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CN106700095A - Preparation method of large-particle-size high-viscosity methyl silicon oil emulsion - Google Patents

Preparation method of large-particle-size high-viscosity methyl silicon oil emulsion Download PDF

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Publication number
CN106700095A
CN106700095A CN201611255954.2A CN201611255954A CN106700095A CN 106700095 A CN106700095 A CN 106700095A CN 201611255954 A CN201611255954 A CN 201611255954A CN 106700095 A CN106700095 A CN 106700095A
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China
Prior art keywords
oil emulsion
silicone oil
preparation
particle diameter
parts
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CN201611255954.2A
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Chinese (zh)
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CN106700095B (en
Inventor
姜宇嵘
伞振鑫
龙娇秀
黄素萄
武丽美
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/12Preparations containing hair conditioners
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00Characterised 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
    • C08J2383/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Polymers & Plastics (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dermatology (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a preparation method of large-particle-size high-viscosity methyl silicon oil emulsion. The high-viscosity methyl silicon oil emulsion is prepared by adopting advanced efficient-shear emulsion equipment. The large-particle-size methyl silicon oil emulsion with the particle size D50 of more than 20mum is prepared by selecting high-viscosity methyl silicon oil as well as a surfactant and water that are added for adjustment. The large-particle-size high-viscosity methyl silicon oil emulsion prepared by the invention is simple and efficient in preparation process and easy in process operation, and has a prominent application effect in personal care products; especially, the large-particle-size high-viscosity methyl silicon oil emulsion can be compounded with small-particle-size silicon oil emulsion in hair care products, so that hair has excellent dry-wet combing performance and smooth and soft handfeel.

Description

A kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high
Technical field
It is adapted in individual the present invention relates to a kind of preparation technology of super large particle diameter viscous methyl-silicone oil emulsion high, especially one kind Nurse the preparation technology of the super large particle diameter viscous methyl-silicone oil emulsion high of industry.
Background technology
Dimethicone due to the sense of touch as excellent smooth, hydrophobic, ventilative, UV resistant and silk, in individual Had a wide range of applications in care product, the big high viscosity dimethicone of relative molecular mass then has lasting retention, into Film is good, can be used to repair the damage of hair and improves cardability, with unique lubricating function, as skin moisturizing agent, hair Hair conditioner has excellent application performance.But then, silicone oil is difficult to disperse due to its hydrophobicity in water phase, and straight Scoop out for hair fiber, then feel, fastness and elasticity are undesirable, therefore, after commercially needing to be prepared into silicone oil emulsion Can apply.But the oily stickiness of high-viscosity methyl-silicone oil is strong, it is difficult to emulsify, it is difficult to meet in the market to emulsion of high-viscosity silicon oil The need for.
Because 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 that hair is astringent to be hardened.And big particle diameter amino-modified silicone oil can effectively change It is apt to this shortcoming, this kind of product has been developed and has been successfully applied in shampoo class product abroad.Patent CN200580043307 Big particle diameter emulsion is prepared under the conditions of 55-70 DEG C, CN201010166365 uses semi-continuous seed emulsion polymerization technique to increase The particle diameter of emulsion.
The content of the invention
It is an object of the invention to pass through machinery emulsification method use in personal care is prepared on high-efficient shear emulsifying equipment Super large particle diameter viscous methyl-silicone oil emulsion high.Super large particle diameter 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 There is excellent dry and wet comb performance, excellent waxy feeling assigned in hair is caused in washing and caring hair product.
Method it is another object of the present invention to provide above-mentioned super large particle diameter viscous methyl-silicone oil emulsion high is prepared.This hair The preparation method production of bright proposition is efficient, it is easy to procedure, and normal temperature and pressure is operated, and without production safety hidden danger, can preferably be expired The need for sufficient actual production, particularly its excellent production efficiency and technology stability high make it in organosilicon personal nursing emulsion Field has wide actual application value.
A kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high, comprises the following steps:
A:The component of following mass fraction is added in high-efficient shear emulsifying equipment:50-70 parts of 10000-1000000cs bis- Methyl-silicone oil, the water of 1-4 parts of emulsifying agent and 7-14 part, is well mixed;
B:15-30 parts of the dilution water toward A, 0.1-1 parts of assistant for emulsifying agent and 0.1-1 parts of thickener, are well mixed, and obtain final product.
Preparation process is reacted at normal temperatures and pressures.
Wherein, in step A, dimethicone is preferably 60-70 parts, and emulsifying agent 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, emulsifying agent is the one kind or several in anion, cation, nonionic, amphoteric surfactant Kind, preferably nonionic or amphoteric surfactant, one kind in alkylation APEO most preferably or glycine betaine or It is several.
Wherein, in step B, assistant for emulsifying agent be anion, cation, nonionic, amphoteric surfactant in one kind or It is several, the preferably fatty alcohol polyethenoxy ether class of nonionic.
Wherein, in step B, thickener is 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, the method for the present invention has following technical characterstic 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℃
Particle diameter >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 advantage of the invention is that:
1. the method for the present invention, the methyl-silicone oil emulsion particle diameter of preparation(D50)More than 20 μm, and with higher stability(Room Warm December, 50 DEG C 30 days)Different from the conventional product emulsion of in the market.
2. in the method for the present invention, methyl-silicone oil viscosity used is 10000-1000000cs, and viscosity is higher than in the market Methyl-silicone oil viscosity in existing washing and caring hair product.
3. the method for the present invention uses high-efficient shear emulsifying equipment, and operation is intelligent, technique normal temperature (20-30 DEG C) normal pressure (Atmospheric pressure), it is strong to high viscosity emulsion emulsifiers ability, emulsion efficiency high is produced, it is using excellent in industrial mass production It is good.
4. the method for the present invention, technical process is simple, easy to operate, batch time 10h, is advised beneficial to procedure and industrialization Prepared by mould, actual application prospect is good.
Super large particle diameter methyl-silicone oil emulsion prepared by the present invention is used for having good application effect in personal care product, Especially compounded with small particle silicone oil in washing and caring hair product so that hair has excellent dry and wet comb performance, excellent cunning soft Feel.
Specific embodiment
With reference to specific embodiment, invention is expanded on further, it should be noted that:Following examples are only with illustrating and not to Limitation technical scheme described in the invention, all equivalent exchanges made on the basis of technical scheme each fall within the present invention Protection domain.
Embodiment 1
The viscosity that 60 parts are added in high-efficient shear emulsifying equipment is the dimethicone of 60000cs, adds 4 parts of glycine betaine, 10 parts of water is added, is stirred, add 24 parts of dilution water, after stirring, add 1 part of guar gum, add 1 The AEO of part.The methyl-silicone oil emulsion particle diameter being prepared into is 31.47 μm, and the room temperature shelf-life is more than 12 Month, 50 DEG C are more than 30 days.
Embodiment 2
The viscosity that 60 parts are added in high-efficient shear emulsifying equipment is the dimethicone of 300000cs, adds 4 parts of glycine betaine, 10 parts of water is added, is stirred, add 25 parts of dilution water, after stirring, add 1 part of guar gum.The first being prepared into Base silicone oil emulsion particle diameter is 34.18 μm, and the room temperature shelf-life is more than 12 months, and 50 DEG C are more than 30 days.
The method of testing of properties is same as Example 1 with testing standard in the present embodiment.
Embodiment 3
The viscosity that 60 parts are added in high-efficient shear emulsifying equipment is the dimethicone of 500000cs, adds 4 parts of beet Alkali, adds 1 part of guar gum, adds 10 parts of water, stirs, and adds 25 parts of dilution water, after stirring, adds 1 The AEO of part.The methyl-silicone oil emulsion particle diameter being prepared into is 38.56 μm, and the room temperature shelf-life is more than 12 months, 50 DEG C are more than 30 days.
The method of testing of properties is same as Example 1 with testing standard in the present embodiment.

Claims (8)

1. the preparation method of a kind of super large particle diameter viscous methyl-silicone oil emulsion high, it is characterized by:Comprise the following steps:
A:The component of following mass fraction is added in high-efficient shear emulsifying equipment:50-70 parts of 10000-1000000cs bis- Methyl-silicone oil, the water of 1-4 parts of emulsifying agent and 7-14 part, is well mixed;
B:15-30 parts of the dilution water toward A, 0.1-1 parts of assistant for emulsifying agent and 0.1-1 parts of thickener, are well mixed, and obtain final product.
2. a kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high as claimed in claim 1, it is characterized by:Prepared Journey is reacted at normal temperatures and pressures.
3. a kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high as claimed in claim 1, it is characterized by:Step A In, dimethicone is preferably 60-70 parts, and emulsifying agent is preferably 2-4 parts, and water is preferably 10-13 parts.
4. a kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high as claimed in claim 1, it is characterized by:Step A In, dimethyl-silicon oil viscosity is preferably 200000-700000 cs.
5. a kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high as claimed in claim 1, it is characterized by:Step A In, emulsifying agent is one or more in anion, cation, nonionic, amphoteric surfactant, preferably nonionic or two Property surfactant, most preferably alkylation APEO or glycine betaine in one or more.
6. a kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high as claimed in claim 1, it is characterized by:Step B In, assistant for emulsifying agent is one or more in anion, cation, nonionic, amphoteric surfactant, preferably nonionic Fatty alcohol polyethenoxy ether class.
7. a kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high as claimed in claim 1, it is characterized by:Step B In, thickener is cellulose family, polyacrylic acid lipid or natural polymer and its derivative species, preferably natural polymer and Its derivative species.
8. a kind of preparation method of super large particle diameter viscous methyl-silicone oil emulsion high as claimed in claim 1, it is characterized by:Efficiently cut Cut emulsifying device preferably EKATO KOAX equipment.
CN201611255954.2A 2016-12-30 2016-12-30 A kind of super large partial size height glues the preparation method of methyl-silicone oil emulsion Active CN106700095B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108498376A (en) * 2018-04-02 2018-09-07 榛硕(武汉)智能科技有限公司 A kind of methyl-silicone oil emulsion and preparation method thereof
CN109438990A (en) * 2018-11-16 2019-03-08 山东道安新材料有限公司 A kind of compound silicone oil emulsion and preparation method thereof
CN110885559A (en) * 2019-12-18 2020-03-17 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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CN1711305A (en) * 2002-11-14 2005-12-21 瓦克化学有限公司 Highly concentrated oil-in-water silicone emulsions
CN101080440A (en) * 2004-12-15 2007-11-28 瓦克化学股份公司 Manufacturation of stable polysiloxane emulsion
CN101130634A (en) * 2007-08-08 2008-02-27 浙江大学 Amino silicone oil microemulsion with high solid content and preparation method thereof
CN105199395A (en) * 2015-09-28 2015-12-30 江苏惠丰润滑材料股份有限公司 Organosilicon waterborne emulsion and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108498376A (en) * 2018-04-02 2018-09-07 榛硕(武汉)智能科技有限公司 A kind of methyl-silicone oil emulsion and preparation method thereof
CN109438990A (en) * 2018-11-16 2019-03-08 山东道安新材料有限公司 A kind of compound silicone oil emulsion and preparation method thereof
CN110885559A (en) * 2019-12-18 2020-03-17 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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