第 43 卷第 2 期 Vol. 43 No. 2 2013 年 4 月 Apr 2013

所属栏目：农药及中间体 三光气法合成苯磺隆的工艺研究

崔玉杰1，2，姚日生1* （1. 合肥工业大学 医学工程学院，安徽 合肥 230009；2. 安徽安生生物化工科技有限公司，安徽 合肥 230001）

摘　要：对三光气法合成苯磺隆工艺进行了改进。通过对催化剂、三光气（BTC）用量及加料方式、温度4个因素的考察，结果表明：BTC用量远高于理论量值主要是由于BTC在高温下快速分解。由此，将原利用单级反应瓶的合成工艺改为两级串联合成工艺，把第一级反应瓶逸出的光气通入第二级反应瓶进行反应，使过量的光气得到了有效的利用。在n（邻甲酸甲酯苯磺酰胺）∶n（催化剂）=1∶1，2个反应瓶内邻甲酸甲酯苯磺酰胺等量，第一级反应瓶温度由110℃升至120℃，第二级反应瓶温度控制在130±5℃的工艺条件下，BTC耗量由原来理论量的253%降低至148%，收率由84.8 %提高至91.0 %。

关键词：苯磺隆；三光气；合成工艺

中图分类号：S482.4　　文献标识码：A　　文章编号：1009-9212（2013）02-0022-03

Study on the Synthesis of Tribenuron-methyl from Triphosgene

CUI Yu-jie1，2，YAO Ri-sheng1* （1. School of Medical Engineering，Hefei University of Technology，Hefei 230009，China；2. Anhui Ansheng Biochemical Science and Technology Co.，Ltd.，Hefei 230001，China）

Abstract：Synthesis of tribenuron-methyl from methyl 2-sulfamoylbenzoate （MeSAB）　and triphosgene　（BTC） was optimized. The effects of catalyst，reaction temperature，BTC amount and feeding method on the reaction yield were investigated. The results showed that the consumption of BTC was much higher than the theoretical value because of its rapid decomposition at high temperature. Thus，an improvement was made by dividing the MeSAB into two reactors in successional stage in stead of single-stage. The excess phosgene escaped from the first reactor was charged into the second reactor，so that the phosgene had been effectively utilized. Suitable conditions were as follows：the ratio of MeSAB to catalyst was 1 to 1，the loadings of MeSAB in two reactors were the same，the reaction temperature in first reactor was slowly increased to 120℃ and in the second was controlled at 130±5℃. Under these conditions，the BTC consumption was reduced to 148 % from 253% of the theory，and the yield increased from 84.8% to 91.0%.

Key words：tribenuron-methyl；triphosgene；synthesis process

作者简介：崔玉杰（1981-），男，内蒙古赤峰人，硕士研究生，研究方向：精细化工。（E-mail：cuiyj_co@126.com）

联 系 人：姚日生，教授，博士，研究方向：精细化工与制药工程。（E-mail：yaors@hfut.edu.cn）

收稿日期：2013-04-07