CN102144955A - Polymer conditioner for hairs as well as preparation method and application thereof - Google Patents
Polymer conditioner for hairs as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a polymer conditioner for hairs as well as a preparation method and an application thereof. The preparation method comprises the following steps: adding deionized water into a reaction kettle; adding cationic monomer, anionic monomer, nonionic monomer and functional monomer under stirring; uniformly stirring, regulating the pH to be between 6.00 and 7.00 with a pH regulating agent; stirring and heating to the temperature of between 65 and 85 DEG C, adding an initiator and a chain transfer agent to react for 5 to 8 hours, cooling to room temperature, and standing for 12 to 15 hours; and stirring and heating to the temperature of between 55 and 65 DEG C, vacuumizing in reduced pressure, adding polyether-polysiloxane, and keeping on stirring for 3 to 5 hours to obtain a target product. In the polymer conditioner, the viscosity at 25 DEG C is between 6,000 and 20,000mpa.s, and the content of effective substances is between 15 and 40 percent. The polymer conditioner for hairs can be applied to shampoos to sufficiently play roles of synergic function of different ions and adsorption function of quaternary ammonium nitrogen and improve the dry/wet combing performance and static resistance.
Description
Technical field
The present invention relates to a kind of preparation method and application of conditioner for hair, particularly a kind of preparation method and application of hair macromolecule conditioner.
Background technology
In the last few years, had one's hair wash in the whole world, the hair products market development is swift and violent, equally also makes people stronger to the demand of top grade hair washing, hair conditioner.In the face of being growing more intense of the market competition, provide excellent more product to become the problem that all manufacturers must face to people.Under the base starting material room for improvement condition of limited of hair washing, hair products, develop novel conditioner or improve the quality that has conditioner now becoming particularly important.
Domestic conditioner for hair commonly used has the conditioner of cation polyquaternary ammonium salt, quaternary ammonium salt, type siloxane and other types at present.They have some common effects is exactly to allow hair when washing and wash easily combing of back (comprising wet comb and doing the comb performance), a softer and smoother touch, makes hair be rich in gloss.
The cation polyquaternary ammonium salt that generally uses has at present: polyquaternary ammonium salt-6, polyquaternary ammonium salt-7, polyquaternary ammonium salt-10, polyquaternary ammonium salt-39, polyquaternary ammonium salt-47 and cation guar gum etc.
Cation polyquaternary ammonium salt such as polyquaternary ammonium salt-6, polyquaternary ammonium salt-7, polyquaternary ammonium salt-39, polyquaternary ammonium salt-47 are because the cost performance height is widely-used as conditioner.This series products mostly is homopolymer or the cationic/nonionic binary polymer or the cationic/nonionic/anion ter-polymers of cationic monomer.By design to cationic monomer, non-ionic monomer, anionic monomer, function monomer, can obtain the CHARGE DISTRIBUTION rule, give full play to the synergism of different ions and the adsorption of quaternary nitrogen, make it have excellent doing/wet cardability, antistatic behaviour.
Quaternary ammonium compound can be widely used in hair washing, hair care conditioning, and it also can be subdivided into three classes, that is: alkyl quaternary ammonium salts, ethoxylated quaternary and esters quaternary ammonium salt.The alkyl quaternary ammonium salts compounds is mainly used in hair conditioner as 1631,1831,1227 etc., is used with aliphatic alcohol usually, can significantly improve the lubricated flexibility that reaches of hair; The dissolubility of ethoxylated quaternary is relevant with oxyethyl chain, is often used as the conditioning additive.What of cardability and ethoxylate molecule are relevant, ethoxylate molecule the more, its cardability is relatively poor relatively; The quaternary ammonium salt that contains ester group belongs to the good type raw material of environment, for conditioning dried, moist hair, all can play improvement effect preferably.
Articles for use market is leading still based on anion surfactant or non-ionic surface active agent owing to have one's hair wash at present, defend the doctrine, when quaternary ammonium salt and polyquaternary ammonium salt compounds use in prescription, should be noted that the collision problem of prescription, prevent the unsettled situation of prescription.
The type siloxane conditioner has amino modified siloxanes, alkylsiloxane, polyether silicone, quaternized siloxanes etc.; siloxanes has the volatility of appropriateness; can on skin, hair, form fine and smooth, uniform organosilicon protective layer; therefore using silicone conditioning agent in hair product mainly is the conditioning performance that improves hair product with it, gives hair glossiness, smoothness, pliability.Because siloxanes mostly is polymeric macromolecular material, be difficult in the water-soluble equal solvent, therefore usually silicone conditioning agent and surfactant are used for the compositions of hair product by the form of emulsifying formation emulsion or microemulsion, as the product of companies such as Dow Corning.Because the granule of silicone emulsion has certain size, therefore in the compositions of hair product, also will consider the stability problem of emulsion, composite thickening agent of meeting or suspending agent improve stability in hair product usually.
Summary of the invention
Primary and foremost purpose of the present invention is to concentrate the advantage of polyquaternary ammonium salt and type siloxane conditioner; the synergism of two kinds of conditioners of performance; a kind of polyquaternary ammonium salt and siloxanes conditioning functions of having concurrently is provided, has hair macromolecule conditioners soft and conditioning functions such as protection hair quality, the dried comb of increase and wet comb effect.Another object of the present invention is to provide the preparation method of described hair macromolecule conditioner; A further object of the present invention is to provide the application of described hair macromolecule conditioner.Purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of hair macromolecule conditioner may further comprise the steps:
(1) in reactor, adds the deionized water of 60 ~ 85 mass parts, stir the cationic monomer that adds 2 ~ 10 mass parts down successively, the anionic monomer of 2 ~ 5 mass parts, the non-ionic monomer of 2 ~ 5 mass parts, the function monomer of 2 ~ 5 mass parts;
(2) stir the back with the pH regulator agent pH is transferred to 6.00 ~ 7.00;
(3) stirring is warming up to 65 ~ 85 ℃, adds the initiator of 0.01 ~ 0.03 mass parts, and the chain-transferring agent of 0.5 ~ 1.0 mass parts is reduced to room temperature behind reaction 5 ~ 8h, leaves standstill 12 ~ 15h;
(4) stirring is warming up to 55 ~ 65 ℃, decompression vacuum pumping, and the polyether modified siloxane of adding 7 ~ 15 mass parts continues to stir 3 ~ 5h, obtains target product.
Described cationic monomer is a kind of in pi-allyl trimethyl ammonium chloride, acryloxy ethyl-trimethyl salmiac, methacryloxyethyl trimethyl ammonium chloride, acrylamide propyl trimethyl ammonium chloride, the Methacrylamide oxypropyl trimethyl ammonium chloride or several;
Described anionic monomer is a kind of in maleic anhydride, acrylic acid, 2-acrylamide methyl propane sulfonic acid sodium, methacrylic acid, the 2-acrylamide C3-C14 alkyl sulfonic acid or several;
Described non-ionic monomer is a kind of in acrylic acid methyl ester., ethyl acrylate, butyl acrylate, methyl methacrylate, ethyl methacrylate, the butyl methacrylate or several;
Described function monomer is a kind of in acrylamide, styrene, chitosan, the chitosan quaternary ammonium salt or several;
Described pH regulator agent is a kind of in potassium hydroxide, sodium hydroxide, ammonia, monoethanolamine, diethanolamine, triethanolamine, aminomethyl propanol, acetic acid, hydrochloric acid, phosphoric acid, the citric acid or several;
Described initiator is a kind of in sodium peroxydisulfate, potassium peroxydisulfate, Ammonium persulfate., benzoyl peroxide, the azodiisobutyronitrile or several;
Described chain-transferring agent is mercaptan, sodium thiosulfate, sodium sulfite, a kind of in Potassium acid sulfite, sodium hypophosphite, the potassium hypophosphite or several;
Described polyether modified siloxane is a kind of in Polyethylene Glycol-10-polydimethylsiloxane (PEG-10 polydimethylsiloxane), Polyethylene Glycol-12-polydimethylsiloxane (PEG-12 polydimethylsiloxane), the Polyethylene Glycol-15-polypropylene glycol-15-polydimethylsiloxane (PEG/PPG-15/15 polydimethylsiloxane) or several;
Preparation-obtained macromolecule conditioner viscosity is 6000-20000mpa.s(25 ℃), working substance content is 15 ~ 40%.
Polyquaternary ammonium salt and type siloxane conditioner all have excellent conditioning functions, and the mechanism of action is different.By polyquaternary ammonium salt and siloxanes are organically combined, can give full play to the synergism of two kinds of conditioners, to give full play to soft and protection hair quality, the dried comb of increase and wet comb effect, further raising is to the opsonic action of hair.
Compared with prior art, at first adopt aqueous solution multi-component copolymer system,, can obtain the polyquaternary ammonium salt intermediate product of CHARGE DISTRIBUTION rule by appropriate design to cationic monomer, non-ionic monomer, anionic monomer, function monomer in the present invention; Then polyquaternary ammonium salt intermediate product and the polysiloxanes that obtains further acted on, siloxane molecule is distributed on the polyquaternary ammonium salt structure.Because product combines the character of polyquaternary ammonium salt and siloxanes, polyquaternary ammonium salt can be given full play to the synergism of different ions and the adsorption of quaternary nitrogen on the one hand, the opposing party's polyquaternary ammonium salt has promoted the adsorption of siloxanes on hair, and has improved the sustainability of absorption.Therefore, the prepared macromolecule conditioner of the present invention compare other conditioners improve to do/aspects such as wet cardability, antistatic behaviour have more obvious effect.
Description of drawings
Fig. 1 improves comparison diagram for embodiment 4 being attacked by dampness combings.
Fig. 2 improves comparison diagram for embodiment 4 does combing.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1
In the four-hole bottle that has agitator and water-bath, drop into the deionized water of 60g, the pi-allyl trimethyl ammonium chloride that adds 10g, 2.5g acrylic acid, 2.5g the acrylic acid methyl ester. of maleic anhydride, 5g, the acrylamide of 5g, the reuse aminomethyl propanol is regulated pH to 6.00, at 65 ℃ of following constant temperature, drop into 0.01g potassium peroxydisulfate initiator initiated polymerization again, and add 1.0g mercaptan and make chain and shift, react after 8 hours and lower the temperature.Leave standstill 15h, stir and be warming up to 65 ℃, decompression vacuum pumping adds 15g Polyethylene Glycol-10-polydimethylsiloxane, stirring reaction 5h, and cooling obtains the macromolecule conditioner.
The macromolecule conditioner viscosity for preparing is about 20000mpa.s(25 ℃), working substance content (quality) is about 40%.
Embodiment 2
In the four-hole bottle that has agitator and water-bath, drop into the deionized water of 85g, the methacryloxyethyl trimethyl ammonium chloride that adds 2g, the methacrylic acid of 2g, the 2-acrylamide methyl propane sulfonic acid of 2g, the acrylamide of 2g, reuse ammonia is regulated pH to 6.50, at 85 ℃ of following constant temperature, drop into 0.03g ammonium persulfate initiator initiated polymerization again, and adding 0.5g sodium thiosulfate is done the chain transfer, react cooling after 5 hours, leave standstill 12h, stir and be warming up to 55 ℃, decompression vacuum pumping adds 7g Polyethylene Glycol-12-polydimethylsiloxane, stirring reaction 3h, cooling obtains the macromolecule conditioner.
The macromolecule conditioner viscosity for preparing is about 6000mpa.s(25 ℃), working substance quality content is about 15%.
In the four-hole bottle that has agitator and water-bath, drop into the deionized water of 80g, the acrylamide propyl trimethyl ammonium chloride that adds 3g, the 2-acrylamide propane sulfonic acid sodium of 3g, the methyl methacrylate of 3g, the styrene of 1g, the 2g chitosan is regulated pH to 7.00 with acetic acid, at 75 ℃ of following constant temperature, drop into 0.02g azodiisobutyronitrile initiator initiated polymerization again, and add the 0.8g sodium sulfite and make chain-transferring agent, lower the temperature behind the reaction 6h, after 14h is left standstill in cooling, stirring is warming up to 60 ℃, and decompression vacuum pumping adds 8g Polyethylene Glycol-10-polydimethylsiloxane, stirring reaction 4h, cooling obtains the macromolecule conditioner.
The macromolecule conditioner viscosity for preparing is about 10000mpa.s(25 ℃), working substance quality content is about 20%.
Embodiment 4: conditioning performance detects
Reference formulation sees Table 1.
Table 1
Preparation method: with AES, K
12A, 6501, CAB-35, EDTA-2Na and water heated and stirred dissolving back cooling adds after reducing to 40～45 ℃, Pearl Concentrate, macromolecule conditioner, the back that stirs adds antiseptic, essence and regulates viscosity with NaCl, adjusts pH value with citric acid.
Blank shampoo does not promptly add the shampoo of macromolecule conditioner.
The sense organ property testing:
Take the mode of volunteer's sensory evaluation, promptly ask flying away property, gloss and the feel of two groups of human shampoo washing hair aftersensation hairs, estimate and adopt 7 fens systems, 7 are divided into best result, and 1 is divided into minimum branch.
The result is as shown in table 2.
Table 2
Instrument test:
Adopt Dia-Stron MTT160 tension measuring device
Method of testing:
Take by weighing the shampoo of 3g reference formulation preparation, be dissolved in the 200ml warm water mix homogeneously.To test topknot and immerse, and hand-launder after the taking-up, the water flushing does not produce to there being tangible foam then.Wet comb test is carried out after processing at once, soaks to be no more than 5 minutes in water.Do the combing test and treat that topknot carries out after drying naturally under the condition of room temperature, humidity 65 ﹪.
Test result is following illustrated in figures 1 and 2.Sensory evaluation and instrument tension test result show, shampoo with the prepared macromolecule conditioner preparation of the present invention has significant conditioning performance, smoothness and flexibility have been increased, sense of touch is smooth, be easy to do comb and wet comb, so the macromolecule conditioner that the present invention makes can be used as high-grade conditioner for hair.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a hair macromolecule conditioner may further comprise the steps:
(1) in reactor, adds the deionized water of 60 ~ 85 mass parts, stir the cationic monomer that adds 2 ~ 10 mass parts down, the anionic monomer of 2 ~ 5 mass parts, the non-ionic monomer of 2 ~ 5 mass parts, the function monomer of 2 ~ 5 mass parts;
(2) stir the back with the pH regulator agent pH is transferred to 6.00 ~ 7.00;
(3) stirring is warming up to 65 ~ 85 ℃, adds the initiator of 0.01 ~ 0.03 mass parts, and the chain-transferring agent of 0.5 ~ 1.0 mass parts is reduced to room temperature behind reaction 5 ~ 8h, leaves standstill 12 ~ 15h;
(4) stirring is warming up to 55 ~ 65 ℃, decompression vacuum pumping, and the polyether modified siloxane of adding 7 ~ 15 mass parts continues to stir 3 ~ 5h, obtains target product.
2. according to the described preparation method of claim 1, it is characterized in that described cationic monomer is more than one in pi-allyl trimethyl ammonium chloride, acryloxy ethyl-trimethyl salmiac, methacryloxyethyl trimethyl ammonium chloride, acrylamide propyl trimethyl ammonium chloride, the Methacrylamide oxypropyl trimethyl ammonium chloride.
3. according to the described preparation method of claim 1, it is characterized in that described anionic monomer is more than one in maleic anhydride, acrylic acid, 2-acrylamide methyl propane sulfonic acid sodium, methacrylic acid, the 2-acrylamide C3-C14 alkyl sulfonic acid; Described non-ionic monomer is more than one in acrylic acid methyl ester., ethyl acrylate, butyl acrylate, methyl methacrylate, ethyl methacrylate, the butyl methacrylate.
4. according to the described preparation method of claim 1, it is characterized in that described function monomer is a kind of in acrylamide, styrene, chitosan, the chitosan quaternary ammonium salt or several.
5. according to the described preparation method of claim 1, it is characterized in that described pH regulator agent is more than one in potassium hydroxide, sodium hydroxide, ammonia, monoethanolamine, diethanolamine, triethanolamine, aminomethyl propanol, acetic acid, hydrochloric acid, phosphoric acid, the citric acid.
6. according to the described preparation method of claim 1, it is characterized in that described initiator is more than one in sodium peroxydisulfate, potassium peroxydisulfate, Ammonium persulfate., benzoyl peroxide, the azodiisobutyronitrile.
7. according to the described preparation method of claim 1, it is characterized in that described chain-transferring agent is mercaptan, sodium thiosulfate, sodium sulfite, more than one in Potassium acid sulfite, sodium hypophosphite, the potassium hypophosphite.
8. according to the described preparation method of claim 1, it is characterized in that described polyether modified siloxane is more than one in Polyethylene Glycol-10-polydimethylsiloxane (PEG-10 dimethyl siloxane), Polyethylene Glycol-12-polydimethylsiloxane (PEG-12 dimethyl siloxane), the Polyethylene Glycol-15-polypropylene glycol-15-polydimethylsiloxane (PEG/PPG-15/15 polydimethylsiloxane).
9. the hair macromolecule conditioner that is made by the described preparation method of claim 1 is characterized in that 25 ℃ of following viscosity are 6000-20000mpa.s, and working substance content is 15 ~ 40%.
10. the described hair macromolecule of claim 9 conditioner is used in shampoo.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104323929A (en) * | 2014-10-31 | 2015-02-04 | 重庆环驰科技有限公司 | Shampoo with controllable viscosity and preparation method thereof |
| CN112301729A (en) * | 2019-07-30 | 2021-02-02 | 株式会社钟化 | Method for producing regenerated collagen fiber, and fiber bundle containing same |
| CN114796018A (en) * | 2022-05-12 | 2022-07-29 | 苏州绿叶日用品有限公司 | Silicon-free shampoo and preparation method thereof |
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| CN1654497A (en) * | 2005-01-14 | 2005-08-17 | 华南理工大学 | Chitosan graft ternary polymerization polymeric flocculant and its preparation method and use |
| CN1994943A (en) * | 2006-11-30 | 2007-07-11 | 华南理工大学 | Amphoteric ion high polymer sludge dehydration agent and its preparation method |
| CN101407582A (en) * | 2007-10-10 | 2009-04-15 | 戈尔德施米特有限公司 | Linear poly(dialkyl) organosiloxane having poly(oxyalkylene), amino functional group and end alkoxy |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322876A (en) * | 2000-05-08 | 2001-11-21 | 广东爱齐美科技有限公司 | Prepn of water soluble quarternary copolymer softener |
| CN1654497A (en) * | 2005-01-14 | 2005-08-17 | 华南理工大学 | Chitosan graft ternary polymerization polymeric flocculant and its preparation method and use |
| CN1994943A (en) * | 2006-11-30 | 2007-07-11 | 华南理工大学 | Amphoteric ion high polymer sludge dehydration agent and its preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104323929A (en) * | 2014-10-31 | 2015-02-04 | 重庆环驰科技有限公司 | Shampoo with controllable viscosity and preparation method thereof |
| CN104323929B (en) * | 2014-10-31 | 2017-08-29 | 重庆环驰科技有限公司 | Controllable shampoo of a kind of viscosity and preparation method thereof |
| CN112301729A (en) * | 2019-07-30 | 2021-02-02 | 株式会社钟化 | Method for producing regenerated collagen fiber, and fiber bundle containing same |
| CN114796018A (en) * | 2022-05-12 | 2022-07-29 | 苏州绿叶日用品有限公司 | Silicon-free shampoo and preparation method thereof |
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Effective date of registration: 20161229 Address after: 510640 Tianhe District, Guangdong, No. five road, No. 381, Patentee after: Huana Science and Engineering Univ. Patentee after: Zhongshan Aihu Commodity Co., Ltd. Address before: 510640 Tianhe District, Guangdong, No. five road, No. 381, Patentee before: Huana Science and Engineering Univ. Patentee before: Foshan Sears Daily Necessities Ltd. |