CN102002242A - Organosilicon emulsion and preparation method thereof - Google Patents
Organosilicon emulsion and preparation method thereof Download PDFInfo
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- CN102002242A CN102002242A CN 201010513349 CN201010513349A CN102002242A CN 102002242 A CN102002242 A CN 102002242A CN 201010513349 CN201010513349 CN 201010513349 CN 201010513349 A CN201010513349 A CN 201010513349A CN 102002242 A CN102002242 A CN 102002242A
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- 239000000839 emulsion Substances 0.000 title claims abstract description 92
- 238000004945 emulsification Methods 0.000 title claims description 15
- 238000002360 preparation method Methods 0.000 title abstract description 23
- 229920000570 polyether Polymers 0.000 claims abstract description 68
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000013543 active substance Substances 0.000 claims abstract description 53
- -1 polysiloxane Polymers 0.000 claims abstract description 41
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 28
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 23
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000007762 w/o emulsion Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 69
- 239000010703 silicon Substances 0.000 claims description 68
- 229910052710 silicon Inorganic materials 0.000 claims description 68
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 10
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000600 sorbitol Substances 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 230000002209 hydrophobic effect Effects 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 239000001593 sorbitan monooleate Substances 0.000 claims description 4
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 4
- 235000011069 sorbitan monooleate Nutrition 0.000 claims description 4
- 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 description 3
- 239000005639 Lauric acid Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 229960001866 silicon dioxide Drugs 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 239000001587 sorbitan monostearate Substances 0.000 claims description 2
- 235000011076 sorbitan monostearate Nutrition 0.000 claims description 2
- 229940035048 sorbitan monostearate Drugs 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 238000012512 characterization method Methods 0.000 claims 1
- 239000000470 constituent Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 239000004721 Polyphenylene oxide Substances 0.000 abstract description 7
- 230000001804 emulsifying effect Effects 0.000 abstract description 5
- 230000008719 thickening Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 239000010985 leather Substances 0.000 abstract description 2
- 238000009941 weaving Methods 0.000 abstract description 2
- 239000000084 colloidal system Substances 0.000 abstract 1
- 239000002537 cosmetic Substances 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 239000007764 o/w emulsion Substances 0.000 abstract 1
- 238000009987 spinning Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 17
- 239000007787 solid Substances 0.000 description 8
- 239000002562 thickening agent Substances 0.000 description 8
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 7
- 229940069338 potassium sorbate Drugs 0.000 description 7
- 235000010241 potassium sorbate Nutrition 0.000 description 7
- 239000004302 potassium sorbate Substances 0.000 description 7
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002518 antifoaming agent Substances 0.000 description 3
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Chemical compound [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- HOWGUJZVBDQJKV-UHFFFAOYSA-N docosane Chemical compound CCCCCCCCCCCCCCCCCCCCCC HOWGUJZVBDQJKV-UHFFFAOYSA-N 0.000 description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical compound C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 description 1
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000002511 behenyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229960001631 carbomer Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 125000002811 oleoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Abstract
The invention discloses an organosilicon emulsion which comprises active substances, high-grade fatty alcohol polyether, an emulsifying agent, polyether modified polysiloxane and water, wherein the active substrates are obtained from polysiloxane and lyophobic particles under the action of a catalyst. A preparation method of the organosilicon emulsion comprises the steps of: A, fully mixing the active substances, the high-grade fatty alcohol polyether, the emulsifying agent and the polyether modified polysiloxane for 10-50min through stirring; B, raising the temperature of the system in the step A to 55-85 DEG C; C, keeping the temperature of the system, slowly adding the water, increasing the stirring speed to ensure that a water-in-oil emulsion is changed into an oil-in-water emulsion, and continuously adding the water until the mass concentration is 40-70 percent; and D, further emulsifying crude emulsion through a colloid mill, and finally, diluting without thickening water until the needed emulsion concentration is reached. The organosilicon emulsion prepared by the method has stable property, and can be widely applied to the industries of papermaking, spinning and weaving, coating, leather, medicine, cosmetics and the like.
Description
Technical field
The present invention relates to a kind of organic silicon emulsion and preparation method, organic silicon emulsion is important fine chemicals additive, and therefore, the present invention is under the jurisdiction of technical field of fine chemical preparations.
Technical background
Organic silicon emulsion is one of important organosilicon product, because its special performance and characteristics, be widely used industrial, be widely used in industrial circles such as papermaking, weaving, slurry, coating, building, leather, medicine, makeup, and Application Areas is also in continuous expansion, and it is very big to use potential.In above-mentioned Application Areas, organosilicon uses the most economical, convenient, safety with the form of water miscible liquid, meets environmental protection requirement simultaneously.
The organic silicon emulsion that uses in the commercial run mainly is an oil-in-water-type, the oil-in-water-type organic silicon emulsion mainly contains following two kinds of preparation methods, first kind forms by the polymeric method, organosilane monomer is polymerized under effects such as catalyzer and initiator and tensio-active agent, as fabric water repllents etc.; Second kind is the method preparation by machinery, various components with the preparation emulsion, comprise compositions such as oil phase component, emulsifying agent, water, stablizer, get by mode decentralized systems such as heated and stirred, mechanical shearing, colloidal mill, clarifixators, as defoamer, releasing agent or the like.
Difference according to the organic silicon emulsion use, the polysiloxane of selection different viscosity, modified polyorganosiloxane are as active substance, these polysiloxane have plenty of linear structure, has plenty of space three-dimensional structure, active substance is scattered in the water with existing emulsion preparation method is the very thing of difficulty of part, patent CN1807512 and CN101298027 then are scattered in full-bodied organosilicon mixture in the water by adding some auxiliary substances, are prepared into organic silicon emulsion.
Estimate a kind of organic silicon emulsion, usually its function and all the other relevant natures are closely connected together, for example, the silicone antifoam agent emulsion also must be considered dilution stability, shear resistant, stability in storage and heatproof stability of product or the like when guaranteeing antifoam performance, if the organosilicon emulsion defoaming agents that stability is bad is applied to dyeing such as cotton, chemical fibre in the textile industry and goes up and eliminate harmful foamy words, just be easy to form " silicon spot ", badly influence the quality of painted efficient and the finished product, cause heavy losses economically.Therefore, the stability of organic silicon emulsion is quite important.
The key ingredient emulsifying agent of organic silicon emulsion mainly is used for the dispersed activity material.A large amount of experiment experiences show that emulsifying agent is too much, can have influence on the major function of organic silicon emulsion; Emulsifying agent is very few, and the organic silicon emulsion that obtains is then very unstable, may cause damage.Therefore, a lot of organic silicon emulsion investigators pay close attention to " when guaranteeing the performance security of organic silicon emulsion, how reducing the ratio between emulsifying agent and the active substance? ", to give full play to the function of active substance, reduce chemical oxygen demand and biological oxygen demand (BOD), realize low-carbon economy and environmental protection and economy.
At present, adopt silicon polyethers, anhydrous sorbitol polyether derivative, alkyl phenol polyether derivative etc. to disperse organosilicon mixture usually, but the emulsifying power of these emulsifying agents remain further to be improved as emulsifying agent.
The present inventor passes through lot of experiments, preferably include organopolysiloxane materials such as polydimethylsiloxane, poly-di-ethyl siloxane, poly-methyl trifluoro propyl siloxanes, poly-ethylene methacrylic radical siloxane, again with described organopolysiloxane and hydrophobic particles the reaction product under catalyst action as active substance, study in conjunction with emulsifying process, pass through preferred emulsifier, introduce materials such as polyether-modified polysiloxane (being commonly called as the silicon polyethers), high fatty alcohol polyethers, processing and preparing becomes stable organic silicon emulsion.Test-results shows, adds the high fatty alcohol polyethers when the emulsification organosilicon mixture in mixture, can improve the emulsifying power of emulsifying agent greatly, obtains more stable organic silicon emulsion, so also just can promote the function of active substance greatly.
Summary of the invention
The purpose of this invention is to provide a kind of organic silicon emulsion and preparation method, the organic silicon emulsion of using the present invention's preparation has better stability, has increased its applicable scope.
The organic silicon emulsion of the present invention's preparation is characterized in that comprising following several component:
1, active substance:
Active substance of the present invention is organopolysiloxane, the reaction product of hydrophobic particles under catalyst action.
(1) general structure of described organopolysiloxane is as follows:
R
aSiO
(4-a)/2
Wherein R is the monovalence alkyl of replacement or non-replacement, carbonatoms is 1～20, these groups comprise alkyl (as methyl, ethyl, propyl group, sec.-propyl, butyl, isobutyl-), aryl (phenyl, tolyl, phenmethyl) and alkylene (comprising vinyl, propenyl), hydrogen atom in these groups can part be replaced by halogen atom, for example 3,3, the 3-trifluoro propyl, the value of a is 1.9～2.2.
The organopolysiloxane that satisfies above condition is a lot, preferred polydimethylsiloxane, poly-di-ethyl siloxane, poly-methyl trifluoro propyl siloxanes, poly-ethylene methacrylic radical siloxane among the present invention.The viscosity of described organopolysiloxane is 10～100, and 000mPas is preferably 100～10, and 000mPas, consumption are 80～98% of active substance total mass, preferred 90～95%.
(2) described hydrophobic particles comprises silicon-dioxide, magnesium oxide, zinc oxide, aluminium sesquioxide.What the present invention selected is water drain silica, and specific surface area is 50m at least
2/ g, preferred 150～250m
2/ g.Consumption accounts for 1～18% of active substance, and preferred 3～8%.
(3) described catalyzer is to make to react between polysiloxane and the silicon-dioxide, to improve the hydrophobicity of water drain silica.Catalyzer commonly used comprises LiOH, CsOH, NaOH, KOH, Me
4NOH, H
2SO
4, H
3PO
4, the preferred NaOH of the present invention.Catalyst consumption is 0.5～3% of an active substance, preferred 1～2%.
The preparation technology of described active substance is as follows: will mix under organopolysiloxane and the hydrophobic particles room temperature earlier, to keep abundant contact.Be warming up to 50～300 ℃ then, preferred 100～200 ℃, add catalyst reaction 2～8h, preferred 4～6h.Reaction finishes and is cooled to room temperature and promptly gets active substance.In whole organic silicon emulsion is 100 mass parts, and the consumption of actives is 10-30 part.
2, high fatty alcohol polyethers
The used high fatty alcohol polyethers of the present invention is to be initiator with the high fatty alcohol, under the effect of catalyzer and the polymkeric substance that obtains of oxyethane (EO), propylene oxide (PO) polymerization reaction take place, its preparation method can be inquired about on the professional technique data and learn, the general formula of the high fatty alcohol polyethers of formation is as follows:
R
1O(EO)
m(PO)
nH
In the formula, R
1For carbonatoms is 12～24 straight or branched alkyl, comprise dodecyl, tetradecyl, hexadecyl, octadecyl and docosyl.R
1Preferred carbonatoms is 16～20 straight chained alkyl.M, n are the polymerization degree in the formula, and m is 5～50 integer, and be preferred 10～25, and n is 10～80 integer, preferred 20～50.
In whole organic silicon emulsion is 100 mass parts, and the consumption of high fatty alcohol polyethers is 1-3 part.
3, emulsifying agent
Emulsifying agent among the present invention, it comprises nonionogenic tenside, anion surfactant, cats product and amphoterics.
The example of nonionogenic tenside is a polyoxyethylene nonylphenol ether, polyoxyethylene octylphenol ether, the lauric acid Soxylat A 25-7, oleic acid polyoxyethylene, sorbitan monostearate, sorbitan monooleate, the anhydrous sorbitol tristearate, Witconol AL 69-66, anhydrous sorbitol Stearinsaeure polyoxyethylene ether-ester, anhydrous sorbitol list oleic acid polyoxyethylene ester, anhydrous sorbitol three stearic acid polyoxyethylene ether esters, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene and the like.
Examples of anionic surfactants is the tensio-active agent of polyoxyethylene nonylphenol ether vitriol, polyoxyethylene octylphenol ether vitriol, alkylphosphonic and the like.
The example of cats product is the tensio-active agent of salt of alkyl benzyl ammonium salt, lauric acid imidazoline, oleoyl tetrahydroglyoxaline, hexadecylamine and the like.
The example of amphoterics is the amphoterics of the own lactones type of alkyltrimethylammonium, phosphoric acid ester type.
Preferred nonionic surfactants, the nonionogenic tenside of use are one or more mixture, preferred multiple mixture.
In whole organic silicon emulsion is 100 mass parts, and the consumption of emulsifying agent is 0.5-5 part.
4, polyether-modified polysiloxane
Polyether-modified polysiloxane is commonly called as the silicon polyethers, is by hydrogen containing siloxane and unsaturated polyether addition reaction to take place under the effect of catalyzer to prepare.The kinetic viscosity of described silicon polyethers in the time of 25 ℃ is 10～30, and 000mPas is preferably at 25 ℃ and descends 60～5,000mPas.The structural formula of silicon polyethers is as follows:
Wherein, letter r
2Be methyl, ethyl, propyl group, butyl or phenyl: R
3Be hydrogen atom, methyl, ethyl, propyl group or butyl; Subscript r, s are the polymerization degree of silicon chain link, and s is 1～50 integer, and r is 1～200 integer; Subscript e and f are respectively the polymerization degree of oxyethane (EO) and propylene oxide (PO), and e and f are 1～50 integer; Subscript t is-CH
2The polymerization degree, be 1～6 integer.
In whole organic silicon emulsion is 100 mass parts, and the consumption of silicon polyethers is 5-15 part.
5, water
In whole organic silicon emulsion is 100 mass parts, and the consumption of water is 50-80 part.
According to requirement to emulsion viscosity, can add thickening material, thickening material comprises polyacrylamide, carbomer, xanthan gum, polyacrylic ester, cellulose ethers, the dosage of thickening material is adjusted according to the viscosity of emulsion.Need add sterilant and sanitas during standing storage, as clorox, potassium sorbate, s-triazine, triumphant pine etc.
The method for preparing emulsion has " agent-in-water method ", " agent-in-oil method ", " nascent soap method " or the like, and the present invention selects the water-dispersion emulsion of " agent-in-oil method " preparation high-viscosity organosilicon composition for use, and concrete grammar is as follows:
Under the room temperature, with active substance, high fatty alcohol polyethers, emulsifying agent, silicon polyethers thorough mixing 10～50min under agitation, preferred 15min～30min; Temperature with above-mentioned system is increased to 55 ℃～85 ℃ maintenance system temperatures then, add entry lentamente, improve stirring velocity and make it become emulsion oil-in-water, continue to add water to needed mass concentration by water-in-oil emulsion, be generally 40%～70%, be preferably 50%～65%; Thick emulsion is by the further emulsification of colloidal mill; Be diluted to needed emulsion concentration with viscous water at last.
Embodiment:
The preparation of active substance:
Adopt reaction raw materials and condition in the following table,, make active substance A, B, C and D according to the preparation method of above-mentioned active substance.
Table 1
The preparation of silicon polyethers:
Preparation silicon polyethers E
1, E
2, E
3And E
4, its structural formula is:
R wherein
2, R
3, r, s, e, f, t value see Table 2.
Table 2
| The silicon polyethers | E 1 | E 2 | E 3 | E 4 |
| R 2 | -CH 3 | -C 2H 5 | -CH 3 | -C 3H 7 |
| R 3 | -H | -CH 3 | -C 2H 5 | -CH 3 |
| r | 2 | 152 | 84 | 195 |
| s | 3 | 45 | 26 | 38 |
| e | 48 | 22 | 2 | 15 |
| f | 30 | 24 | 46 | 3 |
| t | 3 | 4 | 1 | 6 |
The preparation of high fatty alcohol polyethers:
Preparation high fatty alcohol polyethers F
1, F
2, F
3And F
4, its general structure is R
1O (EO)
m(PO)
nH, R
1, m and n value see Table 3.
Table 3
| The high fatty alcohol polyethers | F 1 | F 2 | F 3 | F 4 |
| R 1 | Dodecyl | N-hexadecyl | The n-docosane base | N-hexadecyl |
| m | 5 | 15 | 50 | 20 |
| n | 35 | 10 | 80 | 40 |
The preparation of emulsion:
Embodiment 1:
The emulsion moiety is:
Active substance A 5%
Active substance B 15%
Silicon polyethers E
13%
Silicon polyethers E
23%
Octyl phenol polyoxy ethene (9) ether 0.5%
High fatty alcohol polyethers F
11.5%
Acrylic thickener 1%
Potassium sorbate 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, high fatty alcohol polyethers, silicon polyethers thorough mixing 35min under agitation, temperature with above-mentioned system after finishing is increased to 60 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 28% emulsion H
1
Embodiment 2:
The emulsion moiety is:
Active substance C 10%
Active substance D 15%
Silicon polyethers E
14%
Silicon polyethers E
32.5%
Sorbitan monooleate 1.0%
High fatty alcohol polyethers F
22.5%
Acrylic thickener 2%
Triumphant loose 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, high fatty alcohol polyethers, silicon polyethers thorough mixing 40min under agitation, temperature with above-mentioned system after finishing is increased to 80 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 60%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 35% emulsion H
2
Embodiment 3:
The emulsion moiety is:
Active substance B 15%
Active substance C 6%
Silicon polyethers E
23%
Silicon polyethers E
43%
Witconol AL 69-66 1%
High fatty alcohol polyethers F
32%
Acrylic thickener 1.5%
Potassium sorbate 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, high fatty alcohol polyethers, silicon polyethers thorough mixing 25min under agitation, temperature with above-mentioned system after finishing is increased to 70 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 55%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 30% emulsion H
3
Embodiment 4:
The emulsion moiety is:
Active substance A 10%
Active substance D 4%
Silicon polyethers E
33%
Silicon polyethers E
42.5%
Alkylphenol-polyethenoxy (3) ether 0.5%
High fatty alcohol polyethers F
41%
Acrylic thickener 2.5%
Potassium sorbate 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, high fatty alcohol polyethers, silicon polyethers thorough mixing 30min under agitation, temperature with above-mentioned system after finishing is increased to 75 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 21% emulsion H4.
Comparative Examples 1:
The emulsion moiety is:
Active substance B 10%
Active substance A 5%
Silicon polyethers E
16%
Silicon polyethers E
24%
Octyl phenol polyoxy ethene (9) ether 3%
Acrylic thickener 1%
Potassium sorbate 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, emulsifying agent, silicon polyethers thorough mixing 35min under agitation, temperature with above-mentioned system after finishing is increased to 65 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 28% emulsion T
1
Comparative Examples 2:
The emulsion moiety is:
Active substance D 9%
Active substance C 8%
Silicon polyethers E
17%
Silicon polyethers E
36%
Sorbitan monooleate 5%
Acrylic thickener 2%
Potassium sorbate 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, emulsifying agent, silicon polyethers thorough mixing 40min under agitation, temperature with above-mentioned system after finishing is increased to 75 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 60%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 35% emulsion T
2
Comparative Examples 3:
The emulsion moiety is:
Active substance B 10%
Active substance C 5%
Silicon polyethers E
25%
Silicon polyethers E
46%
Witconol AL 69-66 4%
Acrylic thickener 1.5%
Triumphant loose 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, emulsifying agent, silicon polyethers thorough mixing 25min under agitation, temperature with above-mentioned system after finishing is increased to 70 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 55%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 30% emulsion T
3
Comparative Examples 4:
The emulsion moiety is:
Active substance A 7%
Active substance D 4%
Silicon polyethers E
33.5%
Silicon polyethers E
44%
Alkylphenol-polyethenoxy (3) ether 2.5%
Acrylic thickener 2.5%
Potassium sorbate 0.1%
Water surplus
Amount to 100%
Under the room temperature, with active substance, emulsifying agent, silicon polyethers thorough mixing 30min under agitation, temperature with above-mentioned system after finishing is increased to 75 ℃, then, keeps system temperature, add entry lentamente, improving stirring velocity and make it become the emulsion oil-in-water phase inversion by water-in-oil emulsion, continue to add water to needed mass concentration, is 50%, thick emulsion is by the further emulsification of colloidal mill, and being diluted to solid content with the vinylformic acid viscous water at last is 21% emulsion T
4
According to the prescription in the foregoing description and the Comparative Examples, can draw each components contents, see the following form:
Each components contents in table 4 emulsion
From the result of table 4 as can be seen, added the high fatty alcohol polyethers, the ratio between (silicon polyethers+emulsifying agent+high fatty alcohol polyethers)/active substance has all diminished, and this explanation emulsifying power has improved.
Testing method:
The performance of the high-viscosity organosilicon composition emulsion of the inventive method preparation is mainly assessed from the following aspects:
(1) dilution stability of emulsion:
Organic silicon emulsion according to 1% joins in 99% the water, after being uniformly dispersed, observes the liquid level situation of water diluent.
(2) the floating oil temperature of emulsion:
Organic silicon emulsion according to 1% joins in 99% the water, the liquid level situation that water diluent is observed in the back of heating up.
(3) anti-shear performance of emulsion:
Under the normal temperature, emulsion stoste is placed on the hunting of frequency 30min of 100 times/min on the horizontal oscillator tube, according to the method for (1), comparative emulsion liquid level situation.
The performance test contrast of table 5 emulsion
Consolidated statement 4 and table 5 are introduced the stability that the high fatty alcohol polyethers can improve organic silicon emulsion to a great extent; Add the high fatty alcohol polyethers, can also improve the shared proportion of actives, thereby reduce the use of silicon polyethers and emulsifying agent.
Claims (3)
1. organic silicon emulsion is characterized in that moiety is:
(1) active substance of 10-30 part: prepare under catalyst action by organopolysiloxane, hydrophobic particles, that is: organopolysiloxane, hydrophobic particles are at room temperature mixed; Be warmed up to 50～300 ℃, add catalyst reaction 2～8h; Be cooled to room temperature and promptly get active substance;
Wherein:
Described organopolysiloxane is selected from polydimethylsiloxane, poly-di-ethyl siloxane, poly-methyl trifluoro propyl siloxanes, poly-ethylene methacrylic radical siloxane, its kinetic viscosity in the time of 25 ℃ is 10～100,000mPas, its consumption accounts for 80～98% of active substance quality;
Described hydrophobic particles is specific surface area 50m at least
2The silicon-dioxide of/g, its consumption accounts for 1～18% of active substance quality;
Described catalyzer is NaOH, and its consumption accounts for 0.5～3% of active substance quality;
(2) the high fatty alcohol polyethers of 1-3 part: its general formula is R
1O (EO)
m(PO)
nH, R in the formula
1It for carbonatoms the alkyl of 12～24 straight or branched; Subscript m, n are the polymerization degree, and m is 5～50 integer, and n is 10～80 integer;
(3) emulsifying agent of 0.5-5 part: be nonionogenic tenside, be selected from the mixture of following a kind of material or multiple material, comprise: polyoxyethylene nonylphenol ether, polyoxyethylene octylphenol ether, the lauric acid Soxylat A 25-7, oleic acid polyoxyethylene, sorbitan monostearate, sorbitan monooleate, the anhydrous sorbitol tristearate, Witconol AL 69-66, anhydrous sorbitol Stearinsaeure polyoxyethylene ether-ester, anhydrous sorbitol list oleic acid polyoxyethylene ester, anhydrous sorbitol three stearic acid polyoxyethylene ether esters, castor oil polyoxyethylene ether or alkylphenol polyoxyethylene;
(4) the polyether-modified polysiloxane of 5-15 part: its kinetic viscosity in the time of 25 ℃ is 10～30,000mPas, and its structural formula is:
Wherein, letter r
2Be methyl, ethyl, propyl group, butyl or phenyl; R
3Be hydrogen atom, methyl, ethyl, propyl group or butyl; Subscript s is 1～50 integer, and r is 1～200 integer; Subscript e and f are 1～50 integer; Subscript t is 1～6 integer;
(5) water of 50-80 part;
Each above-mentioned constituent mass sum is 100 parts.
2. the described a kind of organic silicon emulsion of claim 1 is characterized in that (2) described high fatty alcohol polyethers, the R in its general formula
1It for carbonatoms 16～20 alkyl; Subscript m is 10～25 integer, and n is 20～50 integer.
3. prepare the described a kind of organic silicon emulsion of claim 1, its characterization step is:
A, with active substance, high fatty alcohol polyethers, emulsifying agent, polyether-modified polysiloxane thorough mixing 10～50min under agitation;
B, the temperature of above-mentioned system is increased to 55 ℃～85 ℃;
C, maintenance system temperature add entry lentamente, improve stirring velocity and make it become emulsion oil-in-water by water-in-oil emulsion;
D, with thick emulsion by the further emulsification of colloidal mill, be diluted to needed emulsion concentration with viscous water at last.
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| CN115028840A (en) * | 2022-04-12 | 2022-09-09 | 浙江新安化工集团股份有限公司 | Polysiloxane emulsion and preparation method and application thereof |
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