SU157107A1 - - Google Patents
Info
- Publication number
- SU157107A1 SU157107A1 SU777615A SU777615A SU157107A1 SU 157107 A1 SU157107 A1 SU 157107A1 SU 777615 A SU777615 A SU 777615A SU 777615 A SU777615 A SU 777615A SU 157107 A1 SU157107 A1 SU 157107A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- reaction
- viscous
- molecular weight
- ammonia
- temperature
- Prior art date
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- WGGNJZRNHUJNEM-UHFFFAOYSA-N 2,2,4,4,6,6-hexamethyl-1,3,5,2,4,6-triazatrisilinane Chemical compound C[Si]1(C)N[Si](C)(C)N[Si](C)(C)N1 WGGNJZRNHUJNEM-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910002794 Si K Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 aliphatic diamines Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 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
- 238000002360 preparation method Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
Description
Известен способ получени полиалкилсилазапов взаимодействием .диметилдихлорсилана с этплепдиамином с последующей координацией полимеров безводной хлористой медью. Однако способ сложен, получаемые по этому способу полимеры имеют небольшой молекул рный вес.A known method for producing polyalkylsilazapes by reacting dimethyldichlorosilane with ethpledediamine, followed by coordination of the polymers with anhydrous copper chloride. However, the method is complex, the polymers obtained by this method have a low molecular weight.
Предложенный способ получени полиалкилсилазаиов отличаетс от известного те.м, что алкилциклосилазаиы обрабатывают алифатическими диаминами при нагревании.The proposed method for the preparation of polyalkylsilazates differs from the known method that alkylcyclosylazases are treated with aliphatic diamines when heated.
Способ основан на разрыве св зи Si - К в циклос 1лазане и заключаетс в иагревании смеси полиалкилциклосилазаиов и органических диаминов. Из пол}чепной после нагревани массы отгон ют избыток этилендиалгина и получают целевой продукт с выходом 98%. Полученный полимер представл ет собой бесцветиый в зкий продукт в виде густого масла.The method is based on breaking the bond of Si-K in cyclos-lazane and consists in heating a mixture of polyalkyl cyclosyl and organic diamines. After heating the mass, an excess of ethylene dialgin is distilled off from the mass and the desired product is obtained in a yield of 98%. The resulting polymer is a colorless, viscous product in the form of a thick oil.
Пример 1. В трехгорлую колбу, снабженную мешалкой, обратным холодильником с системой поглощени аммиака, капельной воронкой и термометром, загружают 21,9 г гексаметилциклотрисилазана, после чего из капельной воронки при температуре 40С ввод т 18.0 г этилендиамина. Затем те мпературу медленно довод т до 160°С, при которой реакци продолл аетс в течение 10-12 час. При температуре 95-100 С наблюдаетс бурное выделение аммиака. Общее количество выделивщегос аммиака составл ет 91,0% в пересчете на имеющийс азот в тримере. В результате реакции получают в зкую массу, из которой отгонкой в вакууме выдел ют избыток этилендиамина. В колбе остаетс бесцветный в зкий иродукт в виде густого масла. Выход иолимера 98%.Example 1. In a three-necked flask equipped with a stirrer, a reflux condenser with an ammonia absorption system, a dropping funnel and a thermometer, 21.9 g of hexamethylcyclotrisilazane was charged, after which 18.0 g of ethylene diamine was introduced from a dropping funnel at 40 ° C. Then the temperature was slowly adjusted to 160 ° C, at which the reaction was continued for 10-12 hours. At a temperature of 95-100 ° C, there is a rapid release of ammonia. The total amount of ammonia released is 91.0% based on the nitrogen in the trimer. As a result of the reaction, a viscous mass is obtained, from which an excess of ethylene diamine is distilled off in vacuum. A colorless, viscous and product as a thick oil remains in the flask. The output of the iolimer 98%
N° 157107N ° 157107
Вычислено дл CsHgSiN в %: С -41,80: Н - 9,36; Si - 32,59; N - 16,25. Отношение Si : N 1,00.Calculated for CsHgSiN in%: C -41.80: H - 9.36; Si - 32.59; N - 16.25. The ratio of Si: N 1,00.
Найдено в %: С -41,20; Н - 9,40; Si-32,40; N-17,02. Молекул рный вес 2116.Found in%: С -41,20; H - 9.40; Si-32.40; N-17.02. Molecular weight 2116.
Пример 2. В реакционную колбу (см. пример 1) загружают 34,8г гексаметилендиалшна и из канельной воронки нри температуре 40°С ввод т 21,9 г гексаметилциклотрисилазана. Затем температуру медленно довод т до 190-200°С, при которой реакци продолжаетс в течение 57 час. В ходе реакции наблюдаетс выделение аммиака. В результате получают в зкую массу, из которой отгонкой в вакуу.ме удал ют избыток гексаметилендиамина. В колбе остаетс прозрачный, в зкий, темножелтого цвета полимер.Example 2. 34.8 g of hexamethylenedialne was charged into the reaction flask (see example 1) and 21.9 g of hexamethylcyclotrisilazane was introduced from a channel funnel at a temperature of 40 ° C. The temperature is then slowly brought to 190-200 ° C, at which the reaction continues for 57 hours. Ammonia is released during the reaction. The result is a viscous mass, from which excess hexamethylenediamine is removed by distillation in vacuo. A transparent, viscous, dark yellow polymer remains in the flask.
Вычислено дл в %: С - 52,6; Н-10,55; Si-24.5; N-12 ,25. Отношение ,00.Calculated for dL in%: C - 52.6; H-10.55; Si-24.5; N-12, 25. Attitude, 00.
Найдено в %: С -52,1; Н - 10,8; Si -24,11; N- 12,98. Молекул рный вес 2002,6.Found in%: C -52.1; H - 10.8; Si -24.11; N- 12.98. Molecular weight 2002.6.
Предмет изобретени Subject invention
Способ получени полиалкилсилазанов с использованием органических диаминов, отличающийс тем, что, с целью упрощени способа Н увеличени молекул рного веса нолучаемых полимеров, алкилциклосилазаны обрабатывают алифатическими диа.минами при нагревании.A process for producing polyalkylsilazanes using organic diamines, characterized in that, in order to simplify the process H of increasing the molecular weight of the polymers obtained, alkyl cyclosilazanes are treated with aliphatic diamina by heating.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU157107A1 true SU157107A1 (en) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3354098A (en) * | 1966-05-31 | 1967-11-21 | James D Byrd | Elastomeric silazane polymers and process for preparing the same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3354098A (en) * | 1966-05-31 | 1967-11-21 | James D Byrd | Elastomeric silazane polymers and process for preparing the same |
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