General introduction of the present invention
The present invention relates to xanthan gum, especially carried out heat treated xanthan gum, in hair cosmetic compositions as the application of setting agent.The advantage of xanthan gum is to use with other hairspray, can provide the effect of rheology modifying and some other character, comprise splendid hardness, gloss, do comb property, wet comb property, not shattered crack (non-flake), antistatic, sense of touch and high humility are curled retention.Detailed description of the present invention
The present invention relates to xanthan gum, especially carried out heat treated xanthan gum, in hair cosmetic compositions as the application of setting agent.
Xanthan gum can be used with purified form, also can heat-treat.The heat treatment of xanthan gum generally is to carry out under the condition of low humidity, preferred humidity is lower than about 25%, preferredly be lower than about 8%, especially preferredly be lower than approximately 1%, employed temperature is at least about 60 ℃, more preferably at least about 100 ℃, especially preferably at least about 105 ℃, the time of handling is about 30 minutes, preferably at least 1 hour, and more preferably at least 2.5 hours.
Those skilled in the art can adjust heat treated moisture, pH, temperature and time, to obtain needed viscosity, dispersibility, colloform texture (gel texture), solution clarity and other character.It further depends on employed material (grade, viscosity, molecular weight and granularity).Generally speaking, improve heat treated effect with low humidity.But under any given humidity, increase temperature or time generally can make the viscosity of xanthan gum be increased to maximum, further heat the viscosity that can reduce xanthan gum under the used concentration of the present invention.Acid pH is generally more suitable; The pH of 2-4 is optimum.
The heat treatment of xanthan gum can be finished with the whole bag of tricks known in the art, and these methods include but not limited to baking oven, fluid bed, infrared ray and microwave heating.The carrying out of gained the granularity of heat treated xanthan gum can adjust with method as known in the art, wherein said known method is as grinding.
Xanthan gum before and after heat-treating can further be modified.This xanthan gum can or be sheared by oxidation, enzymatic conversion, acid hydrolysis, heat and/or sour dextrinize and transform.Xanthan gum also can carry out chemistry, enzyme or physical modification.Suitable chemical derivative comprises ester, for example acetate and half fat, for example succinate, octenyl succinate and tetradecene base (tetradecenyl) succinate; Phosphate derivative; Ether, for example hydroxyalkyl ether and cation ether; Or any other derivant and their mixture.This modification also can be chemical crosslinking.Here the cross-linking agent of Shi Yonging comprises phosphoryl chloride phosphorus oxychloride, epoxychloropropane, sodium trimetaphosphate (sodium trimetaphosphate) and adipic acid-vinegar stock anhydride.This method also is known in the prior art.Generally speaking, except crosslinked or heat treatment, xanthan gum can not carry out other modification.
As long as heat treatment is unaffected substantially, just can come xanthan gum is carried out purification, to remove xanthan gum abnormal smells from the patient and color natural or that in modification or heat treatment process, produce with any method well known in the prior art.
Especially the carrying out of Shi Heing heat treated xanthan gum be that its 1% viscosity in aqueous solution is greater than about 4000cps, more preferably greater than about 6000cps, most preferably greater than the xanthan gum of about 8000cps, and its intersection strain (crossover strain) is less than about 100, more preferably less than about 90, most preferably be less than about 80.Viscosity is to measure under the rotating speed of 10rpm with the Broolfield DV-1 viscometer that has No. 6 rotating shafts.Here said intersection strain be with controlled pressure or strain flow velocity device under the condition of 1rad/s and 25 ℃, measure.The tangent of phase tangent of an angle, δ (tandelta) is to the strain amplitude mapping, and the strain that intersects is the point that the δ tangent equals 1.
The dispersibility of gained heat treatment xanthan gum is improved, and under given temperature and stirring condition, compares the general minimizing 25% of fully decentralized time of gained xanthan gum, more remarkable minimizing 50%, the most remarkable minimizing 70% with the xanthan gum of not heat-treating.
Natural or carried out the character that heat treated xanthan gum can provide typing for hair cosmetic compositions, wherein said make-up composition comprises hair jelly, gel such as hair jelly gel (spray gels), typing become visible (styling lotions), suppurative mastitis, pomade and mousse.The application of xanthan gum not only influences the hardness of hair, but also is very suitable for keeping curling under the high humility situation.Here said high humility situation refers to 22 ℃ temperature and 90% relative humidity.
Because xanthan gum can provide limpid translucent transparency, so it is particularly useful for gel, and since its can be scattered in heat or the cold water and not need and carry out neutralization reaction, so xanthan gum is easy to use.Xanthan gum is for salt and extreme pH, especially in about 2 to 12 pH scope, also has toleration.Last point, therefore xanthan gum energy biodegrade can be flagged as crude.
The hot repair of xanthan gum decorations have improved the simplification of its application, comprise that to be easy to be scattered in the trend that forms flake in the solution simultaneously low.The hot repair decorations also can be used to improve its thickening usefulness and colloform texture, reduce fibroid or the mucus of long flow structure (long texture).In addition, in the four corner of commonly used pH of hair cosmetic compositions and salt, the heat treatment of xanthan gum can increase its viscosity.Different with carbomer, xanthan gum can with anion, cation and non-ionic copolymer compatibility, this just makes it to use preparation with various hair cosmetic additives commonly used.Though xanthan gum uses the character that typing just can be provided separately; but it also can be with some other setting agent be used in combination; wherein said other setting agent comprises polyoxythylenated vinyl acetic acid esters/butenoic acid copolymer without limitation; vinylacetate butenoic acid (90/10) copolymer; vinylacetate/butenoic acid/vinyl neodecanoate terpolymer; N-octyl acrylamide/methacrylate/hydroxypropyl methyl acrylate/acrylic acid/tert-butyl aminoethyl methacrylate copolymer; and vinyl methylether/maleic anhydride (50/50) copolymer that becomes monoesters with butanols or ethanol; acrylic acid/ethyl acrylate/N-tert-butyl-acrylamide copolymer; and poly-(methacrylic acid/acrylic acylamino-methyl propane sulfonic acid); acrylate copolymer; octyl acrylamide/acrylate/butyl nitrilo acetic acid methacrylate copolymer; acrylate/octyl acrylamide copolymer; VA/ crotonates/vinyl Neodeanoate copolymer; poly-(N-vinyl acetamide); poly-(N-vinyl formamide); modified corn starch; kayexalate; season hydroxyethyl-cellulose (polyquaterniums) is as season hydroxyethyl-cellulose-4; season hydroxyethyl-cellulose-7; season hydroxyethyl-cellulose-10; season hydroxyethyl-cellulose-11; season hydroxyethyl-cellulose-16; season hydroxyethyl-cellulose-28; season hydroxyethyl-cellulose-29; season hydroxyethyl-cellulose-46; polyethers-1; polyurethanes; VA/ acrylate/dodecyl methyl acrylate copolymer; adipic acid/dimethylamino hydroxypropyl diethylidene AMP/ acrylate copolymer; methacrylol ethyl betanin/acrylate copolymer; PVP/ dimethyl amino ethyl methacrylate copolymer; the PVP/DMAPA acrylate copolymer; PVP/ ethyl caprolactam/DMAPA acrylate copolymer; caprolactam/PVP/ dimethyl amino ethyl methacrylate copolymer; VA/ butyl maleate/iso-bornyl acrylate copolymer; VA/ crotonates copolymer; acrylate/acrylamide copolymer; VA/ crotonates/vinyl propionic ester copolymer; vinyl pyrrolidone/vinyl acetic acid esters/vinyl propionic ester terpolymer; the VA/ crotonates; cation and amphoteric guar gum; polyvinylpyrrolidone (PVP); polyvinylpyrrolidone/vinylacetic acid ester copolymer; the PVP acrylate copolymer; vinyl acetic acid esters/.beta.-methylacrylic acid/vinyl propionic ester; acrylate/acrylamide; acrylate/octyl acrylamide; acrylate/hydroxy acrylate copolymer; and the Arrcostab of polyvinyl methyl ether/maleic anhydride; diethylene glycol/cyclohexanedimethanol/isophthalate (isophthalates)/sulfoisophthalic acid ester copolymer; vinyl acetic acid esters/butyl maleate and iso-bornyl acrylate copolymer; caprolactam/PVP/ dimethyl amino ethyl methacrylate; the acrylamide copolymer that vinyl acetic acid esters/alkyl maleate half fat/N-replaces; caprolactam/vinyl pyrrolidone/methacryl amidopropyl trimethyl ammonium chloride terpolymer; methacrylate/acrylate copolymer/amine salt; Vinylcaprolactam homopolymer; polyurethane; hydroxypropyl guar gum; hydroxypropyl guar gum hydroxypropyl chlorination three ammoniums (trimmoiumchloride); poly-(methacrylic acid/acrylamide group methyl propane sulfonic acid; polyurethane/acrylate copolymer and hydroxypropyl chlorination three ammonium guar gum, especially acrylate copolymers; octyl acrylamide/acrylate/butyl amino-ethyl methylpropanoic acid ester copolymer; acrylate/octyl acrylamide copolymer; VA/ crotonates/vinyl Neodeanoate copolymer; poly-(N-vinyl acetamide); poly-(N-vinyl formamide); polyurethane; modified corn starch; kayexalate; season hydroxyethyl-cellulose-4; season hydroxyethyl-cellulose-10; and polyurethane/acrylate copolymer.
Also can in hair cosmetic compositions of the present invention, add the additive of dispensable routine so that the character of this some change of combination results.These additives comprise silicone and silicone derivative; Wetting agent; Wetting agent; Plasticizer is as glycerol, ethylene glycol and phthalate ester and ether; Softening agent, lubricant and penetrating agent are as the lanoline chemical compound; Spice and aromatic; The UV absorbent; Dyestuff, pigment and other coloring agent; Corrosion inhibitor; Antioxidant; Put stick (detackifying agents)); Combing auxiliary agent and conditioner; Antistatic additive; Nertralizer; Polishing material; Antiseptic; Protein, protein derivatives and aminoacid; Vitamin; Emulsifying agent; Surfactant; Viscosity modifier, thickening agent and rheology modifier; Gel; Opacifier; Stabilizing agent; Chelating agen; Chelating agent; Pearling agent; Aesthstic reinforcing agent; Fatty acid, aliphatic alcohol and triglyceride; Plant extract; Film former; And clarifier.These additives that are usually used in the hair cosmetic compositions are known in the prior art.The addition of these additives is amounts a spot of, that can effectively finish its function, generally is to calculate with composition total weight, and every part of weight contains has an appointment 0.01 to 10%, and accounts for about 0.01 to 20% of gross weight.
Aesthstic reinforcing agent comprise without limitation starch ocentyl succinic aluminum, modified corn starch, starch ocentyl succinic aluminum (with) dodecanoyl lysine and starch ocentyl succinic aluminum (with) boron nitride.Thickening agent and rheology modifier comprise acrylate/steareth-20 methylene-succinic acid copolymer without limitation; acrylate/ceteth-20 methylene-succinic acid copolymer; modified potato starch; the hydroxypropyl starch phosphate ester; acrylate/amino acrylates/C10-30 alkyl PEG-20 methylene-succinic acid copolymer; carbomer; acrylate/C10-30 alkyl acrylate intersection copolymer; hydroxypropyl cellulose; hydroxyethyl-cellulose; sodium carboxymethyl cellulose; polyacrylamide (with) the C13-14 isoparaffin (with) laureth-7; acrylamide copolymer (with) mineral oil (with) the C13-14 isoparaffin (with) tween (polysorbate 85); hydroxy ethyl methacrylate/acryloyl group (acrylol) dimethyl sodium taurocholate copolymer.
Xanthan gum can be added in the hair cosmetic compositions with any level that required character can be provided.Generally speaking, the amount of the natural xanthan gum that is used is at least about 0.01%, and preferably at least 0.2%, more preferably at least about 1.0% and be less than approximately 20%, preferably be less than approximately 10%, preferredly be less than 3%.In contrast, the use amount of having carried out heat treated xanthan gum is at least about 0.01%, preferably at least about 0.5%, especially preferably at least about 0.75% and be less than approximately 20%, preferably is less than approximately 2%, preferredly is less than about 1.5%.Employed amount not only depends on the desired character that obtains, but also depends on heat treated degree and other additive.For example, can reach identical typing effect by using less xanthan gum and adding another kind of hair fixing copolymer commonly used simultaneously.
Hair cosmetic compositions can be by being scattered in xanthan gum in the water, remaining hair cosmetic component such as any styling polymer, conditioning polymer or other additive of wanting mixed being prepared then with it.
Transmission system is water in most cases.But, also can use solvent.Because environmental legislation restriction VOC (VOCs) is diffused in the atmosphere, so the VOCs diffusate in the hairspray is limited to 55% in some cases, may very fast meeting further be restricted to lower level.VOC calculates with the wt/wt% of hair cosmetic preparation.Here employed VOC contains 1 to 10 carbon atom, and this compounds has the vapour pressure of 0.1mm Hg at least under 20 ℃, and has photochemical activity.Therefore water can substitute at least a portion VOC usually, has become component bigger in the hair cosmetic compositions.
Generally speaking, the amount of solvent can be less be higher than 55% to the content of VOC.For mousse, the amount of solvent is general even can be less be higher than 6% to the content of VOC.Though can use any solvent well known in the prior art, this solvent generally can be rudimentary (C1-C4) alcohol, particular methanol, ethanol, propanol, isopropyl alcohol or butanols.
VOC also can comprise optional propellant.Such propellant comprises ether without limitation, as dimethyl ether; One or more lower boiling hydrocarbons such as C3-C6Straight chain and branched-chain hydrocarbons, for example propane, butane and iso-butane; Halogenated hydrocarbon, as the hydrogenated carbon fluorine compounds, for example, and 1,1-Difluoroethane and 1,1,1, the 2-tetrafluoroethane exists with the form of liquefied gas; And Compressed Gas, for example nitrogen, air and carbon dioxide.
Hair cosmetic compositions can be prepared character to obtain wanting with xanthan gum.The amount that for example can adjust xanthan gum is with the hardness that obtains wanting and the reservation degree that curls.Generally speaking, the hair gel has at least about 5, the viscosity of 000cps, more preferably at least about 6, the viscosity of 000cps, most preferably at least about 8, the viscosity of 000cps, at least about 70%, preferably at least about 80%, most preferably, be not higher than 100NTU at least about 2 hours high humiditys of 90% reservation degree that curls, preferably be not higher than 50NTU, most preferably be not higher than the turbidity of 30NTU.
Embodiment
The following examples are that the present invention will be further elaborated and explain, and should not be counted as restriction that the present invention is carried out.Employed percentage ratio is all based on w/w.Embodiment 1-contains natural and has carried out the hair styling gel of heat treated xanthan gum
Preparation 1 preparation 2 component %w/w %w/wA part propylene acid ester copolymers1(50%) 8.0 8.0 deionized water 40.0 40.0 amino methyl propanol20.56 0.56B part xanthan gum31.0-carried out heat treated xanthan gum4An amount of segment angle albumen 0.2 0.2 propane diols 2.0 2.0 polysorbas20s of an amount of anticorrisive agent of-1.0 deionized waters50.5 0.5 aromatic0.10.1
100 1001Balance 0/55 (National Starch and Chemical Co.)2AMP-95 (Angus)3Keltrol T (Kelco)4Carried out heat treated Keltrol T (fluidized-bed reactor under 235,60 minutes)5Polysorbas20 (ICI surfactant)
The component of A part is merged, mix until clarification.In the another one container, with xanthan gum or carried out heat treated xanthan gum and under appropriateness stirs, be scattered in the water and (for preparation 1, under 700rpm, mixed 30 minutes, for preparation 2, under 700rpm, mixed 10 minutes, obtain uniform B part).Then A part and C part are merged under appropriateness stirs, add the C part then.
Xanthan gum and carried out heat treated xanthan gum and can both be scattered in cold water.But, carried out heat treated xanthan gum than the easier dispersion of natural xanthan gum.In addition, use xanthan gum and do not need to carry out neutralization.
Preparation 1 obtains a kind of clarification, colourless mucus (Brookfield viscosity: use sprindle#4@20rpm, 3200cps).Preparation 2 obtains a kind of clarification, colourless gel (Brookfield viscosity: use sprindle4@20rpm, 8200cps).The ratio of viscosities preparation 1 of preparation 2 is high a lot, and this shows that having carried out heat treated xanthan gum can provide better thickening usefulness.Compare with preparation 1, preparation 2 is also more as gel, or has viscoloid structure shorter and still less.The clarity of two kinds of preparations is all fine.The various hair styling gels of embodiment 2-
Preparation 3 preparations 4 preparations 5 preparations 6 preparations 7 component A part %w/w %w/w %w/w %w/w %w/w acrylate copolymers1(50%) 8.0----octyl acrylamide/acrylate-4.0---/butyl amino-ethyl methacrylate copolymer2Acrylate/octyl acrylamide copolymer3--4.0--octyl acrylamide/acrylate/---4.0-butyl amino-ethyl methacrylate copolymer4PVP5----4.0 deionized water 40.0 40.0 40.0 40.0 40.0 amino methyl propanol60.56 0.94 1.13 0.77-B has partly carried out heat treated xanthan gum70.85 0.85 0.85 0.85-carbomer8An amount of an amount of antiseptic of----0.5 amino methyl propanol----0.29 deionized waterIn right amountIn right amountIn right amountIn right amountIn right amount
100 100 100 100 1001Balance 0/55 (National Starch and Chemical Co.)2Balance 47 (National Starch and Chemical Co.)3Amphomer HC (National Starch and Chemical Co.)4Amphomer (National Starch and Chemical Co.)5PVP K-30 (ISP)6AMP-95 (Angus)7Carried out heat treated Keltrol T (fluidized-bed reactor, under 235 °F, 60 minutes9Carbopol 940 (BF Goodrich)
Preparation 3-6 obtains clarifying translucent hair gel, its viscosity＞7000cps (Brookfield viscosity sprindle#4@20rpm).In contrast, preparation 7 is basic preparations the most frequently used in the commercial hair fixing.This embodiment has shown various anionic shaped copolymers and the compatibility of having carried out heat treated xanthan gum.
Preparation 8 preparations 9 preparations 10 preparations 11 component A part %w/w %w/w %w/w %w/w acrylate copolymers1(50%) 8.0---octyl acrylamide/acrylate/butyl amino-ethyl methacrylate-4.0--copolymer2Acrylate/octyl acrylamide copolymer3--4.0-octyl group acrylic acid-acrylamide/acrylate/butyl amino-ethyl methacrylate---4.0 copolymer4Deionized water 40.0 40.0 40.0 40.0 amino methyl propanol50.56 0.94 1.13 0.77B part carbomer60.5 an amount of antiseptic of 0.5 0.5 0.5 amino methyl propanol, 0.29 0.29 0.29 0.29 deionized waterIn right amountIn right amountIn right amountIn right amount
100??????100???????100??????1001Balance?0/55(National?Starch?and?Chemical?Co.)2Balance?47(National?Starch?and?Chemical?Co.)3Amphomer?HC(National?Starch?and?Chemical?Co.)4Amphomer(National?Starch?and?Chemical?Co.)5AMP-95(Angus)6Carbopol?940(BF?Goodrich)
What preparation 8-11 obtained is low viscous troubled liquor mixture.This shows that various anionic shaped copolymers and carbomer are incompatible.
Preparation 12 preparations 13 preparations 14 preparations 15
Component
％w/w???％w/w????％w/w????％w/w
Xanthan gum 2.0---
Carried out heat treated xanthan gum-1.0 2.0 0.85
Deionized water is an amount of
AntisepticIn right amountIn right amountIn right amountIn right amount
100??????100??????100?????100
Preparation 12-15 shows that hair styling gel can only contain the xanthan gum of wanting level or carry out heat treated xanthan gum, and water and antiseptic.Owing to can improve the solution rheology, thus can use less amount carrying out heat treated xanthan gum, and can more be resembled the product of gel.
Preparation 21 preparations 22 preparations 23
Component
A part %w/w %w/w %w/w
Acrylate copolymer1(50%) 8.0 4.0 8.0
Amino methyl propanol 0.56 0.28 0.56
Deionized water 40.0 40.0 40.0
The B part
Carried out heat treated xanthan gum21.0 1.0-
Xanthan gum3--1.0
Deionized water is an amount of an amount of
AntisepticIn right amountIn right amountIn right amount
100 100 1001Balance 0/55 (National Starch and Chemical Co.)2Carried out heat treated Keltrol T (fluidized-bed reactor, under 235,60 minutes)3Keltrol T (Kelco)
These preparations have further been represented the xanthan gum under the different application level and have been carried out the different components of heat treated xanthan gum and anion and nonionic shaping copolymer.
Preparation 26 preparations 27 preparations 28 preparations 29 preparations 30
Component
A part %w/w %w/w %w/w %w/w %w/w
Acrylate copolymer1(50%) 8.0 8.0 8.0 8.0 8.0
Amino methyl propanol 0.56 0.56 0.56 0.56 0.56
Deionized water 40.0 40.0 40.0 40.0 40.0
The B part
Carried out heat treated xanthan gum21.0----
Carried out heat treated xanthan gum3-1.0---
Carried out heat treated xanthan gum4--1.0--
Carried out heat treated xanthan gum5---1.0-
Carried out heat treated xanthan gum6----1.0
Deionized water is an amount of an amount of
AntisepticIn right amountIn right amountIn right amountIn right amountIn right amount
100 100 100 100 1001Balance 0/55 (National Starch and Chemical Co.)2Carried out heat treated Keltrol T (fluidized-bed reactor, under 220,240 minutes)3Carried out heat treated Keltrol T (fluidized-bed reactor, under 220,150 minutes)4Carried out heat treated Keltrol T (fluidized-bed reactor, under 228,90 minutes)5Carried out heat treated Keltrol T (fluidized-bed reactor, under 235,30 minutes)6Carry out heat treated Keltrol T (baking oven, under 250,120 minutes) preparation 26-30 and represented to use the hair gel that under different condition, has carried out heat treated xanthan gum sample.
Preparation 31 preparations 32 preparations 33 preparations 34 preparations 35 component A part %w/w %w/w %w/w %w/w %w/w are poly-, (N-vinyl acetamide) 3.0 1.0---poly-, (N-vinyl formamide)--3.0--polyurethane---3.0-modified corn starch1----1.0 deionized water 40.0 40.0 40.0 40.0 40.0B have partly carried out heat treated xanthan gum21.0 an amount of an amount of antiseptic of 1.0 1.0 1.0 1.0 deionized watersIn right amountIn right amountIn right amountIn right amountIn right amount
100 100 100 100 1001Amaze (National Starch and Chemical Co.)2Carried out heat treated Keltrol T (fluidized-bed reactor, under 235,60 minutes)
These embodiment represent the hair gel with the shaping copolymer preparation of having carried out heat treated xanthan gum and various different application levels.
Preparation 36 preparations 37 component A part %w/w %w/w season hydroxyethyl-celluloses-410.15-Jiization hydroxyethyl-cellulose-102-0.15 deionized water 40.0 40.0B have partly carried out heat treated xanthan gum31.0 an amount of antiseptic of 1.0 deionized watersIn right amountIn right amount
100 1001Celquat H-100 or L-200 (National Starch and Chemical Co.)2Celquat SC-230M or Celquat SC-240C (National Starch and Chemical Co.)3Carried out heat treated Keltrol T (fluidized-bed reactor, under 235,60 minutes)
These preparations represent that cationic styling agent/conditioning copolymer can low-levelly use with having carried out heat treated xanthan gum, produce clarifying, have good performance and a rheol hair gel.
Preparation 38 preparations 39 preparations 40 preparations 41 component A part %w/w %w/w %w/w %w/wGellan Gum10.3 0.3--carbomer2--0.1 0.3 deionized water 40.0 40.0 40.0 40.0 amino methyl propanol3--in right amount partly carried out heat treated xanthan gum to pH6B in right amount to pH641.0-1.0-xanthan gum5An amount of antiseptic of-1.0-1.0 deionized watersIn right amountIn right amountIn right amountIn right amount
100 100 100 1001Kelcogel (Kelco)2Carbopol 940 (BF Goodrich)3AMP-95 (Angus)4Carried out heat treated Keltrol T (fluidized-bed reactor, under 235,60 minutes)5Keltrol T (Kelco)
Preparation 38-41 has shown that the hair gel can be by with xanthan gum or carried out heat treated xanthan gum and other rheology modifier/thickening agent, as Gellan glue or carbomer in conjunction with being prepared.
The embodiment 3-hair styling gel performance (I) and the reservation degree that curls
Curling retention to hair setting composition of the present invention is measured, and three kinds of primary commercial hair styling gel compositionss that it had " limit (ultimate) " hair hold facility with these are compared.The known curling reservation of those skilled in the art directly keeps with the hair pattern or keeps relevant, is one of most important character of hair fixing product.This experiment is to place to carry out in 2 hours under the relative humidity of 72 (22 ℃) and 90%.This method can be carried out statistical analysis to the preparation variable.Being calculated as follows of the percent retention of curling: curling keeps %=100 * (L-Lt) (L-Ln), the length of L=hair full extension wherein, L0The curling length of=beginning, Lt=curling length in preset time during t.
This experiment is with 10 " the long bundle (9 parallel assay bundles of every group of sample) of the European virgin's sepia hair of long * 2 grams carries out.The wet topknot of cleaning is carried out combing, be entangled with and too much moisture to remove.The hair gel sample of 0.5 gram is applied on every bundle hair, on its " being applied to " hair gently, and the combing smoothness.With1/2 "The politef of diameter (Teflon) axle is produced curling, places it in the pallet, is placed on dried overnight in the baking oven.The curly hair of doing is taken out from baking oven, make it to be cooled to room temperature.Allow on this curly hair dangles transparent curling retention plate from the topknot end.Putting the initial length that plate and curly hair are measured curly hair before entering environmental chamber.Write down the length of perming respectively at the 15th minute, 30 minutes, 60 minutes, 90 minutes and 2 hours.Calculate curly hair reservation degree then.The result of the curly hair reservation degree after 2 hours has been made into table 1.This result shows that all contain the hair setting composition of xanthan gum, especially contains the hair composition that has carried out heat treated xanthan gum, compares with current commodity, all shows the advantage of interest in the reservation of curling.This is good brings out the retention of curling and can realize by the styling polymer that adds or do not add other.The type of the setting agent of Jia Ruing and quantity can not the appreciable impact xanthan gum or have been carried out the curling reserve capability that heat treated xanthan gum showed in addition.When replacing xanthan gum with carbomer, when especially having carried out heat treated xanthan gum, the curling reservation result who obtains significantly reduces.
Table 1
| The hair styling gel compositions | Average curling keeps time=2 hour T=72 of %: RH=90% |
| 1% has carried out heat treated xanthan gum (preparation 13) | ????91 |
| 2% has carried out heat treated xanthan gum (preparation 12) | ????93 |
| 4% acrylate copolymer+1% has carried out heat treated xanthan gum (preparation 21) | ????93 |
| 4% acrylate copolymer+1% xanthan gum of not heat-treating (preparation 23) | ????91 |
| 2% acrylate copolymer+1% has carried out heat treated xanthan gum (preparation 22) | ????89 |
| 3%PVP+1% has carried out heat treated xanthan gum (preparation 18) | ????95 |
| 4%PVP+1% has carried out heat treated xanthan gum (preparation 17) | ????84 |
| 4%PVP+0.5% carbomer (preparation 16) | ????48 |
| 3% poly-(N-vinyl acrylamide)+1% has carried out heat treated xanthan gum (preparation 31) | ????93 |
| 1% poly-(N-vinyl acrylamide)+l% has carried out heat treated xanthan gum (preparation 32) | ????91 |
| Commercial hair gel I (comprising PVP, carbomer and other additive) | ????34 |
| Commercial hair gel II (comprising the PVP/VA copolymer, carbomer and other additive) | ????47 |
| Commercial hair gel III (comprising the PVP/VA copolymer, PVP, carbomer and other additive) | ????11 |
Embodiment 4-hair styling gel character, hardness and other attribute
Test 1-the subjective assessment of hair setting composition of heat treated xanthan gum compositions that comprised the carrying out that contain PVP and carbomer
The coffee-like bundle of hair group in Europe (10 " long, 2 grammes per square metres) match with 0.5 gram hair setting composition, by 8 judging panels, estimate for a series of character of every group of sample to the marking of 5 (best) with 1 (the worst).Tested attribute of performance group comprises hardness, moistening sense of touch, wet comb property, dry finish, dry sense of touch, does comb property, dry shattered crack (dry flake) and antistatic behaviour.Hardness is to represent with the flintiness of sending out body, and it also is the measurement of maintenance dose (amout of hold) that hair setting composition is produced.This class testing and similar sense organ test are the personal nursing well known to those of ordinary skill in the art and the performance evaluation of cosmetics.The summary of result of the test sees Table 2.It is all better in hardness, gloss, the combination property done aspect comb property, wet comb property, shattered crack, antistatic and the sense of touch to contain the hair composition that carried out heat treated xanthan gum, or can with PVP/ carbomer hair gel phase ratio.When the amount of the styling polymer that adds is identical, all carrying out that comprises gel heat treated xanthan gum can both provide than the better hardness of PVP/ carbomer.Preparation 1 also provides moistening sense of touch, wet comb property, dry sense of touch and the dried comb property of improving comparable with the PVP/ carbomer gel.
The result of table 2. subjective test 1
| Attribute | Based on the average mark of 1 (the worst) to 5 (best) equal interval scale |
| Preparation 3 | Preparation 4 | Preparation 5 | Preparation 7 |
| Moistening sense of touch | ?3.8??S | ??2.7??NS | ??2.8??NS | ??2.8 |
| Wet comb property | ?3.8??S | ??2.5??NS | ??2.6??NS | ??2.9 |
| Dry finish | ?3.4??NS | ??2.7??NS | ??3.1??NS | ??3.2 |
| Hardness | ?3.8??S | ??3.6??S | ??3.6??S | ??2.3 |
| Do comb property | ?3.9??S | ??2.8??NS | ??2.7??NS | ??3.2 |
| Dry shattered crack | ?2.8??NS | ??3.0??NS | ??3.1??NS | ??3.2 |
| Antistatic | ?1.9??NS | ??2.1??NS | ??2.2??NS | ??2.1 |
| Dry sense of touch | ?3.4??S | ??2.9??NS | ??2.7??NS | ??2.7 |
S=sample and reference substance have the nature difference that statistical significance is arranged significantly under 95% confidence level
NS=sample and reference substance do not have the nature difference that statistical significance is arranged significantly under 95% confidence level
Test 2
Six kinds of hair setting compositions and three kinds of main commercial hair styling gels are used for number of people topknot, with the subjective scoring grade attribute of performance group of hardness, gloss and dry shattered crack are assessed then.Balanced Incomplete Block scheme is used in the assessment of this sense organ, and this scheme is that the intensity with set of properties is to mark in the basis.Nine experts estimate bipartite nine samples.For every pair of sample, 1 fen lower hardness of expression, higher dry shattered crack and lower gloss, the higher hardness of expression in 2 fens, lower dry shattered crack and higher gloss.On the basis of this design, preparation amounts to 36 (or to) samples.Calculate the scoring summation of every each attribute of batch sample.The scoring summation that is higher than minimum significant difference (LSD=3.5) show more than 90% sample all with our conjecture or to simulate desired sample immediately different separately.This topknot preparation process is identical with employed process in subjective test 1.The summary of this result of the test sees Table 3.Higher sequence runtime value shows each set of properties preferable performance.The sequence summation is considered to do not have significant difference under 90% confidence level less than the difference of LSD (3.5).This evaluation test is for tendency or the style that shows sample room designs, rather than the specific paired comparison sample that is used for.Commercialization gel phase ratio with main comprises xanthan gum, and the hair composition that has especially carried out heat treated xanthan gum shows hardness equivalence or better, gloss and shattered crack set of properties.
The result of table 3. subjective test 2
| The hair styling gel compositions | Scoring summation (LSD=3.5) |
| Hardness | Gloss | Shattered crack |
| Commercialization gel I (comprising PVP, carbomer, and other additive) | 12 | ?11 | ?12 |
| Commercialization gel II (comprising the PVP/VA copolymer, carbomer, and other additive) | 11 | ?12 | ?12 |
| Commercialization gel III (comprising the PVP/VA copolymer, PVP, carbomer, and other additive) | 8 | ?12 | ?9 |
| 4%PVP+0.5% carbomer (preparation 16) | 15 | ?9 | ?10 |
| 4%PVP+1% has carried out heat treated xanthan gum (preparation 17) | 15 | ?13 | ?11 |
| 4% acrylate copolymer+1% has carried out heat treated xanthan gum (preparation 21) | 11 | ?11 | ?15 |
| 1% has carried out heat treated xanthan gum (preparation 13) | 11 | ?15 | ?13 |
| 2% acrylate copolymer+1% has carried out heat treated xanthan gum (preparation 22) | 12 | ?12 | ?14 |
| 4% acrylate copolymer+1% xanthan gum of not heat-treating (preparation 23) | 13 | ?13 | ?12 |
The mensuration of embodiment 5-colloform texture
Pressure viscosity agent Rheometrics DSR SR-200 with control carries out all mensuration.Under 25 ℃,, in 2 to 1000Pa pressure, carry out the oscillatory shear pressure scanning, obtain cross stress (crossover stress) with the frequency of 1rads/s.The phase tangent of an angle, the δ tangent is mapped to strain amplitude, and the strain that intersects is defined in the strain at tand=1 place.This method is only applicable to have in δ tangent＜1 under the low pressure and descends then and have material greater than 1 value under high pressure.This intersection strain is generally low for the material with short structure, and the material height of long in having, coherent or viscosity structure.This intersection strain data of the hair gel of selecting sees Table 4.The shortcoming that contains the main commercialization hair gel of carbomer and PVP also is used as contrast and measures.Have been found that good concordance is arranged between the subjective evaluation of cross stress data and colloform texture.As shown in table 4, the shortcoming of xanthan gum gel depends on heat treated degree.Untreated xanthan gum provides more tacky, longer colloform texture.Higher treatment temperature and/or longer processing time help to provide the colloform texture shorter, that viscosity is lower.When selecting suitable heat-treat condition, the short colloform texture that can significantly improve, this kind gel approaches the most frequently used carbomer gel (a kind of Polyacrylate thickeners).
Table 4
| The hair styling gel compositions | Intersection strain (%) |
| 4% acrylic copolymer+1% xanthan gum of not heat-treating (preparation 23) | ????155 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Hua @220,120 minutes) | ????131 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @220,150 minutes) | ????88 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @228,60 minutes) | ????150 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @228,90 minutes) | ????120 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @235,60 minutes) | ????96 |
| 1% has carried out heat treated xanthan gum (Liu Huachuan @235,60 minutes) | ????82 |
| Commercialization hair gel (comprising PVP, carbomer, and other additive) | ????73 |
The transparency of embodiment 6-hair gel is measured
The transparency of hair gel is measured with Hach Laboratory Turbidimeter (Model 2100N).This instrument is designed to measure the turbidity from 0 to 4000NTU (Nephelometric turbidity unit), and this instrument has automatic range and selects and the arithmetic point keyed jointing.Low turbidity reads is represented the high grade of transparency.Comprising xanthan gum is listed in the table 5 with the turbidity value that has carried out the translucent hair gel of heat treated xanthan gum.Three kinds clearly the turbidity value of commercialization hair gel also be listed as a reference.
Table 5
| The hair styling gel compositions | Turbidity (NTU) |
| 4% acrylate copolymer+1% xanthan gum of not heat-treating (preparation 19) | ????18.5 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @220,120 minutes) | ????24.2 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @220,150 minutes) | ????25.2 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @228,60 minutes) | ????23.7 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @228,90 minutes) | ????24.5 |
| 4% acrylic copolymer+1% has carried out heat treated xanthan gum (Liu Huachuan @235,60 minutes) | ????25.3 |
| 1% has carried out heat treated xanthan gum (Liu Huachuan @235,60 minutes) | ????24.2 |
| Commercialization hair gel (comprising PVP, PVP/VA, carbomer, and other additive) | ????15.0 |
| Commercialization hair gel (comprising PVP, carbomer, and other additive) | ????14.0 |
| Commercialization hair gel (comprising PVP, carbomer, and other additive) | ????10.9 |
| Deionized water | ????0.04 |
Embodiment 7-contains the hair jelly gel of xanthan gumComponent %w/w %w/wA part propylene acid ester copolymer
1(50%) 8.0 8.0 deionized water 40.0 40.0 amino methyl propanol
20.56 0.56B part xanthan gum
30.5-carried out heat treated xanthan gum
4An amount of an amount of the addition of C segment angle of anticorrisive agent albumen 0.2 0.2 propane diols 2.0 2.0 polysorbas20s of-0.3 deionized water
40.5 0.5 aromatic 0.1 0.1
1Balance 0/55 (National Starch and Chemical Co.)
2AMP-95 (Angus)
3Keltrol T (Kelco)
4Carried out heat treated Keltrol T (fluidized-bed reactor, under 235,60 minutes)
5Polysorbas20 (ICI surfactant)
Embodiment 8-contain the hair mousse of xanthan gum
AContain the hair mousse that xanthan gum does not contain surfactantComponent %w/w
Acrylate copolymer1(50%) 8.0
Deionized water 40.0
The amino methyl propanol20.56
Xanthan gum30.4
Deionized water is an amount of
Antiseptic is an amount of
The C part
Iso-butane/propane46.01Balance 0/55 (National Starch and Chemical Co.)2AMP-95 (Angus)3Keltrol T (Kelco)4Propellant A-46B. contain the 6%VOC mousse that has carried out heat treated xanthan gumComponent %w/w %w/w %w/w has carried out heat treated xanthan gum10.6 0.6 0.6 propylene glycol, 1.0 1.0 1.0 Brijs 3020.4 0.2-DC 19330.2 0.2 0.2Dowicil 20040.2 0.2 0.2 deionized waters, 91.6 91.8 92.0 propellant (Propellant) A-4656.06.06.0
100 100 1001Carried out heat treated ADM xanthan gum (fluid bed, 220,180 minutes)2Laureth-4 (Uniqema)3Dimethicone Copolyol (Dow Corning)4Quaternium-15 (Dow Chemical Co.)5Iso-butane/propane
Xanthan gum is applicable to the hair styling mousse of any kind, comprises the 6%VOC mousse and does not contain the mousse of surfactant.Except the support effect that mousse is provided, the sense of touch that xanthan gum helps to nurse one's health and is not clamminess.Embodiment 9-hair styling mousseComponent %w/w kayexalate110.0 polysorbas2020.4Nonoxynol-1530.4Oleth-1040.4 xanthan gum50.5 deionized water 68.3SD alcohol 40 10.0 iso-butanes10.0
100
1Flexan?130(National?Starch?and?Chemical?Co.)
2Polysorbas20 (Uniqema)
3Tergitol?Np-15(Uniqema)
4Brij 97 (Uniqema)
5Keltrol T (Kelko)Embodiment 10-aerosol hair sprayComponent %w/w octyl acrylamide/acrylate/butyl amino-ethyl methacrylate copolymer18.0 amino methyl propanol21.38 xanthan gum30.3 an amount of dimethyl ether of the deionized water 45.32SD alcohol an amount of antiseptic of 40 20.0 aromatic25.0
1001Balance 47 (National Starch and Chemical Co.)2AMP (Angus)3Keltrol T (Kelco)Embodiment 11-hair fixing and conditioning suppurative mastitisComponent %w/wA part deionized water has carried out heat treated xanthan gum in right amount10.7Quaterium-420.15B partial glycerol stearate32.0 an amount of antiseptic of jojoba oil 2.0C part aromaticIn right amount
1001Carried out heat treated Keltrol T (fluidized-bed reactor, 235,60 minutes)2Celquat H-100 (National Starch and Chemical Co.)3Cerasynt SD (ISP)Embodiment 12-has carried out the various viscosity of heat treated xanthan gum and the strain that intersects
Severally carried out heat treated xanthan gum and tested employed in the above-described embodiments to measure their viscosity in 1% aqueous solution and to intersect strain.Xanthan gum can have been bought, and the result is as follows.
| Sample | Viscosity*(cps) | Intersection strain (%) |
| At 220 ADM xanthan gum of having handled 180 minutes | ?35600 | ?25 |
| At 235 Keltrok T that handled 60 minutes | ?13100 | ?82 |
| At 220 Keltrok T that handled 240 minutes | ?18200 | ?35 |
*Viscosity is with the Brookfield DV-1 viscometer that has Sprindle#6@, measures under the condition of 10rpm
Additional embodiment
1. the hair cosmetic compositions that comprises the xanthan gum of the effective dose of finalizing the design.
2. as enforcement scheme 1 described compositions, wherein said xanthan gum has been carried out heat treatment, and this heat treatment is to be less than about 25%, temperature in moisture to carry out under at least about 60 ℃ condition, carries out at least 30 minutes.
3. as enforcement scheme 2 described compositionss, it is characterized in that used temperature is at least 100 ℃.
4. as enforcement scheme 3 described compositionss, it is characterized in that used temperature is at least 105 ℃.
5. as enforcement scheme 2 described compositionss, it is characterized in that this moisture is less than about 8%.
6. as enforcement scheme 3 described compositionss, it is characterized in that this moisture is less than about 1%.
7. as enforcement scheme 2 described compositionss, it is characterized in that this heat treatment carried out at least about 1 hour.
8. as enforcement scheme 3 described compositionss, it is characterized in that this heat treatment carried out at least about 2.5 hours.
9. as enforcement scheme 2 described compositionss, it is characterized in that this heat treatment be moisture be less than about 1% and temperature be at least under about 105 ℃ and carry out at least about 2.5 hours.
10. as enforcement scheme 1 described compositions, it is characterized in that said composition is selected from hair jelly, mousse, becomes visible, suppurative mastitis, pomade and gel.
11., it is characterized in that said composition is a gel as enforcement scheme 10 described compositionss.
12. as implementing the described compositions of scheme l, it is characterized in that its viscosity is at least about 8000cps, the turbidity that the high humility at least about 80% is curled the reservation degree and is not higher than 100NTU (Nephelometric turbidity unit).
13. as enforcement scheme 1 described compositions, said composition further comprises second kind of styling polymer.
14. as enforcement scheme 13 described compositionss, wherein said second kind of styling polymer is selected from acrylate copolymer, octyl acrylamide/acrylate/butyl amino-ethyl methacrylate copolymer, acrylate/octyl acrylamide copolymer, VA/ crotonates/vinyl Neodeanoate copolymer, poly-(N-vinyl acetamide), poly-(N-vinyl formamide), polyurethane, modified corn starch, kayexalate, season hydroxyethyl-cellulose-4, season hydroxyethyl-cellulose-10 and polyurethane/acrylate copolymer.
15. as enforcement scheme 2 described compositionss, wherein said compositions is a gel.
16. as enforcement scheme 15 described compositionss, said composition further comprises second kind of styling polymer.
17. as enforcement scheme 16 described compositionss, wherein said second kind of styling polymer is selected from acrylate copolymer, octyl acrylamide/acrylate/butyl amino-ethyl methacrylate copolymer, acrylate/octyl acrylamide copolymer, VA/ crotonates/vinyl Neodeanoate copolymer, poly-(N-vinyl acetamide), poly-(N-vinyl formamide), polyurethane, modified corn starch, kayexalate, season hydroxyethyl-cellulose-4, season hydroxyethyl-cellulose-10 and polyurethane/acrylate copolymer.
18. preparation is as enforcement scheme 1 described method for compositions, this method comprises xanthan gum is scattered in the water; Mix with other hair cosmetic composition then.
19. preparation is as enforcement scheme 2 described method for compositions, this method comprises xanthan gum is scattered in the water; Mix with other hair cosmetic composition then.
20. preparation is as enforcement scheme 15 described method for compositions, this method comprises xanthan gum is scattered in the water; Mix with other hair cosmetic composition then.
21. one kind for hair provides the method for typing character, this method comprises the compositions that applies as enforcement scheme 1.
22. the method that the reservation degree that curls is provided under high humidity, this method comprises the compositions that applies as enforcement scheme 1.
23., it is characterized in that said composition is the hair mousse that does not contain surfactant as enforcement scheme 1 described compositions.
24. a hair cosmetic compositions is characterized in that this setting agent is made up of xanthan gum substantially.
25. as enforcement scheme 24 described compositionss, it is characterized in that said composition is selected from hair jelly, mousse, becomes visible, suppurative mastitis, pomade and gel.
26., it is characterized in that said composition is a gel as enforcement scheme 25 described compositionss.
27. as enforcement scheme 24 described compositionss, it is characterized in that its viscosity is at least about 8000cps, the turbidity that the high humility at least about 80% is curled and kept and be not higher than 100NTU (Nephelometric turbidity unit).
28., it is characterized in that said composition is the hair mousse that does not contain surfactant as enforcement scheme 24 described compositionss.
29. as enforcement scheme 1 described compositions, xanthan gum wherein has at least about the viscosity of 4000cps in 1% aqueous solution and is less than about 100 intersection strain.
30. as enforcement scheme 29 described compositionss, wherein said xanthan gum has at least about the viscosity of 6000cps and is less than about 90 intersection strain.
31. as enforcement scheme 29 described compositionss, wherein said xanthan gum has at least about the viscosity of 8000cps and is less than about 80 intersection strain.
32. as enforcement scheme 29 described compositionss, wherein said compositions is a gel.
33., it is characterized in that said composition further comprises second kind of setting agent polymer as enforcement scheme 32 described compositionss.
34. as enforcement scheme 32 described compositionss, wherein said second kind of styling polymer is selected from acrylate copolymer, octyl acrylamide/acrylate/butyl amino-ethyl methacrylate copolymer, acrylate/octyl acrylamide copolymer, VA/ crotonates/vinyl Neodeanoate copolymer, poly-(N-vinyl acetamide), poly-(N-vinyl formamide), polyurethane, modified corn starch, kayexalate, season hydroxyethyl-cellulose 4, season hydroxyethyl-cellulose-10 and polyurethane/acrylate copolymer.