CN109485802A - A kind of hair styling polymer and preparation method thereof - Google Patents
A kind of hair styling polymer and preparation method thereof Download PDFInfo
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- CN109485802A CN109485802A CN201811311965.7A CN201811311965A CN109485802A CN 109485802 A CN109485802 A CN 109485802A CN 201811311965 A CN201811311965 A CN 201811311965A CN 109485802 A CN109485802 A CN 109485802A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/06—Preparations for styling the hair, e.g. by temporary shaping or colouring
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/48—Thickener, Thickening system
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Abstract
The invention belongs to polymer arts, disclose a kind of hair styling polymer, are obtained by following monomer by emulsion polymerization: at least one carboxylic acid monomer of 15-35wt%；(methyl) acrylamide derivative of at least one structure shown in formula I of 20-50wt%；Wherein R1It is hydrogen；R2And R3For hydrogen or C4‑C12Alkyl, but R2With R3It is not simultaneously hydrogen；Alkyl polyoxyethylene ether (methyl) acrylate of at least one structure as shown in Formula II of 10-30wt%；Wherein R4For hydrogen or methyl；N is 7-25, m 11-21；(methyl) the acrylic acid C of 20-45wt%1‑C4Arrcostab.The polymer has the characteristics that light transmittance is high, thickening capabilities are good, curl retention is good under wet environment, meanwhile, the present invention also provides the preparation methods of the polymer.
Description
Technical field
The present invention relates to polymer material fields, and in particular to a kind of hair styling polymer and preparation method thereof.
Background technique
As the improvement of people's living standards, hair styling product increasingly receives the favor of people.Hair styling product
With after spray is shone or is applied on hair, holding forming hair and modification can be played the role of.Pass as hair styling product
Key component, the performances such as quality of forming film, humidity-proof ability, the water solubility of styling polymer have the performance of approved product conclusive
Effect.A good styling polymer, primary need have certain rigidity, so that product is had good fixed effect, that is, have
There is higher curl retention.Second, it is also necessary to have certain flexibility and elasticity, make product have certain toughness without
It is easily broken.Third, styling polymer also need it is easy to clean, in order to which the film formed on hair can be washed off.Finally, fixed
Type polymer also needs transparency with higher, will not generate white bits after forming a film on hair.
Most common styling polymer be polyvinylpyrrolidone and its derivative, commercial product such as BASF's K30Powder、 K90Powder、VA55I etc..This quasi polymer is on hair
The film with certain gloss can be formed, and its hardness and elasticity are also able to satisfy requirement, but humidity-proof ability is poor, in high humidity
Holding capacity of being formed under environment is poor, for needing additionally to use thickener in aqueous hair jelly.
Patent US3927199 discloses a kind of hair styling polymer, which is N- alkyl acrylamide, propylene
The copolymer solution of the monomer compositions such as acid, acrylate, used polymerization are polymerisation in solution.The polymerization of the patent disclosure
The sizing that object is suitable for propellant is spraying, has good style-ability.But because it contains higher volatile organic solvent, no
Easily used in aqueous hair jelly.
Patent CN1890278A disclose it is a kind of using polymerisation in solution preparation can be used as setting agent based on (methyl) third
The copolymer of enoic acid ter-butyl ester, the polymer can be used for preparing the hair spray with strong style-ability.
Patent CN101044176B discloses a kind of amphoteric ethyl methacrylate copolymers solution that can be used as setting agent,
The polymer is prepared using polymerisation in solution.The copolymer of the patent disclosure has good style-ability in low VOC formula, can
It generates good spraying.
CN01136106.9 discloses a kind of cosmetic composition, containing with the following group in cosmetically acceptable carrier
Point: (a) at least one fixed film forming polymer is selected from branched block copolymer, and the branched block copolymer contains work
At least one C1-20 alkyl acrylate and/or at least one N- for principal monomer be mono- or N, N- bis- (C2-12 alkyl) (first
Base) acrylamide and acrylic acid and/or methacrylic acid, (b) at least one thickener, selected from being based on (methyl) propylene
The crosslinking of acid or noncrosslinking homopolymer and copolymer, and (c) at least one thickener altogether, are selected from the non-fibre different from (b)
Tie up plain class thickening polymer；What the program focused on to consider is film forming polymer (a), thickener (b), matching between thickener (c)
It closes, does not solve the problems, such as that style-ability existing in the prior art, humidity-proof ability are poor, while needing additionally using thickening
Agent.
In the art, it is added in hairspray using polyoxyethylene ether substance, mostly using containing poly-
The surfactant of ethylene oxide ether segment, is generally not involved in polymerization.
As: a kind of hair setting composition disclosed in CN201710705556.4, the raw material including following weight percent:
The fatty alcohol polyethenoxy ether class of 10-50%；The setting agent of 10-40%；The poly ethyldiol modified glyceride type of 1-20%；1-
The modified castor oil of 20% polyoxyethylene ether；The modified waxes of 1-20%；The conditioning moisturizer of 10-50%；Deionized water is supplied
To 100%.
Although the polymer of above-mentioned patent disclosure has preferable style-ability, it is substantially using polymerisation in solution system
It is standby, the organic solvents such as alcohols can be used during the preparation process, it is difficult to be used for aqueous hair jelly product.Traditional polyvinylpyrrolidone
And its derivative, although can be used for aqueous hair jelly product, its humidity-proof ability is poor, and needs additionally to use thickener.
Summary of the invention
The object of the present invention is to provide a kind of hair styling polymer；The polymer is high with light transmittance, thickening capabilities are good,
The good feature of curl retention under wet environment, meanwhile, the present invention also provides the preparation methods of the polymer.
Concrete scheme of the invention is as follows: a kind of hair styling polymer, is obtained by following monomer by emulsion polymerization:
At least one carboxylic acid monomer of 15-35wt%；
(methyl) acrylamide derivative of at least one structure shown in formula I of 20-50wt%；
Wherein R1It is hydrogen；R2And R3For hydrogen or C4-C12Alkyl, but R2With R3It is not simultaneously hydrogen；
Alkyl polyoxyethylene ether (methyl) acrylate of at least one structure as shown in Formula II of 10-30wt%.
Wherein R4For hydrogen or methyl；N is 7-25, m 11-21；
(methyl) the acrylic acid C of 20-45wt%1-C4Arrcostab.
In above-mentioned hair styling polymer, the carboxylic acid monomer be selected from acrylic acid, methacrylic acid, itaconic acid,
One of fumaric acid, crotonic acid, aconitic acid, maleic acid are a variety of.
In above-mentioned hair styling polymer, acrylamide derivative described in Formulas I is N tert butyl acrylamide, uncle N-
Octyl acrylamide, N, N- dioctyl acrylamide, N, one or more of N- dodecyl acrylamide.
In above-mentioned hair styling polymer, (methyl) acrylic acid polyoxyethylene ether long-chain alkyl groups described in Formula II are ten
Dialkyl group polyoxyethylene ether (methyl) acrylate, Steareth (methyl) acrylate, eicosyl polyoxy
One or more of vinethene (methyl) acrylate, beheneth (methyl) acrylate.
In above-mentioned hair styling polymer, (methyl) the acrylic acid C1-C4Arrcostab is (methyl) acrylic acid first
Ester, (methyl) ethyl acrylate, (methyl) n-butyl acrylate, (methyl) tert-butyl acrylate, (methyl) propyl acrylate it
One or more.
Meanwhile the invention also discloses the preparation method of such as above-mentioned hair styling polymer, the methods specifically:
Pre-emulsion containing all or part of monomer, the initiator solution containing all or part of initiator are added drop-wise to and contained
Deionized water, the lotion of emulsifier, the monomer of surplus and initiator reactor in, carry out emulsion polymerization and obtain containing hair styling
The polymer emulsion of polymer；
Monomer accounts for 20~40wt% of polymer emulsion total amount.
In the preparation method of above-mentioned hair styling polymer, specifically comprise the following steps:
Step 1: portions of de-ionized water, partial emulsifier, all or part of monomer being added in first reactor, led to
Inert gas is simultaneously opened stirring and is emulsified, and pre-emulsion is configured to；
Step 2: some or all of initiator being added in the desired amount of deionized water and is dissolved, is configured to cause
Agent aqueous solution；
Step 3: remaining deionized water, residual emulsifier, residual monomer being added in second reactor, leads to nitrogen, stirs
It mixes and is warming up to 75~90 DEG C；If monomer is all added in the first reactor of step 1, the step is without being added monomer；
Step 4: after temperature rises to 75~90 DEG C, remaining initiator is added；If whole initiators are added in step 2,
Then the step is without being added initiator；
Step 5: after a certain period of time, starting the initiation of the pre-emulsion and step 2 in 1 first reactor of a dropping step simultaneously
Agent aqueous solution, time for adding are 30min~180min；
Step 6: after pre-emulsion and initiator solution are added dropwise to complete, continuing to keep the temperature 30min~180min；Heat preservation is completed
Polymer emulsion is obtained by filtration in cooling afterwards.
In the preparation method of above-mentioned hair styling polymer, the deionized water accounts for polymer emulsion total weight 54
~79wt%.
In the preparation method of above-mentioned hair styling polymer, the emulsifier accounts for polymer emulsion total weight 0.5
~3wt%；
The emulsifier is anionic emulsifier, nonionic emulsifier or their mixture.
Specifically, the emulsifier can be selected are as follows: sodium sulfate of polyethenoxy ether of fatty alcohol, dodecyl sulphate
Sodium, fatty alcohol polyoxyethylene ether；In general, general anionic emulsifier, nonionic emulsifier can be applied to this
Invention.
In the preparation method of above-mentioned hair styling polymer, the initiator accounts for polymer emulsion total weight
0.05%~3%；
The initiator is one in water-soluble inorganic persulfate, peroxide, peroxy acid and azo-compound
Kind is a variety of.
The invention has the benefit that
Hair styling polymer provided by the invention has the volume under excellent light transmittance, thickening capabilities and wet environment
Bent conservation rate.In aqueous hair jelly, when pH is that active matter dosage is 2~5wt% between 6~9, light transmittance is greater than 90%, glues
Degree is greater than 30000cps, and curl retention in the environment of 25 DEG C, 90%RH is greater than 90%.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but does not constitute any limitation of the invention, any
In the modification for the limited times that scope of the invention as claimed is made, still in scope of the presently claimed invention.
Embodiment 1:
Equipped with nitrogen device, agitating device and peristaltic pump 2L four-hole boiling flask in be added 600g deionized water and
11.25g sodium sulfate of polyethenoxy ether of fatty alcohol and stirring and dissolving.Again by 45g acrylic acid, 120g N, N- dioctyl acrylamide,
60g beheneth (7) methacrylate and 75g methyl methacrylate mixed dissolution are uniformly added afterwards
In four-hole boiling flask, continues to stir and lead to nitrogen, form pre-emulsion.
0.75g sodium peroxydisulfate is added in 100g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
485g deionized water and 3g sodium sulfate of polyethenoxy ether of fatty alcohol are opened and stir and lead to nitrogen, system is made to be warming up to 90 DEG C.
After system temperature rises to 90 DEG C, start while being added dropwise pre-emulsion and initiator solution, controls rate of addition
It is added dropwise to complete pre-emulsion and initiator solution in 90 minutes.After dripping off pre-emulsion and initiator solution, continue 90
DEG C heat preservation 30 minutes.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.The embodiment resulting polymers are denoted as poly-
Close object 1.
Embodiment 2:
400g deionized water and 7.5g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Sodium sulfate of polyethenoxy ether of fatty alcohol and stirring and dissolving.Again by 112.5g methacrylic acid, 90g N, N- dodecyl propylene
Amide, 45g Steareth (12) acrylate and 202.5g methyl methacrylate mixed dissolution it is uniform after
It is added in four-hole boiling flask, continues to stir and lead to nitrogen, form pre-emulsion.
3g ammonium persulfate and 3g potassium peroxydisulfate are added in 60g deionized water, it is water-soluble to form initiator after stirring and dissolving
Liquid.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
575g deionized water opens and stirs and lead to nitrogen, system is made to be warming up to 85 DEG C.
Addition 1.5g ammonium persulfate in 85 DEG C of backward reaction systems is risen to system temperature, starts after a few minutes while being added dropwise
Pre-emulsion and initiator solution, control rate of addition are added dropwise to complete pre-emulsion and initiator solution in 120 minutes.
After dripping off pre-emulsion and initiator solution, continue to keep the temperature 60 minutes at 85 DEG C.The near near room temperature of reaction solution after heat preservation
And it filters and packages.The embodiment resulting polymers are denoted as polymer 2.
Embodiment 3:
400g deionized water and 32g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Sodium sulfate of polyethenoxy ether of fatty alcohol and 8g fatty alcohol polyoxyethylene ether and stirring and dissolving.Again by 210g acrylic acid, 120g uncle N-
Butylacrylamide, 90g dodecyl polyoxyethylene ether (9) base acrylate and 180g n-butyl acrylate mixed dissolution are equal
It is added in four-hole boiling flask after even, continues to stir and lead to nitrogen, form pre-emulsion.
25g potassium peroxydisulfate and 20g sodium peroxydisulfate are added in 150g deionized water, form initiator after stirring and dissolving
Aqueous solution.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
260g deionized water, 4g sodium sulfate of polyethenoxy ether of fatty alcohol and 1g fatty alcohol polyoxyethylene ether open and stir and lead to nitrogen, make
System is warming up to 75 DEG C.
After system temperature rises to 75 DEG C, start while being added dropwise pre-emulsion and initiator solution, controls rate of addition
It is added dropwise to complete pre-emulsion and initiator solution in 180 minutes.After dripping off pre-emulsion and initiator solution, continue 85
DEG C heat preservation 180 minutes.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.The embodiment resulting polymers are denoted as poly-
Close object 3.
Embodiment 4:
450g deionized water and 15g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Lauryl sodium sulfate and stirring and dissolving.It is further continued for 90g itaconic acid, 225g N- t-octyl acrylamide, 45g octadecyl
Polyoxyethylene ether (25) methacrylate and 90g methyl methacrylate mixed dissolution are uniformly added in four-hole boiling flask afterwards,
Continue to stir and lead to nitrogen, forms pre-emulsion.
15g ammonium persulfate is added in 80g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
490g deionized water opens and stirs and lead to nitrogen, system is made to be warming up to 80 DEG C.
After system temperature rises to 80 DEG C, start while being added dropwise pre-emulsion and initiator solution, controls rate of addition
It is added dropwise to complete pre-emulsion and initiator solution in 150 minutes.After dripping off pre-emulsion and initiator solution, continue 80
DEG C heat preservation 120 minutes.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.The embodiment resulting polymers are denoted as poly-
Close object 4.
Embodiment 5:
400g deionized water and 30g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Fatty alcohol polyoxyethylene ether and stirring and dissolving.81g maleic acid, 135g N tert butyl acrylamide, 135g octadecyl are gathered again
Ethylene oxide ether (18) methacrylate and 189g ethyl methacrylate mixed dissolution are uniformly added in four-hole boiling flask afterwards, after
It is continuous to stir and lead to nitrogen, form pre-emulsion.
12g sodium peroxydisulfate is added in 50g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
405g deionized water simultaneously opens stirring, then by 9g acrylic acid, 15g N tert butyl acrylamide, 15g octadecyl polyoxy second
Alkene ether metacrylic acid ester and 21g ethyl methacrylate mixed dissolution are uniformly added in five mouthfuls of flasks afterwards to be continued to stir and lead to
Nitrogen makes system be warming up to 85 DEG C.
After system temperature rises to 85 DEG C, 3g sodium peroxydisulfate is added.Start after a few minutes while pre-emulsion is added dropwise and draws
Agent aqueous solution is sent out, control rate of addition is added dropwise to complete pre-emulsion and initiator solution in 30 minutes.Drip off pre-emulsion and
After initiator solution, continue to keep the temperature 180 minutes at 85 DEG C.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.
The embodiment resulting polymers are denoted as polymer 5.
Embodiment 6:
600g deionized water and 25g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Lauryl sodium sulfate and stirring and dissolving.Again by 20.5g methacrylic acid, 20g itaconic acid, 81g N- t-octyl acrylamide,
After 81g beheneth (25) methacrylate and 67.5g methyl methacrylate mixed dissolution are uniform
It is added in four-hole boiling flask, continues to stir and lead to nitrogen, form pre-emulsion.
12g ammonium persulfate is added in 75g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
480g deionized water and 5g lauryl sodium sulfate simultaneously open stirring, then by 4.5g methacrylic acid, 9g N- t-octyl third
Acrylamide, 9g beheneth methacrylate and 7.5g methyl methacrylate mixed dissolution it is uniform after
It is added in five mouthfuls of flasks and continues to stir and lead to nitrogen, system is made to be warming up to 85 DEG C.
After system temperature rises to 85 DEG C, 3g ammonium persulfate is added.Start after a few minutes while pre-emulsion is added dropwise and draws
Agent aqueous solution is sent out, control rate of addition is added dropwise to complete pre-emulsion and initiator solution in 120 minutes.Drip off pre-emulsion and
After initiator solution, continue to keep the temperature 60 minutes at 85 DEG C.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.It should
Embodiment resulting polymers are denoted as polymer 6.
Comparative example 1
500g deionized water and 12g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Sodium sulfate of polyethenoxy ether of fatty alcohol and stirring and dissolving.Again by 180g N, N- dioctyl acrylamide, 90g docosyl are poly-
Ethylene oxide ether (25) methacrylate and 180g methyl methacrylate mixed dissolution are uniformly added in four-hole boiling flask afterwards, after
It is continuous to stir and lead to nitrogen, form pre-emulsion.
22.5g sodium peroxydisulfate is added in 100g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
435g deionized water and 3g sodium sulfate of polyethenoxy ether of fatty alcohol are opened and stir and lead to nitrogen, system is made to be warming up to 85 DEG C.
After system temperature rises to 85 DEG C, start while being added dropwise pre-emulsion and initiator solution, controls rate of addition
It is added dropwise to complete pre-emulsion and initiator solution in 180 minutes.After dripping off pre-emulsion and initiator solution, continue 85
DEG C heat preservation 120 minutes.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.The embodiment resulting polymers are denoted as pair
Than polymer 1.
Comparative example 2
500g deionized water and 12g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Sodium sulfate of polyethenoxy ether of fatty alcohol and stirring and dissolving.Again by 135g acrylic acid, 135g beheneth (25)
Methacrylate and 135g methyl methacrylate mixed dissolution are uniformly added in four-hole boiling flask afterwards, continue to stir and lead to nitrogen
Gas forms pre-emulsion.
22.5g sodium peroxydisulfate is added in 100g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
435g deionized water and 3g sodium sulfate of polyethenoxy ether of fatty alcohol are opened and stir and lead to nitrogen, system is made to be warming up to 85 DEG C.
After system temperature rises to 85 DEG C, start while being added dropwise pre-emulsion and initiator solution, controls rate of addition
It is added dropwise to complete pre-emulsion and initiator solution in 180 minutes.After dripping off pre-emulsion and initiator solution, continue 85
DEG C heat preservation 60 minutes.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.The embodiment resulting polymers are denoted as pair
Than polymer 2.
Comparative example 3
500g deionized water and 12g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Sodium sulfate of polyethenoxy ether of fatty alcohol and stirring and dissolving.Again by 90g acrylic acid, 180g N- t-octyl acrylamide, 180g methyl
Methyl acrylate mixed dissolution is uniformly added in four-hole boiling flask afterwards, continues to stir and lead to nitrogen, forms pre-emulsion.
22.5g sodium peroxydisulfate is added in 100g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
435g deionized water and 3g sodium sulfate of polyethenoxy ether of fatty alcohol are opened and stir and lead to nitrogen, system is made to be warming up to 90 DEG C.
After system temperature rises to 85 DEG C, start while being added dropwise pre-emulsion and initiator solution, controls rate of addition
It is added dropwise to complete pre-emulsion and initiator solution in 120 minutes.After dripping off pre-emulsion and initiator solution, continue 85
DEG C heat preservation 120 minutes.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.The embodiment resulting polymers are denoted as pair
Than polymer 3.
Comparative example 4
500g deionized water and 15g are added in the 2L four-hole boiling flask equipped with nitrogen device, agitating device and peristaltic pump
Sodium sulfate of polyethenoxy ether of fatty alcohol and stirring and dissolving.Again by 135g acrylic acid, 225g N- t-octyl acrylamide, 90g 20
Dialkyl group polyoxyethylene ether (25) methacrylate mixed dissolution is uniformly added in four-hole boiling flask afterwards, continues to stir and leads to nitrogen
Gas forms pre-emulsion.
22.5g sodium peroxydisulfate is added in 100g deionized water, forms initiator solution after stirring and dissolving.
It is added in five mouthfuls of flasks of 2L equipped with nitrogen device, reflux condensing tube, electric blender, thermometer and peristaltic pump
435g deionized water opens and stirs and lead to nitrogen, system is made to be warming up to 90 DEG C.
After system temperature rises to 90 DEG C, start while being added dropwise pre-emulsion and initiator solution, controls rate of addition
It is added dropwise to complete pre-emulsion and initiator solution in 120 minutes.After dripping off pre-emulsion and initiator solution, continue 90
DEG C heat preservation 60 minutes.It the near room temperature of near reaction solution and is filtered and packaged after heat preservation.The embodiment resulting polymers are denoted as pair
Than polymer 4.
Using test
After hair styling polymer emulsion of the present invention is diluted to a certain concentration and forms hydrogel with alkali neutralization,
Evaluate the performances such as its light transmittance, thickening capabilities and style-ability.
The preparation of hydrogel: after taking the desired amount of polymer emulsion to be diluted with the desired amount of deionized water, addition is neutralized to
Aminomethylpropanol needed for 100% (95%), stirring neutralize and form test performance after hydrogel.
Light transmittance test: using the light transmittance of ultraviolet-uisible spectrophotometer test hydrogel, wavelength 420nm.
Sample: being placed in constant temperature 2h in 25 DEG C of insulating boxs by viscosity test, with BROOKFIELD-RVT viscosimeter test specimens
Product viscosity.
Curl retention test: weighing 0.7g test sample, be evenly coated on 2g topknot, and rolls up at 1.5 centimetres
On curling iron.The topknot spooled is placed in 50 DEG C of electro-heating standing-temperature cultivators 2 hours dry.Topknot is removed from curling iron
(record curl length L0), hang over 25 DEG C, in the environment of 90%RH for 24 hours after and the curl length L after recording for 24 hourst。
Curl retention formula calculates: curl retention %=(L-Lt)/(L-L0) × 100%
Wherein: L=does the topknot length before hai roll
L0=curl length when being removed from curling iron
Lt=for 24 hours after curl length.
Each polymer performance such as the following table 1 described in the embodiment of the present invention and comparative example:
The application test result of table 1 embodiment 1-6 and comparative example 1-4
By above-mentioned test it follows that
1, the present invention using water as continuous phase, the available polymer being easily applied in aqueous hair jelly product,
Humidity-proof ability is good.
2, the present invention uses 4 kinds of essential monomers, long-acting curling, shaping may be implemented and while from thickening capabilities
It improves.
3, when the polymer emulsion that the present invention is prepared is applied in specific formula, it will not influence the light transmittance of product.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of hair styling polymer, which is characterized in that obtained by following monomer by emulsion polymerization:
At least one carboxylic acid monomer of 15-35wt%；
(methyl) acrylamide derivative of at least one structure shown in formula I of 20-50wt%；
Wherein R1It is hydrogen；R2And R3For hydrogen or C4-C12Alkyl, but R2With R3It is not simultaneously hydrogen；
Alkyl polyoxyethylene ether (methyl) acrylate of at least one structure as shown in Formula II of 10-30wt%；
Wherein R4For hydrogen or methyl；N is 7-25, m 11-21；
(methyl) the acrylic acid C of 20-45wt%1-C4Arrcostab.
2. hair styling polymer according to claim 1, which is characterized in that the carboxylic acid monomer be selected from acrylic acid,
One of methacrylic acid, itaconic acid, fumaric acid, crotonic acid, aconitic acid, maleic acid are a variety of.
3. hair styling polymer according to claim 1, which is characterized in that acrylamide derivative described in Formulas I is N-
N-tert-butyl acrylamide, N- t-octyl acrylamide, N, N- dioctyl acrylamide, N, one of N- dodecyl acrylamide
Or it is a variety of.
4. hair styling polymer according to claim 1, which is characterized in that (methyl) acrylic acid polyoxy second described in Formula II
Alkene ether long-chain alkyl groups are dodecyl polyoxyethylene ether (methyl) acrylate, Steareth (methyl) propylene
One of acid esters, eicosyl polyoxyethylene ether (methyl) acrylate, beheneth (methyl) acrylate
Or it is a variety of.
5. hair styling polymer according to claim 1, which is characterized in that (methyl) the acrylic acid C1-C4Alkyl
Ester be (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl) n-butyl acrylate, (methyl) tert-butyl acrylate,
One or more of (methyl) propyl acrylate.
6. a kind of preparation method of hair styling polymer a method as claimed in any one of claims 1 to 5, which is characterized in that the side
Method specifically:
By the pre-emulsion containing all or part of monomer, the initiator solution containing all or part of initiator be added drop-wise to containing go from
In the reactor of the lotion of sub- water, emulsifier, the monomer of surplus and initiator, carries out emulsion polymerization and obtain polymerizeing containing hair styling
The polymer emulsion of object；
Monomer accounts for 20~40wt% of polymer emulsion total amount.
7. the preparation method of hair styling polymer according to claim 6, which is characterized in that specifically include following step
It is rapid:
Step 1: portions of de-ionized water, partial emulsifier, all or part of monomer being added in first reactor, inertia is led to
Gas is simultaneously opened stirring and is emulsified, and pre-emulsion is configured to；
Step 2: some or all of initiator being added in the desired amount of deionized water and is dissolved, initiator water is configured to
Solution；
Step 3: remaining deionized water, residual emulsifier, residual monomer being added in second reactor, lead to nitrogen, stirring is simultaneously
It is warming up to 75~90 DEG C；If monomer is all added in the first reactor of step 1, the step is without being added monomer；
Step 4: after temperature rises to 75~90 DEG C, remaining initiator is added；It, should if whole initiators are added in step 2
Step is without being added initiator；
Step 5: after a certain period of time, starting the initiator water of the pre-emulsion and step 2 in 1 first reactor of a dropping step simultaneously
Solution, time for adding are 30min~180min；
Step 6: after pre-emulsion and initiator solution are added dropwise to complete, continuing to keep the temperature 30min~180min；It is dropped after the completion of heat preservation
Polymer emulsion is obtained by filtration in temperature.
8. the preparation method of hair styling polymer according to claim 6 or 7, which is characterized in that the deionization
Water accounts for 54~79wt% of polymer emulsion total weight.
9. the preparation method of hair styling polymer according to claim 6 or 7, which is characterized in that the emulsifier
Account for 0.5~3wt% of polymer emulsion total weight；
The emulsifier is anionic emulsifier, nonionic emulsifier or their mixture.
10. the preparation method of hair styling polymer according to claim 6 or 7, which is characterized in that the initiator
Account for polymer emulsion total weight 0.05%~3%；
The initiator be one of water-soluble inorganic persulfate, peroxide, peroxy acid and azo-compound or
Person is a variety of.
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|---|---|---|---|---|
| CN1980633A (en) * | 2004-07-02 | 2007-06-13 | 莱雅公司 | Cosmetic compositions containing at least one conditioning agent and at least one ethylene polymer with polyethylene glycol grafts |
| CN102793634A (en) * | 2012-08-22 | 2012-11-28 | 珀莱雅(湖州)化妆品有限公司 | Hair styling composition |
| CN102906136A (en) * | 2010-04-28 | 2013-01-30 | 巴斯夫欧洲公司 | Rheology modifying and setting polymer, composition thereof and method for making it |
| CN103442687A (en) * | 2011-03-28 | 2013-12-11 | 可泰克斯公司 | Comb polymers for the hair |
| CN106062021A (en) * | 2014-02-26 | 2016-10-26 | 巴斯夫欧洲公司 | A polymer suitable for use in hair styling |
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2018
- 2018-11-06 CN CN201811311965.7A patent/CN109485802A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1980633A (en) * | 2004-07-02 | 2007-06-13 | 莱雅公司 | Cosmetic compositions containing at least one conditioning agent and at least one ethylene polymer with polyethylene glycol grafts |
| US20080286218A1 (en) * | 2004-07-02 | 2008-11-20 | Franck Giroud | Cosmetic Compositions Containing at Least One Conditioning Agent and at Least One Ethylene Polymer with Polyethylene Glycol Grafts |
| CN102906136A (en) * | 2010-04-28 | 2013-01-30 | 巴斯夫欧洲公司 | Rheology modifying and setting polymer, composition thereof and method for making it |
| CN103442687A (en) * | 2011-03-28 | 2013-12-11 | 可泰克斯公司 | Comb polymers for the hair |
| CN102793634A (en) * | 2012-08-22 | 2012-11-28 | 珀莱雅(湖州)化妆品有限公司 | Hair styling composition |
| CN106062021A (en) * | 2014-02-26 | 2016-10-26 | 巴斯夫欧洲公司 | A polymer suitable for use in hair styling |
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