对甲氧基苯基硫脲的合成工艺.pdfVIP

学兔兔 化 工 进 展 ·3l10· CHEMICAL INDUSTRY AND ENGINEERING PROGRESS 2015年第34卷第8期 对甲氧基苯基硫脲的合成工艺 陶红玲，张新慧，钱阳，丁浩，陈天云 (合肥工业大学化学与化工学院，安徽 合肥 230009) 摘要：以对氨基苯甲醚、硫氰酸铵为原料在酸催化下制备了对甲氧基苯基硫脲，通过单因素实验方法研究了反 应原料的配比、反应时间及反应温度等工艺参数对合成对甲氧基苯基硫脲收率的影响，获得的较佳合成工艺条 件为：对氨基苯甲醚5．7g，硫氰酸铵3．1g，盐酸3．3mL，水量8mL，反应温度90~C，反应时间为9h。平行放大 实验结果表明，产品的收率大于95％，产品的纯度为99．4％，红外光谱和核磁共振谱测试的结果表明所合成的化 合物为对甲氧基苯基硫脲。该合成技术工艺过程简单，生产安全，环境友好，产品收率高，易于生产。 关键词：对甲氧基苯硫脲；对氨基苯甲醚；硫氰酸铵 中图分类号：TQ 224．7 文献标志码：A 文章编号：1000—6613(2015)08—3110—04 DoI：10．160858．issn．1000．6613．2015．08．032 Synthetic process of 1一(4·meth0xypheny1)thi0urea TAOHongling，ZHANGXinhui，QIANYang，DINGHao，CHENTianyun (School ofChemistry and Chemical Engineering，Hefei University ofTechnology，Hefei 230009，Anhui，China) Abstract：I—r4一methoxypheny1)thiourea was effectively prepared from P—anisidine and ammonium thiocyanate with acidic catalyst． The effects of technical parameters on the yield of 1一r4-methoxypheny1)thiourea were studied through single—factor experimental method，such as raw materials ratio，reaction time and reaction temperature，etc．The optimal condition was P—anisidine 5．7g，ammonium thiocyanat 3．1 g，hydrochloric acid 3．3mL，water 8mL，reaction temperature 90~C， and reaction time 9h．The results of larger scale experiments proved that the average yield was 95％ and the pureness was 99．4％．The FTIR and NMR spectrum suggest that the synthetic compounds was l—r4一methoxypheny1)thiourea．The process of this synthesis technology was facile，safe，environment friendly with high product yield and easy production．