钛硅复合氧化物催化合成长链二元腈

以四氯化钛和硅酸乙酯为原料,制备了复合氧化物催化剂TiO2-SiO2(TSO),应用于催化十三碳二元酸氨化反应制得十三碳二元腈。按正交实验设计方法考察了催化剂组成、催化剂用量、温度、反应时间、搅拌速度及氨气流量对反应的影响。结果表明,最佳反应条件为:钛硅原子个数比3∶1,采用程序升温方式(280℃2 h,300℃3 h,320℃1 h),催化剂用量为酸质量的10%,搅拌速度1000 r/min,氨气流量120 L/h。最佳反应条件下制备的产物十三碳二腈的质量分数达96.70%,收率达86.28%。用TLC、IR、GC-MS检测产物的纯度和结构,并合成了一系列长链二元腈。

Synthesis of long-chain dicarboxylic acid dinitrile catalyze by composite TiO2-SiO2

Composite catalyst TiO2-SiO2(TSO) was prepared from TiCl4 and Si(OC2H5)4.And it was used in the synthesis of long-chain dicarboxylic acid dinitrile with ammonia and tridecane dicarboxylic acid as reactants.Effects of the catalyst composition and dosage,reaction temperature and time,stirring rate and ammonia flux were investigated.The choice of reaction conditions was based on orthogonal experimental design.The optimal recation conditions were:n(Ti) ∶n(Si)=3 ∶1,the amount of catalyst is 10%(weight percent of the acid),stirring rate is 1 000 r/min,ammonia flow rate is 120 L/h,at the programme temperature control(280 ℃ 2 h,300 ℃ 3 h,320 ℃ 1 h).The yield of product was 86.28% with purity of 96.70%.The purity and structure of the product were analysed by TLC,IR and GC-MS.And then a series of long-chain dicarboxylic acid dinitrile were synthesizes in the same reaction conditions successfully.