李亚豪毕业设计论文

丙烯酸五溴苄酯的合成及其对聚双环戊二烯的阻燃研究

郑州轻工业学院成人教育

本科毕业论文

丙烯酸五溴苄酯的合成及其对聚双环戊二烯的

阻燃研究

学生姓名 李亚豪 专业班级 一班 学 号 院 （系） 继续教育学院 指导教师(职称) 高讲 完成时间 2013年 5月 10 日

郑州轻工业学院继续教育学院

I

丙烯酸五溴苄酯的合成及其对聚双环戊二烯的阻燃研究

丙烯酸五溴苄酯的合成及其对聚双环戊二烯的

阻燃研究

摘 要

聚双环戊二烯（PDCPD）具有高模量、高抗冲性和高抗蠕变性，

特别适用于反应注射成型制造大型且结构复杂的构件。但是它的阻燃性不好，限制了在某些领域的应用。阻燃剂是用以提高材料抗燃性，即阻止材料被引燃及抑制火焰传播的助剂，主要用于合成及天然高分子材料，使之具有难燃性、自熄性和消烟性等特点。因此，本论文采用丙烯酸五溴苄酯与双环戊二烯（DCPD）同步聚合的方法实现PDCPD的阻燃。

首先，进行了五溴甲苯与五溴苄基溴的合成，探索了反应温度对五溴苄基溴产率的影响，并对产物五溴苄基溴进行红外表征。

然后，以制得的五溴苄基溴为原料，在一定条件下与丙烯酸进行酯化反应制备丙烯酸五溴苄酯。探索了反应温度对酯化反应的影响，并对产物丙烯酸五溴苄酯进行红外表征。

最后，对丙烯酸五溴苄酯与双环戊二烯同步聚合制备出了阻燃性PDCPD高分子材料，并测定氧指数（OI）测定。结果表明，加入丙烯酸五溴苄酯的聚合物比纯聚双环戊而的阻燃性要好。

关键词：阻燃剂，五溴甲苯，五溴苄基溴，丙烯酸五溴苄酯，双环戊二烯

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丙烯酸五溴苄酯的合成及其对聚双环戊二烯的阻燃研究

Synthesis of Pentabromobenzyl Acrylate and Its Flame Retardance Application to Polydicyclopenadiene

ABSTRACT

The PDCPD has a high modulus, high impact resistance and high creep resistance but its flame retardants is too bad to limit its the applications in some areas. Flame retardant (FR) is a kind of additive which can enhance the materials flame resistance，and it is mainly used for nature or synthesized polymers which make the polymer have many characteristics such as flame retardance, fire resistant, self-extinguish ability, smoke abatement and so on．But most of the flame retardant are small molecule materials so that they are incompatible with polymer and have harmful effect on physical and mechanical properties and processing properties of matrix material．

In this paper, Pentabromobenzyl acrylate was chosen to be as a flame retardant for PDCPD.

Pentabromobenzyl acrylate is a very good flame retardant for PDCPD, its double bond can be polymerize with DCPD, so it has a good compatibility with the PDCPD. Because of the flame retardant components can not migrate out the matrix, it can enhance effectively the materials flame resistance. pentabromotoluene,

brominated

pentabromobenzyl

was

first

synthesized, and investigated the effects of reaction temperature on the yield. Then, pentabromobenzyl acrylate was synthesized by brominated pentabromobenzyl reacted with acryloyl chloride. Products were characterized with infrared spectrometer.

Last, the pentabromobenzyl acrylate and DCPD were polymerized synchronously to prepare a flame resistance PDCPD, and was tested

III

丙烯酸五溴苄酯的合成及其对聚双环戊二烯的阻燃研究

with oxygen index (OI). The results showed that the flame resistance of polymer blends which contain pentabromobenzyl acrylate is better than that of pure PDCPD.

KEY WORDS: Flame Retardant, Pentabromobenzyl Acrylate, Pentabromotoluene, Pentdienecyclopentadiene

IV

丙烯酸五溴苄酯的合成及其对聚双环戊二烯的阻燃研究

目 录

第1章 前 言 ...................................... 7 §1.1 引言 ....................................... 7 §1.2 PDCPD阻燃剂国内发展概况 .................... 7 §1.3 聚丙烯酸五溴苄酯简介 ....................... 8 §1.3.1 阻燃剂聚丙烯酸五溴苄酯 .................. 8 §1.3.2 聚丙烯酸五溴苄酯结构 .................... 8 §1.3.3 聚丙烯酸五溴苄酯合成方法 ................ 9 §1.3.4 中间体五溴甲苯简介 ..................... 10 §1.3.5 中间体五溴苄基溴简介 ................... 10 §1.3.6 单体丙烯酸五溴苄酯 ..................... 11 §1.4 本课题的研究意义 .......................... 11 第2章 实验部分 .................................. 12 §2.1 实验原材料及基本配方 ...................... 12 §2.2 实验设备及仪器 ............................ 12 §2.3 实验步骤 .................................. 13 §2.3.1 五溴甲苯的制备 ......................... 13 §2.3.2 五溴苄基溴的制备 ....................... 13 §2.3.3 丙烯酸五溴苄酯的制备 ................... 14 §2.3.4 丙烯酸五溴苄酯与DCPD的共聚合 .......... 14 §2.4 PDCPD阻燃性能测定 ......................... 14 §2.5 红外光谱表征 .............................. 14 §2.6 氧指数测试 ................................ 15 第3章 结果与讨论 ................................ 16 §3.1 五溴甲苯的合成与表征 ...................... 16 §3.1.1 五溴甲苯的合成方法 ..................... 16 §3.1.2 五溴甲苯的表征 ......................... 17 §3.2 五溴苄基溴的合成 .......................... 17

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