SU199396A1 - METHOD OF OBTAINING SILICON ORGANIC OLIGOMERS - Google Patents
METHOD OF OBTAINING SILICON ORGANIC OLIGOMERSInfo
- Publication number
- SU199396A1 SU199396A1 SU1032737A SU1032737A SU199396A1 SU 199396 A1 SU199396 A1 SU 199396A1 SU 1032737 A SU1032737 A SU 1032737A SU 1032737 A SU1032737 A SU 1032737A SU 199396 A1 SU199396 A1 SU 199396A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- silicon organic
- obtaining silicon
- organic oligomers
- oligomers
- aryl
- Prior art date
Links
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title 1
- 229910052710 silicon Inorganic materials 0.000 title 1
- 239000010703 silicon Substances 0.000 title 1
- -1 methylsiloxane Chemical class 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- KSMWLICLECSXMI-UHFFFAOYSA-N sodium;benzene Chemical compound [Na+].C1=CC=[C-]C=C1 KSMWLICLECSXMI-UHFFFAOYSA-N 0.000 description 2
- UDHSHGAIIVHYFW-UHFFFAOYSA-N C1(=CC=CC=C1)[SiH2]O[SiH](O[SiH2]C1=CC=CC=C1)C1=CC=CC=C1 Chemical compound C1(=CC=CC=C1)[SiH2]O[SiH](O[SiH2]C1=CC=CC=C1)C1=CC=CC=C1 UDHSHGAIIVHYFW-UHFFFAOYSA-N 0.000 description 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Известно получение кремнийорганических олигомеров путем взаимодействи а, ш-дихлорполиди метилсилокеана с алкил- или ариллитием при охлаждении. Дл получени олигомеров с высокой термои радиационной стойкостью и качестве исходных соединений берут и, со-дихлоралкиларилгилоксаны и ведут его взаимодействие с арилпроизводным щелочного металла - арилнатрием . Пример 1. К 14 г фенилнатри , предварительно полученного в трехгорлой колбе с мешалкой, капельной воронкой и термометром, медленно приливают 22,8 г (0,07 моль 1,3-дихлор- ,1,3 диметил-, 1,3-дифенилсилоксана при охлаждении. Реакцию ведут в токе сухого азота . От реакционной смеси отфильтровывают осадок, промывают его толуолом, фильтрат Промывают водой и после отгонки растворител остаток разгон ют в вакууме. При температуре 210-220 С (1 мм. рт. ст.) получают 27 г (91,6% от теоретического) продукта с показател ми 1,5816 (в переохлажденном состо нии); Si 13,8о/о, т. цл. 50°С (перекристаллизованный из спирто-ацетоновой .меси). Пример 2. По методу, описанному в примере 1,32,4 г (0,07 моль) 1,5 дихлор-,1,3,5триметил- , 1, 3, 5-трифенилтрисилоксана медленно приливают при охлаждении в колбу с 4 г (0,14 моль) фенилнатри , суспендированного в толуоле. Разгонкой продукта реакции в вакууме при температуре 250-265°С (1 мм рт. ст.) выдел ют фракцию в количестве 30 г (78,5%, от теоретического) со следуюш,ими пок ател ми. Найдено: п 1,5790; Vjo 167 ест; мол. вес. 529; С 72,77%; Н 6,4%,; Si 15,5о/о. Литературные данные дл трисилоксана: п 1,5785; V-2, 165 ест; мол. вес 546; С 72,6%; Н6,24о/о; Si 15,45%. Предмет изобретени Способ получени кремнийорганических олигомеров путем взаимодействи а, со-дихлорполиорганосилоксанов с арилнроизводным щелочного металла, отличающийс тем, что, с |,елью получени термостойких и радиационностойких кремнийорганических олигомеров, в качестве а, ы-дихлорполиорганосилоксанов используют а, со-дихлоралкиларилсилоксаны, а в качестве арилпроизводного щелочного металла используют арилнатрий.It is known to obtain organosilicon oligomers by reacting a, n-dichloropolyde methylsiloxane with alkyl- or aryllithium during cooling. In order to obtain oligomers with high thermal and radiation resistance and the quality of the starting compounds, they take and co-dichloroalkylarylgiloxanes and interact with the aryl alkali metal derivative - aryl sodium. Example 1. To 14 g of phenyl sodium, previously obtained in a three-necked flask with a stirrer, an addition funnel and a thermometer, slowly pour 22.8 g (0.07 mol of 1,3-dichloro, 1.3 dimethyl, 1,3-diphenylsiloxane with cooling. The reaction is carried out in a stream of dry nitrogen. The precipitate is filtered off from the reaction mixture, washed with toluene, the filtrate is washed with water and after the solvent is distilled off, the residue is distilled in vacuum. At a temperature of 210-220 ° C (1 mmHg), 27 are obtained g (91.6% of theoretical) of the product with indicators of 1.5816 (in the supercooled state); Si 13.8 o / o, so 50 ° (recrystallized from an alcohol-acetone mixture.) Example 2. According to the method described in example 1.32.4 g (0.07 mol) 1.5 dichloro, 1,3,5 trimethyl, 1, 3, 5- triphenyltrisiloxane is slowly poured into a flask with 4 g (0.14 mol) of phenyl sodium suspended in toluene while cooling. Distillation of the reaction product in vacuum at 250–265 ° C (1 mm Hg) separates the fraction of 30 g ( 78.5%, from the theoretical) with the next, by their opponents. Found: p 1.5790; Vjo 167 eats; a pier weight. 529; C, 72.77%; H 6.4%; Si 15.5 / o. Literature data for trisiloxane: n 1,5785; V-2, 165 eats; a pier weight 546; From 72.6%; H6.24o / o; Si 15.45%. The subject of the invention. A method for producing organosilicon oligomers by reacting a, co-dichloropolyorganosiloxanes with an aryl derivative of an alkali metal, characterized in that, with the purpose of obtaining heat-resistant and radiation-resistant organosilicon oligomers, a, i-ades are used as aces, as a, s-dichloropolyorganosiloxanes, which are used by aphors. Aryl sodium is used as an aryl alkali metal.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU199396A1 true SU199396A1 (en) |
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