SU303332A1 - Method for the production of polydimethylsiloxanes - Google Patents
Method for the production of polydimethylsiloxanesInfo
- Publication number
- SU303332A1 SU303332A1 SU1281252A SU1281252A SU303332A1 SU 303332 A1 SU303332 A1 SU 303332A1 SU 1281252 A SU1281252 A SU 1281252A SU 1281252 A SU1281252 A SU 1281252A SU 303332 A1 SU303332 A1 SU 303332A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- catalyst
- polydimethylsiloxanes
- weight
- tetramethylammonium
- production
- Prior art date
Links
- 235000013870 dimethyl polysiloxane Nutrition 0.000 title description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 title description 5
- -1 polydimethylsiloxanes Polymers 0.000 title description 5
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000003054 catalyst Substances 0.000 description 7
- 229920001971 elastomer Polymers 0.000 description 7
- 239000000806 elastomer Substances 0.000 description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N 2,2,4,4,6,6-hexamethyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- ANZPUCVQARFCDW-UHFFFAOYSA-N 2,2,4,4,6,6-hexamethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C[Si]1(C)O[SiH2]O[Si](C)(C)O[Si](C)(C)O1 ANZPUCVQARFCDW-UHFFFAOYSA-N 0.000 description 1
- GETQZCLCWQTVFV-UHFFFAOYSA-N Trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N Trimethylsilyl chloride Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 1
- DDJSWKLBKSLAAZ-UHFFFAOYSA-N cyclotetrasiloxane Chemical compound O1[SiH2]O[SiH2]O[SiH2]O[SiH2]1 DDJSWKLBKSLAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001264 neutralization Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
Description
Изобретение относитс к способу получени полидимети л сил океанов.This invention relates to a method for producing the polydimethic energy of the oceans.
Известен способ получени полидиметилсилоксанов полимеризацией органоциклосплоксанов в присутствии основного катализатора и 1-1,5 вес. % пол рных органических соединений , содержащих серу или азот, с последующей дезактивацией катализатора.A known method for producing polydimethylsiloxanes by the polymerization of organocyclosploxanes in the presence of a basic catalyst and 1-1.5 wt. % polar organic compounds containing sulfur or nitrogen, followed by catalyst deactivation.
С целью получени термостойких полидиметилсилоксановых эластомеров в качестве катализатора примен ют сс,со-тетраметиламмонийтетраметилдисилоксан или а-тетраметил-согидроксиполидиметилсилоксан и полученные эластомеры предпочтительно подвергают термообработке при 150-170°С или обработке триорганохлорсиланом.In order to obtain heat-resistant polydimethylsiloxane elastomers, cc, co-tetramethylammonium tetramethyldisiloxane or a-tetramethyl-cohydroxypolydimethylsiloxane are used as catalyst and the resulting elastomers are preferably heat treated at 150-170 ° C or treated with triorganochlorosilane.
Полимеризации подвергают октаметилциклотетрасилоксан , гексаметилциклотетрасн л океан , гексаметилциклотрисилоксан или их смесь.Polymerizations are subjected to octamethylcyclotetrasiloxane, ocean hexamethylcyclotetra, hexamethylcyclotrisiloxane, or their mixture.
В реакционную смесь органоциклосилоксанов может быть введен 1 мол. % гептаметнлвинилциклотетрасилоксана .In the reaction mixture of organocyclosiloxanes can be entered 1 mol. % heptamethylamine cyclotetrasiloxane.
Пример 1. В круглодо ную колбу помещают 10 г октаметил-, гексаметилциклотрисилоксана или их смеси, 0,01 вес. % а,оз-тетраметиламмонийтетраметилдисилоксана или атетраметиламмоний-й - гидроксиполидиметилсилоксана и 1-1,5 вес. % диметилформамида или димегилсульфоксида. Реакционную смесьExample 1. In a round-bottomed flask was placed 10 g of octamethyl-, hexamethylcyclotrisiloxane, or a mixture thereof, 0.01 weight. % a, oz-tetramethylammonium tetramethyldisiloxane or atetramethylammonium th - hydroxypolydimethylsiloxane and 1-1.5 weight. % dimethylformamide or dimethyl sulfoxide. Reaction mixture
нагревают 1-2 час при 50-80°С, затем температуру бани поднимают до 170°С, колбу присоедин ют к водоструйному насосу и прогревают эластомер с одновременной отгонкой1-2 hours at 50-80 ° C, then the bath temperature is raised to 170 ° C, the flask is connected to a water-jet pump and the elastomer is heated with simultaneous distillation
выдел ющегос триметиламина. При этой же температуре отгон ют и летучие продукты. Выход 92-94%, мол. вес. 500000-700000.trimethylamine. Volatile products are also distilled off at the same temperature. The output of 92-94%, mol. weight. 500,000-700,000.
Пример 2. В круглодонную колбу помещают 10 г октаметилциклотетрасилоксана, гексаметилциклотетрасилоксана или их смеси, 0,01 вес. % а,ш-тетраметиламмоннйтетраметилдисилоксана или а-тетраметиламмоний-ш-гидроксиполидиметплсилоксана и 1 -1,5% диметилформамида или диметилсульфоксида. Реакционную смесь нагревают 1-2 час при 50- 80°С. Полученный эластомер раствор ют в бензоле (10%-ный раствор), нейтрализуют триметилхлорсиланом, вз тым к катализатору в соотношении 1,5 : 1, и раствор обрабатывают пиридином дл св зывани НС1, затем промывают дистиллированной водой до нейтральной реакции. Полимер из раствора осаждают избытком метанола и высущивают в вакуум-сущилке до посто нного веса.Example 2. In a round bottom flask is placed 10 g of octamethylcyclotetrasiloxane, hexamethylcyclotetrasiloxane, or a mixture thereof, 0.01 weight. % a, w-tetramethylammonium tetramethyldisiloxane or a-tetramethylammonium-w-hydroxy polydimethylsiloxane and 1 -1.5% dimethylformamide or dimethyl sulfoxide. The reaction mixture is heated for 1-2 hours at 50-80 ° C. The resulting elastomer is dissolved in benzene (10% solution), neutralized with trimethylchlorosilane taken at a ratio of 1.5: 1 to the catalyst, and the solution is treated with pyridine to bind HC1, then washed with distilled water until neutral. The polymer from the solution is precipitated with excess methanol and dried in a vacuum flask to constant weight.
Выход 92%. Мол. вес. 500000-700000.Yield 92%. Mol weight. 500,000-700,000.
Предмет изобретени 5 вес. % пол рных органических соединений, содержаихих серу илп азот, с последующей дезактивацией катализатора, отличающийс тем, что, с целью получени термостойких полидиметилсилоксановых эластомеров, в качестве5 катализатора примен ют а,ы-тетраметиламмонийтетраметилдисилоксан или сс-тетраметило-гидроксиполидиметилсилоксан . 4 2. Способ но п. 1, отличающийс тем, что дезактивацию катализатора осуществл ют термообработкой эластомера при температуре 150-170°С. 3. Способ но п. 1, отличающийс тем, что дезактивацию катализатора осуществл ют обработкой эластомера триорганохлорсилапом.The subject of the invention 5 wt. % polar organic compounds containing sulfur or nitrogen, followed by catalyst deactivation, characterized in that, in order to obtain heat-resistant polydimethylsiloxane elastomers, a, s-tetramethylammonium tetramethyl disiloxane or cc-tetramethyl-hydroxypolydimethyloxychloroxyloxychloroxyloxychloroxyloxychloroxyloxychloroxyloxychloroxyloxychloroxychloroxydioxymethylsiloxane or cc-tetramethylhydroxypolydimethyloxychloroxychloroxyloxychloroxyloxychloroxyloxychloroxychloroxydioxychloride 4 2. Method of claim 1, characterized in that the deactivation of the catalyst is carried out by heat treatment of the elastomer at a temperature of 150-170 ° C. 3. A method according to claim 1, characterized in that the deactivation of the catalyst is carried out by treating the elastomer with triorganochlorosilap.
Publications (1)
Publication Number | Publication Date |
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SU303332A1 true SU303332A1 (en) |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4008261A (en) * | 1975-01-02 | 1977-02-15 | Dow Corning Corporation | Method of preparing phosphonium siloxanes and products thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4008261A (en) * | 1975-01-02 | 1977-02-15 | Dow Corning Corporation | Method of preparing phosphonium siloxanes and products thereof |
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