CN106700095B - A kind of super large partial size height glues the preparation method of methyl-silicone oil emulsion - Google Patents
A kind of super large partial size height glues the preparation method of methyl-silicone oil emulsion Download PDFInfo
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- CN106700095B CN106700095B CN201611255954.2A CN201611255954A CN106700095B CN 106700095 B CN106700095 B CN 106700095B CN 201611255954 A CN201611255954 A CN 201611255954A CN 106700095 B CN106700095 B CN 106700095B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
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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
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
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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
- A61Q5/02—Preparations for cleaning the hair
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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
- A61Q5/12—Preparations containing hair conditioners
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses the preparation methods that a kind of super large partial size height glues methyl-silicone oil emulsion.High viscosity methyl-silicone oil emulsion is prepared using advanced high-efficient shear emulsifying equipment.By selecting highly viscous methyl-silicone oil and adjusting the amount of the surfactant and water that are added, the super large partial size methyl-silicone oil emulsion that partial size D50 is greater than 20 μm can be prepared into.Super large partial size methyl-silicone oil emulsion preparation process prepared by the present invention is simple and efficient, it is easy to procedure, for having application effect outstanding in personal care product, especially it is used in compounding with small particle silicone oil emulsion and makes hair that there is excellent dry and wet comb performance and waxy feeling in washing and caring hair product.
Description
Technical field
The present invention relates to the preparation process that a kind of super large partial size height glues methyl-silicone oil emulsion, especially one kind is suitble in individual
The super large partial size height for nursing industry glues the preparation process of methyl-silicone oil emulsion.
Background technique
Sense of touch of the dimethicone as with excellent smooth, hydrophobic, ventilative, UV resistant and silk, in individual
It being had a wide range of applications in care product, the big high viscosity dimethicone of relative molecular mass then has lasting retention, at
Film property is good, can be used for repairing the damage of hair and improves cardability, has unique lubricating function, as skin moisturizing agent, hair
Sending out conditioner has excellent application performance.But then, silicone oil is difficult to disperse in water phase due to its hydrophobicity, and straight
It scoops out for hair fiber, then feel, fastness and elasticity are undesirable, therefore, after needing to be prepared into silicone oil emulsion on the market
It can apply.However highly viscous methyl-silicone oil oil stickiness is strong, it is difficult to emulsify, it is difficult to meet in the market to emulsion of high-viscosity silicon oil
Needs.
Since emulsion particle diameter is smaller in conventional emulsions, the chance being attached on hair is greatly increased, and washing and dehydrating integrated machine can be reduced,
The degree accumulated on hair after being used for multiple times is high, easily makes hair is astringent to be hardened.And big partial size amino-modified silicone oil can effectively change
It is apt to this disadvantage, this kind of product has been developed in foreign countries and has been successfully applied in shampoo class product.Patent CN200580043307
Big partial size lotion is prepared under the conditions of 55-70 DEG C, CN201010166365 uses semi-continuous seed emulsion polymerization technique to increase
The partial size of lotion.
Summary of the invention
It is an object of the invention to prepare use in personal care on high-efficient shear emulsifying equipment by machinery emulsification method
Super large partial size height glues methyl-silicone oil emulsion.Super large partial size methyl-silicone oil emulsion particle diameter distribution prepared by the present invention is narrow, internal phase viscosities
Height, storage stability is high, especially multiple with small particle methyl-silicone oil for having good application effect in personal care product
Assigned in making hair that there is excellent dry and wet to comb performance, excellent waxy feeling in washing and caring hair product.
It is another object of the present invention to provide the methods for preparing the viscous methyl-silicone oil emulsion of above-mentioned super large partial size height.This hair
The preparation method production of bright proposition efficiently, is easy to procedure, and normal temperature and pressure operates, no production safety hidden danger can preferably expire
The needs of sufficient actual production, especially its excellent production efficiency and high technology stability make it in organosilicon personal nursing lotion
Field has wide practical application value.
A kind of super large partial size height glues the preparation method of methyl-silicone oil emulsion, comprising the following steps:
A: the component of following mass fraction: 50-70 parts of 10000- is added in high-efficient shear emulsifying equipment
1000000cs dimethicone, the water of 1-4 parts of emulsifier and 7-14 part, is uniformly mixed；
B: 15-30 parts of the dilution water into A, 0.1-1 parts of assistant for emulsifying agents and 0.1-1 parts of thickener are uniformly mixed, i.e.,
?.
Preparation process is reacted at normal temperatures and pressures.
Wherein, in step A, dimethicone is preferably 60-70 parts, and emulsifier is preferably 2-4 parts, and water is preferably 10-13
Part.
Wherein, in step A, dimethyl-silicon oil viscosity is preferably 200000-700000 cs.
Wherein, in step A, emulsifier is one of anion, cation, nonionic, amphoteric surfactant or several
Kind, preferably non-ionic or amphoteric surfactant, one of alkylation polyoxyethylene ether most preferably or glycine betaine or
It is several.
Wherein, in step B, assistant for emulsifying agent be one of anion, cation, nonionic, amphoteric surfactant or
Several, preferably non-ionic fatty alcohol polyethenoxy ether class.
Wherein, in step B, thickener be cellulose family, polyacrylic acid lipid or natural polymer and its derivative species,
Preferably natural polymer and its derivative species.
Wherein high-efficient shear emulsifying equipment is preferably EKATO KOAX equipment.
Compared with other technologies, method of the invention has technical characterstic below and effect:
| This patent | Certain method (screw extruder technique) | Certain method (super-pressure emulsion polymerization technique) | Certain method (anionic polymerization process) | |
| Pressure | Normal pressure | Micro-vacuum | >1Mpa | Normal pressure |
| Temperature | 20-30℃ | 60℃ | 10-50℃ | 85℃ |
| Partial size | >20 um | 0.3 um | 0.4 um | <0.5 um |
| Internal phase viscosities | 10,000-1,000,000 cs | 1,000,000,000 cs | 300,000 cs | 113,000 cs |
The present invention has the advantages that
1. method of the invention, the methyl-silicone oil emulsion partial size (D50) of preparation is greater than 20 μm, and has higher stability
(room temperature December, 50 DEG C 30 days) is different from product emulsion conventional in the market.
2. in method of the invention, methyl-silicone oil viscosity used is 10000-1000000cs, viscosity is higher than in the market
Methyl-silicone oil viscosity in existing washing and caring hair product.
3. method of the invention uses high-efficient shear emulsifying equipment, operation is intelligent, technique room temperature (20-30 DEG C) normal pressure
(atmospheric pressure), strong to high viscosity emulsion emulsifiers ability, production lotion is high-efficient, is in industrial mass production using excellent
It is good.
4. method of the invention, technical process is simple, easy to operate, batch time 10h, is conducive to procedure and industrialization rule
Mould preparation, actual application prospect are good.
Super large partial size methyl-silicone oil emulsion prepared by the present invention is used to have good application effect in personal care product,
It is especially compounded with small particle silicone oil and hair is made to have excellent dry and wet comb performance, excellent cunning soft in washing and caring hair product
Feel.
Specific embodiment
Combined with specific embodiments below, invention is further described, it is noted that following embodiment be only to illustrate rather than
It limits the technical scheme described by the invention, all equivalent exchanges made on the basis of technical scheme each fall within the present invention
Protection scope.
Embodiment 1
The dimethicone that the viscosity that 60 parts are added in high-efficient shear emulsifying equipment is 60000cs, is added 4 parts of sweet tea
Dish alkali adds 10 parts of water, stirs evenly, and 24 parts of dilution water is added, and after mixing evenly, 1 part of guar gum is added, then
1 part of fatty alcohol polyoxyethylene ether is added.The methyl-silicone oil emulsion partial size being prepared into is 31.47 μm, and the room temperature shelf-life is greater than
12 months, 50 DEG C were greater than 30 days.
Embodiment 2
The dimethicone that the viscosity that 60 parts are added in high-efficient shear emulsifying equipment is 300000cs, is added 4 parts of sweet tea
Dish alkali adds 10 parts of water, stirs evenly, and 25 parts of dilution water is added, 1 part of guar gum is added after mixing evenly.It is prepared into
Methyl-silicone oil emulsion partial size be 34.18 μm, the room temperature shelf-life be greater than 12 months, 50 DEG C be greater than 30 days.
The test method with testing standard of properties are same as Example 1 in the present embodiment.
Embodiment 3
The dimethicone that the viscosity that 60 parts are added in high-efficient shear emulsifying equipment is 500000cs, is added 4 parts of sweet tea
Dish alkali is added 1 part of guar gum, adds 10 parts of water, stir evenly, and 25 parts of dilution water is added, after mixing evenly, then plus
Enter 1 part of fatty alcohol polyoxyethylene ether.The methyl-silicone oil emulsion partial size being prepared into is 38.56 μm, and the room temperature shelf-life is greater than 12
Month, 50 DEG C are greater than 30 days.
The test method with testing standard of properties are same as Example 1 in the present embodiment.
Claims (5)
1. a kind of super large partial size height glues the preparation method of methyl-silicone oil emulsion, it is characterized in that: the following steps are included:
A: the component of following mass fraction: 50-70 parts of 10000-1000000cs bis- is added in high-efficient shear emulsifying equipment
Methyl-silicone oil, the water of 1-4 parts of emulsifier and 7-14 part, is uniformly mixed；
B: 15-30 parts of dilution water, 0.1-1 parts of assistant for emulsifying agents and 0.1-1 parts of thickener are added into A, is uniformly mixed, i.e.,
?；
Wherein, the high-efficient shear emulsifying equipment is EKATO KOAX equipment；
Wherein, preparation process is normal temperature and pressure；
Wherein, in step A, emulsifier is one or more of nonionic, amphoteric surfactant；
Wherein, in step B, assistant for emulsifying agent is one or more of anion, cation, nonionic, amphoteric surfactant；
Thickener is polyacrylate, natural polymer.
2. a kind of super large partial size height as described in claim 1 glues the preparation method of methyl-silicone oil emulsion, it is characterized in that: step A
In, emulsifier is alkylation one or more of polyoxyethylene ether or glycine betaine.
3. a kind of super large partial size height as claimed in claim 2 glues the preparation method of methyl-silicone oil emulsion, it is characterized in that: step B
In, assistant for emulsifying agent is non-ionic fatty alcohol polyethenoxy ether class.
4. a kind of super large partial size height as described in any one of claims 1-3 glues the preparation method of methyl-silicone oil emulsion, feature
Are as follows: in step A, dimethicone is preferably 60-70 parts, and emulsifier is preferably 2-4 parts, and water is preferably 10-13 parts.
5. a kind of super large partial size height as claimed in claim 4 glues the preparation method of methyl-silicone oil emulsion, it is characterized in that: step A
In, dimethyl-silicon oil viscosity is preferably 200000-700000 cs.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611255954.2A CN106700095B (en) | 2016-12-30 | 2016-12-30 | A kind of super large partial size height glues the preparation method of methyl-silicone oil emulsion |
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| CN201611255954.2A CN106700095B (en) | 2016-12-30 | 2016-12-30 | A kind of super large partial size height glues the preparation method of methyl-silicone oil emulsion |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108498376B (en) * | 2018-04-02 | 2020-11-13 | 榛硕（武汉）智能科技有限公司 | Methyl silicone oil emulsion and preparation method thereof |
| CN109438990B (en) * | 2018-11-16 | 2021-02-02 | 山东道安新材料有限公司 | Composite silicone oil emulsion and preparation method thereof |
| CN110885559B (en) * | 2019-12-18 | 2021-12-31 | 广东灵捷制造化工有限公司 | High-viscosity dimethyl silicone oil emulsion and preparation method thereof |
| CN112646487A (en) * | 2020-12-24 | 2021-04-13 | 南京曦瑞生物科技有限公司 | Water-based silicone oil and preparation method thereof |
| CN113214498A (en) * | 2021-04-29 | 2021-08-06 | 南京威尔生物科技有限公司 | Preparation method of emulsified silicone oil with high viscosity and good stability |
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2016
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