有机硅高分子阻尼材料的制备与表征
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摘要
以乙二胺和甲基三氯硅烷为主要原料，通过逐步偶联聚合制备了梯形聚硅氧烷(PMSQ)；以八甲基环四硅氧烷为主要原料，碱催化下通过控制滴加去离子水的量制备了不同黏度的端羟基聚硅氧烷(PDMS)。以合成的PMSQ和PDMS为原料进行了如下工作：
1．PDMS与含有活性氯的封端剂反应，制备成可用于紫外光固化的乙烯基聚硅氧烷。
通过FTIR分析了封端剂的结构特征。在光引发剂存在下进行了紫外光固化实验，结果证明：合成的乙烯基聚硅氧烷可以实现在紫外光下固化。
2．以聚硅氧烷(PDMS，PMSQ)为预聚体与丙烯酸酯进行互穿网络聚合，制备性能优良的高分子阻尼材料。
分别从组分配比、交联剂用量、PDMS和PMSQ不同比例等方面研究了材料的阻尼性能，并应用原子力显微镜(AFM)对IPN微相结构进行了观察。借助MTS测试了材料的阻尼性能，研究表明：聚甲基丙烯酸丁酯(PBMA)和聚硅氧烷(PDMS)存在最佳组分配比80:20，材料的阻尼因子tgδ_(max)可达0.9。固定组分配比改变交联剂二乙二醇二丙烯酸酯(DEGDA)的用量，测试材料的阻尼性能，结果表明：当交联剂的用量达到8％时材料的阻尼因子tgδ_(max)可达1.4。固定最佳组分配比80:20交联剂用量8％，用合成的不同黏度PDMS为预聚体制备阻尼材料，测试结果表明：特征粘度为54.5mpa.s时材料的阻尼性能良好。把制备的PMSQ代替部分PDMS为预聚体与PBMA制备成阻尼材料，测试表明：PMSQ加入5％时材料的阻尼性能优良，tgδ_(max)可达1.3。研究了甲基丙烯酸甲酯(MMA)、甲基丙烯酸丁酯(BMA)共聚物／聚硅氧烷IPN阻尼材料，实验证明，MMA的加入不利于提高材料在室温下的阻尼性能。
Hydroxy-terminated ladder-like polysiloxane was synthesized from ethylene diamine and monomethyltrichlorosilane by stepwise coupling polymerization. Meanwhile, hydroxy-terminated single-chain polysiloxane with different viscosity was also synthesized from octamethylcyclotetrasiloxane by alkali-catalyzed method.
After that, some following experiments were completed :
1. Hydroxy-terminated single-chain polysiloxane and active chlorine- contained end-capping reagent were used to synthesis polysiloxane which can be solidified under ultraviolet. The characteristic functional groups of end-capping reagent were proved by FTIR. Meanwhile, ultraviolet curing experiment was done when a certain photoinitiator was in existence, and the result showed that ethenyl-terminal polysiloxane could be solidified under ultraviolet.
2. High quality polymer damping material was synthesized by interpenetrating networks polymerization using polysiloxane and acrylate.
Some affected factors to damping property were studied, such as the compounding ratio of component, the quantity of crosslinking agent, and the ratio of single-chain to ladder-like polysiloxane. And the morphology of damping material was also observed by AFM. The damping property was measured by MTS and the result showed that when the optimal ratio of poly (n-butyl methacrylate) to polysiloxane was 80:20, the damping factor tg δ_(max) was 0.9. And then changing the quantity of crosslinking agent, the result showed that the damping factor tg δ_(max) was up to 1.4 when the ratio of crosslinking agent was 8%. Under the optimal ratio and quanlity of crosslinking agent, damping material was synthesized using different viscosity of polysiloxane as prepolymer. The result was that when the characteristic viscosity was 54.5mpas, the damping property was optimal. Using hydroxy-terminated ladder-like polysiloxane to replace some hydroxy-terminated single-chain polysiloxane, the result showed when the ratio
1．PDMS与含有活性氯的封端剂反应，制备成可用于紫外光固化的乙烯基聚硅氧烷。
通过FTIR分析了封端剂的结构特征。在光引发剂存在下进行了紫外光固化实验，结果证明：合成的乙烯基聚硅氧烷可以实现在紫外光下固化。
2．以聚硅氧烷(PDMS，PMSQ)为预聚体与丙烯酸酯进行互穿网络聚合，制备性能优良的高分子阻尼材料。
分别从组分配比、交联剂用量、PDMS和PMSQ不同比例等方面研究了材料的阻尼性能，并应用原子力显微镜(AFM)对IPN微相结构进行了观察。借助MTS测试了材料的阻尼性能，研究表明：聚甲基丙烯酸丁酯(PBMA)和聚硅氧烷(PDMS)存在最佳组分配比80:20，材料的阻尼因子tgδ_(max)可达0.9。固定组分配比改变交联剂二乙二醇二丙烯酸酯(DEGDA)的用量，测试材料的阻尼性能，结果表明：当交联剂的用量达到8％时材料的阻尼因子tgδ_(max)可达1.4。固定最佳组分配比80:20交联剂用量8％，用合成的不同黏度PDMS为预聚体制备阻尼材料，测试结果表明：特征粘度为54.5mpa.s时材料的阻尼性能良好。把制备的PMSQ代替部分PDMS为预聚体与PBMA制备成阻尼材料，测试表明：PMSQ加入5％时材料的阻尼性能优良，tgδ_(max)可达1.3。研究了甲基丙烯酸甲酯(MMA)、甲基丙烯酸丁酯(BMA)共聚物／聚硅氧烷IPN阻尼材料，实验证明，MMA的加入不利于提高材料在室温下的阻尼性能。
Hydroxy-terminated ladder-like polysiloxane was synthesized from ethylene diamine and monomethyltrichlorosilane by stepwise coupling polymerization. Meanwhile, hydroxy-terminated single-chain polysiloxane with different viscosity was also synthesized from octamethylcyclotetrasiloxane by alkali-catalyzed method.
After that, some following experiments were completed :
1. Hydroxy-terminated single-chain polysiloxane and active chlorine- contained end-capping reagent were used to synthesis polysiloxane which can be solidified under ultraviolet. The characteristic functional groups of end-capping reagent were proved by FTIR. Meanwhile, ultraviolet curing experiment was done when a certain photoinitiator was in existence, and the result showed that ethenyl-terminal polysiloxane could be solidified under ultraviolet.
2. High quality polymer damping material was synthesized by interpenetrating networks polymerization using polysiloxane and acrylate.
Some affected factors to damping property were studied, such as the compounding ratio of component, the quantity of crosslinking agent, and the ratio of single-chain to ladder-like polysiloxane. And the morphology of damping material was also observed by AFM. The damping property was measured by MTS and the result showed that when the optimal ratio of poly (n-butyl methacrylate) to polysiloxane was 80:20, the damping factor tg δ_(max) was 0.9. And then changing the quantity of crosslinking agent, the result showed that the damping factor tg δ_(max) was up to 1.4 when the ratio of crosslinking agent was 8%. Under the optimal ratio and quanlity of crosslinking agent, damping material was synthesized using different viscosity of polysiloxane as prepolymer. The result was that when the characteristic viscosity was 54.5mpas, the damping property was optimal. Using hydroxy-terminated ladder-like polysiloxane to replace some hydroxy-terminated single-chain polysiloxane, the result showed when the ratio
引文
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