CN101130634A - Amino silicone oil microemulsion with high solid content and preparation method thereof - Google Patents
Amino silicone oil microemulsion with high solid content and preparation method thereof Download PDFInfo
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- CN101130634A CN101130634A CNA2007100704989A CN200710070498A CN101130634A CN 101130634 A CN101130634 A CN 101130634A CN A2007100704989 A CNA2007100704989 A CN A2007100704989A CN 200710070498 A CN200710070498 A CN 200710070498A CN 101130634 A CN101130634 A CN 101130634A
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- silicone oil
- solid content
- high solid
- amido
- oil microemulsion
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- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 42
- 239000007787 solid Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920013822 aminosilicone Polymers 0.000 title abstract 6
- 229920002545 silicone oil Polymers 0.000 claims abstract description 32
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- -1 Amido silicon Chemical compound 0.000 claims description 27
- 125000003368 amide group Chemical group 0.000 claims description 27
- 239000003921 oil Substances 0.000 claims description 23
- 229910052710 silicon Inorganic materials 0.000 claims description 21
- 239000010703 silicon Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000012875 nonionic emulsifier Substances 0.000 claims description 2
- 239000008041 oiling agent Substances 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 23
- 239000000839 emulsion Substances 0.000 abstract description 11
- 238000004945 emulsification Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 238000010790 dilution Methods 0.000 abstract description 3
- 239000012895 dilution Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000007957 coemulsifier Substances 0.000 abstract 2
- 239000003792 electrolyte Substances 0.000 abstract 2
- 239000000835 fiber Substances 0.000 description 7
- OBFQBDOLCADBTP-UHFFFAOYSA-N aminosilicon Chemical compound [Si]N OBFQBDOLCADBTP-UHFFFAOYSA-N 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000000593 microemulsion method Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical group CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 1
- BVTJGGGYKAMDBN-UHFFFAOYSA-N Dioxetane Chemical compound C1COO1 BVTJGGGYKAMDBN-UHFFFAOYSA-N 0.000 description 1
- XVTJVGIQSVHBPO-UHFFFAOYSA-L N(=O)[O-].[Na+].[Cl-].[Na+] Chemical compound N(=O)[O-].[Na+].[Cl-].[Na+] XVTJVGIQSVHBPO-UHFFFAOYSA-L 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- AZFNGPAYDKGCRB-XCPIVNJJSA-M [(1s,2s)-2-amino-1,2-diphenylethyl]-(4-methylphenyl)sulfonylazanide;chlororuthenium(1+);1-methyl-4-propan-2-ylbenzene Chemical compound [Ru+]Cl.CC(C)C1=CC=C(C)C=C1.C1=CC(C)=CC=C1S(=O)(=O)[N-][C@@H](C=1C=CC=CC=1)[C@@H](N)C1=CC=CC=C1 AZFNGPAYDKGCRB-XCPIVNJJSA-M 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002979 fabric softener Substances 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical group CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010289 potassium nitrite Nutrition 0.000 description 1
- 239000004304 potassium nitrite Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- Colloid Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明公开了一种高固含量氨基硅油微乳液，重量百分比组成为：氨基硅油1％～60％；乳化剂5％～19％；助乳化剂2.5％～10％；电解质0.01％～0.1％；水15％～90％。本发明高固含量氨基硅油微乳液的制备采用为逆相(反相)乳化法，首先由乳化剂和硅油混合，然后通过加助乳化剂、水和电解质制备出介于O/W和W/O之间的双连续相结构的乳液，使用时通过稀释变成O/W的氨基硅油微乳液。本发明的氨基硅油微乳液为双连续型结构，稀释后具有粒径小、分布窄、固含量可达较高，为20％～80％(w/w)。并且制备过程简单、过程易控制。The invention discloses an amino silicone oil microemulsion with high solid content, which is composed of amino silicone oil 1%-60%; emulsifier 5%-19%; co-emulsifier 2.5%-10%; electrolyte 0.01%-0.1% ; Water 15% to 90%. The preparation of the high solid content amino silicone oil microemulsion of the present invention adopts the inverse phase (inverted phase) emulsification method, at first mixed by emulsifier and silicone oil, then by adding co-emulsifier, water and electrolyte to prepare a mixture between O/W and W/ The emulsion with bicontinuous phase structure between O can be diluted into O/W amino silicone oil microemulsion when used. The amino silicone oil microemulsion of the present invention has a bicontinuous structure, and after dilution, has small particle size, narrow distribution and high solid content of 20%-80% (w/w). Moreover, the preparation process is simple and easy to control.
Description
Technical field
The present invention relates to textiles auxiliary agent field, relate in particular to a kind of high solid content amido silicone oil microemulsion and preparation method.
Background technology
Amido silicon oil has excellent adsorption, becomes the characteristics of mould and favorable orientation, can give fabric sofetening mild feel, improves the flexibility and the smooth property of fabric greatly, is the most popular soft finishing agent in textile auxiliary agent field in recent years.Amido silicon oil and methyl-silicone oil backbone structure are similar, molecular backbone chain is very submissive, it is a kind of bent volution linear chain structure of easily disturbing, alternately form by Siliciumatom and Sauerstoffatom, methyl is almost nil around the free energy of Si-O key rotation, very free, can 360 ° of rotations, this characteristic makes silicone oil become the best fabric softener, and amino can with the hydroxyl of fiber surface, interactions such as Suo Ji, be orientated very securely and be adsorbed on the fiber, form very firm film at fiber surface, the static friction coefficient of fiber is descended, just can make with very little power to begin between the fiber to slide, make fabric produce good soft and smooth property, so amido silicon oil have better effect than the silicone oil of other kind.Chinese market year needs about 400,000 tons of textiles soft finishing agent at present, and wherein the consumption of amido silicon oil soft finishing agent has surpassed 20,000 tons.
Amido silicon oil is many to be used with emulsion state, the high viscosity of amido silicon oil and low surface tension have determined its more difficult emulsification, particle size of emulsion and distribution thereof have bigger influence to the result of use of amino silicon oil emulsion, when amido silicon oil uses with the microemulsion state, the moulding property of fiber, the film density, performances such as pliability all are greatly improved, therefore microemulsion can effectively improve the use properties of amido silicon oil, and the many solid contents of amido silicone oil microemulsion that oneself prepare on the Chinese market are lower, bring a lot of inconvenience for storage and transportation, higher solids content and stable amido silicone oil microemulsion have abroad been arranged, but the amido silicone oil microemulsion of import often mixes emulsifying agent and other additives, makes that cost is higher and it is inconvenient to use.
Summary of the invention
The invention provides a kind of simple to operate, lower-cost high solid content amido silicone oil microemulsion and preparation method.
A kind of high solid content amido silicone oil microemulsion, weight percent consists of:
Amido silicon oil 1%～60%
Emulsifying agent 5%～19%
Assistant for emulsifying agent 2.5%～10%
Ionogen 0.01%～0.1%
Water 15%～90%
Described amido silicon oil viscosity is 50mPas～5000mPas, and the ammonia value is 0.1～1.5.
Described amino silicon monomer is N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane or γ-divinyl triammonium propyl group methyl dimethoxysilane.
Described emulsifying agent is that nonionic emulsifier is composite, is nonyl phenol oxyethylene ether and Fatty Alcohol(C12-C14 and C12-C18) oxyethylene ether, and the hydrophile-lipophile balance value (HLB) of the emulsifying agent after composite is 12.0～13.8.
Described assistant for emulsifying agent is a carbonatoms less than 6 low mass molecule alcohol and/or carbonatoms less than 6 low molecular acid.When low mass molecule alcohol and low molecular acid mixing use can be arbitrary proportion.
Described low mass molecule alcohol can be at least a in ethanol, propyl alcohol, propyl carbinol, Pentyl alcohol or the polyoxyethylene glycol, and described low molecular acid can be at least a in acetate or the oxalic acid.
Described ionogen is an an alkali metal salt, as: Repone K, sodium-chlor, Sodium Nitrite, potassium nitrite, saltpetre, sodium sulfate etc.
The preparation method of described high solid content amido silicone oil microemulsion may further comprise the steps:
Add amido silicon oil and emulsifying agent in the reactor, stir 40～60min, add assistant for emulsifying agent (alcohol, organic acid) and water then, continue to stir 40～60min, add ionogen and water, stir 40～60min and obtain high solid content amido silicone oil microemulsion.
The strong stirring rake of shearing of the employing of described stirring, mixing speed is 50r/min～2000r/min.
The temperature that described preparation method suits is 5 ℃～80 ℃, when winter temperature is low, needs suitably heating.
Described preparation method is anti-phase (anti-phase) emulsion process, at first mix by emulsifying agent and silicone oil, then by add assistant for emulsifying agent, power and water is separated the emulsion that matter is prepared the co-continuous phase structure between O/W and W/O, becomes the amido silicone oil microemulsion of O/W during use by dilution.
The high viscosity of amido silicon oil and low surface tension have determined its more difficult emulsification, the many solid contents of amino silicon oil emulsion on the domestic market are not high now, be below 40%, what adopt is that the emulsion polymerization solid content is high or adopt the positive emulsion process to cause particle diameter bigger more, and particle size of emulsion and distribution thereof have bigger influence to the result of use of amino silicon oil emulsion, particle diameter is more little, and performances such as the moulding property of fiber, film density, pliability can be greatly improved.The present invention adopts the anti-phase emulsion process to prepare the high solids content microemulsion of (surpassing 70%), and particle diameter greatly reduces the transportation and the storage cost of amino silicon oil emulsion below 100nm, and smaller particle size has improved its use properties.
The amido silicone oil microemulsion of the inventive method preparation is a doubly-linked ideotype structure, has after the dilution that particle diameter is little, narrowly distributing, solid content can reach higherly, are 20%～80% (w/w).And preparation process is simple, process is easy to control.
Embodiment
Embodiment 1
Adding 140g viscosity in the beaker of 250ml is 850mPas, the ammonia value is 0.38 amido silicon oil, add the composite emulsifying agent of secondary octyl phenol polyethenoxy ether (TX-7 and TX-10), HLB value after emulsifying agent is composite is 13.0, the emulsifying agent consumption is 29% of an amido silicon oil quality, stirs 40min down with the strong stirring rake 400r/min that shears, and adds assistant for emulsifying agent, assistant for emulsifying agent comprises 10% propyl carbinol, 1.15% acetate, water 15g continues to stir 40min, the KCl (being dissolved in advance in the 8g water) of adding 0.1%, add the about 10g of water, continue to stir 40min, can contain the viscous emulsion of more white bubble, bubble collapse after placement for some time is transparence.It is amido silicone oil microemulsion of the present invention.
Weighting method claims to such an extent that solid content is about 78%, when being diluted with water to solid content 10%, obtains the blue light transparent micro emulsion, and it is 5.7 that acidometer is measured its pH value, and recording particle size of emulsion with laser particle analyzer is 23.2nm less than the equal particle diameter of body, and number average bead diameter is 13.6nm.
Annotate: the propyl carbinol of 10% described in the embodiment, 1.15% acetate, 0.1% KCl are benchmark with the quality of amido silicon oil all.
Embodiment 2
According to the operation of embodiment 1, amido silicon oil is used instead and is that viscosity 1000mPas, composite emulsifier use instead and is HLB value 12.8, and other conditions are constant, the preparation amido silicone oil microemulsion.Solid content is 72 ± 2%, and the particle diameter that laser particle analyzer records microemulsion is 64.6nm.
Embodiment 3
According to the operation of embodiment 1, amido silicon oil is used instead and is that viscosity 500mPas, composite emulsifier use instead and is HLB value 13.1, and other conditions are constant, the preparation amido silicone oil microemulsion.Solid content is that the particle diameter that 76 ± 2% laser particle analyzers record microemulsion is 24.6nm
Embodiment 4
According to the operation of embodiment 1, the composite type of emulsifying agent is used instead and is TX-7 and fatty alcohol-polyoxyethylene ether (AEO-9), and other conditions are constant, the preparation amido silicone oil microemulsion.Solid content is about 75%, and the particle diameter that laser particle analyzer records microemulsion is 83.2nm.
Embodiment 5
According to the operation of embodiment 1, propyl carbinol is used instead and is n-propyl alcohol and Pentyl alcohol mixture in the assistant for emulsifying agent, and n-propyl alcohol and Pentyl alcohol part by weight are 2.5: 1, and other conditions are constant, the preparation amido silicone oil microemulsion.Solid content is 73 ± 2%, and the particle diameter that laser particle analyzer records microemulsion is 60.3nm.
Embodiment 6
According to the operation of embodiment 1, amido silicon oil is used instead to the ammonia value is 0.26, acetate consumption 1% in the assistant for emulsifying agent, and other conditions are constant, the preparation amido silicone oil microemulsion.Solid content is about 75%, and the particle diameter that laser particle analyzer records microemulsion is 56.2nm.
Embodiment 7
According to the operation of embodiment 1, ionogen is used instead and is sodium-chlor, and other conditions are constant, the preparation amido silicone oil microemulsion.Solid content is about 77%, and the particle diameter that laser particle analyzer records microemulsion is 63.2nm.
Claims (9)
1. high solid content amido silicone oil microemulsion is characterized in that weight percent consists of:
Amido silicon oil 1%～60%
Emulsifying agent 5%～19%
Assistant for emulsifying agent 2.5%～10%
Ionogen 0.01%～0.1%
Water 15%～90%
2. high solid content amido silicone oil microemulsion according to claim 1 is characterized in that: described amido silicon oil viscosity is 50mPas～5000mPas, and the ammonia value is 0.1～1.5.
3. high solid content amido silicone oil microemulsion according to claim 1 is characterized in that: described emulsifying agent is that nonionic emulsifier is composite, and hydrophile-lipophile balance value is 12.0～13.8.
4. high solid content amido silicone oil microemulsion according to claim 1 is characterized in that: described emulsifying agent is that polyoxyethylene nonylphenol ether and fatty alcohol-polyoxyethylene ether are composite.
5. high solid content amido silicone oil microemulsion according to claim 1 is characterized in that: described assistant for emulsifying agent is a carbonatoms less than 6 low mass molecule alcohol and/or carbonatoms less than 6 low molecular acid.
6. high solid content amido silicone oil microemulsion according to claim 5, it is characterized in that: described low mass molecule alcohol is at least a in ethanol, propyl alcohol, propyl carbinol, Pentyl alcohol or the polyoxyethylene glycol, and described low molecular acid is at least a in acetate or the oxalic acid.
7. high solid content amido silicone oil microemulsion according to claim 1 is characterized in that: described ionogen is an an alkali metal salt.
8. the preparation method of high solid content amido silicone oil microemulsion according to claim 1, may further comprise the steps: add amido silicon oil and emulsifying agent in the reactor, stir 40～60min, add assistant for emulsifying agent then, continue to stir 40～60min, add ionogen and water, stir 40～60min and obtain high solid content amido silicone oil microemulsion.
9. preparation method according to claim 9 is characterized in that: temperature is 5 ℃～80 ℃ in the reaction process, and the rotating speed of stirring is 50r/min～2000r/min.
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Cited By (9)
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| CN101497744B (en) * | 2008-07-29 | 2011-01-12 | 浙江传化股份有限公司 | Amino silicon oil emulsion and preparation thereof |
| CN102995443A (en) * | 2012-11-29 | 2013-03-27 | 常熟市三利经纬编织造有限公司 | Manufacture method of waterproof polyester fabric |
| CN103059829A (en) * | 2013-01-25 | 2013-04-24 | 中国石油大学(华东) | Nanometer emulsion type water control fracturing fluid for tight gas reservation well and preparation method thereof |
| CN106633103A (en) * | 2016-12-30 | 2017-05-10 | 江西蓝星星火有机硅有限公司 | Preparation method of high-internal-phase-viscosity polysiloxane emulsion |
| CN106700095A (en) * | 2016-12-30 | 2017-05-24 | 江西蓝星星火有机硅有限公司 | Preparation method of large-particle-size high-viscosity methyl silicon oil emulsion |
| CN109280171A (en) * | 2018-08-28 | 2019-01-29 | 上海树脂厂有限公司 | Small particle amido silicone oil microemulsion and its preparation method and application |
| 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 |
| CN113185710A (en) * | 2021-04-26 | 2021-07-30 | 广东赛安特新材料有限公司 | Amino silicone oil emulsion and preparation method thereof |
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| CN1167729C (en) * | 2001-03-07 | 2004-09-22 | 华东理工大学 | Preparation method of aminoalkyl polyorganosiloxane |
| EP1258503A1 (en) * | 2001-05-15 | 2002-11-20 | Clariant International Ltd. | Modified polyorganosiloxanes, aqueous emulsions, preparation and use thereof |
| CN1539866A (en) * | 2003-11-01 | 2004-10-27 | 唐昌军 | Preparation method for flexible balancing ammonia alkyl polyorganosiloxane and microcmulsion fluid, and application |
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| CN101497744B (en) * | 2008-07-29 | 2011-01-12 | 浙江传化股份有限公司 | Amino silicon oil emulsion and preparation thereof |
| CN102995443A (en) * | 2012-11-29 | 2013-03-27 | 常熟市三利经纬编织造有限公司 | Manufacture method of waterproof polyester fabric |
| CN103059829A (en) * | 2013-01-25 | 2013-04-24 | 中国石油大学(华东) | Nanometer emulsion type water control fracturing fluid for tight gas reservation well and preparation method thereof |
| CN103059829B (en) * | 2013-01-25 | 2014-08-20 | 中国石油大学(华东) | Nanometer emulsion type water control fracturing fluid for tight gas reservation well and preparation method thereof |
| CN106633103B (en) * | 2016-12-30 | 2019-06-04 | 江西蓝星星火有机硅有限公司 | A kind of preparation method of the polysiloxane emulsion of high internal phase viscosities |
| CN106633103A (en) * | 2016-12-30 | 2017-05-10 | 江西蓝星星火有机硅有限公司 | Preparation method of high-internal-phase-viscosity polysiloxane emulsion |
| CN106700095A (en) * | 2016-12-30 | 2017-05-24 | 江西蓝星星火有机硅有限公司 | Preparation method of large-particle-size high-viscosity methyl silicon oil emulsion |
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| CN109280171A (en) * | 2018-08-28 | 2019-01-29 | 上海树脂厂有限公司 | Small particle amido silicone oil microemulsion and its preparation method and application |
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Assignee: Zhejiang in Yiwu Province Li industry and Trade Co., Ltd. Assignor: Zhejiang University Contract record no.: 2011330000316 Denomination of invention: High solid content amido silicone oil microemulsion and method of producing the same Granted publication date: 20110112 License type: Exclusive License Open date: 20080227 Record date: 20110420 |
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