
gels including spray gels, styling lotions, creams, pomades, and
mousses. The use of xanthan gum imparts not only stiffness, but is
also highly suitable for retention of curls under high humidity
conditions. High humidity conditions, as used herein, is intended
to mean at 22.degree. C. and 90% relative humidity.
[0016] Xanthan gum is particularly suitable for gels as it provides
clear to translucent clarity and is easy to use as it is
dispersible in either hot or cold water and needs no
neutralization. Xanthan gum also exhibits tolerance to salt and
extreme pH, particularly in the range of about 2 to about 12.
Finally, it is biodegradable and may be labeled as natural.
[0017] The heat modification of xanthan gum improves the ease of
use, including the ease of dispersing in solution with less
tendency to form fish eyes. Heat modification also may be used to
improve thickening efficiency and gel texture, reducing the
stringiness or pituitousness of the long texture. In addition, heat
treatment of xanthan increases its viscosity throughout the pH and
salt ranges typically used in hair cosmetic compositions. Unlike
Carbomer, xanthan gum is compatible with anionic, cationic or
nonionic polymers, allowing it to be formulated with a variety of
commonly used hair cosmetic additives. Although xanthan gum alone
provides fixative properties, it may be used in combination with
other fixatives, including without limitation polyoxythylenated
vinyl acetate/crotonic acid copolymers, vinyl acetate crotonic acid
(90/10) copolymers, vinyl acetate/crotonic acid/vinyl neodecanoate
terpolymers, N-octylacrylamide/methylacrylate/hydroxypropyl
methacrylate/acrylic acid/tert-butylaminoethyl methacrylate
copolymers, and methyl vinyl ether/maleic anhydride (50/50)
copolymers monoesterified with butanol or ethanol, acrylic
acid/ethyl acrylate/N-tert-butyl-acrylamide terpolymers, and poly
(methacrylic acid/acrylamidomethyl propane sulfonic acid),
acrylates copolymer, octylacrylamide/acrylates/butylaminoethyl
methacrylate copolymer, acrylates/octylacrylamide copolymer,
VA/crotonates/vinyl Neodeanoate copolymer, poly(N-vinyl acetamide),
poly(N-vinyl formamide), corn starch modified, sodium polystyrene
sulfonate, polyquaterniums such as polyquaternium-4,
polyquaternium-7, polyquaternium-10, polyquaternium-11,
polyquarternium-16, polyquaternium-28, polyquaternium-29,
polyquaternium-46, polyether-1, polyurethanes, VA/acrylates/lauryl
methacrylate copolymer, adipic acid/dimethylaminohydroxypropyl
diethylene AMP/acrylates copolymer, methacrylol ethyl
betaine/acrylates copolymer, PVP/dimethylaminoethylmeth- acrylate
copolymer, PVP/DMAPA acrylates copolymer, PVP/vinylcaprolactam/DM-
APA acrylates copolymer, vinyl caprolactam/PVP/dimethylaminoethyl
methacrylate copolymer, VA/butyl maleate/isobornyl acrylate
copolymer, VA/crotonates copolymer, acrylate/acrylamide copolymer,
VA/crotonates/vinyl propionate copolymer, vinylpyrrolidone/vinyl
acetate/vinyl propionate terpolymers, VA/crotonates, cationic and
amphoteric guar, polyvinylpyrrolidone (PVP),
polyvinylpyrrolidone/vinyl acetate copolymer, PVP acrylates
copolymer, vinyl acetate/crotonic acid/vinyl proprionate,
acrylates/acrylamide, acrylates/octylacrylamide,
acrylates/hydroxyacrylates copolymer, and alkyl esters of
polyvinylmethylether/maleic anhydride,
diglycol/cyclohexanedimethanol/iso- phthalates/sulfoisophthalates
copolymer, vinyl acetate/butyl maleate and isobornyl acrylate
copolymer, vinylcaprolactamlPVP/dimethylaminoethyl methacrylate,
vinyl acetatefalkylmaleate half ester/N-substituted acrylamide
terpolymers, vinyl caprolactam/vinylpyrrolidonel
methacryloamidopropyl trimethylammonium chloride terpolymer,
methacrylates/acrylates copolymer/amine salt, polyvinylcaprolactam,
polyurethanes, hydroxypropyl guar, hydroxypropyl guar hydroxypropyl
trimmonium chloride, poly (methacrylic acid/acrylamidomethyl
propane sulfonic acid, poylurethane/acrylate copolymers and
hydroxypropyl trimmonium chloride guar, particularly acrylates
copolymer, octylacrylamide/acrylates/butylaminoethyl methacrylate
copolymer, acrylates/octylacrylamide copolymer, VA/crotonates/vinyl
Neodeanoate copolymer, poly(N-vinyl acetamide), poly(N-vinyl
formamide), polyurethane, corn starch modified, sodium polystyrene
sulfonate, polyquaternium-4, polyquarternium-10, and
polyurethane/acrylates copolymer.
[0018] Optional conventional additives may also be incorporated
into the hair compositions of this invention to provide certain
modifying properties to the composition. Included among these
additives are silicones and silicone derivatives; humectants;
moisturizers; plasticizers, such as glycerine, glycol and phthalate
esters and ethers; emollients, lubricants and penetrants, such as
lanolin compounds; fragrances and perfumes; UV absorbers; dyes,
pigments and other colorants; anticorrosion agents; antioxidants;
detackifying agents; combing aids and conditioning agents;
antistatic agents; neutralizers; glossifiers; preservatives;
proteins, protein derivatives and amino acids; vitamins;
emulsifiers; surfactants; viscosity modifiers, thickeners and
rheology modifiers; gelling agents; opacifiers; stabilizers;
sequestering agents; chelating agents; pearling agents; aesthetic
enhancers; fatty acids, fatty alcohols and triglycerides; botanical
extracts; film formers; and clarifying agents. 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 0.01 to 10%
by weight each, and from about 0.01 to 20% by weight total, based
on the weight of the composition.
[0019] Aesthetic enhancers is intended to include without
limitation aluminum starch octenyl succinate, corn starch modified,
aluminum starch octenylsuccinate (and) lauroyl lysine, and aluminum
starch octenylsuccinate (and) boron nitride. Thickeners and
rheology modifiers is intended to include without limitation
acrylates/steareth-20 itaconate copolymer, acrylates/ceteth-20
itaconate copolymer, potato starch modified, hydroxypropyl starch
phosphate, acrylates/aminoacrylates/C10-30 alkyl PEG-20 itaconate
copolymer, carbomer, acrylates/C10-30 alkyl acrylate crosspolymer,
hydroxypropylcellulose, hydroxyethylcellulose, sodium
carboxymethylcellulose, polyacrylamide (and) C13-14 isoparaffin
(and) laureth-7, acrylamides copolymer (and) mineral oil (and)
C13-14 isoparaffin (and) polysorbate 85,
hydroxyethylacrylate/sodium acrylol dimethyltaurate copolymer, and
hydroxyethylacrylate/sodium acrylol dimethyltaurate copolymer.
[0020] Xanthan gum may be formulated into hair cosmetic
compositions at any level which provides the desired properties.
Typically, native xanthan gum will be used in an amount of at least
about 0.01%, particularly at least about 0.2%, more particularly at
least about 1.0% and less than about 20%, particularly less than
about 10%, more particularly less than about about 3%. In contrast,
heat treated xanthan gum will be used in an amount of at least
about 0.01%, particularly at least about 0.5%, more particularly at
least about 0.75% and less than about 20%, particularly less than
about 2%, more particularly less than about 1.5%. The amount used
will depend not only upon the properties desired, but also upon the
heat treatment levels and other additives. For example, the same
amount of fixative property may be achieved by using less xanthan
gum and adding another commonly used hair fixative polymer.
[0021] The hair cosmetic composition may be prepared by dispersing
xanthan gum in water and then mixing in the remaining hair cosmetic
components such as any fixative polymers, conditioning polymers or
other additives as desired.
[0022] The delivery system in most cases will be water. However, it
is possible to use a solvent. In general, the amount of solvent
will be small to achieve a VOC (volatile organic compounds) content
of no more than 55%. Typically, the solvent will be a lower
(C.sub.1-4) alcohol, particularly methanol, ethanol, propanol,
isopropanol, or butanol, though any solvent known in the art may be
used. VOC will also include any optional propellant(s).
[0023] The hair cosmetic composition may be formulated with xanthan
gum to achieve the desired properties. For example the amount of
xanthan gum may be adjusted to achieve the desired stiffness and
curl retention. In general, a hair gel will have a viscosity of at
least about 5,000 cps, more particularly at least about 6,000 cps
and most particularly at least about 8,000 cps, a high humidity
curl retention for 2 hours of at least about 70%, more particularly
at least about 80% and most particularly about 90%, and turbidity
of no greater than 100 NTU, particularly no greater than 50 NTU,
most particularly no greater than 30 NTU.
EXAMPLES
[0024] The following examples are presented to further illustrate
and explain the present invention and should not be taken as
limiting in any regard. All percents used are on a weight/weight
basis.
Example 1
Hair Styling Gels with Native and Heat-Treated Xanthan Gum
[0025]
1 Formula 1 Formula 2 Ingredients % w/w % w/w Part A Acrylates
Copolymer.sup.1 (50%) 8.0 8.0. Deionized Water 40.0 40.0
Aminomethyl Propanol.sup.2 0.56 0.56 Part B Xanthan gum.sup.3 1.0
-- Heat-treated Xanthan gum.sup.4 -- 1.0 Deionized Water q.s. q.s.
Preservative q.s. q.s. Part C Keratin Protein 0.2 0.2 Propylene
Glycol 2.0 2.0 Polysorbate 20.sup.5 0.5 0.5 Fragrance 0.1 0.1 100
100 .sup.1Balance 0/55 (National Starch and Chemical Co.)
.sup.2AMP-95 (Angus) .sup.3Keltrol T (Kelco) .sup.4Heat-treated
Keltrol T (Fluid bed reactor at 235.degree. F. for 60 minutes)
.sup.5Tween 20 (ICI Surfactants)
[0026] The ingredients in part A were combined and mixed until
clear. In a separate container, xanthan or heat-treated xanthan gum
was dispersed into water with moderate mixing (for formula 1, mix
for 30 minutes at 700 rpm, and for formula 2, mix for 10 minutes at
700 rpm to achieve uniform part B). Parts A and B were combined
while stirring moderately and then part C was added.
[0027] Both the xanthan and heat-treated xanthan gum were cold
water dispersible. However, the heat-treated xanthan gum was easier
to disperse than the native xanthan gum. In addition, no
neutralization was needed with the use of xanthan gum.
[0028] Formula 1 produced a clear, colorless viscous liquid
(Brookfield viscosity: 3200 cps with sprindle#4@20 rpm). Formula 2
produced a clear, colorless gel (Brookfield viscosity: 8200 cps
with sprindle#4@20 rpm). Formula 2 had much higher viscosity than
formula 1, which demonstrated that the heat-treated xanthan gum
provides better thickening efficiency. Formula 2 was also much more
gel-like, or with shorter and less stringy gel texture compared to
formula 1. Both formulas had very good clarity.
Example 2
Various Hair Styling Gel Formulations
[0029]
2 Formula 3 Formula 4 Formula 5 Formula 6 Formula 7 Ingredients %
w/w % w/w % w/w % w/w % w/w Part A Acrylates Copolymer.sup.1 (50%)
8.0 -- -- -- -- Octylacrylamide/Acrylates/ -- 4.0 -- -- --
Butylaminoethyl Methacrylate Copolymer.sup.2
Acrylates/Octylacrylamide -- -- 4.0 -- -- Copolymer.sup.3
Octylacrylamide/Acrylates/ -- -- -- 4.0 -- Butylaminoethyl
Methacrylate Copolymer.sup.4 PVP.sup.5 -- -- -- -- 4.0 Deionized
Water 40.0 40.0 40.0 40.0 40.0 Aminomethyl Propanol.sup.6 0.56 0.94
1.13 0.77 -- Part B Heat-treated Xanthan gum.sup.7 0.85 0.85 0.85
0.85 -- Carbomer.sup.8 -- -- -- -- 0.5 Aminomethyl Propanol -- --
-- -- 0.29 Deionized Water q.s. q.s. q.s. q.s. q.s. Preservative
q.s. q.s. q.s. q.s. q.s. 100 100 100 100 100 .sup.1Balance 0/55
(National Starch and Chemical Co.) .sup.1Balance 47 (National
Starch and Chemical Co.) .sup.3Amphomer HC (National Starch and
Chemical Co.) .sup.4Amphomer (National Starch and Chemical Co.)
.sup.5PVP K-30 (ISP) .sup.6AMP-95 (Angus) .sup.7Heat-treated
Keltrol T (Fluid bed reactor at 235.degree. F. for 60 minutes)
.sup.8Carbopol 940 (BF Goodrich)
[0030] Formulas 3-6 produced clear to translucent hair gels with
viscosity >7000 cps (Brookfield viscosity spindle #4@20 rpm). As
a comparison, formula 7 is a basic formula for the most commonly
used commercial hair styling gel. This example shows the
compatibility of various anionic fixative polymers with
heat-treated xanthan gum.
3 Formula Formula Formula Formula 8 9 10 11 Ingredients % w/w % w/w
% w/w % w/w Part A Acrylates Copolymer.sup.1 (50%) 8.0 -- -- --
Octylacrylamide/Acrylates/ -- 4.0 -- -- Butylaminoethyl
Methacrylate Copolymer.sup.2 Acrylates/Octylacrylamide -- -- 4.0 --
Copolymer.sup.3 Octylacrylamide/Acrylates/ -- -- -- 4.0
Butylaminoethyl Methacrylate Copolymer.sup.4 Deionized Water 40.0
40.0 40.0 40.0 Aminomethyl Propanol.sup.5 0.56 0.94 1.13 0.77 Part
B Carbomer.sup.6 0.5 0.5 0.5 0.5 Aminomethyl Propanol 0.29 0.29
0.29 0.29 Deionized Water q.s. q.s. q.s. q.s. Preservative q.s.
q.s. q.s. q.s. 100 100 100 100 .sup.1Balance 0/55 (National Starch
and Chemical Co.) .sup.1Balance 47 (National Starch and Chemical
Co.) .sup.3Amphomer HC (National Starch and Chemical Co.)
.sup.4Amphomer (National Starch and Chemical Co.) .sup.5AMP-95
(Angus) .sup.6Carbopol 940 (BF Goodrich)
[0031] Formulas 8-11 resulted in cloudy liquid mixtures with low
viscosity. This demonstrates the incompatibility of various anionic
fixative polymers with Carbomer.
4 Formula Formula Formula Formula 12 13 14 15 Ingredients % w/w %
w/w % w/w % w/w Xanthan gum 2.0 -- -- -- Heat-treated -- 1.0 2.0
0.85 Xanthan gum Deionized Water q.s. q.s. q.s. q.s. Preservative
q.s. q.s. q.s. q.s. 100 100 100 100
[0032] Formulas 12-15 show that hair styling gels can simply
contain xanthan gum or heat-treated xanthan gum at desired levels,
as well as water and preservatives. Due to the improvement in
solution rheology, heat-treated xanthan gum may be used at much
lower level than untreated xanthan gum and produce more gel-like
product.
5 Formula 21 Formula 22 Formula 23 Ingredients % w/w % w/w % w/w
Part A Acrylates Copolymer.sup.1 (50%) 8.0 4.0 8.0 Aminomethyl
Propanol 0.56 0.28 0.56 Deionized Water 40.0 40.0 40.0 Part B
Heat-treated Xanthan gum.sup.2 1.0 1.0 -- Xanthan gum.sup.3 -- --
1.0 Deionized Water q.s. q.s. q.s Preservative q.s. q.s. q.s. 100
100 100 .sup.1Balance 0/55 (National Starch and Chemical Co.)
.sup.2Heat-treated Keltrol T (Fluid bed reactor at 235.degree. F.
for 60 minutes) .sup.3Keltrol T (Kelco)
[0033] These formulas further show different combinations of
xanthan and heat-treated xanthan gum with anionic and nonionic
fixative polymers at different use levels.
6 Formula 26 Formula 27 Formula 28 Formula 29 Formula 30
Ingredients % w/w % w/w % w/w % w/w % w/w Part A Acrylates
Copolymer.sup.1 (50%) 8.0 8.0 8.0 8.0 8.0 Aminomethyl Propanol 0.56
0.56 0.56 0.56 0.56 Deionized Water 40.0 40.0 40.0 40.0 40.0 Part B
Heat-treated Xanthan gum.sup.2 1.0 -- -- -- -- Heat-treated Xanthan
gum.sup.3 -- 1.0 -- -- -- Heat-treated Xanthan gum.sup.4 -- -- 1.0
-- -- Heat-treated Xanthan gum.sup.5 -- -- -- 1.0 -- Heat-treated
Xanthan gum.sup.6 -- -- -- -- 1.0 Deionized Water q.s. q.s. q.s.
q.s. q.s. Preservative q.s. q.s. q.s. q.s. q.s. 100 100 100 100 100
.sup.1Balance 0/55 (National Starch and Chemical Co.)
.sup.2Heat-treated Keltrol T (Fluid bed reactor at 220.degree. F.
for 240 minutes) .sup.3Heat-treated Keltrol T (Fluid bed reactor at
220.degree. F. for 150 minutes) .sup.4Heat-treated Keltrol T (Fluid
bed reactor at 228.degree. F. for 90 minutes) .sup.5Heat-treated
Keltrol T (Fluid bed reactor at 235.degree. F. for 30 minutes)
.sup.6Heat-treated Keltrol T (oven at 250.degree. F. for 120
minutes)
[0034] Formulas 26-30 show hair gels using xanthan gum samples that
are heat-treated under different conditions.
7 Formula 31 Formula 32 Formula 33 Formula 34 Formula 35
Ingredients % w/w % w/w % w/w % w/w % w/w Part A Poly (N-vinyl
acetamide) 3.0 1.0 -- -- -- Poly (N-vinyl formamide) -- -- 3.0 --
-- Polyurethane -- -- -- 3.0 -- Corn Starch Modified.sup.1 -- -- --
-- 1.0 Deionized Water 40.0 40.0 40.0 40.0 40.0 Part B Heat-treated
Xanthan gum.sup.2 1.0 1.0 1.0 1.0 1.0 Deionized Water q.s. q.s.
q.s. q.s. q.s. Preservative q.s. q.s. q.s. q.s. q.s. 100 100 100
100 100 .sup.1Amaze (National Starch and Chemical Co.)
.sup.2Heat-treated Keltrol T (Fluid bed reactor at 235.degree. F.
for 60 minutes)
[0035] These examples show hair gels made with heat-treated xanthan
gum and various fixative polymers at different use levels.
8 Formula 36 Formula 37 Ingredients % w/w % w/w Part A
Polyquaternium-4.sup.1 0.15 -- Polyquaternium-10.sup.2 -- 0.15
Deionized Water 40.0 40.0 Part B Heat-treated Xanthan gum.sup.3 1.0
1.0 Deionized Water q.s. q.s. Preservative q.s. q.s. 100 100
.sup.1Celquat H-100 or L-200 (National Starch and Chemical Co.)
.sup.1Celquat SC-230M or Celquat SC-240C (National Starch and
Chemical Co.) .sup.2Heat-treated Keltrol T (Fluid bed reactor at
235.degree. F. for 60 minutes)
[0036] These formulas show that cationic fixative/conditioning
polymers can be used at lower levels with heat-treated xanthan gum
to produce clear hair gels with good performance and rheology.
9 Formula Formula Formula Formula 38 39 40 41 Ingredients % w/w %
w/w % w/w % w/w Part A Gellan Gum.sup.1 0.3 0.3 -- --
Carbomer.sup.2 -- -- 0.1 0.3 Deionized Water 40.0 40.0 40.0 40.0
Aminomethyl Propanol.sup.3 -- -- q.s. to q.s. to pH 6 pH 6 Part B
Heat-treated Xanthan gum.sup.4 1.0 -- 1.0 -- Xanthan gum.sup.5 --
1.0 -- 1.0 Deionized Water q.s. q.s. q.s. q.s. Preservative q.s.
q.s. q.s. q.s. 100 100 100 100 .sup.1Kelcogel (Kelco)
.sup.2Carbopol 940 (BF Goodrich) .sup.3AMP-95 (Angus)
.sup.4Heat-treated Keltrol T (Fluid bed reactor at 235.degree. F.
for 60 minutes) .sup.5Keltrol T (Kelco)
[0037] Formulas 38-41 demonstrate that hair gels can be made by
combining xanthan or heat-treated xanthan gum with other rheology
modifiers/thickeners, such as Gellan gum or carbomer.
Example 3
Hair Styling Gel Performance (I) and Curl Retention
[0038] The curl retention properties of the hair styling
compositions of the present invention were measured and compared to
those of three leading commercial hair styling gel compositions
with "ultimate" hair holding power. It is known to one skilled in
the art that curl retention correlates directly to hair style
retention, or hold, which is one of the most important performance
attribute for a hair styling product. The test was conducted at
72.degree. F. (22.degree. C.) and 90% Relative Humidity over a
period of 2 hours. The procedure allows for statistical analysis of
formulation variables. The percentage curl retention was calculated
by: Curl Retention %=100.times.(L-L.sub.t)/(L-L.sub.o). where
L=iength of hair fully extended, L.sub.o=initial curl length,
L.sub.t=curl length at a givin time t.
[0039] The test was performed on 10" long.times.2 gram tresses of
European virgin brown hair (9 replicate tresses per sample).
Cleaned wet hair tresses were combed through to remove tangles and
excess water is removed. 0.5 gram of sample hair gel was applied to
each tress, gently "worked into" the hair tress and combed through.
Curls of hair were made using 1/2" diameter Teflon mandrel, placed
on a tray and dried in an oven overnight. The dried curls were
removed from the oven and allowed to cool to room temperature. The
curls were suspended from the bound end of the tress on graduated
transparent curl retention boards. An initial curl length reading
was taken before placing boards and curls into the environment
chamber. Then curl lengths were recorded at 15 minutes, 30 minutes,
60 minutes, 90 minutes and 2 hours. Curl retention averages were
then calculated.
[0040] The curl retention results after 2 hours are tabulated in
Table 1. The results demonstrate that all the hair styling
compositions containing xanthan gum, particularly heat-treated
xanthan gum, exhibited dramatically superior curl retention
compared to the leading commercial products. This superior curl
retention property was achieved with and without other fixative
polymers. The type and amount of additional fixative polymers did
not vary the curl retention capability significantly with xanthan
or heat-treated xanthan gum present. Significantly lower curl
retention results were obtained when carbomer is used in the
composition instead of xanthan gum, particularly heat-treated
xanthan gum.
10TABLE 1 Average % Curl Retention Time = 2 hours Hair Styling Gel
Compositions T = 72.degree. F.; RH = 90% 1% heat-treated xanthan
gum (Formula 13) 91 2% heat-treated xanthan gum (Formula 12) 93 4%
Acrylates Copolymer + 93 1% heat-treated xanthan gum (Formula 21)
4% Acrylates Copolymer + 91 1% untreated xanthan gum (Formula 23)
2% Acrylates Copolymer + 89 1% heat-treated xanthan gum (Formula
22) 3% PVP + 95 1% heat-treated xanthan gum (Formula 18) 4% PVP +
84 1% heat-treated xanthan gum (Formula 17) 4% PVP + 48 0.5%
Carbomer (Formula 16) 3% Poly (N-vinyl acetamide) + 93 1%
heat-treated xanthan gum (Formula 31) 1% Poly (N-vinyl acetamide) +
91 1% heat-treated xanthan gum (Formula 32) Commercial hair gel I
(containing PVP, 34 carbomer, and other additives) Commercial hair
gel II (containing PVP/VA 47 copolymer, carbomer, and other
additives) Commercial hair gel III (containing PVP/VA 11 copolymer,
PVP, carbomer, and other additives)
Example 4
Hair Styling Gel Performance, Stiffness and Other Attributes
[0041] Test 1--Subjective evaluation of hair styling compositions
containing heat-treated xanthan gum compositions containing PVP and
carbomer. European dark brown hair tresses panelists (10"long, 2
grams weight) with 0.5 grams of the hair styling composition were
each rated by eight panelists by giving the samples a score of 1
(worst) to 5 (best) for a variety of properties. The performance
attributes tested included stiffness, wet feel, wet comb, dry
gloss, dry feel, dry comb, dry flake, and anti-static. Stiffness is
used to describe the hardness of hair body, which is also a measure
of the amount of hold produced by hair styling compositions. This
and similar types of sensory tests are well known by those in the
art for the performance assessment of personal care and cosmetic
products. A summary of the test results is shown in Table 2.
[0042] The overall performance of the hair compositions containing
heat-treated xanthan gum was better or comparable to a PVP/carbomer
hair gel in stiffness, gloss, dry comb, wet comb, flake,
anti-static, and feel. All of the heat-treated xanthan gum
containing gels provided better stiffness than the PVP/carbomer gel
with the same amount of additional fixative polymers. Formula 1
also provided improved wet feel, wet comb, dry feel, and dry comb
comparing to the PVP/carbomer gel.
11TABLE 2 Results of Subjective Test 1 Average score based on 1
(worst) to 5 (best) rating scale Formula 7 Attribute Formula 3
Formula 4 Formula 5 (control) wet feel 3.8 S 2.7 NS 2.8 NS 2.8 wet
comb 3.8 S 2.5 NS 2.6 NS 2.9 dry gloss 3.4 NS 2.7 NS 3.1 NS 3.2
Stiffness 3.8 S 3.6 S 3.6 S 2.3 dry comb 3.9 S 2.8 NS 2.7 NS 3.2
dry flake 2.8 NS 3.0 NS 3.1 NS 3.2 anti-static 1.9 NS 2.1 NS 2.2 NS
2.1 dry feel 3.4 S 2.9 NS 2.7 NS 2.7 S = differences in performance
between the sample and the control are regarded as being
statistically significant at the 95% confidence level NS = no
differences in performance between the sample and the control are
regarded as being statistically significant at the 95% confidence
level
[0043] Test 2
[0044] Subjective ranking of six hair styling compositions and
three leading commercial hair styling gels was performed on human
hair tresses for the performance attributes of stiffness, gloss,
and dry flake. This sensory evaluation used a Balanced Incomplete
Block Design, with which ranking is based on the intensity of
attributes. Nine samples were ranked in groups of two by nine
panelists. For each pair of samples, a score of 1 was given for
less stiffness, more dry flake, and less gloss, and a score of 2
was given for more stiffness, less dry flake, and more gloss. Based
on the design, a total of 36 blocks (or pairs) of samples were
prepared. The ranking sum of each attribute for each sample was
calculated. Rank sums that differed by more than the least
significant difference (LSD=3.5) indicates samples which differed
by more than 90% of what we would expect from guessing or random
stimuli alone. The hair tress preparation procedure was the same
with that used in subjective Test 1. A summary of the test results
is shown in Table 3. The higher rank run value indicates better
performance on each attribute. The differences in rank sum that
were less than LSD (3.5) are considered as no significant
difference at 90% confidence level. This ranking test was designed
for showing trends or patterns among the samples, but not
particularly for the comparison of samples in pairs. Compared to
the leading commercial gels, hair compositions containing xanthan
gum, particularly heat-treated xanthan gum showed equivalent or
better stiffness, gloss, and flake attributes.
12TABLE 3 Results of Subjective Test 2 Rank Sums (LSD = 3.5) Hair
Styling Gel Compositions Stiffness Gloss Flake Commercial hair gel
I (containing PVP, 12 11 12 carbomer, and other additives)
Commercial hair gel II (containing PVP/VA 11 12 12 copolymer,
carbomer, and other additives) Commercial hair gel III (containing
PVP/VA 8 12 9 copolymer, PVP, carbomer, and other additives) 4% PVP
+ 0.5% Carbomer (Formula 16) 15 9 10 4% PVP + 15 13 11 1%
heat-treated xanthan gum (Formula 17) 4% Acrylates Copolymer + 11
11 15 1% heat-treated xanthan gum (Formula 21) 1% heat-treated
xanthan gum (Formula 13) 11 15 13 2% Acrylates Copolymer + 12 12 14
1% heat-treated xanthan gum (Formula 22) 4% Acrylates Copolymer +
13 13 12 1% untreated xanthan gum (Formula 23)
Example 5
Measurement of Gel Texture
[0045] A Rheometrics DSR SR-200 controlled stress rheometer was
used for all measurements. The crossover strain was obtained from
an oscillatory shear stress sweep run at a frequency of 1 rad/s,
from a stress of 2 to 1000 Pa at 25C. The tangent of the phase
angle, tandelta was plotted versus the strain amplitude and the
crossover strain was defined as the strain at which the tand=1.
This method was applied only to materials which had values of
tandelta<1 at low stresses and which then broke down and had
values greater than 1 at high stresses. The crossover strain was
typically low for materials with short texture and high for
materials with long, cohesive, or stringy textures. The crossover
strain data for selected hair gels is in Table 4. The shortness of
a leading commercial hair gel containing Carbomer and PVP was also
measured as a comparison. Good agreement between the crossover
strain data and subjective assessment of the gel texture has been
found. As shown in Table 4, the shortness of xanthan gel depended
on the degree of heat treatment. The untreated xanthan gum gave
more stringy and longer gel texture. The higher treatment
temperature and/or longer treatment time tended to give shorter,
less stringy gel texture. When appropriate heat treatment
conditions were selected, one obtained significantly improved
shorter gel texture, which was close to the most commonly used
Carbomer gel (a polyacrylic acid thickener).
13TABLE 4 Hair Styling Gel Compositions Crossover Strain (%) 4%
Acrylates Copolymer + 155 1% untreated xanthan gum (Formula 23) 4%
Acrylates Copolymer + 131 1% heat-treated xanthan gum (fluid bed
@220.degree. F. for 120 minutes) 4% Acrylates Copolymer + 88 1%
heat-treated xanthan gum (fluid bed @220.degree. F. for 150
minutes) 4% Acrylates Copolymer + 150 1% heat-treated xanthan gum
(fluid bed @228.degree. F. for 60 minutes) 4% Acrylates Copolymer +
120 1% heat-treated xanthan gum (fluid bed @228.degree. F. for 90
minutes) 4% Acrylates Copolymer + 96 1% heat-treated xanthan gum
(fluid bed @235.degree. F. for 60 minutes) 1% heat-treated xanthan
gum (fluid bed 82 @235.degree. F. for 60 minutes) Commercial hair
gel (containing PVP, 73 carbomer, and other additives)
Example 6
Clarity Measurement of Hair Gels
[0046] The clarity of hair gels were measured by using Hach
Laboratory Turbidimeter (Model 2100N). The instrument is designed
for measurement of turbidity from 0 to 4000NTU (Nephelometric
Turbidity Units) with automatic range selection and decimal point
placement. Low turbidity reading represents high clarity. The
turbidity values of clear to translucent hair gels containing
xanthan gum and heat-treated xanthan gum are listed in Table 5. The
turbidity values of three clear commercial hair gels are also
listed as a reference.
14TABLE 5 Hair Styling Gel Compositions Turbidity (NTU) 4%
Acrylates Copolymer + 18.5 1% untreated xanthan gum (Formula 19) 4%
Acrylates Copolymer + 24.2 1% heat-treated xanthan gum (fluid bed
@220.degree. F. for 120 minutes) 4% Acrylates Copolymer + 25.2 1%
heat-treated xanthan gum (fluid bed @220.degree. F. for 150
minutes) 4% Acrylates Copolymer + 23.7 1% heat-treated xanthan gum
(fluid bed @228.degree. F. for 60 minutes) 4% Acrylates Copolymer +
24.5 1% heat-treated xanthan gum (fluid bed @228.degree. F. for 90
minutes) 4% Acrylates Copolymer + 25.3 1% heat-treated xanthan gum
(fluid bed @235.degree. F. for 60 minutes) 1% heat-treated xanthan
gum (fluid bed 24.2 @235.degree. F. for 60 minutes) Commercial hair
gel (containing PVP, PVP/VA, 15.0 carbomer, and other additives)
Commercial hair gel (containing PVP, 14.0 carbomer, and other
additives) Commercial hair gel (containing PVP, 10.9 carbomer, and
other additives) Deionized water 0.04
Example 7
Hair Spray Gel with Xanthan Gum
[0047]
15 Ingredients % w/w % w/w Part A Acrylates Copolymer.sup.1 (50%)
8.0 8.0. D.I. Water 40.0 40.0 Aminomethyl Propanol.sup.2 0.56 0.56
Part B Xanthan gum.sup.3 0.5 -- Heat-treated Xanthan gum.sup.4 --
0.3 Deionized Water q.s. q.s. Preservative q.s. q.s. Part C Keratin
Protein 0.2 0.2 Propylene Glycol 2.0 2.0 Polysorbate 20.sup.4 0.5
0.5 Fragrance 0.1 0.1 .sup.1Balance 0/55 (National Starch and
Chemical Co.) .sup.2AMP-95 (Angus) .sup.3Keltrol T (Kelco)
.sup.4Heat-treated Keltrol T (Fluid bed reactor at 235.degree. F.
for 60 minutes) .sup.5Tween 20 (ICI Surfactants)
Example 8
Surfactant-Free Hair Mousse with Xanthan Gum
[0048]
16 Ingredients % w/w Acrylates Copolymer.sup.1 (50%) 8.0 D.I. Water
40.0 Aminomethyl Propanol.sup.2 0.56 Xanthan gum.sup.3 0.4
Deionized Water q.s. Preservative q.s. Part C
Isobutane/Propane.sup.4 6.0 100 .sup.1Balance 0/55 (National Starch
and Chemical Co.) .sup.2AMP-95 (Angus) .sup.3Keltrol T (Kelco)
.sup.4Propellant A-46
Example 9
Styling Mousse
[0049]
17 Ingredients % w/w Sodium Polystyrene Sulfonate.sup.1 10.0
Polysorbate 20.sup.2 0.4 Nonoxynol-15.sup.3 0.4 Oleth-10.sup.4 0.4
Xanthan gum.sup.5 0.5 Deionized Water 68.3 SD Alcohol 40 10.0
Isobutane 10.0 100 .sup.1Flexan 130 (National Starch and Chemical
Co.) .sup.2Tween 20 (Uniqema) .sup.3Tergitol NP-15 (Uniqema)
.sup.4Brij 97 (Uniqema) .sup.5Keltrol T (Kelko)
Example 10
Aerosol Hair Spray
[0050]
18 Ingredients % w/w Octylacrylamide/Acrylates/ 8.0 Butylaminoethyl
Methacrylate Copolymer.sup.1 Aminomethyl Propanol.sup.2 1.38
Xanthan gum.sup.3 0.3 Deionized Water 45.32 SD Alcohol 40 20.0
Fragrance q.s. Preservative q.s. Dimethyl Ether 25.0 100
.sup.1Balance 47 (National Starch and Chemical Co.) .sup.2AMP
(Angus) .sup.3Keltrol T (Kelko)
Example 11
Hair Styling and Conditioning Cream
[0051]
19 Ingredients % w/w Part A Deionized Water q.s. Heat-treated
xanthan gum.sup.1 0.7 Quaternium-4.sup.2 0.15 Part B Glyceryl
Stearate.sup.3 2.0 Jojoba oil 2.0 Part C Fragrance q.s.
Preservative g.s. 100 .sup.1Heat-treated Keltrol T (Fluid bed
reactor at 235.degree. F. for 60 minutes) .sup.2Celquat H-100
(National Starch and Chemical Co.) .sup.3Cerasynt SD (ISP)
* * * * *