| 第 43 卷第 2 期 |  | Vol. 43 No. 2 | | 2013 年 4 月 | Apr 2013 |
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所屬欄目：農藥及中間體
三光氣法合成苯磺隆的工藝研究 |
| 崔玉杰1，2，姚日生1*
（1. 合肥工業(yè)大學(xué) 醫學(xué)工程學(xué)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：對三光氣法合成苯磺隆工藝進(jìn)行了改進(jìn)。通過(guò)對催化劑、三光氣（BTC）用量及加料方式、溫度4個(gè)因素的考察，結果表明：BTC用量遠高于理論量值主要是由于BTC在高溫下快速分解。由此，將原利用單級反應瓶的合成工藝改為兩級串聯(lián)合成工藝，把第一級反應瓶逸出的光氣通入第二級反應瓶進(jìn)行反應，使過(guò)量的光氣得到了有效的利用。在n（鄰甲酸甲酯苯磺酰胺）∶n（催化劑）=1∶1，2個(gè)反應瓶?jì)揉徏姿峒柞ケ交酋０返攘�，第一級反應瓶溫度�?10℃升至120℃，第二級反應瓶溫度控制在130±5℃的工藝條件下，BTC耗量由原來(lái)理論量的253%降低至148%，收率由84.8 %提高至91.0 %。 |
| 關(guān)鍵詞：苯磺��；三光氣；合成工藝 |
| 中圖分類(lèi)號：S482.4 文獻標識碼：A 文章編號：1009-9212（2013）02-0022-03 |
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| 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�。˙TC） 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 |
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作者簡(jiǎn)介：崔玉杰（1981-），男，內蒙古赤峰人，碩士研究生，研究方向：精細化工。（E-mail：cuiyj_co@126.com）
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聯(lián) 系 人：姚日生，教授，博士，研究方向：精細化工與制藥工程。（E-mail：yaors@hfut.edu.cn）
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收稿日期：2013-04-07
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