U.S. patent application number 15/630411 was filed with the patent office on 2018-01-04 for shampoo compositions comprising a chelant.
The applicant listed for this patent is The Procter & Gamble Company. Invention is credited to Casey Patrick Kelly, Jennifer Mary MARSH, Mark Robert Sivik.
Application Number | 20180000705 15/630411 |
Document ID | / |
Family ID | 59270174 |
Filed Date | 2018-01-04 |
United States Patent
Application |
20180000705 |
Kind Code |
A1 |
MARSH; Jennifer Mary ; et
al. |
January 4, 2018 |
Shampoo Compositions Comprising a Chelant
Abstract
Described herein is a shampoo composition and methods of using
the same, the shampoo composition including a copper chelant, a
detersive surfactant, and a carrier.
Inventors: |
MARSH; Jennifer Mary;
(Deerfield Twp., OH) ; Kelly; Casey Patrick;
(Wyoming, OH) ; Sivik; Mark Robert; (Mason,
OH) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
The Procter & Gamble Company |
Cincinnati |
OH |
US |
|
|
Family ID: |
59270174 |
Appl. No.: |
15/630411 |
Filed: |
June 22, 2017 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
62356943 |
Jun 30, 2016 |
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Current U.S.
Class: |
1/1 |
Current CPC
Class: |
A61Q 5/002 20130101;
A61K 8/41 20130101; A61K 8/44 20130101; A61K 2800/51 20130101; A61K
2800/596 20130101; A61K 2800/5922 20130101; A61Q 5/02 20130101;
A61K 8/463 20130101 |
International
Class: |
A61K 8/41 20060101
A61K008/41; A61Q 5/02 20060101 A61Q005/02; A61K 8/44 20060101
A61K008/44; A61K 8/46 20060101 A61K008/46; A61Q 5/00 20060101
A61Q005/00 |
Claims
1. A shampoo composition comprising: (a) from about 0.005% to about
5% of one or more chelants, by weight of the shampoo composition,
wherein the one or more chelants have a molecular structure as
follows: ##STR00008## wherein n is 2 or 3; m is 1, 2, 3, or 4; and
Y and Z are independently selected from the group consisting of
hydrogen, methyl, ethyl, propyl, butyl, pentyl,
--CH.sub.2CH.sub.2OH, --CH.sub.2CH(CH.sub.3)OH),
--CH.sub.2CH.sub.2NH.sub.2, --CH.sub.2CH(CH.sub.3)NH.sub.2, and
combinations thereof; and wherein the one or more chelants
comprise: (1) log of the formation constant log K.sub.ML of its
complex with copper is higher than 6; (2) log P value is from about
-5 to about 2; and (3) molecular weight of from about 50 to about
500; (b) from about 2% to about 50% of one or more detersive
surfactants, by weight of the shampoo composition; and (c) from
about 75% to about 98% of an aqueous carrier, by weight of the
shampoo composition; wherein the shampoo composition has a pH of
about 3 to about 8.
2. The shampoo composition of claim 1, wherein the detersive
surfactant is selected from the group consisting of anionic
surfactants, cationic surfactants, non-ionic surfactants,
amphoteric surfactants, and mixtures thereof.
3. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 5% to about 25% of the detersive
surfactant by weight of the shampoo composition.
4. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 7% to about 22% of the detersive
surfactant by weight of the shampoo composition.
5. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 9% to about 18% of the detersive
surfactant by weight of the shampoo composition.
6. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 11% to about 15% of the detersive
surfactant by weight of the shampoo composition.
7. The shampoo composition of claim 1, wherein the log P value of
the one or more chelants is from about -4 to about 1.
8. The shampoo composition of claim 1, wherein the log P value of
the one or more chelants is from about -3 to about 0.
9. The shampoo composition of claim 1, wherein the molecular weight
of the one or more chelants is from about 75 to about 400.
10. The shampoo composition of claim 1, wherein the molecular
weight of the one or more chelants is from about 100 to about
350.
11. The shampoo composition of claim 1, wherein the molecular
weight of the one or more chelants is from about 125 to about
325.
12. The shampoo composition of claim 1, wherein the molecular
weight of the one or more chelants is from about 140 to about
300.
13. The shampoo composition of claim 1, further comprising a gel
network, wherein the gel network comprises a fatty alcohol and a
surfactant.
14. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 0.01% to about 3% of the one or
more chelants.
15. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 0.01% to about 1% of the one or
more chelants.
16. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 0.01% to about 0.5% of the one or
more chelants.
17. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 0.01% to about 0.1% of the one or
more chelants.
18. The shampoo composition of claim 1, wherein the shampoo
composition comprises from about 0.025% to about 0.05% of the one
or more chelants.
19. The shampoo composition of claim 1, wherein the one or more
chelants are selected from the group consisting of
2,3-triethylenetetramine, tetraethylenepentamine,
2,4-tetraethylenepentamine, pentaethylenehexamine,
tris(2-aminoethyl)amine, ethylenedinitrilotetrapropan-2-ol,
1,1',1'',1'''
[(2-hydroxypropyl)imino]bis(2,1ethanediylnitrilo)]tetrakis-2-propanol,
tetraethylenepentaamine-(1-EO), 1,5,9,13-Tetraazatridecane, and
mixtures thereof.
20. A method of inhibiting copper deposition on hair and
facilitating the removal of copper deposited on hair comprising: a.
applying to the hair the shampoo composition of claim 1; and b.
rinsing the shampoo composition from the hair.
Description
FIELD OF THE INVENTION
[0001] Described herein are shampoo compositions comprising a
detersive surfactant, a chelant, and a carrier, wherein the shampoo
composition inhibits both deposition/penetration of copper salts
and other transition metal salts in the hair and removes such salts
from hair fiber. A method of cleansing hair with such shampoo
compositions is also described herein.
BACKGROUND OF THE INVENTION
[0002] Many water sources that are used by consumers for personal
care contain elevated levels of calcium and magnesium salts, as
well as undesirable levels of redox metals (e.g., copper and/or
iron) salts. As such, using chelants to sequester trace redox
metals often proves to be ineffective because most chelants also
competitively bind calcium and/or magnesium.
[0003] It has been found that even trace quantities of copper can
deposit on the hair surface and in between the cuticle layers of
hair. This deposition of copper on hair is especially problematic
because transition metal ions, such as copper and iron, can
facilitate reduction-oxidation (redox) reactions during hair
coloring treatments and during UV exposure. These reactions
generate reactive oxygen species (ROS), which in turn can cause
damage to the hair. In addition, they can interfere with the
oxidative color formation chemistry and lead to reduced color
uptake for hair colorant users.
[0004] Accordingly, there is a need for improved shampoo
compositions that can inhibit copper depositing on hair, as well as
facilitate the removal of copper already deposited thereon.
SUMMARY OF THE INVENTION
[0005] Described herein is a shampoo composition comprising: [0006]
(a) from about 0.005% to about 5% of one or more chelants, by
weight of the shampoo composition, wherein the one or more chelants
have a molecular structure as follows:
[0006] ##STR00001## [0007] wherein n is 2 or 3; m is 1, 2, 3, or 4;
and [0008] Y and Z are independently selected from the group
consisting of hydrogen, methyl, ethyl, propyl, butyl, pentyl,
--CH.sub.2CH.sub.2OH, --CH.sub.2CH(CH.sub.3)OH),
--CH.sub.2CH.sub.2NH.sub.2, --CH.sub.2CH(CH.sub.3)NH.sub.2, and
combinations thereof; [0009] and wherein the one or more chelants
comprise: [0010] (1) log of the formation constant log K.sub.ML of
its complex with copper is higher than 6; [0011] (2) log P value is
from about -5 to about 2; and [0012] (3) molecular weight of from
about 50 to about 500; [0013] (b) from about 2% to about 50% of one
or more detersive surfactants, by weight of the shampoo
composition; and [0014] (c) from about 75% to about 98% of an
aqueous carrier, by weight of the shampoo composition; wherein the
shampoo composition has a pH of about 3 to about 8.
DETAILED DESCRIPTION OF THE INVENTION
[0015] While the specification concludes with claims particularly
pointing out and distinctly claiming the invention, it is believed
that the shampoo composition described herein will be better
understood from the following description.
[0016] As used herein, the term "fluid" includes liquids and
gels.
[0017] As used herein, the term "log x" refers to the common (or
decadic) logarithm of x.
[0018] As used herein, the articles including "a" and "an" when
used in a claim, are understood to mean one or more of what is
claimed or described.
[0019] All percentages are by weight of the total composition,
unless stated otherwise. All ratios are weight ratios, unless
specifically stated otherwise. All ranges are inclusive and
combinable. The number of significant digits conveys neither a
limitation on the indicated amounts nor on the accuracy of the
measurements. The term "molecular weight" or "M.Wt." as used herein
refers to the weight average molecular weight unless otherwise
stated. "QS" means sufficient quantity for 100%.
[0020] As used herein, "mixtures" is meant to include a simple
combination of materials and any compounds that may result from
their combination.
[0021] All numerical amounts are understood to be modified by the
word "about" unless otherwise specifically indicated. Unless
otherwise indicated, all measurements are understood to be made at
25.degree. C. and at ambient conditions, where "ambient conditions"
means conditions under about one atmosphere of pressure and at
about 50% relative humidity. All such weights percents (wt %) as
they pertain to listed ingredients are based on the active level
and do not include carriers or by-products that may be included in
commercially available materials, unless otherwise specified.
[0022] Unless otherwise noted, all component or composition levels
are in reference to the active portion of that component or
composition, and are exclusive of impurities, for example, residual
solvents or by-products, which may be present in commercially
available sources of such components or compositions.
[0023] Herein, "comprising" means that other steps and other
ingredients which do not affect the end result can be added. This
term encompasses the terms "consisting of" and "consisting
essentially of". The compositions, methods, uses, kits, and
processes of the shampoo composition described herein can comprise,
consist of, and consist essentially of the elements and limitations
of the invention described herein, as well as any of the additional
or optional ingredients, components, steps, or limitations
described herein. As used herein, the terms "include," "includes,"
and "including," are meant to be non-limiting and are understood to
mean "comprise," "comprises," and "comprising," respectively.
[0024] The term "substantially free from" or "substantially free
of" as used herein means less than about 1%, or less than about
0.8%, or less than about 0.5%, or less than about 0.3%, or about
0%, by total weight of the composition.
[0025] "Hair," as used herein, means mammalian hair including scalp
hair, facial hair and body hair, particularly on hair on the human
head and scalp.
[0026] "Cosmetically acceptable," as used herein, means that the
compositions, formulations or components described are suitable for
use in contact with human keratinous tissue without undue toxicity,
incompatibility, instability, allergic response, and the like. All
compositions described herein which have the purpose of being
directly applied to keratinous tissue are limited to those being
cosmetically acceptable.
[0027] "Derivatives," as used herein, includes but is not limited
to, amide, ether, ester, amino, carboxyl, acetyl, acid, and/or
alcohol derivatives of a given compound.
[0028] "Polymer," as used herein, means a chemical formed from the
polymerisation of two or more monomers, which may be the same or
different. The term "polymer" as used herein shall include all
materials made by the polymerisation of monomers as well as natural
polymers. Polymers made from only one type of monomer are called
homopolymers. A polymer comprises at least two monomers. Polymers
made from two or more different types of monomers are called
copolymers. The distribution of the different monomers can be
calculated statistically or block-wise--both possibilities are
suitable for the shampoo composition. Except if stated otherwise,
the term "polymer" used herein includes any type of polymer
including homopolymers and copolymers.
[0029] The term "charge density" as used herein, means the ratio of
the number of positive charges on a monomeric unit of which a
polymer is comprised to the M.Wt. of said monomeric unit. The
charge density multiplied by the polymer M.Wt. determines the
number of positively charged sites on a given polymer chain. For
cationic guars, charge density is measured using standard elemental
analysis of percentage nitrogen known to one skilled in the art.
This value of percentage nitrogen, corrected for total protein
analysis, can then be used to calculate the number or equivalence
of positive charges per gram of polymer. For the cationic
copolymers, the charge density is a function of the monomers used
in the synthesis. Standard NMR techniques know to one skilled in
the art would be used to confirm that ratio of cationic and
non-ionic monomers in the polymer. This would then be used to
calculate the number or equivalence of positive charges per gram of
polymer. Once these values are know, the charge density is reported
in milliequivalence (meq) per gram of cationic polymer.
[0030] The term log P is the n-octanol/water partition coefficients
of the material.
[0031] All percentages, parts and ratios are based upon the total
weight of the compositions of the present invention, unless
otherwise specified. All such weights as they pertain to listed
ingredients are based on the active level and, therefore, do not
include carriers or by-products that may be included in
commercially available materials.
[0032] Unless otherwise noted, all component or composition levels
are in reference to the active portion of that component or
composition, and are exclusive of impurities, for example, residual
solvents or by-products, which may be present in commercially
available sources of such components or compositions.
[0033] It should be understood that every maximum numerical
limitation given throughout this specification includes every lower
numerical limitation, as if such lower numerical limitations were
expressly written herein. Every minimum numerical limitation given
throughout this specification will include every higher numerical
limitation, as if such higher numerical limitations were expressly
written herein. Every numerical range given throughout this
specification will include every narrower numerical range that
falls within such broader numerical range, as if such narrower
numerical ranges were all expressly written herein.
Shampoo Composition
[0034] Described herein is a shampoo composition comprising (a)
from about 0.005% to about 5% of one or more chelants; (b) from
about 2% to about 50% of one or more detersive surfactants, by
weight of the shampoo composition; (c) from about 75% to about 98%
of an aqueous carrier, by weight of the shampoo composition,
wherein the shampoo composition has a pH of about 3 to about 8, and
wherein the shampoo inhibits copper deposition on hair and
facilitates the removal of copper deposited on hair. The shampoo
composition also delivers consumer desired shampooing in addition
to inhibiting the deposition of copper (i.e. from the water used to
rinse) on the hair.
[0035] A. Chelants
[0036] The shampoo composition comprises from about 0.005% to about
5%, alternatively from about 0.01% to about 3%, alternatively from
about 0.01% to about 1%, alternatively from about 0.01% to about
0.5%, alternatively from about 0.01% to about 0.1%, and
alternatively from about 0.025% to about 0.05% of one or more
chelants by weight of the shampoo composition, wherein the one or
more chelants have a molecular structure as follows:
##STR00002## [0037] wherein n is 2 or 3; m is 1, 2, 3, or 4; and
[0038] Y and Z are independently selected from the group consisting
of hydrogen, methyl, ethyl, propyl, butyl, pentyl,
--CH.sub.2CH.sub.2OH, --CH.sub.2CH(CH.sub.3)OH),
--CH.sub.2CH.sub.2NH.sub.2, --CH.sub.2CH(CH.sub.3)NH.sub.2, and
combinations thereof; [0039] and wherein the one or more chelants
comprise: [0040] (1) log of the formation constant log K.sub.ML of
its complex with copper is higher than 6; [0041] (2) log P value is
from about -5 to about 2; and [0042] (3) molecular weight of from
about 50 to about 500.
Stability Constants of Exemplary Chelants
[0043] The relative affinity of a chelant at a specified pH for
Cu.sup.+2 can be assessed by its Stability Constant. The Stability
Constant of a metal chelant interaction is defined as:
K ML = [ ML ] [ M ] [ L ] ##EQU00001##
where: [ML] is the concentration of metal ligand complex at
equilibrium; [M] is the concentration of free metal ion; [L] is the
concentration of free ligand in a fully deprotonated form; and
K.sub.ML is the stability constant for the metal chelant
complex.
[0044] The stability constants of chelant-metal ion complexes are
well documented in the literature for commonly used chelants (see,
for example, Arthur Martell & Robert M Smith, Critically
Selected Stability Constants of Metal Complexes Database, Version
3.0 and above, incorporated herein by reference). When not
documented the constants can be measured using various analytical
methods (see "Metal Complexes in Aqueous Solutions", Martel and
Hancock, edition Modem Inorganic Chemistry, p. 226-228,
incorporated herein by reference).
[0045] It has been found that effective chelants need to have a
high affinity for copper in order to preferentially bind copper
found in hair. However, it has been found that also important to
efficacy is the ability for the chelant to penetrate inside the
hair fibers rapidly during the shampoo lathering process (which
typically lasts between 30 seconds and 1 minute). The copper to be
removed is inside the hair and the chelant needs to penetrate
inside hair and form a strong copper-chelant complex. This
copper-chelant complex needs to be water soluble and thus easily
removed during the rinsing process. To be able to do this, two
additional parameters have been shown to be important for chelant
efficacy. These are log P, the octanol/water partitioning
coefficient, and the molecular weight of the chelant. Both are
related to the ability of the chelant to penetrate into hair and
also form a water soluble copper-chelant complex
[0046] The one or more chelants for use in the shampoo composition
may be selected from the group consisting of triethylenetetramine,
tetraethylenepenatmine, pentaethylenehexamine,
tris(2-aminoethyl)amine, ethylenedinitrilotetrapropan-2-ol,
1,1',1''-[[2-hydroxypropyl)imino]bis(2,1-ethanediylnitrilo)]tetrakis-2-pr-
opanol, tetraethylenepentaamine-(1-EO), 1,5,9,13-tetraazatridecane,
and mixtures thereof.
##STR00003## ##STR00004##
[0047] Table 1 provides relevant properties and performance of the
one or more copper chelants described herein. Details on
determination of copper removing performance is described in the
Examples section.
TABLE-US-00001 TABLE 1 Properties of representative chelants Copper
Removing Log Performance K.sub.ML Log Chelant from Shampoo Cu P MW
2,3-Triethylenetetramine (TETA) 70% 20.1 -2.3 146
2,4-Tetraethylenepentamine 60% 22.8 -2.7 189 (TEPA)
Pentaethylenehexamine (PEHA) 55% -3.1 232 Tris(2-aminoethyl)amine
(tren) 45% 18.8 -2.2 146 Ethylenedinitrilotetrapropan-2-ol 30% 9.8
-0.2 292 (EDTP) 1,1,1'',1'''[(2- No data -0.2 394
hydroxypropyl)imino] bis(2,1- collected
ethanediylnitrilo)]tetrakis-2- Propanol (Pentrol)
Tetraethylenepentaamine-(1-EO) No data -2.9 498 collected
1,5,9,13-Tetraazatridecane 15% 17.1 -2.1 188 (Thermine)
[0048] The log of the formation constant log K.sub.ML of its
complex with copper can be higher than 6, alternatively higher than
8, alternatively higher than 9, alternatively higher than 10,
alternatively higher than 12, alternatively higher than 14,
alternatively higher than 16, alternatively higher than 17,
alternatively higher than 18, and alternatively higher than 20. The
log of the formation constant log K.sub.ML of its complex with
copper can be from about 6 to about 28, alternatively from about 8
to about 27, alternatively from about 9 to about 26, alternatively
from about 10 to about 25, alternatively from about 12 to about 24,
alternatively from about 14 to about 24, alternatively from about
16 to about 24, alternatively from about 17 to about 24,
alternatively from about 18 to about 24, and alternatively from
about 20 to about 23.
[0049] The log P value of the one or more chelants can be from
about -5 to about 2, alternatively from about -4 to about 1,
alternatively from about -3.5 to about 0, and alternatively from
about -2.9 to about -2.5.
[0050] The molecular weight of the one or more chelants can be from
about 50 to about 500, alternatively from about 75 to about 400,
alternatively from about 100 to about 350, alternatively from about
125 to about 325, alternatively from about 140 to about 300,
alternatively from about 140 to about 200.
[0051] The copper removing performance of the shampoo composition
is determined by treating hair with clarifying shampoo containing
the corresponding chelant for 20 cycles and comparing the copper
content of the hair compared to the same treatment using shampoo
without the chelant.
[0052] Other chelants that can be used to reduce copper content of
hair have the following general structure:
##STR00005##
wherein M is hydrogen or a metal ion; p is 1 or 2; q is 1 or 2; and
X is selected from the group containing hydrogen, methyl, ethyl,
propyl, --CH.sub.2CH.sub.2OH, --CH.sub.2CH(CH.sub.3)OH),
--CH.sub.2CH.sub.2NH.sub.2, --CH.sub.2CH(CH.sub.3)NH.sub.2,
--CH.sub.2COOM, or --CH.sub.2CH.sub.2SH, and
--CH.sub.2CH(CH.sub.3)SH).
[0053] Non-limiting examples include iminodiacetic acid,
N-(2-hydroxyethyl)iminodiacetic acid, N-methyliminodiacetic acid,
N-(2-aminoethyl)iminodiacetic acid, N-propyliminodiacetic acid, and
nitrilotriacetic acid.
##STR00006##
[0054] It is found that treatment with shampoo composition
containing 0.1 wt % iminodiacetic acid reduces copper by 40% and
shampoo composition containing 0.1 wt %
N-(2-hydroxyethyl)iminodiacetic acid reduces copper by 30% after 20
cleaning cycles compared to comparative treatment with shampoo that
does not contain the chelant.
[0055] B. Detersive Surfactant
[0056] The shampoo composition comprises from about 2% to about
50%, alternatively from about 5% to about 25%, alternatively from
about 7% to about 22%, alternatively from about 9% to about 18%,
and alternatively from about 11% to about 15% of one or more
detersive surfactants by weight of the shampoo composition. The
concentration of the detersive surfactant component in the shampoo
composition should be sufficient to provide the desired cleaning
and lather performance.
[0057] The one or more detersive surfactants can be selected from
the group consisting of anionic surfactants, amphoteric or
zwitterionic surfactants, or mixtures thereof. The one or more
detersive surfactants can also be selected from the group
consisting of anionic surfactants, cationic surfactants, non-ionic
surfactants, amphoteric surfactants, and mixtures thereof. Various
examples and descriptions of detersive surfactants are set forth in
U.S. Pat. No. 6,649,155; U.S. Patent Application Publication No.
2008/0317698; and U.S. Patent Application Publication No.
2008/0206355, which are incorporated herein by reference in their
entirety.
[0058] Anionic surfactants suitable for use in the compositions are
the alkyl and alkyl ether sulfates. Other suitable anionic
surfactants are the water-soluble salts of organic, sulfuric acid
reaction products. Still other suitable anionic surfactants are the
reaction products of fatty acids esterified with isethionic acid
and neutralized with sodium hydroxide. Other similar anionic
surfactants are described in U.S. Pat. Nos. 2,486,921; 2,486,922;
and 2,396,278, which are incorporated herein by reference in their
entirety.
[0059] Exemplary anionic surfactants for use in the shampoo
composition include ammonium lauryl sulfate, ammonium laureth
sulfate, triethylamine lauryl sulfate, triethylamine laureth
sulfate, triethanolamine lauryl sulfate, triethanolamine laureth
sulfate, monoethanolamine lauryl sulfate, monoethanolamine laureth
sulfate, diethanolamine lauryl sulfate, diethanolamine laureth
sulfate, lauric monoglyceride sodium sulfate, sodium lauryl
sulfate, sodium laureth sulfate, potassium lauryl sulfate,
potassium laureth sulfate, sodium lauryl sarcosinate, sodium
lauroyl sarcosinate, lauryl sarcosine, cocoyl sarcosine, ammonium
cocoyl sulfate, ammonium lauroyl sulfate, sodium cocoyl sulfate,
sodium lauroyl sulfate, potassium cocoyl sulfate, potassium lauryl
sulfate, triethanolamine lauryl sulfate, triethanolamine lauryl
sulfate, monoethanolamine cocoyl sulfate, monoethanolamine lauryl
sulfate, sodium tridecyl benzene sulfonate, sodium dodecyl benzene
sulfonate, sodium cocoyl isethionate and combinations thereof. In a
further embodiment, the anionic surfactant is sodium lauryl sulfate
or sodium laureth sulfate.
[0060] Suitable amphoteric or zwitterionic surfactants for use in
the shampoo composition include those which are known for use in
shampoo or other personal care cleansing. Concentrations of such
amphoteric surfactants range from about 0.5 wt % to about 20 wt %,
and from about 1 wt % to about 10 wt %. Non limiting examples of
suitable zwitterionic or amphoteric surfactants are described in
U.S. Pat. Nos. 5,104,646 and 5,106,609, which are incorporated
herein by reference in their entirety.
[0061] Amphoteric detersive surfactants suitable for use in the
shampoo composition include those surfactants broadly described as
derivatives of aliphatic secondary and tertiary amines in which the
aliphatic radical can be straight or branched chain and wherein one
of the aliphatic substituents contains from about 8 to about 18
carbon atoms and one contains an anionic group such as carboxy,
sulfonate, sulfate, phosphate, or phosphonate. Exemplary amphoteric
detersive surfactants for use in the present shampoo composition
include cocoamphoacetate, cocoamphodiacetate, lauroamphoacetate,
lauroamphodiacetate, and mixtures thereof.
[0062] Zwitterionic detersive surfactants suitable for use in the
shampoo composition include those surfactants broadly described as
derivatives of aliphatic quaternaryammonium, phosphonium, and
sulfonium compounds, in which the aliphatic radicals can be
straight or branched chain, and wherein one of the aliphatic
substituents contains from about 8 to about 18 carbon atoms and one
contains an anionic group such as carboxy, sulfonate, sulfate,
phosphate or phosphonate. In another embodiment, zwitterionics such
as betaines are selected.
[0063] Non limiting examples of other anionic, zwitterionic,
amphoteric or optional additional surfactants suitable for use in
the shampoo composition are described in McCutcheon's, Emulsifiers
and Detergents, 1989 Annual, published by M. C. Publishing Co., and
U.S. Pat. Nos. 3,929,678, 2,658,072; 2,438,091; 2,528,378, which
are incorporated herein by reference in their entirety.
[0064] The shampoo composition may also comprise a cationic
conditioning polymer, an aqueous carrier, and other additional
ingredients described herein.
[0065] C. Cationic Conditioning Polymers
[0066] The shampoo composition described herein may comprise one or
more cationic conditioning polymers. This polymer may be selected
from the group consisting of (a) a cationic guar polymer, (b) a
cationic non-guar polymer, (c) a cationic tapioca polymer, (d) a
cationic copolymer of acrylamide monomers and cationic monomers,
(e) a synthetic, non-crosslinked, cationic polymer, which forms
lyotropic liquid crystals upon combination with the detersive
surfactant, and (f) mixtures thereof.
[0067] D. Carrier
[0068] The shampoo composition further comprises from about 75% to
about 98%, alternatively from about 80% to about 98% of a
cosmetically acceptable carrier, by weight of the shampoo
composition. The carrier can be an aqueous carrier. The amount and
chemistry of the carrier is selected according to the compatibility
with other components and other desired characteristic of the
product. In an embodiment, the carrier is selected from the group
consisting of: water and water solutions of lower alkyl alcohols.
Lower alkyl alcohols useful herein are monohydric alcohols having 1
to 6 carbons, such as ethanol and/or isopropanol. In an embodiment,
the cosmetically acceptable carrier is a cosmetically acceptable
aqueous carrier and is present at a level of from about 20% to
about 95%, or from about 60% to about 85%.
[0069] The pH of the shampoo composition can be from about pH 3 to
about pH 8, alternatively from about pH 4 to about pH 7, and
alternatively from about pH 5 to about pH 6.
[0070] E. Benefit Agent
[0071] The shampoo composition may further comprise one or more
benefit agents. Exemplary benefit agents include, but are not
limited to, silicone emulsions, anti-dandruff actives, perfume
microcapsules, gel networks, colorants, particles, and other
insoluble skin or hair conditioning agents such as skin silicones,
natural oils such as sun flower oil or castor oil.
[0072] (1). Silicone Emulsion
[0073] The silicone emulsions suitable for use herein include
emulsions of insoluble polysiloxanes prepared in accordance with
the descriptions provided in U.S. Pat. No. 4,476,282 and U.S.
Patent Application Publication No. 2007/0276087. Accordingly,
insoluble polysiloxanes referred to herein for the purpose of the
invention include polysiloxanes such as alpha, omega
hydroxy-terminated polysiloxanes or alpha, omega alkoxy-terminated
polysiloxanes having a molecular weight within the range from about
50,000 to about 500,000 g/mol. As used herein, "insoluble
polysiloxane" means that the water solubility of the polysiloxane
is less than 0.05 wt %. In another embodiment, the water solubility
of the polysiloxane is less than 0.02 wt %, or less than 0.01 wt %,
or less than 0.001 wt %. According to an embodiment, the insoluble
polysiloxane is present in the shampoo composition in an amount
within the range from about 0.1 wt % to about 3 wt %, based on the
total weight of the composition. For example, the insoluble
polysiloxane can be present in an amount within the range from
about 0.2 wt % to about 2.5 wt %, or from about 0.4 wt % to about
2.0 wt %, or from about 0.5 wt % to about 1.5 wt %, based on the
total weight of the composition.
[0074] According to one aspect of the silicone emulsion, the
insoluble polysiloxane used herein include alpha, omega hydroxy- or
alkoxy-terminated polysiloxanes having a general formula I:
R.sup.1[O--SiR.sub.2].sub.n--OR.sup.1,
wherein `n` is an integer, R is a substituted or unsubstituted
C.sub.1 to C.sub.10 alkyl or aryl, and R.sup.1 is a hydrogen or a
substituted or unsubstituted C.sub.1 to C.sub.10 alkyl or aryl.
Non-limiting examples of R and R.sup.1 may be independently
selected from alkyl groups such as methyl, ethyl, n-propyl,
isopropyl, n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl,
neopentyl, tertpentyl, hexyl such as n-hexyl, heptyl such as
n-heptyl, octyl such as n-octyl and isooctyl such as
2,2,4-trimethyl-pentyl, nonyl such as n-nonyl, decyl such as
n-decyl, dodecyl such as n-dodecyl, octadecyl such as n-octadecyl;
or aryl groups such as phenyl, naphthyl, anthryl and phenanthryl.
In an embodiment, the insoluble polysiloxane has a general formula
H--[O--SiR.sub.2].sub.n--OH.
[0075] According to another aspect of the silicone emulsion, the
insoluble polysiloxane has an average molecular weight within the
range from about 50,000 to about 500,000 g/mol. For example, the
insoluble polysiloxane may have an average molecular weight within
the range from about 60,000 to about 400,000; from about 75,000 to
about 300,000; from about 100,000 to about 200,000; or the average
molecular weight may be about 150,000 g/mol.
[0076] According to another aspect of the silicon emulsion, total
content of a cyclic polysiloxane having a general formula:
##STR00007##
wherein R is as defined above, and wherein m is 4 or 5, is present
in the silicone emulsion in an amount less than about 2.5 wt %
based on the total weight of all polysiloxanes. For example,
dimethiconol may include significant quantities of cyclic
polysiloxanes, such as octamethylcyclotetrasiloxane (D4) and
decamethylcyclotetrasiloxane (D5). In an embodiment, the amount of
D4 is less than about 2.0%, or less than about 1.5%, or less than
about 1.0%, or less than about 0.5%, based on the total weight of
all polysiloxanes. In an embodiment, the amount of D5 is less than
about 0.5%, or less than about 0.4%, or less than about 0.3%, or
less than about 0.2%, based on the total weight of all
polysiloxanes.
[0077] According to yet another aspect of the silicone emulsion,
the emulsion has a viscosity up to about 500,000 cPs. For example,
the viscosity may be within the range from about 75,000 to about
300,000, from about 100,000 to about 200,000, or about 150,000
cPs.
[0078] According to yet another aspect of the silicone emulsion,
the insoluble polysiloxane has an average particle size within the
range from about 30 nm to about 10 micron. The average particle
size may be within the range from about 40 nm to about 5 micron,
from about 50 nm to about 1 micron, from about 75 nm to about 500
nm, or about 100 nm, for example.
[0079] The average molecular weight of the insoluble polysiloxane,
the viscosity of the silicone emulsion, and the size of the
particle comprising the insoluble polysiloxane are determined by
methods commonly used by those skilled in the art, such as the
methods disclosed in Smith, A. L. The Analytical Chemistry of
Silicones, John Wiley & Sons, Inc.: New York, 1991. For
example, the viscosity of the silicone emulsion can be measured at
30.degree. C. with a Brookfield viscosimeter with spindle 6 at 2.5
rpm.
[0080] According to another aspect of the silicone emulsion, the
emulsion further includes an anionic surfactant that participates
in providing high internal phase viscosity emulsions having
particle sizes in the range from about 30 nm to about 10 micron.
The anionic surfactant is selected from organic sulfonic acids.
Most common sulfonic acids used in the present process are
alkylaryl sulfonic acid; alkylaryl polyoxyethylene sulphonic acid;
alkyl sulfonic acid; and alkyl polyoxyethylene sulfonic acid.
General formulas of the sulfonic acids are as shown below:
R.sup.2C.sub.6H.sub.4SO.sub.3H (II)
R.sup.2C.sub.6H.sub.4O(C.sub.2H.sub.4O).sub.mSO.sub.3H (III)
R.sup.2SO.sub.3H (IV)
R.sup.2O(C.sub.2H.sub.4O).sub.mSO.sub.3H (IV)
Where R.sup.2, which may differ, is a monovalent hydrocarbon
radical having at least 6 carbon atoms. Non-limiting examples of
R.sup.2 include hexyl, octyl, decyl, dodecyl, cetyl, stearyl,
myristyl, and oleyl. `m` is an integer from 1 to 25. Exemplary
anionic surfactants include but are not limited to octylbenzene
sulfonic acid; dodecylbenzene sulfonic acid; cetylbenzene sulfonic
acid; alpha-octyl sulfonic acid; alpha-dodecyl sulfonic acid;
alpha-cetyl sulfonic acid; polyoxyethylene octylbenzene sulfonic
acid; polyoxyethylene dodecylbenzene sulfonic acid; polyoxyethylene
cetylbenzene sulfonic acid; polyoxyethylene octyl sulfonic acid;
polyoxyethylene dodecyl sulfonic acid; and polyoxyethylene cetyl
sulfonic acid. Generally, 1 to 15% anionic surfactant is used in
the emulsion process. For example, 3-10% anionic surfactant can be
used to obtain an optimum result.
[0081] The silicone emulsion may further include an additional
emulsifier together with the anionic surfactant, which along with
the controlled temperature of emulsification and polymerization,
facilitates making the emulsion in a simple and faster way.
Non-ionic emulsifiers having a hydrophilic lipophilic balance (HLB)
value of 10 to 19 are suitable and include polyoxyalkylene alkyl
ether, polyoxyalkylene alkylphenyl ethers and polyoxyalkylene
sorbitan esters. Some useful emulsifiers having an HLB value of 10
to 19 include, but are not limited to, polyethylene glycol octyl
ether; polyethylene glycol lauryl ether; polyethylene glycol
tridecyl ether; polyethylene glycol cetyl ether; polyethylene
glycol stearyl ether; polyethylene glycol nonylphenyl ether;
polyethylene glycol dodecylphenyl ether; polyethylene glycol
cetylphenyl ether; polyethylene glycol stearylphenyl ether;
polyethylene glycol sorbitan monostearate; and polyethylene glycol
sorbitan monooleate.
[0082] In accordance with another embodiment, the composition may
further comprise an anti-dandruff active, which may be an
anti-dandruff active particulate.
[0083] F. Other components
[0084] The shampoo composition can also additionally comprise any
suitable optional ingredients as desired. Such optional ingredients
should be physically and chemically compatible with the components
of the composition, and should not otherwise unduly impair product
stability, aesthetics, or performance. The CTFA Cosmetic Ingredient
Handbook, Tenth Edition (published by the Cosmetic, Toiletry, and
Fragrance Association, Inc., Washington, D.C.) (2004) (hereinafter
"CTFA"), describes a wide variety of nonlimiting materials that can
be added to the composition herein.
[0085] In accordance with another embodiment of the invention, a
method of making a shampoo composition comprising a detersive
surfactant, a cationic conditioning polymer, a chelant, and a
carrier is provided. The method includes (i) combining the
detersive surfactant and the cationic conditioning polymer in
suitable carrier, and (ii) combining a chelant and a carrier
composition that includes a product of step (i) to form the shampoo
composition.
[0086] In an embodiment, the shampoo composition has a viscosity of
4,000 cP to 20,000 cP, or from about 6,000 cP to about 12,000 cP,
or from about 8,000 cP to about 11,000 cP, measured at 26.6.degree.
C. with a Brookfield R/S Plus Rheometer at 2 s.sup.-1. cP means
centipoises.
[0087] Also described herein is a method of inhibiting copper
deposition on hair and facilitating the removal of copper deposited
on hair comprising applying to the hair a shampomo composition
described herein and rinsing the shampoo composition from the
hair.
[0088] Inhibition of copper deposition on hair and facilitation of
the removal of copper deposited on hair may also be achieved by
applying a leave-on treatment to the hair after rinsing the
conditioner from the hair. The leave-on treatment may deliver
consumer desired conditioning in addition to inhibiting the
deposition of copper (i.e. from the water used to rinse) on the
hair. The leave-on treatment described herein may comprise from
about 0.025% to about 0.50%, alternatively from about 0.05% to
about 0.25% of one or more chelants described herein, by weight of
the leave-on treatment. The leave-on treatment may also comprise
one or more rheology modifiers and an aqueous carrier.
[0089] The shampoo composition can be prepared by conventional
formulation and mixing techniques. It will be appreciated that
other modifications of the shampoo composition within the skill of
those in the hair care formulation art can be undertaken without
departing from the spirit and scope of this invention. All parts,
percentages, and ratios herein are by weight unless otherwise
specified. Some components may come from suppliers as dilute
solutions. The amount stated reflects the weight percent of the
active material, unless otherwise specified.
Test Methods
Shampoo Treatment Protocol
[0090] All testing are performed on colored hair switches (see
Method of Measurement of Copper on Hair below) weighing
approximately 4.0 grams and having a length of approximately 6
inches. The hair switches are commercially available from IHIP
(International Hair Importers). Three hair switches per shampoo
composition are used. An amount of 0.20 g of shampoo is spread via
a syringe onto separate hair switch. That is, the dosage is 0.10 g
of shampoo per g of hair. Each application consists of adding
shampoo to the hair, milking for 30 seconds followed by rinsing for
30 seconds. Shampoo is then reapplied (0.1 g/g), milked for 30
seconds and rinsed for 30 seconds. Excess water is squeezed from
the hair switches and left to air dry or treated with a rinse-off
conditioner and/or a leave-on treatment composition. This protocol
is repeated for a number of times/cycles (as indicated in the
tables below, which describe the details of hair treatments).
Method of Measurement of Copper on Hair
[0091] The following test method is used to assess the ability of
the compositions and regimens to remove copper from the hair and to
inhibit copper deposition onto the hair.
[0092] Hair switches are colored once with an oxidative hair
colorant. An extra blonde shade is used for the testing. The hair
switches are washed for 10 or 20 repeat wash cycles in tap water
containing 7 grains per gallon water hardness (Ca/Mg) and 0.06
.mu.g/g copper ions. Each wash cycle consists of two applications
of 0.1 g/g a shampoo to the hair switches. Each application
consists of adding shampoo to the hair, milking for 30 secs
followed by rinsing for 30 secs. Shampoo is then reapplied 0.1 g/g,
milked for 30 secs, rinsed for 30 secs and then dried in a heat box
(60.degree. C.) until dry.
[0093] Samples of 100 mg of hair are digested overnight with 2 ml
of high purity concentrated nitric acid. The digestive mixture also
contains 150 .mu.L of 100 .mu.g/g Yttrium internal standard
(Inorganic Ventures, Christianburg, Va., USA). Following digestion,
samples are heated to 70-80.degree. C. for one hour, cooled to room
temperature and diluted to 15 mL with deionized water. Copper
content of the hair switches is determined by inductively coupled
plasma atomic spectroscopy (ICP-OES)). For each leg, 3 different
samples are analyzed.
EXAMPLES & DATA
[0094] The following are non-limiting examples of the shampoo
composition described herein. The examples are given solely for the
purpose of illustration and are not to be construed as limitations
of the shampoo composition, as many variations thereof are possible
without departing from the spirit and scope of the shampoo
composition, which would be recognized by one of ordinary skill in
the art.
[0095] The shampoo composition described herein is generally
prepared by conventional methods. Such methods typically involve
mixing of the ingredients in one or more steps to a relatively
uniform state, with or without heating, cooling, application of
vacuum, and the like. The compositions are prepared such as to
optimize stability (physical stability, chemical stability,
photostability) and/or delivery of the active materials. The
shampoo composition may be in a single phase or a single product,
or the shampoo composition may be in a separate phases or separate
products. If two products are used, the products may be used
together, at the same time, or sequentially. Sequential use may
occur in a short period of time, such as immediately after the use
of one product, or it may occur over a period of hours or days.
[0096] In order to minimize the variability of the resulting copper
content on hair that is related to (a) lot-to-lot viariability due
to hair switches and (b) day-to-day variability of the water used
during shampoo and conditioner treatments, a single lot of hair
switches is used for each experimental series and a separate
control experiment/treatment is run for each experimental series
(see below).
Experimental Series I:
[0097] Investigation of treatments with clarifying shampoos
containing simple surfactants and 2,3-Triethylenetetramine.
TABLE-US-00002 Ex. 1 Control Ex. 2 Components Wt % Wt % Sodium
Laureth-1 Sulfate.sup.1 10.50 10.50 Sodium Lauryl Sulfate.sup.2
1.50 1.50 Cocamidopropyl betaine 1.00 1.00 Sodium benzoate 0.25
0.25 Citric Acid 0.70 0.70 Methylchloroisothiazolinone/ 0.0005
0.0005 Methylisothiazolinone.sup.3 Sodium chloride 1.00 1.00
Tetrasodium EDTA dihydrate 0.16 0.16 2,3-Triethylenetetramine
(TETA) 0.00 0.10 Deionized water Q.S. Q.S. pH adjusted to 6.0 6.0
.sup.1Sodium laureth-3-sulfate available from BASF as Standapol
ES-3 (28 wt. % active). .sup.2Sodium Lauryl Sulfate available from
BASF as Standapol WAQ-LC (29 wt. % active). .sup.3Kathon CG
available from Dow (1.5 wt % active).
Results of Experimental Series I
TABLE-US-00003 [0098] Composition of Ex. 1 Ex. 2 Summary
Description of Control Clarifying Clarifying shampoo Composition
shampoo with with simple simple surfactant surfactant and chelant
Concentration of Chelant in 0.0% 0.10% Shampoo Chelant used -- 2,3-
Triethylenetetramine Shampoo pH 6.0 6.0 Shampoo cycles 10 10
Average final copper 84 33 concentration in hair (ppm) Standard
deviation 4.2 1.1 Relative content of Copper 100 33 content on hair
after treatment (versus control shampoo treatment)
[0099] Chelant 2,3-Triethylenetetramine contributes to significant
reduction of copper content on hair after 10 shampoo cycle
treatments compared to treatment with shampoo composition that does
not comprise the chelant.
Experimental Series II:
[0100] Investigation of treatments with clarifying shampoos
containing simple surfactants and 2,3-Triethylenetetramine in two
different pH values.
TABLE-US-00004 Ex. 3 Ex. 4 Control Control Ex. 5 Ex. 6 Components
Wt % Wt % Wt % Wt % Sodium Laureth-1 Sulfate.sup.1 10.50 10.50
10.50 10.50 Sodium Lauryl Sulfate.sup.2 1.50 1.50 1.50 1.50
Cocamidopropyl betaine 1.00 1.00 1.00 1.00 Sodium benzoate 0.25
0.25 0.25 0.25 Citric Acid 0.70 1.00 0.70 1.00
Methylchloroisothiazolinone/ 0.0005 0.0005 0.0005 0.0005
Methylisothiazolinone.sup.3 Sodium chloride 1.00 1.00 1.00 1.00
Tetrasodium EDTA dihydrate 0.16 0.16 0.16 0.16
2,3-Triethylenetetramine 0.00 0.00 0.10 0.10 Deionized water Q.S.
Q.S. Q.S. Q.S. to 100 to 100 to 100 to 100 pH adjusted to 6.0 4.25
6.0 4.25 .sup.1Sodium laureth-3-sulfate available from BASF as
Standapol ES-3 (28 wt. % active). .sup.2Sodium Lauryl Sulfate
available from BASF as Standapol WAQ-LC (29 wt. % active).
.sup.3Kathon CG available from Dow (1.5 wt % active).
Results of Experimental Series II
TABLE-US-00005 [0101] Composition of Ex. 3 Ex. 4 Ex. 5 Ex. 6
Summary Control Control Clarifying Clarifying Description of
Clarifying Clarifying shampoo shampoo Composition shampoo shampoo
with simple with simple with simple with simple surfactant
surfactant surfactant surfactant and chelant and chelant
Concentration 0.0% 0.0% 0.10% 0.10% of Chelant in Shampoo Chelant
used -- -- 2,3- 2,3- Triethylene- Triethylene- tetramine tetramine
Shampoo pH 6.0 4.25 6.0 4.25 Shampoo 20 20 20 20 cycles Average
final 92 62 34 36 copper concentration in hair (ppm) Standard 11
4.8 3.1 3.6 deviation Relative 100.0 67 v. 39 v. 37 v. content of
Control Control Control Copper content on hair after treatment
(versus control shampoo treatment)
[0102] The presence of 2,3-Triethylenetetramine acid contributes to
an effective removal of copper from hair after 20 shampoo cycles
both at low and a higher pH value. Without the chelant, lower pH
shows higher copper removal from hair.
Experimental Series III:
[0103] Investigation of treatments with clarifying shampoos
containing simple surfactants (pH=6) and various chelants described
herein.
TABLE-US-00006 Ex. 7 Control Ex. 8 Ex. 9 Ex. 10 Ex. 11 Components
Wt % Wt % Wt % Wt % Wt % Sodium Laureth-1 10.50 10.50 10.50 10.50
10.50 Sulfate.sup.1 Sodium Lauryl 1.50 1.50 1.50 1.50 1.50
Sulfate.sup.2 Cocamidopropyl betaine 1.00 1.00 1.00 1.00 1.00
Sodium benzoate 0.25 0.25 0.25 0.25 0.25 Citric Acid 0.70 0.70 0.70
1.00 1.00 Methylchloro- 0.0005 0.0005 0.0005 0.0005 0.0005
isothiazolinone/ Methyl- isothiazolinone.sup.3 Sodium chloride 1.00
1.00 1.00 1.00 1.00 Tetrasodium EDTA 0.16 0.16 0.16 0.16 0.16
dihydrate 2,3-Triethylenetetramine 0.00 0.10 0.00 0.00 0.00
Tetraethylenepentamine 0.00 0.00 0.10 0.00 0.00
Tris(2-aminoethyl)amine 0.00 0.00 0.00 0.00 0.00
Pentaethylenehexamine 0.00 0.00 0.00 0.00 0.10 Deionized water Q.S.
Q.S. Q.S. Q.S. Q.S. to 100 to 100 to 100 to 100 to 100 pH adjusted
to 6.0 6.0 6.0 6.0 6.0 .sup.1Sodium laureth-3-sulfate available
from BASF as Standapol ES-3 (28 wt. % active). .sup.2Sodium Lauryl
Sulfate available from BASF as Standapol WAQ-LC (29 wt. % active).
.sup.3Kathon CG available from Dow (1.5 wt % active).
Results of Experimental Series III
TABLE-US-00007 [0104] Composition of Ex. 7 Ex. 8 Ex. 9 Ex. 10 Ex.
11 Summary Control Clarifying shampoo Clarifying shampoo Clarifying
shampoo Clarifying shampoo Description of Clarifying with simple
with simple surfactant with simple surfactant with simple
surfactant Composition shampoo with surfactant and and chelant and
chelant and chelant simple surfactant chelant Concentration of 0.0%
0.10% 0.10% 0.10% 0.10% Chelant in Shampoo Chelant used -- 2,3-
Tetraethylenepentamine Tris(2- Pentaethylenehexamine
Triethylenetetramine aminoethyl)amine Chelant Class -- Class III
Class III Shampoo pH 6.0 6.0 6.0 6.0 6.0 Shampoo cycles 20 20 20 20
20 Average final copper 115 37 49 62 53 concentration in hair (ppm)
Standard deviation 14 2.8 2.7 3.8 10.5 Relative content of 100 32
43 54 46 Copper content on hair after treatment (versus control
shampoo treatment)
[0105] All chelants from Class III evaluated in a 20 cycle cleaning
treatment using a clarifying shampoo containing simple surfactants
shows reduction of copper hair content compared to the control
shampoo treatment. 2,3-Triethylenetetramine and
Tetraethylenepentamine show more effective treatments.
Experimental Series IV:
[0106] Investigation of treatments with clarifying shampoos
containing simple surfactants (pH=6) and
ethylenedinitrilotetrapropan-2-ol chelant.
TABLE-US-00008 Ex. 12 Control Ex. 13 Components Wt % Wt % Sodium
Laureth-1 Sulfate.sup.1 10.50 10.50 Sodium Lauryl Sulfate.sup.2
1.50 1.50 Cocamidopropyl betaine 1.00 1.00 Sodium benzoate 0.25
0.25 Citric Acid 0.70 0.70 Methylchloroisothiazolinone/ 0.0005
0.0005 Methylisothiazolinone.sup.3 Sodium chloride 1.00 1.00
Tetrasodium EDTA dihydrate 0.16 0.16
Ethylenedinitrilotetrapropan-2-ol 0.00 0.40 Deionized water Q.S. to
100 Q.S. to 100 pH adjusted to 6.0 6.0 .sup.1Sodium
laureth-3-sulfate available from BASF as Standapol ES-3 (28 wt. %
active). .sup.2Sodium Lauryl Sulfate available from BASF as
Standapol WAQ-LC (29 wt. % active). .sup.3Kathon CG available from
Dow (1.5 wt % active).
Results of Experimental Series IV
TABLE-US-00009 [0107] Composition of Ex.12 Ex.13 Summary Control
Clarifying Clarifying shampoo Description of shampoo with simple
with simple Composition surfactant surfactant and chelant
Concentration of 0.00% 0.40% Chelant in Shampoo Chelant used --
Ethylenedinitrilotetrapropan- 2-ol Shampoo pH 6.0 6.0 Shampoo
cycles 20 20 Average final copper 70 50 concentration in hair (ppm)
Standard deviation 2.6 0.4 Relative content of 100 71 Copper
content on hair after treatment (versus control shampoo
treatment)
[0108] The presence of ethylenedinitrilotetrapropan-2-ol acid (at a
concentration of 0.40 wt %) contributes to an effective removal of
copper from hair after 20 shampoo cycles compared to the
corresponding treatment with control shampoo that does not contain
the chelant.
Experimental Series V:
[0109] Investigation of treatments with clarifying shampoos
containing simple surfactants, a rheology modifier and
tris-2-aminoethylamine
TABLE-US-00010 Ex. 14 Control Ex. 15 Components Wt % Wt % Sodium
Laureth-3 Sulfate.sup.1 6.00 6.00 Sodium Lauryl Sulfate.sup.2 9.50
9.50 Cocamidopropyl betaine 1.88 1.88 Tetrasodium EDTA dihydrate
0.16 0.16 Citric Acid (Anhydrous) 0.28 0.28 Sodium benzoate 0.25
0.25 Methylchloroisothiazolinone/ 0.0005 0.0005
Methylisothiazolinone.sup.3 Sodium chloride 0.57 0.57
Hydroxypropylmethylcellulose 0.25 0.25 Tris-2-aminoethylamine 0.00
0.10 Perfume 0.40 0.40 Distilled Water Q.S. Q.S. .sup.1Sodium
laureth-3-sulfate available from BASF as Standapol ES-3 (28 wt. %
active). .sup.2Sodium Lauryl Sulfate available from BASF as
Standapol WAQ-LC (29 wt. % active). .sup.3Kathon CG available from
Dow (1.5 wt % active).
Results of Experimental Series V
TABLE-US-00011 [0110] Composition of Ex.14 Ex.15 Summary Control
Clarifying Clarifying shampoo with Description of shampoo with
simple simple surfactant, a Composition surfactant and Rheology
Rheology Modifier and a Modifier chelant Concentration of 0.00%
0.10% Chelant in Shampoo Chelant used -- Tris-2-aminoethylamine
Shampoo pH 6.0 6.0 Shampoo cycles 10 10 Average final copper 94 62
concentration in hair (ppm) Standard deviation 15 9.5 Relative
content of 100 66 Copper content on hair after treatment (versus
control shampoo treatment)
[0111] The presence of tris-2-aminoethylamine acid contributes to
an effective removal of copper from hair after 10 shampoo cycles
compared to the corresponding treatment with control clarifying
shampoo that does not contain the chelant.
Experimental Series VI:
[0112] Investigation of treatments with clarifying shampoos
containing simple surfactants, a rheology modifier and chelants
having 2-aminodiacetic acid molecular structures.
TABLE-US-00012 Ex. 16 Control Ex. 17 Ex. 18 Components Wt % Wt % Wt
% Sodium Laureth-3 Sulfate.sup.1 6.00 6.00 6.00 Sodium Lauryl
Sulfate.sup.2 9.50 9.50 9.50 Cocamidopropyl betaine 1.88 1.88 1.88
Tetrasodium EDTA dihydrate 0.16 0.16 0.16 Citric Acid (Anhydrous)
0.28 0.28 0.28 Sodium benzoate 0.25 0.25 0.25
Methylchloroisothiazolinone/ 0.0005 0.0005 0.0005
Methylisothiazolinone.sup.3 Sodium chloride 0.57 0.57 0.57
Hydroxypropylmethylcellulose 0.25 0.25 0.25 Iminodiacetic acid 0.00
0.10 0.00 N-(2-hydroxyethyl)iminodiacetic acid 0.00 0.00 0.10
Perfume 0.40 0.40 0.40 Distilled Water Q.S. Q.S. Q.S. .sup.1Sodium
laureth-3-sulfate available from BASF as Standapol ES-3 (28 wt. %
active). .sup.2Sodium Lauryl Sulfate available from BASF as
Standapol WAQ-LC (29 wt. % active). .sup.3Kathon CG available from
Dow (1.5 wt % active).
Results of Experimental Series VI
TABLE-US-00013 [0113] Composition of Ex.16 Ex.17 Ex.18 Summary
Control Clarifying Clarifying shampoo Clarifying shampoo
Description of shampoo with simple with simple with simple
surfactant, Composition surfactant and surfactant, a a Rheology
Modifier Rheology Modifier Rheology Modifier and a chelant and a
chelant Concentration of 0.00% 0.10% 0.10% Chelant in Shampoo
Chelant used -- Iminodiacetic acid N-(2- hydroxyethyl)iminodiacetic
acid Shampoo pH 6.0 6.0 6.0 Shampoo cycles 20 20 20 Average final
copper 84 51 56 concentration in hair (ppm) Standard deviation 6.5
2.7 1.7 Relative content of 100 61 67 Copper content on hair after
treatment (versus control shampoo treatment)
[0114] The presence of chelants having 2-aminodiacetic acid
molecular structures contributes to an effective removal of copper
from hair after 20 shampoo cycles compared to the corresponding
treatment with control clarifying shampoo that does not contain the
chelant.
Experimental Series VII:
[0115] Investigation of treatments using shampoos and rinse-off
conditioner and leave-on treatments containing
2,3-Triethylenetetramine chelant.
Conditioning Shampoo Compositions
TABLE-US-00014 [0116] Ex. 19 Control Ex. 20 Components Wt % Wt %
Sodium Laureth-3 Sulfate.sup.1 6.10 6.10 Sodium Lauryl
Sulfate.sup.2 4.00 4.00 Cocoamide MEA.sup.3 0.90 0.90 Guar
hydroxypropyltrimonium chloride.sup.4 0.25 0.25 Glycol distearate
1.50 1.50 Dimethicone.sup.5 1.00 1.00 Tetrasodium EDTA dihydrate
0.16 0.16 Citric Acid (Anhydrous) 0.18 0.18 Sodium benzoate 0.27
0.27 Methylchloroisothiazolinone/ 0.0006 0.0006
Methylisothiazolinone.sup.6 Sodium chloride 0.20 0.20 Hydrochloric
acid (6N) 0.06 0.06 2,3-Triethylenetetramine (TETA) 0.00 0.10
Perfume 0.40 0.40 Distilled Water Q.S. Q.S. .sup.1Sodium
laureth-3-sulfate available from BASF as Standapol ES-3 (28 wt. %
active). .sup.2Sodium Lauryl Sulfate available from BASF as
Standapol WAQ-LC (29 wt. % active). .sup.3Cocamide MEA available
from BASF as Comperlan CMEA (85 wt. % active). .sup.4Jaguar C-500
available from Ashland. .sup.5Silicone oil with viscosity of
330.000 cP .sup.6Kathon CG available from Dow (1.5 wt %
active).
Clarifying Shampoo Compositions
TABLE-US-00015 [0117] Ex. 19(a) Control Ex. 21 Components Wt % Wt %
Sodium Laureth-3 Sulfate.sup.1 6.00 6.00 Sodium Lauryl
Sulfate.sup.2 9.50 9.50 Cocamidopropyl betaine 1.88 1.88
Tetrasodium EDTA dehydrate 0.16 0.16 Citric Acid (Anhydrous) 0.28
0.28 Sodium benzoate 0.25 0.25 Methylchloroisothiazolinone/ 0.0005
0.0005 Methylisothiazolinone.sup.3 Sodium chloride 0.57 0.57
Hydroxypropylmethylcellulose 0.25 0.25 2,3-Triethylenetetramine
(TETA) 0.0 0.10 Perfume 0.40 0.40 Distilled Water Q.S. Q.S.
.sup.1Sodium laureth-3-sulfate available from BASF as Standapol
ES-3 (28 wt. % active). .sup.2Sodium Lauryl Sulfate available from
BASF as Standapol WAQ-LC (29 wt. % active). .sup.3Kathon CG
available from Dow (1.5 wt % active).
Hair Repair Shampoo Compositions
TABLE-US-00016 [0118] Ex. 22 Control Ex. 23 Components Wt % Wt %
Ammonium lauryl sulfate 16.00 16.00 Cocoamide MEA.sup.1 0.8 0.8
Cetyl alcohol 0.9 0.9 Polyquatemium-10.sup.2 0.5 0.5 Polyethylene
glycol 7M.sup.3 0.10 0.10 Dimethicone.sup.4 2.00 2.00 Glycol
distearate 1.50 1.50 Sodium benzoate 0.25 0.25 Disodium EDTA 0.13
0.13 Citric acid 0.04 0.04 Sodium citrate dehydrate 0.45 0.45
Sodium chloride 0.03 0.03 Methylchloroisothiazolinone/ 0.0005
0.0005 Methylisothiazolinone.sup.5 Perfume 0.50 0.50
2,3-Triethylenetetramine (TETA) 0.00 0.10 Distilled Water Q.S. Q.S.
.sup.1Cocamide MEA available from BASF as Comperlan CMEA (85 wt. %
active). .sup.2Quaternized hydroxyethyl cellulose avaliable from
Dow Unival LR30M. .sup.3Available by Dow. .sup.4Silicone oil with
viscosity of 330.000 cP. .sup.5Kathon CG available from Dow (1.5 wt
% active).
Smoothing Rinse-Off Conditioner Compositions
TABLE-US-00017 [0119] Ex. 24 Control Ex. 25 Components Wt % Wt %
Stearyl alcohol 2.32 2.32 Cetyl alcohol 0.93 0.93 Dicetyldimonium
chloride 0.34 0.34 Behentrimonium methosulfate 1.16 1.16 Propylene
glycol 0.16 0.16 Isopropyl alcohol 0.28 0.28 Disodium EDTA
Dihydrate 0.13 0.13 Terminal amodimethicone.sup.1 0.75 0.75
Methylchloroisothiazolinone/ 0.0005 0.0005
Methylisothiazolinone.sup.2 Benzyl alcohol 0.40 0.40
2,3-Triethylenetetramine (TETA) 0.00 0.10 Distilled Water Q.S. Q.S.
.sup.1Terminal amodimethicone with visc. Of 10,000 cP at 25.degree.
C. is available by Momentive Performance Materials. .sup.2Kathon CG
available from Dow (1.5 wt % active)
Volumizing Rinse-Off Conditioner Compositions
TABLE-US-00018 [0120] Ex. 25(a) Control Ex. 26 Components Wt % Wt %
Hydroxypropyl guar.sup.1 0.35 0.35 DTDMAC (Quaternium-18.sup.2)
0.75 0.75 Stearamidopropyldimethylamine 1.00 1.00 Glyceryl
monostearate 0.25 0.25 Emulsifying wax NF (Polywax NF) 0.50 0.50
Cetyl alcohol 1.20 1.20 Stearyl alcohol 0.80 0.80 Oleyl alcohol
0.25 0.25 Citric acid 0.13 0.13 EDTA 0.10 0.10 Terminal
amodimethicone.sup.3 0.50 0.50 2,3-Triethylenetetramine (TETA) 0.00
0.10 Methylchloroisothiazolinone/ 0.0005 0.0005
Methylisothiazolinone.sup.4 Benzyl alcohol 0.4 0.4 Distilled Water
Q.S. Q.S. .sup.1Jaguar HP-105 supplied by Rhodia
.sup.2Diatallowdimethylammonium chloride .sup.3Terminal
amodimethicone with visc. Of 10,000 cP at 25.degree. C. is
available by Momentive Performance Materials. .sup.4Kathon CG
available from Dow (1.5 wt % active).
Hair Repair Rinse-Off Conditioner Compositions
TABLE-US-00019 [0121] EX. 27 Control EX. 28 Components Wt % Wt %
Behentrimonium chloride 2.28 2.28 Stearyl alcohol 4.64 4.64 Cetyl
alcohol 0.93 0.93 Isopropyl alcohol 0.57 0.57 Disodium EDTA
Dihydrate 0.13 0.13 Dimethicone.sup.1 4.20 4.20 Sodium hydroxide
0.02 0.02 Methylchloroisothiazolinone/ 0.0005 0.0005
Methylisothiazolinone.sup.2 Benzyl alcohol 0.40 0.40
2,3-Triethylenetetramine 0.00 0.10 Distilled Water Q.S. Q.S.
.sup.1Mixture of silicone gum and silicone oil XF49-B1747 available
from Momentive Performance Materials. .sup.2Kathon CG available
from Dow (1.5 wt % active).
Leave-on Treatment Composition
TABLE-US-00020 [0122] Ex. 29 Components Wt % Amodimethicone and
Cetrimonium 0.35 chloride and Trideceth-12.sup.1
Polyquatemium-11.sup.2 0.75 PEG-40 Hydrogenated castor oil 0.50
PPG-2 Methyl ether 0.5 DMDM Hydantoin 0.20 Disodium EDTA 0.14
Poysorbate 80 0.12 Aminomethyl propanol 0.1 Citric acid anhydrous
0.08 2,3-Triethylenetetramine 0.10 Distilled Water Q.S.
.sup.1Siameter MEM-0949 Emulsion available from Dow Corning; it
contains 35% aminosilicone .sup.2Copolymer of vinylpyrrolidone and
quaternized dimethylaminoethyl methacrylate; Gafquat 755 NH
available by Ashland
Results of Experimental Series VII
[0123] Each treatment (regimen) includes cleaning with conditioning
shampoo followed by a rinse-off conditioner, followed by a leave-on
treatment spray (when indicated).
TABLE-US-00021 Shampoo Ex. 19 Control Ex. 20 Ex. 19 Control Ex. 19
Control Composition Conditioning SH Conditioning Conditioning
Conditioning SH (SH) SH SH Smoothing Ex. 24 Control Ex. 24 Control
Ex. 25 Ex. 24 Control Rinse-off Smoothing ROC Smoothing Smoothing
Smoothing ROC conditioner ROC ROC composition (ROC) Leave-on No LOT
No LOT No LOT Ex. 29 treatment LOT composition (LOT) Summary SH
Control SH w/ chelant SH Control SH Control Description of ROC
Control ROC Control ROC w/ chelant ROC Control Composition No LOT
No LOT No LOT LOT w/ chelant Concentration 0% in SH 0.1% in SH 0%
in SH 0% in SH of Chelant 0% in ROC 0% in ROC 0.1% in ROC 0% in ROC
No LOT No LOT No LOT 0.1% in LOT Chelant used -- 2,3- 2,3- 2,3-
Triethylenetetramine Triethylenetetramine Triethylenetetramine
Cycles 20 20 20 20 Average final 84 30 25 43 copper concentration
in hair (ppm) Standard 5.6 2.1 1.7 0.2 deviation Relative content
100 36 30 51 of Copper v. Treatment v. Treatment v. Treatment AM
content on hair AM AM after treatment (versus control shampoo
treatment) Shampoo Ex. 21 Ex. 19(a) Ex. 23 Ex. 22 Control
Composition Clarifying SH Control Repair SH Repair SH (SH)
Clarifying SH Rinse-off Ex. 25(a) Control Ex. 26 Ex. 27 Control Ex.
28 conditioner Volumizing ROC Volumizing Repair ROC Repair ROC
composition ROC (ROC) Leave-on No LOT No LOT No LOT No LOT
treatment composition (LOT) Summary SH w/chelant SH Control SH w/
chelant SH Control Description of ROC Control ROC w/ chelant ROC
Control ROC w/ chelant Composition No LOT No LOT No LOT
Concentration 0.1% in SH 0% in SH 0.1% in SH 0.1% in SH of Chelant
0% in ROC 0.1% in ROC 0% in ROC 0% in ROC No LOT No LOT No LOT No
LOT Chelant used -- 2,3- 2,3- 2,3- Triethylenetetramine
Triethylenetetramine Triethylenetetramine Cycles 20 20 20 20
Average final 32 28 35 26 copper concentration in hair (ppm)
Standard 1.6 3.4 4.5 0.7 deviation Relative content 35 30 38 28 of
Copper v. Treatment v. Treatment v. Treatment v. Treatment AM
content on hair AM AM AM after treatment (versus control shampoo
treatment)
[0124] Addition of 2,3-Triethylenetetramine in any of the products
of the regimen contributes to an effective removal of copper from
hair after 20 conditioning shampoo/rinse-off conditioner/leave-on
treatment regimen cycles compared to the corresponding treatment
with control conditioning shampoo/control rinse-off conditioner.
The regimen where the chelant is added in the leave-on treatment is
particularly effective in removing copper form hair.
[0125] The dimensions and values disclosed herein are not to be
understood as being strictly limited to the exact numerical values
recited. Instead, unless otherwise specified, each such dimension
is intended to mean both the recited value and a functionally
equivalent range surrounding that value. For example, a dimension
disclosed as "40 mm" is intended to mean "about 40 mm."
[0126] Every document cited herein, including any cross referenced
or related patent or application, is hereby incorporated herein by
reference in its entirety unless expressly excluded or otherwise
limited. The citation of any document is not an admission that it
is prior art with respect to any invention disclosed or claimed
herein or that it alone, or in any combination with any other
reference or references, teaches, suggests or discloses any such
invention. Further, to the extent that any meaning or definition of
a term in this document conflicts with any meaning or definition of
the same term in a document incorporated by reference, the meaning
or definition assigned to that term in this document shall
govern.
[0127] While particular embodiments of the present invention have
been illustrated and described, it would be obvious to those
skilled in the art that various other changes and modifications can
be made without departing from the spirit and scope of the
invention. It is therefore intended to cover in the appended claims
all such changes and modifications that are within the scope of
this invention.
* * * * *