摘要
以2,4-二胺基甲苯(TDA)和二甲基二硫为原料,以卤化亚铜配合物为催化剂,制备二甲硫基2,4-二胺基甲苯(DMTDA)。考察了工艺参数对制备DMTDA的收率和选择性的影响,适宜的工艺条件是:在常压下反应温度为150°C,反应时间为6h,催化剂与TDA的摩尔比为0.05。由实验还可知配位催化剂失活是由于二甲基二硫与催化剂中的部分配体发生了反应,催化剂配体的流失是催化剂活性降低的主要原因。
Activity of a copper-halogen coordination catalyst used to prepare dimethyl-(thioltoluenediamine)(DMTDA) is estimated. This paper describes the inactivity reasons of complex catalyst and factors affecting the alkylthiolation of toluenediamine. When the agitator speeds is higher and catalyst grains are finer, catalysis powder particles are suspended in the mixture with a state of pseudo-homogenous suspension, the mass-transfer resistances at the outer surface of the catalyst and inside the catalyst are considered to be negligible, on the condition of which the alkylthiolation of toluenediamine is considered to be carried out in pseudo-homogenous system. Higher yield and selectivity of DMTDA are reached when the reaction temperature is 150 (°C), the mole ratio of catalyst to TDA is 0.05 and reaction time is about 6 h under the atmosphere. The experiment results show that loss of coordination from coordination catalyst results from the inactivity of catalysts.
出处
《华东理工大学学报（自然科学版）》
CAS
CSCD
北大核心
2004年第3期241-244,共4页
Journal of East China University of Science and Technology
关键词
二胺基甲苯
二甲基二硫
配位催化剂
选择性
toluenediamine
dimethyl disulfide
coordination catalyst
selectivity
