SU203683A1 - METHOD OF OBTAINING ORGANO-HYDRIDHLOROSILANE - Google Patents
METHOD OF OBTAINING ORGANO-HYDRIDHLOROSILANEInfo
- Publication number
- SU203683A1 SU203683A1 SU1106994A SU1106994A SU203683A1 SU 203683 A1 SU203683 A1 SU 203683A1 SU 1106994 A SU1106994 A SU 1106994A SU 1106994 A SU1106994 A SU 1106994A SU 203683 A1 SU203683 A1 SU 203683A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- hydridhlorosilane
- organohydride
- mol
- organo
- obtaining
- Prior art date
Links
- -1 chlorine tin Chemical compound 0.000 claims description 3
- KOPOQZFJUQMUML-UHFFFAOYSA-N Chlorosilane Chemical class Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 2
- 239000005046 Chlorosilane Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 150000004756 silanes Chemical class 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K Aluminium chloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 229910006647 SnH Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- SOYVLBDERBHIME-UHFFFAOYSA-N chloro(diethyl)silicon Chemical compound CC[Si](Cl)CC SOYVLBDERBHIME-UHFFFAOYSA-N 0.000 description 1
- GTPDFCLBTFKHNH-UHFFFAOYSA-N chloro(phenyl)silicon Chemical compound Cl[Si]C1=CC=CC=C1 GTPDFCLBTFKHNH-UHFFFAOYSA-N 0.000 description 1
- BYLOHCRAPOSXLY-UHFFFAOYSA-N dichloro(diethyl)silane Chemical compound CC[Si](Cl)(Cl)CC BYLOHCRAPOSXLY-UHFFFAOYSA-N 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- KXCAEQNNTZANTK-UHFFFAOYSA-N stannane Chemical compound [SnH4] KXCAEQNNTZANTK-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
- 229910000083 tin tetrahydride Inorganic materials 0.000 description 1
Description
Известен способ получени органогидридхлорсиланов реакцией диспропорционировани в присутствии хлористого алюмини в качестве катализатора.A known method for producing organohydridechlorosilanes by disproportionation reaction in the presence of aluminum chloride as a catalyst.
С целью расширени сырьевой базы и проведени направленного синтеза, предложено органогидридхлорсиланы получать взаимодействием органогидридсиланов с хлорным оловом , желательно при температуре 30-80°С в среде серного эфира.In order to expand the raw material base and carry out directional synthesis, it has been proposed to obtain organohydride chlorosilanes by the interaction of organohydride silanes with chlorine tin, preferably at a temperature of 30-80 ° C in a medium of sulfur ether.
Пример 1. В четырехгорлую колбу, снабженную мешалкой, термометром, капельной воронкой, соединенную с ловушкой, охлаждаемой жидким азотом, загружают 10,8 г (ОД моль) CcnsSiHs, растворенного в 50 мл абсолютного серного эфира, и прибавл ют 26,5 г (0,1 моль) SnClj. В ловушке собирают SnH.i. Наблюдаетс выделение На. После внесени всего хлорного олова реакционную смесь перемешивают 40-60 мин при комнатной температуре. Разгонкой выдел ют 11 г (выход 83%) фенилхлорсилана C(iH5SiH2Cl с т. кип. 161 -162°С.Example 1. A four-necked flask equipped with a stirrer, a thermometer, an addition funnel connected to a liquid nitrogen-cooled trap was charged with 10.8 g (OD mol) of CcnsSiHs dissolved in 50 ml of absolute sulfuric ether and 26.5 g added ( 0.1 mol) SnClj. SnH.i is trapped. There is a selection of On. After all the chlorine tin has been added, the reaction mixture is stirred for 40-60 minutes at room temperature. Distillation gave 11 g (yield 83%) of phenylchlorosilane C (iH5SiH2Cl with bp 161-162 ° C.
Найдено, %: С1 25,0, 24,9.Found%: C1 25.0, 24.9.
Вычислено, %: С1 24,8.Calculated,%: C1 24.8.
(0,1 моль) (C2H5)SiH2, к которому по капл м прибавл ют 32 г (0,1 моль) . После прибавлени первых капель наблюдаетс разогревание , температуру реакционной зоны поддерживают не выше 80°С. Отмечаетс образование белого осадка SnCL, в ловушке собирают SnH4. Разгонкой выдел ют 9,2 г (выход 58,3%) диэтилхлорсилана и 1,9 г (выход 8%) диэтилдихлорсилана.(0.1 mol) (C2H5) SiH2 to which 32 g (0.1 mol) is added dropwise. After the addition of the first drops, heating is observed, the temperature of the reaction zone is maintained not higher than 80 ° C. The formation of a white precipitate of SnCL is noted, and SnH4 is collected in the trap. Distillation gave 9.2 g (yield: 58.3%) of diethylchlorosilane and 1.9 g (yield: 8%) of diethyldichlorosilane.
(C,H5)2SiHCl: т. кип. 100-101°С; DD 1,4118. Найдено, % : С1 28,5, 28,7. Вычислено, %: С1 28,7. (C.Hg)2SiCl.,: т. кин. 129-130°С. Найдено, %: С1 44,7, 45,0. Вычислено, %: С1 45,13.(C, H5) 2SiHCl: T. Kip. 100-101 ° C; DD 1.4118. Found,%: C1 28.5, 28.7. Calculated,%: C1 28.7. (C.Hg) 2SiCl.,: T. Kin. 129-130 ° C. Found,%: C1 44.7, 45.0. Calculated,%: C1 45.13.
Предмет изобретени Subject invention
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU203683A1 true SU203683A1 (en) |
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