CN108727590B - 一种硅树脂废弃料的回收再利用方法 - Google Patents
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Abstract
本发明涉及聚硅氧烷应用技术领域，为解决现有硅树脂废弃料造成环境污染的问题，提出一种硅树脂废弃料回收再利用方法，是以硅树脂废弃料为原料，在催化剂和水的作用下，在有机溶剂中进行反应，得到环型、笼型、半笼型、双甲板型或者梯型聚倍半硅氧烷中一种，本发明的回收方法具有反应条件温和、能耗低、效率高、产品提纯过程简单易行等优点。
Description
技术领域
本发明涉及聚硅氧烷应用技术领域，特别是涉及硅树脂废弃料的一种回收再利用方法。
背景技术
聚硅氧烷具有耐热、耐辐射、耐腐蚀、阻燃、无毒等优越性能，广泛应用于包封材料、密封材料、航空航天、化妆品等领域。但是，硅树脂在合成或者使用过程中会产生不符合性能要求的无规或者交联结构，只能进行废弃处理，对环境造成污染。以这些硅树脂废弃料为原料合成结构有序的聚硅氧烷，如环型、笼型、半笼型、双甲板型或者梯型聚倍半硅氧烷，可以有效减少环境污染。文献中报道的合成环型、笼型、半笼型、双甲板型或者梯型聚倍半硅氧烷的原料一般为三官能团化合物，如苯基三甲氧基硅烷(Polymer Journal，2007，39，230-238；Inorganic Chemistry，2002，41，6892-6904)。以硅树脂废弃料为原料合成结构有序的聚硅氧烷的工作未见报道。
发明内容
为解决现有硅树脂废弃料造成环境污染的问题，本发明提出一种硅树脂废弃料回收再利用方法，是以硅树脂废弃料为原料，在催化剂和水的作用下，在有机溶剂中进行反应，得到环型、笼型、半笼型、双甲板型或者梯型聚倍半硅氧烷中一种，本发明的回收方法具有反应条件温和、能耗低、效率高、产品提纯过程简单易行等优点。
本发明是通过以下技术方案实现的：一种硅树脂废弃料的回收再利用方法为：以硅树脂废弃料为原料，在催化剂和水的作用下，在有机溶剂中进行反应，得到环型、笼型、半笼型、双甲板型、梯型聚倍半硅氧烷中一种。
反应过程为：
反应式中，X、Y、Z、Q、R分别独立地选自氢、烷基、烯基、炔基、芳香基、环氧基、酯基、磺酸基、羧基、腈基、卤代烷基、卤代烯基、卤代炔基中一种，m、n为正整数。
所述的催化剂选自酸、碱、金属中一种，作为优选，催化剂选自盐酸、硝酸、硫酸、磷酸、乙酸、甲酸、四甲基氢氧化铵、四乙基氢氧化铵以及钾、钠、铁、钴、镍、钌、铑、铂、钯、锇、铱、金、银、铜、锡、锌、钛、锆、铬、锰或镧系金属的单质或金属化合物中一种，
硅树脂废弃料与催化剂的质量比为1∶0.0001～0.1。
硅树脂废弃料与水的质量比为1∶0.001～1。
所述有机溶剂选自烷烃、芳香烃、醚类、酮类中一种，作为优选，所述有机溶剂选自正己烷、环己烷、甲苯、乙醚、正丁醚、四氢呋喃、1，4-二氧六环、丙酮、环己酮、甲基异丁基酮、乙酸乙酯中一种，所用的量为使溶质溶解的量。
所述反应温度为0～120℃，反应时间为30分钟～24小时。
作为优选，所述回收反应完成后，还经过真空烘干、柱色谱、重结晶或者沉淀的后处理过程。
本发明实现硅树脂废弃料的高效回收再利用，回收率可以达到60～95％。产物结构通过基质辅助飞行时间质谱、红外光谱、核磁共振等进行了表征。
与现有技术相比，本发明的有益效果是：以硅树脂废弃料为原料合成结构有序聚倍半硅氧烷，变废为宝，并具有反应条件温和、能耗低、效率高、产品提纯过程简单易行等优点。
附图说明
图1为实施例1中由硅树脂废弃料回收得到的双甲板型聚倍半硅氧烷的基质辅助飞行时间质谱；
图2为实施例1中由硅树脂废弃料回收得到的双甲板型聚倍半硅氧烷的氢谱核磁共振谱图；
图3为实施例1中由硅树脂废弃料回收得到的双甲板型聚倍半硅氧烷的硅谱核磁共振谱图。
具体实施方式
下面通过实施例对本发明作进一步详细说明，实施例中所用原料均可市购或采用常规方法制备。
实施例1：由含有苯基的硅树脂废弃料制备双甲板型聚倍半硅氧烷
在0℃温度下，将99克水加到装有100克含有苯基的硅树脂废弃料、10克四甲基氢氧化铵与200毫升丙酮的500毫升三口烧瓶中，搅拌反应30分钟后，加入100克活性炭，搅拌30分钟，过滤并经过真空烘干，得到白色固体的双甲板型聚倍半硅氧烷，回收率90％。
由硅树脂废弃料回收得到的双甲板型聚倍半硅氧烷的基质辅助飞行时间质谱如图1所示；由硅树脂废弃料回收得到的双甲板型聚倍半硅氧烷的氢谱核磁共振谱图如图2所示；由硅树脂废弃料回收得到的双甲板型聚倍半硅氧烷的硅谱核磁共振谱图如图3所示。
实施例2：由含有氢的硅树脂废弃料制备环型聚倍半硅氧烷
在30℃温度下，将0.017克水加到装有3.9克含氢的硅树脂废弃料、0.01克盐酸与50毫升丁醚的100毫升三口烧瓶中，搅拌反应3小时后，加入5克活性炭，搅拌20分钟，过滤并经过真空烘干，得到白色固体的环型聚倍半硅氧烷，回收率75％。
实施例3：由含有丙烯酸乙酯基的硅树脂废弃料制备笼型聚倍半硅氧烷
在70℃温度下，将0.19克水加到装有9克含有丙烯酸乙酯基的废硅树脂废弃料、0.001克氯化钯与60毫升环己酮的100毫升三口烧瓶中，搅拌反应9小时后，加入5克活性炭，搅拌30分钟，过滤并经过真空烘干，得到白色固体的笼型聚倍半硅氧烷，回收率60％。
实施例4：由含有甲基的硅树脂废弃料制备半笼型聚倍半硅氧烷
在120℃温度下，将1克水加到装有70克含有甲基的硅树脂废弃料、0.01克三氧化二铁与300毫升甲苯的500毫升三口烧瓶中，搅拌反应12小时后，通过柱色谱除去催化剂，过滤并经过真空烘干，得到白色固体的半笼型聚倍半硅氧烷，回收率95％。
实施例5：由含有苯基的硅树脂废弃料制备梯型聚倍半硅氧烷
在20℃温度下，将8克水加到装有24克含有苯基的硅树脂废弃料、0.2克磷酸与60毫升丙酮的100毫升三口烧瓶中，搅拌反应24小时后，加入100毫升正己烷，用去离子水洗反应液至中性并经过真空烘干，得到白色固体的梯型聚倍半硅氧烷，回收率75％。
实施例6：由含有环氧基的硅树脂废弃料制备梯型聚倍半硅氧烷
在120℃温度下，将10克水加到装有150克含有环氧基的硅树脂废弃料、2.5克二茂铁与250毫升1，4-二氧六环的500毫升三口烧瓶中，搅拌反应30分钟后，加入30克活性炭，搅拌15分钟，过滤，将反应液浓缩后倾入甲醇，得到白色固体的梯型聚倍半硅氧烷，回收率86％。
实施例7：由含有乙烯基的硅树脂废弃料制备环型聚倍半硅氧烷
在10℃温度下，将4克水加到装有120克含有乙烯基的硅树脂废弃料、0.02克四氯化钛与300毫升乙酸乙酯的1000毫升三口烧瓶中，搅拌反应15小时后，加入5克活性炭，搅拌10分钟，过滤并经过真空烘干，得到白色固体的环型聚倍半硅氧烷，回收率82％。
实施例8：由含有乙炔基的硅树脂废弃料制备笼型聚倍半硅氧烷
在0℃温度下，将5克水加到装有100克乙炔基的硅树脂废弃料、0.01克氯化铜与300毫升甲苯的500毫升三口烧瓶中，搅拌反应20小时后，加入5克活性炭，搅拌30分钟，过滤并经过真空烘干，得到白色固体的笼型聚倍半硅氧烷，回收率65％。
实施例9：由含有2-氯乙烯基的硅树脂废弃料制备双甲板型聚倍半硅氧烷
在100℃温度下，将4克水加到装有40克含2-氯乙烯基的硅树脂废弃料、0.01克氯化钯与300毫升丁醚的500毫升三口烧瓶中，搅拌反应1小时后，通过柱色谱除去催化剂，并经过真空烘干，得到白色固体的双甲板型聚倍半硅氧烷，回收率65％。
Claims (1)
1.一种硅树脂废弃料的回收再利用方法，其特征在于，在0℃温度下，将99克水加到装有100克含有苯基的硅树脂废弃料、10克四甲基氢氧化铵与200毫升丙酮的500毫升三口烧瓶中，搅拌反应30分钟后，加入100克活性炭，搅拌30分钟，过滤并经过真空烘干，得到双甲板型聚倍半硅氧烷。
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