抗黄变双(乙酰乙酸乙酯)钛酸二异丁酯的研制  

Preparation of Anti-Yellowing Diisobutoxy-bisethylacetoacetatotitanate

作　　者：冯琼华 向冲 王成 肖俊平 FENG Qionghua;XIANG Chong;WANG Cheng;XIAO Junping(Hubei Bluesky New Materials Inc.,Xiantao 433000,Hubei)

机构地区：[1]湖北新蓝天新材料股份有限公司,湖北仙桃433000

出　　处：《有机硅材料》2022年第6期25-29,共5页Silicone Material

摘　　要：以钛酸四异丁酯和乙酰乙酸乙酯或钛酸四异丙酯、乙酰乙酸乙酯和异丁醇为原料,合成抗黄变双(乙酰乙酸乙酯)钛酸二异丁酯,并将其作为催化剂制备脱醇型室温硫化硅橡胶。对比了两种合成双(乙酰乙酸乙酯)钛酸二异丁酯路径的差异,研究了投料比、投料顺序、蒸馏温度等对产物钛含量和颜色的影响,并测试了硅橡胶性能。结果表明,以钛酸四异丁酯和乙酰乙酸乙酯为原料直接合成双(乙酰乙酸乙酯)钛酸二异丁酯的路线具备可行性,且钛酸四异丁酯与乙酰乙酸乙酯物质的量之比控制在1∶(2~2.2)时,既可提高转化率,又能使产物钛含量更接近于理论值。而以钛酸四异丙酯、乙酰乙酸乙酯和异丁醇为原料时,仅在投料顺序为钛酸四异丙酯先与乙酰乙酸乙酯反应,再与过量异丁醇反应才能制得产物,但产物钛含量偏低。相比于采用常规的双(乙酰乙酸乙酯)钛酸二异丙酯,采用双(乙酰乙酸乙酯)钛酸二异丁酯作催化剂制得的硅橡胶贮存性能良好、生产更易控制,且在70℃老化8 d后,胶条基本无黄变。Anti-yellowing diisobutoxy-bisethylacetoacetatotitanate was synthesized from tetraisobutyl titanate and ethyl acetoacetate or tetraisopropyl titanate,ethyl acetoacetate and isobutanol.The dealcoholized RTV silicone rubber was prepared by using it as catalyst.The differences between the two synthetic routes of diisobutoxy-bisethylacetoacetatotitanate were compared,and the effects of feeding ratio,feeding sequence and distillation temperature on the titanium content and color of the product were studied,and the properties of silicone rubber were tested.The results show that the direct synthesis route is feasible with tetraisobutyl titanate and ethyl acetoacetate as raw materials,and the molar feeding ratio controlled at tetraisobutyl titanate∶ethyl acetoacetate=1∶(2-2.2)can not only improve the conversion rate,but also make the product titanium content closer to the theoretical value.Using tetraisopropyl titanate,ethyl acetoacetate and isobutanol as raw materials,the product can be obtained only when the feeding order is that tetraisopropyl titanate first reacts with ethyl acetoacetate and then reacts with excess isobutanol,and the titanium content of the product is relatively low.Compared with the conventional diisobutoxy-bisethylacetoacetatotitanate,the silicone rubber prepared by diisobutoxy-bisethylacetoacetatotitanate as the catalyst has good storage performance,easier controlled production,and after aging at 70℃for 8 d,the adhesive strip had no yellowing.

关 键 词：抗黄变 钛酸四异丁酯 乙酰乙酸乙酯 硅橡胶 

分 类 号：TQ433.438[化学工程]