Zn(OAc)2·2H2O热处理对2,4-甲苯二氨基甲酸甲酯合成的影响  

Effect of thermal treatment of Zn(OAc)·2HO on the synthesis of 2,4-toluene dicarbamate

作　　者：张嘉振 马雪晴[1] 王桂荣[1,2] 王延吉 ZHANG Jiazhen;MA Xueqing;WANG Guirong;WANG Yanji(College of Chemical Engineering,Hebei University of Technology,Tianjin 300130,China;Key Laboratory of Green Chemicals and Energy-Efficient Hebei Province,Tianjin 300130,China)

机构地区：[1]河北工业大学化工学院,天津300130 [2]绿色化工与高效节能河北省重点实验室,天津300130

出　　处：《精细化工》2020年第10期2154-2160,共7页Fine Chemicals

基　　金：国家自然科学基金(21236001,21776057)。

摘　　要：借助TG、FTIR和XRD表征分析了Zn(OAc)2·2H2O在热处理过程中组成的变化。Zn(OAc)2·2H2O在100℃热处理8 h内仅发生脱水反应;在120℃热处理4 h,产物中有Zn4O(OAc)6生成,并且其相对含量随热处理时间的延长而增加;在160℃热处理6h时有ZnO生成,延长至12h后产物大部分为ZnO。将Zn(OAc)2·2H2O在不同热处理条件下得到的产物用于催化合成2,4-甲苯二氨基甲酸甲酯(2,4-TDC)。当反应温度为160℃时,Zn(OAc)2·2H2O在100℃热处理8 h后催化合成2,4-TDC的收率达到88.1%,说明该反应温度下Zn(OAc)2的催化活性较高;当反应温度为180℃时,Zn(OAc)2·2H2O在140℃热处理8h后催化合成2,4-TDC的收率达到92.8%,说明该反应温度下Zn4O(OAc)6拥有更高的催化活性。The composition changes of Zn(OAc)2·2H2O during thermal treatment were characterized and analyzed by TG,FTIR and XRD.Only dehydration reaction occurred after heat treatment of Zn(OAc)2·2H2O at 100℃for 8 h.After thermal treatment of Zn(OAc)2·2H2O at 120℃for 4 h,Zn4O(OAc)6 was formed in the product and its relative content increased with the increase of thermal treatment time.ZnO was formed after thermal treatment of Zn(OAc)2·2H2O at 160℃for 6 h,and most of the products were ZnO after thermal treatment at 160℃12 h.The products of Zn(OAc)2·2H2O under different thermal treatment conditions were used as catalysts for the synthesis of 2,4-toluene dicarbamate(2,4-TDC).At 160℃,the yield of 2,4-TDC catalyzed by the product after thermal treatment of Zn(OAc)2·2H2O at 100℃for 8 h reached 88.1%,indicating that the catalytic activity of Zn(OAc)2 was higher at 160℃.When the reaction temperature reached 180℃,the yield of 2,4-TDC catalyzed by the product after thermal treatment of of Zn(OAc)2·2H2O at 140℃for 8 h was up to 92.8%,which shows that Zn4O(OAc)6 had a higher catalytic activity at 180℃.

关 键 词：乙酸锌 热处理 2 4-甲苯二氨基甲酸甲酯 催化活性 

分 类 号：TQ225.2[化学工程—有机化工]