紫外光固化环氧聚硅氧烷树脂的制备与性能
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TQ31

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国家自然科学基金项目(面上项目,重点项目,重大项目)


Preparation and properties of UV-curable epoxy-polysiloxane resins
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The National Natural Science Foundation of China (General Program, Key Program, Major Research Plan)

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    摘要:

    以1,2-环氧-9-癸烯和双侧氢封端的聚二甲基硅氧烷为反应物,在卡斯特催化剂〔铂(0)-1,3-二乙烯-1,1,3,3-四甲基二硅氧烷〕的催化下发生硅氢加成反应,成功制备了环氧基聚硅氧烷预聚物,并使用阳离子型光引发剂对其进行紫外光固化,制得紫外光固化环氧聚硅氧烷树脂。对合成双端环氧基聚硅氧烷预聚物的反应条件进行优化。利用FTIR和1HNMR对所合成预聚物的结构进行了结构表征,采用热失重分析、差示扫描量热法、接触角、耐碱性、耐醇性、凝胶率、邵氏A硬度和断裂面微观形貌对固化膜的性能和形貌进行了测试。结果表明:在反应温度为75 ℃、催化剂有效成分添加量为0.009‰(以双端含氢聚硅氧烷和1,2-环氧-9-癸烯的质量和为基准,下同)条件下,8 h时反应程度达93.95%;当使用光引发剂BL9380用量为3%(以预聚体质量为基准,下同)、固化时间为20 s时,制得的树脂表面活性能为18.4~18.8 mN/m,耐碱性、耐醇性良好,凝胶率为93.9%,邵氏A硬度为37,空气气氛下两个最大分解速率分别为437.6和511.3 ℃,780 ℃下质量残余率为13.9%,固化膜的综合性能最好。

    Abstract:

    Epoxy-siloxane prepolymer was synthesized through hydrosilylation between 1,2-epoxy-9-decene and hydrogen-terminated polydimethylsiloxane in the presence of a catalytic amount of Karstedt's catalyst [platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane], then cured with cationic light initiator under ultraviolet light to obtain UV-curable epoxy-polysiloxane resin. The reaction conditions for the synthesis of the prepolymer were optimized. The structure of the synthesized prepolymer was characterized by FTIR and 1HNMR. The properties and morphology of the cured film were tested by thermogravimetic analysis (TGA), differential scanning calorimetry (DSC), contact angle, alkali resistance and alcohol resistance, gel rate, Shore A hardness, and fracture surface morphology. The results showed that under the conditions of reaction temperature 75 ℃, reaction time 8 h, dosage of catalyst's active ingredient 0.009‰ (based on the total mass of hydrogen-terminated polydimethylsiloxane and 1,2-epoxy-9-decene, the same below), the reaction degree was 93.95%. When the dosage of photoinitiator BL9380 was 3% (based on the mass of the epoxy-siloxane prepolymer, the same below), and the curing time was 20 s, the cured resin had the best comprehensive performance. The surface activity energy was 18.4~18.8 mN/m, the gel rate was 93.9%, and exhibited dood alkali resistance and alcohol resistance with Shore A hardness of 37. The cured resins exhibited good thermal stability with corresponding temperatures of maximum decomposition rate of 437.6 and 511.3 ℃ in air, and 13.9% of residual weight ratio at 780 ℃.

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于昕仪,李小全,黄振祝,冯超,林树东,胡继文.紫外光固化环氧聚硅氧烷树脂的制备与性能[J].精细化工,2020,37(7):0

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  • 收稿日期:2020-01-16
  • 最后修改日期:2020-03-18
  • 录用日期:2020-03-20
  • 在线发布日期: 2020-04-13
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