甲基乙烯基MQ树脂的制备及对LED封装补强作用的研究

1、摘 要 MQ 树脂是一种很独特的聚硅氧烷树脂，其是由单官能度硅氧烷链节（M）与四官能度硅氧烷缩聚链节（Q）构成的有机硅树脂。MQ 硅树脂性质介于普通无机高分子化合物和有机高分子化合物之间，其具有一般树脂难以达到的耐高温、憎水和耐化学品等性能。此外，MQ 硅树脂还具有优异的电绝缘性能、机械性能、优良的耐热性、耐候性、柔韧性、成膜性和粘接性。MQ 树脂在工业上具有很大的应用价值，主要用作加成型液体硅橡胶的补强填料，硅氧烷压敏胶的填料及增粘剂，以其为基料做成的涂料电绝缘漆、层压材料、模塑料、防潮剂和脱膜剂等各类产品在各个领域都获得了广泛的应用。 本文采用价廉易得的硅酸钠作为原料设计并合成出了甲基乙烯基 MQ 树脂，具体的合成路线为：1）硅酸钠水溶液在酸性条件下水解，然后加入四甲基二乙烯基二硅氧烷（MMVI）、六甲基二硅氧烷（MM）共水解，在回流条件下合成 MQ 萃取溶液。2）MQ萃取溶液和甲苯在回流条件下脱水缩聚。3）将得到的 MQ 树脂溶液水洗到中性，干燥过滤。4）减压蒸馏得到 MQ 树脂。对最终得到的产物进行了核磁、红外和紫外表征确定了所合成化合物的结构。对制备 MQ 树脂各影响因素进行

2、了研究，使其粘度适宜，得出最佳工艺条件为：共水解温度为 40-50，共水解时间 30-40min，回流时间为 3-4h，脱水缩聚时间为 3-4h，脱水缩聚温度在 90-100，催化剂为 2gKOH 配制成浓度为 50的溶液，并且通过脱水缩聚步骤降低了 MQ 树脂的羟基含量，使其含量控制在 1-2，改善了其与乙烯基硅油的相容性。对 MQ 树脂进行了热失重、耐热性性能测试，得出结论：随着 nR/nSi的增大，MQ 树脂的热失重也增大；甲基乙烯基 MQ 树脂在 250仅损失 5，表明 MQ 树脂具有优良的耐热性。 研究了甲基乙烯基 MQ 树脂对 LED 封装补强作用，得出对其补强性能提高了四倍的工艺条件为：乙烯基含量为 1-4的 MQ 树脂；MQ 加入量为乙烯基硅油 20-25；nM/nQ为 0.8-0.9 的 MQ 树脂；粘度为 5000mPa.s 的乙烯基硅油比粘度为 2000mPa.s的乙烯基硅油拉伸性能好。关键词：MQ 树脂、LED 封装材料、补强、拉伸性能 I Abstract MQ resin is unique polysiloxane resin It is made up

3、of single-functional siloane chainand tetrafunctional siloxane chain. The properties of MQ resin is among inorganic polymersand organic polymers.It posses temperature resistance、hydrophobic、resistance to chemicals、excellent electrical insulation、mechanical、excellent heat resistance、weather resistance、flexibility 、 film formation and adhesion.MQ resin had great application value in theindustrymainly for additional liquid silicone rubber reinforcing fillersilicone pressuresensitive adhesive filler

4、 and tackiferAs the base materialit was made of electrical insulatingpaints、laminated materials、molding compounds、moisture-proof agents and mold releaseagents of various products that apply all areas. The cheap and easy to get of sodium is raw material.Methyl Vinyl MQ resin have beensynthesized the synthetic procedures are as follows:1 sodium aqueous solution hydrolysisunder acidic conditionthen add in MMVI、MM and cohydrolysisthus synthesize MQextraction solution in return conditions.2 MQ extrac

5、tion solution and toluene dehydrationcondensation in return conditions.3MQ resin solution washed to neutralitythen driedfilter.4Get MQ resin after vacuum distillation. Their structures were confirmed by IR UVand 1HNMR. It research all the factors of MQ resin in order to reinforce very well.Itsoptimum conditions: the temperature of cohydrolysis was 40-50 the time of cohydrolysiswas 30-40min the time of reflux time was 3-4hthe time of dehydration polycondensationwas 3-4h the temperature of dehydra

6、tion polycondensation was 95-100 the dosage ofcatalyst was 2g KOH with concentration of 50 Solution. It test TG and heat resistance:withnR/nSi increasesTG also increasedMethyl vinyl MQ resin loss at 250 only 5itshowed that MQ resin had excellent heat resistance. MQ resin apply in LED Packaging Reinforcing and text performanceand the preferableprocess was:vinyl content of 1-4 of the MQ resinthe amount of MQ resin was 20-25of vinyl silicone oilM/Q was 0.8.The 5000mPa.s viscosity of vinyl silicone oil is better thanthe 2000mPa.s viscosity of vinyl silicone oil.Keywords: MQ resin、LED packaging materials、reinforce、tensile properties II 目 录摘 要.IAbstract . II第一章 综 述. 1 1.1 引言 . 1 1.2 LED 概述. 1 1.3 LED 封装材料. 2 1.3.1 环氧树脂材料. 2 1.3.2 有机硅改性环氧树脂材料. 2 1.3.3 有机硅材料. 3 1.4 硅橡胶 . 3 1.4.1 加成型液体硅橡胶组分. 4 1.4.1.1 乙烯基硅油 . 4 1.4.1.2 含氢硅油 . 4 1.4.1.3 铂催化剂 . 4 1.4.1.4 抑制剂 .

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