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摘要：本论文以甲基乙烯基二氯硅烷，亚磷酸二甲酯为原料，以无水三氯化铝为催化剂，制备出一种含Si/P反应型阻燃剂。通过改变原料物质量配比、反应时间、反应温度和催化剂用量等，系统研究了各合成因素对产物收率的影响，并通过测定该阻燃剂的羟值、酸值、粘度、固含量等性能指标，筛选出合成该阻燃剂的最优条件。利用傅里叶红外（FTIR)、核磁共振（HNMR）对其进行结构分析。实验结果表明，当甲基乙烯基二氯硅烷与亚磷酸二甲酯物质量之比为1:1.5，反应时间为24 h，反应温度为53℃，催化剂用量为2 g时，得到的阻燃剂收率最大，反应条件最佳。并对该阻燃剂在PU硬泡上进行了性能评价。利用万能试验机对含有该阻燃剂的PU硬泡进行压缩强度测试，利用氧指数仪对其进行氧指数测定，并对表观密度、尺寸稳定性等进行测定。实验结果表明，加入该阻燃剂后PU硬泡的压缩强度和氧指数均有提高。24279
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毕业论文 关键词： 硅/磷；反应型阻燃剂；合成；PU硬泡
Reactive flame retardant Si/P study on synthesis and rigid PU foam
Abstract: in this article, methyl vinyl dichlorosilane and dimethyl phosphite were used as raw materials, with anhydrous aluminum chloride as catalyst, we prepared reactive flame retardant containing Si/P. By varying the ratio of raw material, the amount of catalysts, reaction temperature and time, etc, we systematically studied synthesis effect of factors on yield. By determining hydroxyl value, acid value, viscosity, solids content and other performance indicators, we filtered out the optimum conditions of synthesis of the flame retardant. Fourier transform infrared (FTIR), nuclear magnetic resonance (HNMR) were used for structural analysis. Experimental results showed that, when the ratio of vinyl silane chloride and dimethyl phosphite esters to 1:1.5, the reaction time of 24 h, the reaction temperature of 53℃, the catalyst to 2 g, the reaction conditions were best. And performances of the flame retardant were evaluated on the polyurethane rigid foam. Universal testing machine was used to test the compression strength of polyurethane rigid foam with the flame retardant. Oxygen index apparatus was used to determinate the oxygen index , and the apparent density, dimensional stability, etc, were also measured. The results showed that, after joining the flame retardant to polyurethane rigid foam , the compression strength and oxygen index were increased.
Key Words: Silicon/phosphorous; reactive flame retardant agent; synthesized; rigid PU foam
目 录
1绪论 1
1.1 阻燃剂概述 1
1.1.1 阻燃剂的分类 1
1.1.2 阻燃剂制备方法 2
1.1.3 阻燃剂的优缺点 3
1.1.4 阻燃剂的应用 4
1.1.5 阻燃剂的发展趋势与展望 5
1.2 聚氨酯(PU)硬质泡沫简介 7
1.2.1 PU泡沫塑料的定义 7
1.2.2 PU泡沫塑料的分类 7
1.2.3 PU泡沫塑料的结构 7
1.2.4 PU硬泡的特点 8
1.2.5 PU硬泡的制备方法 8
1.2.6 PU硬泡的应用 9
1.3 阻燃剂在PU上的应用研究 9
1.4 现有问题 10
1.5 本实验的目的和意义 10
1.6 研究内容 11
2 实验部分 12
2.1 原料及试剂 12
2.2 实验方法 13
2.2.1 反应型含Si/P阻燃剂的制备 13
2.2.2 反应型含Si/P阻燃剂体系制备PU硬泡 13
2.3 分析表征 13
2.3.1 红外光谱分析 13
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