SU872531A1 - Способ получени полуретанов - Google Patents
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(54) СПОСОБ ПОЛУЧЕНИЯ ПОЛИУРЕТАНОВ
Изобретение относитс к высокомолекул рным соединени м, а именно к синтезу полиуретанов, нашедших широкое применение в различных област х техники. Известен способ получени полиуретанов конденсацией в растворе диизоциана-. тов с диолами fl. Недостатки известного способа - необходимость синтеза дорогосто щих диизоцианатов , потер растворимости полиуретанами в результате возникновени пространственных сшивок за счет взаимодействи уретановых группировок полимерных цепей с изоцианатными группш-ги с образованием аллофанатнык структур и трудност получени линейных полимеров. Наиболее близким к изобретению по технической сущности вл етс способ по лучени полиуретанов поликонденсацией в растворе производных диолов с диаминами с последуюшим высаживанием полиуретана водой 2. Недостатки такого способа получени полиуретанов - низкие выходы и низкие в зкостные характеристики полимеров, обусловленные протеканием побочшах продеосов взаимодействи хлорформиатных группировок с растворител ми и третичными аминами, используемыми в качестве aibцептрра хлористого водорода, что приводит к гибели функциональных групп; трудность хранени и транспортировки биохпор формиатов, обусловленна легкостью их гидролиза, сопровождающийс образованием монофункциональных примесей и уведачением давлени (при гидролизе выдеп ЮТс CO-i, нее), а также протеканием интенсивной коррозии; неудобство работы с бисхлорформиатами, большинство из которых жидкости; трудность очистки биохлорформиатов , обусловленна их высокими температурами кипени , они рчишакггс лишь перегонкой в вакууме; невозможрность синтеза линейных полиуретанов с боковыми функциональными группами (например ОН-группами), с которыми хлорформиаты активно реагируют . 38 Цепь изобретени - получение полиуретана линейного строени , растворимого в органических растворител х, а также повышение процента его выхода. Указанна цель достигаетс тем, что в качестве производных диопов используют активированные бис-карбонаты диолов обшей формулы -о - Х; :Q). се се R. (CH),-,-(cHi),, -, -(cHi)-, -(CHj),-СН -,, - и поли конденсацию провод т при 7 5-120 Полученные таким образом полиуре таны полностью растворимы в органических растворител х, так как N , N-диметил рмамид (ДМФА), N , (-диметилацетами N -метилпирролидон, М -крезол, смесь тетрахлорэтана с фенолом (3:1). Приведенна в зкость полученных полиуретанов 0,5-1,6 дл/г в м-крезоле, выход 6994% в зависимости от условий реакции и природы активирующей группы. Синтезированные полимеры характеризуютс по пр1веденной в зкости их растч воров и данными ИК-спектрапьного анализа . Пример 1. К раствору 1,16 г (0,О1 мол ) гексаметилендиам1 ра (ГМДА в 16,6 мл N , N - даметипформамида добав Л5ООТ 4,06 г активированн(Лг.о бис-карбон та на основе 1,3-пропандиола и п -нитр фенола при комнатной температуре, На блюдаетс разогревание реакционного рас вора в результате экзотермической реакции . Реакционную смесь перемешивают при комнатной температуре в течение 45 мин, а затем помешают в силиконовую баню при (при комнатной тем пературе полимер Ызгоедает из раствора, при нагревании до - гомогенный раствор). Перемешивание продолжают при 105 С в течение 2,5 ч и гор чий реакционный раствор выпивают в воду. Вы1 павший полимер отфильтровывают, промывают этиловым спиртом, экстрагируют спиртом в аппарате Сокслетта и сушат. Выход 88%; ЧпР Л дп/г в м-крезоле при 25°С, С 0,5 г/дл. Пример 2. Синтез полиурютана существл ют в соответствии с методикой, приведенной в примере 1, с той разницей, что в качестве активированного бис-карбоната используют бис-Г2,4-динитро(карбофенокси )}- ,3-пропандиол (ДНКФП). Выход полиуретана 69%; Р О,6О дл/г в м-крезоле при 25°С, С 0,5 г/дл. Пример 3- Синтез полиуретана осуществл ют в соответствии с методикой, приведенной в примере 1, с той разницей, что в качестве активированного бискарбоната используют ,4,6- рихлор (карбофенокси)-,3-пропандиол (ТХКФП). Выход полиуретана 83%; 1пР 0,61 дл/г, в м-крезоле при 25 С, С 0,5 г/дл. Пример 4. Синтез полиуретана осуществл ют в соответствии с методикой, йриведенной в примере 1, с той разницей, что в качестве активированного карбоната используют бис-пентахлор(карбофенок- си)-1,3-пропандиол (ПХКФП). Выход полиуретана 68%; 7.ПР 0,48 дл/г в м-крезоле при 25С, С 0,5 г/дл. Пример 5. К раствору 1,16 г (0,01 мол ) гексаметилендиамина в 16,7 мм N ,Н - 1иметилформамида добавл ют 4,20 г бис-Г 1 -нитpo(кapбoфeнoкcи- -1,3-бутандиола (ПНКФБ). Наблюдаетс разогревание реакционного раствора в результате экзотермической реакции. Реакционную смесь перемешивают при комнатной температуре в течение 0,5 ч, а затем при 75°С в течение 3 ч (полимер растворим в N , N -диметидформамиде при комнатной температуре). Реакционный раствор выливают в воду. Выпавший полимер отфильтровывают, промывают водой, экстрагируют водой в аппарате Сокслетта и сушат. Выход 91%, ЧПР 0,96 дл/г в м-крезоле при 25С, С 0,5 г/дл. Пример 6. Синтез полимера осуществл ют в соответствии с методикой, приведенной в примере 5, с той лишь раз ,ницей, что используют бис- ентахлор(кар- ;бофенокси)-1,3-бутандиол (ПХКФБ).Вы .ход 71%, tnp 0,43 дл/г в м-крезоле при 25°С, С 0,5 г/дл. Пример 7. Синтез полимера осуществл5пот в соответствии с методикой, приведенной в примере 1, с той р 1зницей, что реакцию провод т в гексамегилфосфортриамиде . Выход полиуретана 89%, 1цр 0,7 дл/г при в м-крезопе, С 0,5 г/дп. Пример 8. Синтез полиуретана осуществл ют в соответствии с методикой приведенной в примере 1, с той разницей что в качествекатализатора в реакционную смесь ввод т триэтиламин (из расчета 2,2 мол триэтиламина на 1 моль диамина ). Выход полиуретана 9О%, tnpl.e дл/г в м-крезоле при 25С, С 0,5 г/дл. Пример 9. Синтез полиуретана осуществл ют в соответствии с примером 2 с той разницей, что в реакционную смесь в качестве катализатора ввод т три этиламин (из расчета 2,2 мол на 1 мол диамина). Выход полиуретана 82%; 1пР 0,75 дл/г в м-крезоле при С 0,5 г/дл. Пример 10. Синтез полиуретана осуществл ют в соответствии с примером 3, с той разницей, что в реакционную смесь в качестве катализатора ввод т триэтиламин (из расчета 2,2 мол на 1 моль диамина). Выход полиуретана 88%, 1,ПР 0,85 дл/г в м-крезоле при 25°С, С 0,5 г/дл. При мер 11. Синтез попиуретана осуществл ют в соответствии с примером 4, с той разницей, что в реакционную смесь в качестве катализатора ввод т три- .этиламин (из расчета 2,2 мол на 1 мопь диамина). Выход 79%;,про,75 дл/г в м-крезоле прт 25 С, С 0,5 г/да. Пример 12. QiHTea осуществл г ют в соответствии с методикой, приведенной в примере 1, с той лищь разницей, что вместо гексаметилендиамина используют 4,4-диаминодифенклметан (ДАДМ) и ре- акцию провод т при 120С. Выход полимера 89%, LnP 0,84 дл/г в мгкрезоде при 25С, С 0,5 г/дл. П р и м е р 13. Синтез осущестап ют в соответствии с методикой, приведен ной в примере 1, с три разницей, го иопользуют 14 -(2-оксиэтил)- типендиамин (ОЭДА), а поликонденсацию провод т при комнатной температуре в течение 16 ч. Выход полимера 94%; 1,06 дп/г в диметилформамиде при 25С, С 0,5 г/дп. С)сновные характеристики полученных полиуретанов приведены в таблице.
872531
8 Продолжение таблицы
Claims (2)
- Формула изобретенияСпособ получения полиуретанов поли— 45 конденсацией в растворе производных ди олов с диаминами с последующим выделением полиуретанов, отличающий— с я тем, что, с целью получения полиуретанов линейного строения, растворимого в органических растворителях, а также повышения выхода и вязкостных характеристик в качестве производных· диолов используют активированные бис—карбонаты диолов общей формулы 0 U х— о — С, — О— R— 0 — 0 — 0—X ,N0^R· , —(CHipg —, —(CHj)4— ( —(сн^-СН -, — СНлСНл—0—СНлСНл — ( сн3 и поликонденсацию проводят при 75-12О°С.Источники информаций, принятые во внимание при экспертизе1. Саундерс Дж. и Фриш К. К. Химия полиуретанов. М., 'Химия', 1968.
- 2. Морган П. У. , Поликонденсацион— ный метод синтеза полимеров. Л.,'Химия', 1970, с. 256 (прототип).
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1979
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