摘要采用新戊二醇,三氯氧磷为原料,在超声场中制备中间体新戊二醇磷酰氯。探讨了超声波对反应的影响,通过超声波技术提高产品的得率,并制备了五种新型膨胀型阻燃剂,在合成1,4-二(5,5-二甲基-1,3-二氧杂-2-磷杂环己基磷酰基)哌嗪(PBNGP)时,设计正交试验,确定最佳工艺条件为以氯仿为溶剂,中间体和哌嗪的物质的量之比为2。0︰1。2,反应温度为50℃。以中间体与苯并三氮唑合成了一种未见文献报道的新型膨胀型阻燃剂,并对其反应机理进行了探讨。通过红外光谱、核磁共振、质谱对所得产品的结构进行表征,测定了阻燃剂的膨胀度、剩炭率,将阻燃剂应用于制备阻燃性聚丙烯,测定阻燃聚丙烯的氧指数和拉伸强度,筛选出性能优良的阻燃剂。76965
毕业论文关键词 膨胀型阻燃剂 新戊二醇磷酰氯 合成 阻燃
毕业设计说明书外文摘要
Title The study on the synthesis of novel intumescent flame retardants of neopentyl glycol
Abstract Neopentyl glycol chlorophosphate was synthesized by using neopentyl glycol and phosphorus oxychloride as the starting material in ultrasonic field。 The effect of ultrasonic on yield was studied。 Five kinds of novel intumescent flame retardants (IFR) were prepared。 The optimal reaction conditions of preparration of 1,4-bis (5,5-dimethyl-1,3-dioxa-2-phosphacyclohexyl phosphoryl) piperazine (PBNGP) were obtained through orthogonal experiment and as fellows: using chloroform as solvent, n (intermediate) : n (piperazine) = 2。0:1。2, reaction temperature is 50℃。 One kind of novel IFR were prepared by reacting intermediate with benzotriazole in this paper,and it hasn't been reported previously, then its reaction mechanism was studied。 The obtained products were characterized by IR、NMR and MS。 The intumenscent degree and char residual of flame retardants were determined。Flame retardants were applied to prepare flame retarding polypropylene。Their oxygen index value and tensile strength of flame retarding polypropylene was determined。The optimal intumescent flame retardant was selected。
Keywords Intumenscent Flame Retardant, Neopentyl glycol chlorophosphate, Synthesis,Flame retardancy
目 次
1 引言 1
1。1 课题概述 1
1。2 阻燃剂的发展 1
1。3 膨胀型阻燃剂的简介 1
1。4 本文研究内容 3
2 新型膨胀型阻阻燃剂的制备研究 4
2。1 新戊二醇磷酰氯(5,5-二甲基-1,3,-二氧杂-2-磷杂环己内酰氯)的制备 4
2。2 1,4-二(5,5-二甲基-1,3-二氧杂-2-磷杂环己基磷酰基)哌嗪(PBNGP)的制备 11
2。3 3-(5,5-二甲基-1,3-二氧杂-2-磷杂环己基磷酰基)苯并咪唑的制备 15
2。4 3-(5,5-二甲基-1,3-二氧杂-2-磷杂环己基磷酰基)苯并三氮唑的制备 19
2。5 1,4-二(5,5-二甲基-1,3-二氧杂己内磷酰亚胺基)苯(NBPAN)的制备 23
2。6 1,2-(5,5-二甲基-1,3-二氧-2-磷环己膦酰胺基)乙烷的制备 28
3 新型膨胀型阻燃剂性能分析 32
3。1 热重分析 32
3。2 膨胀性能的测定