CN103073892A - O/W type polysiloxane nano-emulsion and preparation method thereof - Google Patents
O/W type polysiloxane nano-emulsion and preparation method thereof Download PDFInfo
- Publication number
- CN103073892A CN103073892A CN2013100520552A CN201310052055A CN103073892A CN 103073892 A CN103073892 A CN 103073892A CN 2013100520552 A CN2013100520552 A CN 2013100520552A CN 201310052055 A CN201310052055 A CN 201310052055A CN 103073892 A CN103073892 A CN 103073892A
- Authority
- CN
- China
- Prior art keywords
- polysiloxane
- alcohol
- emulsifying agent
- organic additive
- nanoemulsions
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Cosmetics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses O/W type polysiloxane nano-emulsion and a preparation method thereof. The O/W type polysiloxane nano-emulsion consists of the following components in percentage by weight: 1-30 percent of polysiloxane, 5-25 percent of emulsifying agent, 3-25 percent of organic additive, 0.01-2.0 percent of inorganic additive and the balance of water. The preparation method of the O/W type polysiloxane nano-emulsion comprises the following steps of: firstly mixing the polysiloxane and the emulsifying agent and then heating to 70-90 DEG C to obtain a uniformly dispersed oil phase component; then mixing the organic additive, the inorganic additive and water and then heating to 70-90 DEG C to obtain a uniformly dispersed water phase component; and finally, homogenizing the oil phase component at a homogenizing speed of 15,000-30,000 rpm, meanwhile, adding the water phase component therein, homogenizing for 5-15 minutes, then controlling the stirring speed to be 300-800 rpm and naturally cooling to room temperature to obtain the O/W type polysiloxane nano-emulsion with particle diameter of dispersed phase particles within 100-500 nm.
Description
Technical field
The invention belongs to the makeup technical field, relate to a kind of O/W type polysiloxane nanoemulsions and preparation method thereof.
Background technology
Polysiloxane is that a class has unique siloxane bond structure Si-O-Si, gives larger bond angle and bond distance, and Intermolecular Forces is little, unlike the easy crystallization of organic molecule, therefore, good air permeability; The bond energy that it is higher makes organosilicon polymer have outstanding thermotolerance and excellent flexibility, and the vertical outside of the spirane structure of its molecular chain and methyl makes it to have extremely low surface tension, good water repellency.Because si-h bond (Si-H) has larger activity, can issue unboiled water solution and condensation cross-linking film forming at high temperature and metal-salt effect, function antibiotic, mildew-resistant that the active group of organosilicon quaternary ammonium salt has, because structural singularity, make organosiloxane polymer have lubricated, soft, refuse the series of characteristics such as water, froth breaking, antibacterial and mouldproof, be applicable in the personal-care supplies.Therefore polysiloxane is applied to makeup, will have that lubricity is good, the performance of ultra-violet radiation resisting is good, antistatic property is good, good permeability, stability are high, nontoxic, odorless, tasteless, can not cause skin and to stimulate and irritated, the characteristics such as security is high.Yet the siloxane bond structure Si-O-Si of polysiloxane belongs to nonpolar structure, is difficult to emulsified in application process.
Skin-care cosmetics product great majority belong to emulsion system, and common emulsion system causes the dispersed phase particles particle diameter larger owing to the equal reason of the technique of the composite ratio of recipe ingredient and employing, generally greater than 1 μ m, therefore, the dispersiveness of product, poor stability, the product heterogeneity is scattered in the activeconstituents of common emulsion system for above-mentioned reasons, cause the functional mass poor permeability, be difficult to play the effect of effect.
Summary of the invention
One of purpose of the present invention is in order to solve above-mentioned ordinary emulsion system dispersed phase particles heterogeneity, the technical problem that particle diameter is excessive and a kind of dispersed phase particles uniform particle diameter, O/W type polysiloxane nanoemulsions that particle diameter is less are provided.
Two of purpose of the present invention provides above-mentioned a kind of O/W type polysiloxane nanoemulsions preparation method, namely in the homogeneous oil phase, add water, utilize the low-energy emulsification method, nanoemulsions forms dispersed phase particles uniform particle diameter, O/W type polysiloxane nanoemulsions that particle diameter is less in the phase inversion process.
Technical scheme of the present invention
A kind of O/W type polysiloxane nanoemulsions counts by weight percentage, and composition and the content of its raw material are as follows:
Polysiloxane 1～30%
Emulsifying agent 5～25%
Organic additive 3～25%
Inorganic additives 0.01～2.0%
Surplus is water;
Described polysiloxane is one or more mixtures that form in polydimethyl polysiloxane, methyl phenyl silicone, long chain alkyl modified polysiloxane, cyclic polysiloxanes, amino modified polysiloxane and the carboxy-modified polysiloxane, is preferably polydimethyl polysiloxane, methyl phenyl silicone or long chain alkyl modified polysiloxane;
Described emulsifying agent is sorbitan fatty acid ester, the polyoxyethylene sorbitan fatty acid ester, fatty alcohol-polyoxyethylene ether, cithrol, ethoxylated castor oil, glycerine monofatty ester, the composite mixture that in polyglycerol ester and the sucrose monostearate one or more form, preferred HLB value in the described composite mixture (described HLB value is the size between the hydrophilic group and oleophilic group and the amount of balance of power degree in the surfactant molecule) between 3～8 and HLB composite between 8～18, and the emulsifier content that wherein the HLB value is higher is greater than the content of the lower emulsifying agent of HLB value.
Described organic additive is monohydroxy-alcohol or the polyvalent alcohol of short carbon chain;
The molecular formula of wherein said monohydroxy-alcohol is C
nH
2n+1OH, wherein n is between 1～12;
Wherein said polyvalent alcohol is one or more alcohol mixtures that form in ethylene glycol, 1,2-PD, 1,3-PD, 1,3 butyleneglycol, propylene carbonate and the glycerol, is preferably 1,2-PD, 1,3 butyleneglycol or glycerol;
Described inorganic additives is one or more mixtures that form in sodium-chlor, Repone K, sal epsom, the sodium sulfate, is preferably sodium-chlor, Repone K or sal epsom;
The preparation method of above-mentioned a kind of O/W type polysiloxane nanoemulsions specifically comprises the steps
(1), with polysiloxane and emulsifying agent mixing post-heating to 70～90 ℃, obtain finely dispersed oil phase component;
(2), with organic additive, inorganic additives and water mixing post-heating to 70～90 ℃, obtain finely dispersed water component;
(3), with the oil phase component of homogeneous speed 15000～30000rpm homogenizing step (1) gained, water component with step (2) gained adds wherein simultaneously, behind homogeneous 5～15min, the control stirring velocity is 3200～800rpm, naturally cooling is down to room temperature, namely gets O/W type polysiloxane nanoemulsions.
Beneficial effect of the present invention
A kind of O/W type polysiloxane nanoemulsions of the present invention has adopted the compound scheme of polysiloxane preferably, emulsifying agent, organic additive, inorganic additives and water.Owing to adopting in the preparation process and in the homogeneous oil phase component, adding the water component, namely utilize the low-energy emulsification method, therefore, uniform particle diameter, the particle diameter of the dispersed phase particles of the O/W type polysiloxane nanoemulsions of final gained are less, are between 100～500nm, and its preparation technology is simple, energy consumption is low, the nanoemulsions stable system that forms is transparent or semitransparent outward appearance, and the product skinfeel is good, the activeconstituents of load is easy to infiltration, and then plays the effect of effect.
Description of drawings
The transmission electron microscope picture of the O/W type polysiloxane nanoemulsions of Fig. 1, embodiment 1 gained.
Embodiment
Also by reference to the accompanying drawings the present invention is further set forth below by specific embodiment, but do not limit the present invention.
Used transmission electron microscope is that NEC is made TEM-2100 type transmission electron microscope in the embodiment of the invention.
Embodiment 1
A kind of O/W type polysiloxane nanoemulsions counts by weight percentage, and each raw material composition and content are as follows in the described O/W type polysiloxane nanoemulsions:
Polysiloxane 1%
Emulsifying agent 5%
Organic additive 3%
Inorganic additives 0.01%
Water 90.99%
Described polysiloxane is polydimethylsiloxane, the technical grade product of the used for cosmetic that DOW CORNING (China) organosilicon company limited produces;
Described emulsifying agent is C
18The polyoxyethylenated alcohol mixture is namely by the C of EO=2
18The C of polyoxyethylenated alcohol and EO=21
18The mixture that polyoxyethylenated alcohol forms, the HLB value of mixture is 11.3, wherein the C of EO=2
18Polyoxyethylenated alcohol is that 2%, HLB value is the C of 5, EO=21
18Polyoxyethylenated alcohol is that 3%, HLB value is 15.5, the technical grade product that large (China) company limited of standing grain provides, and described EO is the average ethoxy radix of Soxylat A 25-7;
Described inorganic salt are sodium-chlor, the chemical pure product of Chemical Reagent Co., Ltd., Sinopharm Group;
Described organic additive is 1,2 propylene glycol, the SILVER REAGENT product of Chemical Reagent Co., Ltd., Sinopharm Group.
The preparation method of above-mentioned a kind of polysiloxane nanoemulsions specifically comprises the steps:
(1), with polysiloxane and emulsifying agent mixing post-heating to 70 ℃, obtain finely dispersed oil phase component;
(2), with organic additive, inorganic additives and water mixing post-heating to 70 ℃, obtain finely dispersed water component;
(3), with the oil phase component of homogeneous speed 15000rpm homogenizing step (1) gained, water component with step (2) gained adds wherein simultaneously, the control stirring velocity is that the 300rpm naturally cooling is down to room temperature behind the homogeneous 5min, finally forms the particle diameter of dispersed phase particles at the O/W of 100～300nm type polysiloxane nanoemulsions.
The transmission electron microscope picture of the O/W type polysiloxane nanoemulsions of above-mentioned gained as shown in Figure 1, as can be seen from Figure 1 emulsion particle distribution homogeneous, size is about 150nm.
Embodiment 2
A kind of O/W type polysiloxane nanoemulsions counts by weight percentage, and each raw material composition and content are as follows in the described O/W type polysiloxane nanoemulsions:
Polysiloxane 15%
Emulsifying agent 15%
Organic additive 15%
Inorganic additives 0.5%
Water 54.5%
Described polysiloxane is methyl phenyl silicone, the technical grade product that DOW CORNING (China) organosilicon company limited produces;
Described emulsifying agent is the mixture that is comprised of sorbitan fatty acid ester and polyoxyethylene sorbitan fatty acid ester, the HLB value of mixture is 10.72, wherein sorbitan fatty acid ester is 6%, the HLB value is 4.3, the polyoxyethylene sorbitan fatty acid ester is 9%, the HLB value is 15, the technical grade product that Chemical Reagent Co., Ltd., Sinopharm Group provides;
Described inorganic salt are Repone K, the chemical pure product of Chemical Reagent Co., Ltd., Sinopharm Group;
Described organic additive is glycerol, the SILVER REAGENT product of Chemical Reagent Co., Ltd., Sinopharm Group.
The preparation method of above-mentioned a kind of polysiloxane nanoemulsions specifically comprises the steps:
(1), with polysiloxane and emulsifying agent mixing post-heating to 80 ℃, obtain finely dispersed oil phase component;
(2), with organic additive, inorganic additives and water mixing post-heating to 80 ℃, obtain finely dispersed water component;
(3), with the oil phase component of homogeneous speed 25000rpm homogenizing step (1) gained, water component with step (2) gained adds wherein simultaneously, the control stirring velocity is that the 500rpm naturally cooling is down to room temperature behind the homogeneous 8min, finally forms the particle diameter of dispersed phase particles at the O/W of 300～400nm type polysiloxane nanoemulsions.
Embodiment 3
A kind of O/W type polysiloxane nanoemulsions counts by weight percentage, and each raw material composition and content are as follows in the described O/W type polysiloxane nanoemulsions:
Polysiloxane 30%
Emulsifying agent 25%
Organic additive 25%
Inorganic additives 2.0%
Water 18%
Described polysiloxane is long chain alkyl modified polysiloxane, the technical grade product that DOW CORNING (China) organosilicon company limited produces;
Described emulsifying agent is stearic acid polyglycerol ester mixture, the mixture that is namely formed by the poly-Witepsol W-S 55 of stearic acid and poly-ten glyceryl ester of stearic acid, the HLB value of mixture is 10.6, wherein the poly-Witepsol W-S 55 of stearic acid is 10%, the HLB value is 7, poly-ten glyceryl ester of stearic acid are that 15%, HLB value is 13, the technical grade product that husky (China) company limited of dragon provides;
Described inorganic salt are sal epsom, the chemical pure product of Chemical Reagent Co., Ltd., Sinopharm Group;
Described organic additive is 1,3 butyleneglycol, the SILVER REAGENT product of Chemical Reagent Co., Ltd., Sinopharm Group.
The preparation method of above-mentioned a kind of polysiloxane nanoemulsions specifically comprises the steps:
(1), with polysiloxane and emulsifying agent mixing post-heating to 90 ℃, obtain finely dispersed oil phase component;
(2), with organic additive, inorganic additives and water mixing post-heating to 90 ℃, obtain finely dispersed water component;
(3), with the oil phase component of homogeneous speed 30000rpm homogenizing step (1) gained, water component with step (2) gained adds wherein simultaneously, the control stirring velocity is that the 800rpm naturally cooling is down to room temperature behind the homogeneous 15min, finally forms the particle diameter of dispersed phase particles at the O/W of 400～500nm type polysiloxane nanoemulsions.
Foregoing only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (5)
1. an O/W type polysiloxane nanoemulsions is characterized in that counting by weight percentage, and its raw material composition and content are as follows:
Polysiloxane 1～30%
Emulsifying agent 5～25%
Organic additive 3～25%
Inorganic additives 0.01～2.0%
Surplus is water;
Described polysiloxane is one or more mixtures that form in polydimethyl polysiloxane, methyl phenyl silicone, long chain alkyl modified polysiloxane, cyclic polysiloxanes, amino modified polysiloxane, the carboxy-modified polysiloxane;
Described emulsifying agent is sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, C
8-22One or more composite mixtures that form in polyoxyethylenated alcohol, cithrol, ethoxylated castor oil, glycerine monofatty ester, poly alkyl alcohol glyceryl ester, the sucrose monostearate;
Described organic additive is monohydroxy-alcohol or the polyvalent alcohol of short carbon chain, and the molecular formula of wherein said monohydroxy-alcohol is C
nH
2n+1OH, wherein n is between 1～12; Wherein said polyvalent alcohol is one or more alcohol mixtures that form in ethylene glycol, 1,2-PD, 1,3-PD, 1,3 butyleneglycol, propylene carbonate and the glycerol;
Described inorganic additives is one or more mixtures that form in sodium-chlor, Repone K, sal epsom, the sodium sulfate.
2. a kind of O/W type polysiloxane nanoemulsions as claimed in claim 1 is characterized in that counting by weight percentage, and its raw material composition and content are as follows:
Polysiloxane 1%
Emulsifying agent 5%
Organic additive 3%
Inorganic additives 0.01%
Water 90.99%
Described polysiloxane is polydimethylsiloxane;
Described emulsifying agent is C
8-22The polyoxyethylenated alcohol mixture is namely by the C of EO=2
8-22The C of polyoxyethylenated alcohol and EO=21
8-22The mixture that polyoxyethylenated alcohol forms, the wherein C of EO=2
8-22Polyoxyethylenated alcohol is the C of 2%, EO=21
8-22Polyoxyethylenated alcohol is 3%;
Described inorganic salt are sodium-chlor;
Described organic additive is 1,2 propylene glycol.
3. a kind of O/W type polysiloxane nanoemulsions as claimed in claim 1 is characterized in that counting by weight percentage, and its raw material composition and content are as follows:
Polysiloxane 15%
Emulsifying agent 15%
Organic additive 15%
Inorganic additives 0.5%
Water 54.5%
Described polysiloxane is methyl phenyl silicone;
Described emulsifying agent is the mixture that is comprised of sorbitan fatty acid ester and polyoxyethylene sorbitan fatty acid ester, and wherein sorbitan fatty acid ester is 6%, and the polyoxyethylene sorbitan fatty acid ester is 9%;
Described inorganic salt are Repone K;
Described organic additive is glycerol.
4. a kind of O/W type polysiloxane nanoemulsions as claimed in claim 1 is characterized in that counting by weight percentage, and its raw material composition and content are as follows:
Polysiloxane 30%
Emulsifying agent 25%
Organic additive 25%
Inorganic additives 2.0%
Water 18%
Described polysiloxane is long chain alkyl modified polysiloxane;
Described emulsifying agent is the poly alkyl alcohol glyceride mixture, the mixture that is namely formed by poly alkyl alcohol Witepsol W-S 55 and poly alkyl alcohol ten glyceryl ester, and wherein the poly alkyl alcohol Witepsol W-S 55 is 10%, poly alkyl alcohol ten glyceryl ester are 15%;
Described inorganic salt are sal epsom;
Described organic additive is 1,3 butyleneglycol.
5. such as the preparation method of claims 1,2,3 or 4 described a kind of O/W type polysiloxane nanoemulsions, it is characterized in that specifically comprising the steps:
(1), with polysiloxane and emulsifying agent mixing post-heating to 70～90 ℃, obtain finely dispersed oil phase component;
(2), with organic additive, inorganic additives and water mixing post-heating to 70～90 ℃, obtain finely dispersed water component;
(3), with the oil phase component of homogeneous speed 15000～30000rpm homogenizing step (1) gained, water component with step (2) gained adds wherein simultaneously, the control stirring velocity is that 300～800rpm naturally cooling is down to room temperature behind homogeneous 5～15min, namely gets O/W type polysiloxane nanoemulsions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310052055.2A CN103073892B (en) | 2013-02-18 | 2013-02-18 | O/W type polysiloxane nano-emulsion and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310052055.2A CN103073892B (en) | 2013-02-18 | 2013-02-18 | O/W type polysiloxane nano-emulsion and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103073892A true CN103073892A (en) | 2013-05-01 |
| CN103073892B CN103073892B (en) | 2015-05-20 |
Family
ID=48150596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310052055.2A Expired - Fee Related CN103073892B (en) | 2013-02-18 | 2013-02-18 | O/W type polysiloxane nano-emulsion and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103073892B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107574038A (en) * | 2017-08-14 | 2018-01-12 | 中山大学惠州研究院 | A kind of essence microemulsion and preparation method thereof |
| CN109517191A (en) * | 2018-11-16 | 2019-03-26 | 山东道安新材料有限公司 | A kind of highly stable Modified silicon oil emulsion |
| CN113550150A (en) * | 2021-09-02 | 2021-10-26 | 浙江宝时美化工有限公司 | Preparation method of compound organic silicon softening agent |
| WO2022001575A1 (en) * | 2020-06-30 | 2022-01-06 | 江苏四新科技应用研究所股份有限公司 | Organosilicone emulsion and preparation method |
| CN114249897A (en) * | 2020-09-24 | 2022-03-29 | 深圳市鸿信顺电子材料有限公司 | Impregnation liquid and application thereof in surface treatment process of sheet type element |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1610717A (en) * | 2002-01-25 | 2005-04-27 | 陶氏康宁公司 | Compositions containing silicone oil-in-water emulsions, salts, alcohols and solvents |
-
2013
- 2013-02-18 CN CN201310052055.2A patent/CN103073892B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1610717A (en) * | 2002-01-25 | 2005-04-27 | 陶氏康宁公司 | Compositions containing silicone oil-in-water emulsions, salts, alcohols and solvents |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107574038A (en) * | 2017-08-14 | 2018-01-12 | 中山大学惠州研究院 | A kind of essence microemulsion and preparation method thereof |
| CN109517191A (en) * | 2018-11-16 | 2019-03-26 | 山东道安新材料有限公司 | A kind of highly stable Modified silicon oil emulsion |
| WO2022001575A1 (en) * | 2020-06-30 | 2022-01-06 | 江苏四新科技应用研究所股份有限公司 | Organosilicone emulsion and preparation method |
| CN114249897A (en) * | 2020-09-24 | 2022-03-29 | 深圳市鸿信顺电子材料有限公司 | Impregnation liquid and application thereof in surface treatment process of sheet type element |
| CN113550150A (en) * | 2021-09-02 | 2021-10-26 | 浙江宝时美化工有限公司 | Preparation method of compound organic silicon softening agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103073892B (en) | 2015-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103073892B (en) | O/W type polysiloxane nano-emulsion and preparation method thereof | |
| CN1206301C (en) | Organosilicon water repellent compositions | |
| EP1427772B1 (en) | Clear silicone microemulsions | |
| CN102046139B (en) | The preparation of siloxane microemulsion | |
| KR101451116B1 (en) | Aqueous silicone emulsions for imparting water repellency | |
| CN102264800B (en) | Curable organopolysiloxane composition and porous cured organopolysiloxane material | |
| CN102639607B (en) | Silicone oil emulsion, method of producing same, and silicone oil composition | |
| CN102226072A (en) | Preparation method of organic silicon microcapsule powder waterproof agent | |
| JP2012506469A (en) | Composition comprising a silicon-containing compound | |
| CN103113824A (en) | Film-forming polysiloxane emulsion and preparation method thereof | |
| CN102249593A (en) | Preparation method of organosilicon powder waterproofing agent | |
| CN101061993A (en) | Methods and compositions for epilation | |
| CN107384326A (en) | Gelatin chitosan nano silicon multinuclear microcapsules of storing energy through phase change preparation method | |
| KR20130062284A (en) | Cosmetic raw material | |
| KR100994353B1 (en) | Composite cured silicone powder, method for production thereof and aqueous composition | |
| CN106243364B (en) | A kind of organic silicon modified by polyether lotion and preparation method thereof | |
| EP1660584B1 (en) | Silicone oil-in-water (o/w) emulsions or compositions useful for water repellent applications | |
| CN103690379B (en) | A kind of O/W type shea butter nanoemulsions and preparation method thereof | |
| CN103070787B (en) | O/W type polysiloxane nano-emulsion and a preparation method thereof | |
| TW200301136A (en) | Stabilization of vitamins in water-in-silicone oil (W/O) emulsions | |
| JP5543069B2 (en) | Polyoxyalkylene-alkyl functional siloxane resins and aqueous compositions thereof | |
| EP0992280A2 (en) | Method of making thick water-in-silicone emulsions | |
| Bayer et al. | Superhydrophobic cellulose-based bionanocomposite films from Pickering emulsions | |
| CN107304295A (en) | A kind of preparation method of MQ resin tooths organosilicone elastic silica gel thin film | |
| CN103668941A (en) | Rabbit hair textile anti-static nano-finishing agent and finishing process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150520 Termination date: 20180218 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |