CN101935327A - Preparation method of disiloxane - Google Patents
Preparation method of disiloxane Download PDFInfo
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- CN101935327A CN101935327A CN 201010239025 CN201010239025A CN101935327A CN 101935327 A CN101935327 A CN 101935327A CN 201010239025 CN201010239025 CN 201010239025 CN 201010239025 A CN201010239025 A CN 201010239025A CN 101935327 A CN101935327 A CN 101935327A
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- Prior art keywords
- oxide
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- chlorosilane
- hydrogen
- organic
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 title abstract 5
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000005046 Chlorosilane Substances 0.000 claims abstract description 12
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007791 liquid phase Substances 0.000 claims abstract description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 239000006194 liquid suspension Substances 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- -1 sec.-propyl Chemical group 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 150000004706 metal oxides Chemical class 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 125000004218 chloromethyl group Chemical group [H]C([H])(Cl)* 0.000 claims description 4
- 125000001995 cyclobutyl group Chemical group [H]C1([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 claims description 4
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 4
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 claims description 4
- 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 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000001624 naphthyl group Chemical group 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 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 claims description 4
- 125000000725 trifluoropropyl group Chemical group [H]C([H])(*)C([H])([H])C(F)(F)F 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 229960004643 cupric oxide Drugs 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 230000008030 elimination Effects 0.000 description 4
- 238000003379 elimination reaction Methods 0.000 description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 239000005051 trimethylchlorosilane Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- DCSOPUDOZMRWRP-UHFFFAOYSA-N Cc1cc(C)cc([SiH2]Cl)c1 Chemical compound Cc1cc(C)cc([SiH2]Cl)c1 DCSOPUDOZMRWRP-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- XSDCTSITJJJDPY-UHFFFAOYSA-N chloro-ethenyl-dimethylsilane Chemical compound C[Si](C)(Cl)C=C XSDCTSITJJJDPY-UHFFFAOYSA-N 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003751 zinc Chemical class 0.000 description 2
- WBODDOZXDKQEFS-UHFFFAOYSA-N 1,2,3,4-tetramethyl-5-phenylbenzene Chemical compound CC1=C(C)C(C)=CC(C=2C=CC=CC=2)=C1C WBODDOZXDKQEFS-UHFFFAOYSA-N 0.000 description 1
- AYSQVETWZJWRRH-UHFFFAOYSA-N C1CCC(C1)[Si](CN)(C2=CC=CC=C2)Cl Chemical compound C1CCC(C1)[Si](CN)(C2=CC=CC=C2)Cl AYSQVETWZJWRRH-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- KBAZUXSLKGQRJF-UHFFFAOYSA-N chloro-dimethyl-(3,3,3-trifluoropropyl)silane Chemical compound C[Si](C)(Cl)CCC(F)(F)F KBAZUXSLKGQRJF-UHFFFAOYSA-N 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Silicon Polymers (AREA)
Abstract
The invention relates to a preparation method of disiloxane, aiming to solve the technical problems of waste acid water generation, gas generation and unsafe and difficult control in a production process. The preparation method comprises the following steps of: dropwise adding the metered chlorosilane to a three-mouth bottle filled with a metallic oxide and an organic liquid suspension by stirring for reaction at 0-50 DEG C; after finishing the dropwise addition, continuously reacting until the pH value of a reaction system is 6-7; centrifugally filtering to obtain liquid-phase matter, wherein when the organic liquid in the bottle is the disiloxane as a target product, the obtained liquid-phase matter is the disiloxane, and when the organic liquid in the bottle is an organic solvent, the organic solvent is removed from the obtained liquid-phase matter so that the disiloxane is obtained.
Description
Technical field
The present invention relates to chemical technology field, specifically be a kind of be raw material with chlorosilane and metal oxide, through dechlorination reaction, directly prepare the method for sily oxide.
Background technology
Sily oxide is mainly used in the production of organic chemical industry and medication chemistry, mostly as closure agent, clean-out system, releasing agent etc.The at present main producing hydrolysis process that adopts of sily oxide is about to the trialkylchlorosilane reaction that is hydrolyzed, production sily oxide and dilute hydrochloric acid under acidic conditions.This method production efficiency is low, the yield of product is low, of poor quality, and the acid concentration that produces in the while production process is lower and contain a small amount of organic waste water, so product separation is relatively more difficult, environmental pollution is also relatively more serious, thereby has limited further developing of producing.
In CN 101362777A, wish that it is solid-phase reactant that people such as Ji Cai adopts with carbonate, with the trimethylchlorosilane liquid phase reaction thing, with the hexamethyldisiloxane reaction solvent, by the synthetic hexamethyldisiloxane of liquid-solid reaction.In this method, there is gas to emit in the reaction, increased the difficulty of reaction control and the danger of reaction process.
Summary of the invention
The technical issues that need to address of the present invention are to provide a kind of preparation method of easy sily oxide, the generation of no waste acid water in the production process, also gasless generation, easily control safely.
The preparation method of sily oxide of the present invention is characterized in that may further comprise the steps: the chlorosilane of metering is under agitation dropped in the there-necked flask that metal oxide and organic liquid suspension liquid are housed, be reflected under 0～50 ℃ (being preferably 15～25 ℃) and carry out; Dropwise, continue to react to the pH value of reaction system be 6～7; Centrifuging obtains the liquid phase thing; When the organic liquid in the bottle was the target product sily oxide, the liquid phase thing that obtains was a sily oxide, and when the organic liquid in the bottle was organic solvent, the liquid phase thing that obtains removed organic solvent, obtains sily oxide; Described sily oxide has following structural formula:
R1, R2, R3 are methyl, ethyl, phenyl, vinyl, hydrogen, chloromethyl, sec.-propyl, propyl group, normal-butyl, the tertiary butyl, amyl group, cyclopentyl, hexyl, dodecyl, octadecyl, cyclobutyl, cyclohexyl, methylcyclohexyl, suberyl, phenmethyl, styroyl, xenyl, naphthyl or trifluoro propyl, and when among R1, R2, the R3 one when being hydrogen, all the other two can not be hydrogen;
Described chlorosilane general formula is R1R2R3SiCl, R1, R2, R3 are methyl, ethyl, phenyl, vinyl, hydrogen, chloromethyl, sec.-propyl, propyl group, normal-butyl, the tertiary butyl, amyl group, cyclopentyl, hexyl, dodecyl, octadecyl, cyclobutyl, cyclohexyl, methylcyclohexyl, suberyl, phenmethyl, styroyl, xenyl, naphthyl, trifluoro propyl in the formula, and when among R1, R2, the R3 one when being hydrogen, all the other two can not be hydrogen;
Described metal oxide is selected from zinc oxide, barium oxide, magnesium oxide, calcium oxide or cupric oxide (being preferably zinc oxide), and the mol ratio of metal oxide and chlorosilane is 0.5～1.0: 1(is preferably 0.6: 1);
Described organic liquid is an organic solvent: a kind of in ethyl acetate, methyl acetate, toluene, benzene, dimethylbenzene, gasoline, solvent oil, ether, sherwood oil, normal hexane, hexanaphthene or the ethylene dichloride, the target product sily oxide of organic liquid or liquid state; The mass ratio of chlorosilane and organic liquid be 1: 0.5～5(be preferably 1: 1～2).When using as organic liquid, there is not other organic impurity in the liquid reactants, the product purity height with the target product sily oxide.
Preparation method of the present invention compares with the sily oxide producing hydrolysis process, has avoided the generation of waste water, have simple to operate, product yield is high.With adopting carbonate is that solid formation is compared, and the present invention adopts metal oxide, makes no gas generation in the reaction process, reacts more steady, and production security is better.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1.In the 500ml there-necked flask of stirring, thermometer and dropping funnel is housed, add 39.1g(0.48mol) zinc oxide, the 52.0g hexamethyldisiloxane stirs into suspension liquid, splashes into 103.7g(0.96mol gradually) trimethylchlorosilane.Be reflected at 20 ℃ and carry out, after dropwising, continue to react to the pH value of reaction system be 7.With the centrifugal elimination of insoluble zinc salt, obtain hexamethyldisiloxane 125.9g.Productive rate is that the 95.0%(of theoretical value is by the trimethylchlorosilane amount).
Embodiment 2.In the 500ml there-necked flask of stirring, thermometer and dropping funnel is housed, add 16.0(0.40mol) magnesium oxide, 136.0g toluene stirs into suspension liquid, splashes into 68.0g(0.40mol gradually) the 3,5-dimethylphenyl chlorosilane.Be reflected at 50 ℃ and carry out, after dropwising, continue to react to the pH value of reaction system be 7.With the centrifugal elimination of insoluble magnesium salts.The steaming of toluene in the liquid phase is removed, obtain tetramethyl-phenylbenzene sily oxide 52.6g.Productive rate is that the 92.0%(of theoretical value is by 3,5-dimethylphenyl chlorosilane amount).
Embodiment 3.In the 500ml there-necked flask of stirring, thermometer and dropping funnel is housed, add 16.8g(0.3mol) calcium oxide, the 300g ether stirs into suspension liquid, splashes into 60.0g(0.5mol gradually) the dimethyl vinyl chlorosilane.Be reflected at 5 ℃ and carry out, after dropwising, continue to react to the pH value of reaction system be 6.With the centrifugal elimination of insoluble calcium salt.Ether in the liquid phase obtains tetramethyl divinyl disiloxane 43.7g after steaming and removing.Productive rate is that the 94.0%(of theoretical value is by dimethyl vinyl chlorosilane amount).
Embodiment 4.In the 500ml there-necked flask of stirring, thermometer and dropping funnel is housed, add 48.6g(0.6mol) zinc oxide, 282g tetramethyl-dihydro sily oxide stirs into suspension liquid, splashes into 94.0g(1.0mol gradually) dimethyl silicane hydroxide.Be reflected at 15 ℃ and carry out, after dropwising, continue to react to system pH be 7.With the centrifugal elimination of insoluble zinc salt, obtain 345.2g tetramethyl-dihydro sily oxide.Productive rate is that the 94.3%(of theoretical value is by the dimethyl silicane hydroxide amount).
Embodiment 5.Other uses 73.4g(0.48mol instead with embodiment 1) barium oxide, productive rate is 92.0%.
Embodiment 6.Other uses 0.4mol dimethyl trifluoro propyl chlorosilane instead with embodiment 2, and productive rate is 95.4%.
Embodiment 7.Other uses 0.5mol aminomethyl phenyl cyclopentyl chlorosilane instead with embodiment 3, and productive rate is 93.5%.
Claims (2)
1. the preparation method of a sily oxide is characterized in that may further comprise the steps: the chlorosilane of metering is under agitation dropped in the there-necked flask that metal oxide and organic liquid suspension liquid are housed, be reflected under 0～50 ℃ and carry out; Dropwise, continue to react to the pH value of reaction system be 6～7; Centrifuging obtains the liquid phase thing; When the organic liquid in the bottle was the target product sily oxide, the liquid phase thing that obtains was a sily oxide, and when the organic liquid in the bottle was organic solvent, the liquid phase thing that obtains removed organic solvent, obtains sily oxide; Described sily oxide has following structural formula:
R1, R2, R3 are methyl, ethyl, phenyl, vinyl, hydrogen, chloromethyl, sec.-propyl, propyl group, normal-butyl, the tertiary butyl, amyl group, cyclopentyl, hexyl, dodecyl, octadecyl, cyclobutyl, cyclohexyl, methylcyclohexyl, suberyl, phenmethyl, styroyl, xenyl, naphthyl or trifluoro propyl, and when among R1, R2, the R3 one when being hydrogen, all the other two can not be hydrogen;
Described chlorosilane general formula is R1R2R3SiCl, R1, R2, R3 are methyl, ethyl, phenyl, vinyl, hydrogen, chloromethyl, sec.-propyl, propyl group, normal-butyl, the tertiary butyl, amyl group, cyclopentyl, hexyl, dodecyl, octadecyl, cyclobutyl, cyclohexyl, methylcyclohexyl, suberyl, phenmethyl, styroyl, xenyl, naphthyl, trifluoro propyl in the formula, and when among R1, R2, the R3 one when being hydrogen, all the other two can not be hydrogen;
Described metal oxide is selected from zinc oxide, barium oxide, magnesium oxide, calcium oxide or cupric oxide, and the mol ratio of metal oxide and chlorosilane is 0.5～1.0: 1;
Described organic liquid is an organic solvent: a kind of in ethyl acetate, methyl acetate, toluene, benzene, dimethylbenzene, gasoline, solvent oil, ether, sherwood oil, normal hexane, hexanaphthene or the ethylene dichloride, the target product sily oxide of organic liquid or liquid state; The mass ratio of chlorosilane and organic liquid is 1: 0.5～5.
2. the preparation method of sily oxide according to claim 1 is characterized in that temperature of reaction is 15～25 ℃; The mol ratio of metal oxide and chlorosilane is 0.6: 1; The mass ratio of chlorosilane and organic liquid is 1: 1～2.
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| CN201010239025A CN101935327B (en) | 2010-07-28 | 2010-07-28 | Preparation method of disiloxane |
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| CN201010239025A CN101935327B (en) | 2010-07-28 | 2010-07-28 | Preparation method of disiloxane |
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| CN101935327B CN101935327B (en) | 2012-10-24 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731559A (en) * | 2012-06-11 | 2012-10-17 | 西南科技大学 | Alkyl-substituted disiloxane and preparation method thereof |
| CN109439290A (en) * | 2018-12-05 | 2019-03-08 | 山东恒利热载体工程技术有限公司 | A kind of environmental protection organic heat carrier and preparation method thereof |
| CN109776593A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The preparation method of four ethylene disiloxane of 1,3- dimethyl -1,1,3,3- |
| CN115521331A (en) * | 2022-10-14 | 2022-12-27 | 唐山三友化工股份有限公司 | Continuous efficient hydrolysis method and device for dimethylchlorosilane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4578494A (en) * | 1985-06-14 | 1986-03-25 | Dow Corning Corporation | Preparation of polysiloxanes from halosilanes |
| JPH11322935A (en) * | 1998-05-12 | 1999-11-26 | Nippon Unicar Co Ltd | Manufacture of organosiloxane from monohalosilane |
| CN101362777A (en) * | 2008-09-25 | 2009-02-11 | 江苏宏达新材料股份有限公司 | Preparation method of hexamethyl disiloxane |
-
2010
- 2010-07-28 CN CN201010239025A patent/CN101935327B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4578494A (en) * | 1985-06-14 | 1986-03-25 | Dow Corning Corporation | Preparation of polysiloxanes from halosilanes |
| JPH11322935A (en) * | 1998-05-12 | 1999-11-26 | Nippon Unicar Co Ltd | Manufacture of organosiloxane from monohalosilane |
| CN101362777A (en) * | 2008-09-25 | 2009-02-11 | 江苏宏达新材料股份有限公司 | Preparation method of hexamethyl disiloxane |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731559A (en) * | 2012-06-11 | 2012-10-17 | 西南科技大学 | Alkyl-substituted disiloxane and preparation method thereof |
| CN109776593A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The preparation method of four ethylene disiloxane of 1,3- dimethyl -1,1,3,3- |
| CN109776593B (en) * | 2017-11-14 | 2023-05-09 | 河北圣泰材料股份有限公司 | Preparation method of 1, 3-dimethyl-1, 3-tetraethylenedisiloxane |
| CN109439290A (en) * | 2018-12-05 | 2019-03-08 | 山东恒利热载体工程技术有限公司 | A kind of environmental protection organic heat carrier and preparation method thereof |
| CN109439290B (en) * | 2018-12-05 | 2021-03-16 | 山东恒利热载体工程技术有限公司 | Environment-friendly organic heat carrier and preparation method thereof |
| CN115521331A (en) * | 2022-10-14 | 2022-12-27 | 唐山三友化工股份有限公司 | Continuous efficient hydrolysis method and device for dimethylchlorosilane |
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