三光气法碳酸二苯酯合成及工程放大的分析研究.pdfVIP

三光气法碳酸二苯酯合成与工程放大研究 摘 要 碳酸二苯酯是一种重要的化工产品，可用来合成许多重要的医药、农 药及其它有机化合物。目前国内外合成 DPC 的方法主要有：光气法、苯 酚氧化羰化法、酯交换法和三光气法。三光气与气体光气相比，使用安全， 与环境友好。本论文从实验室里对催化剂的加入时间、溶剂的选择、混料 方式、及产品提纯对产品的质量及收率做了大量研究，总结出选用二氯甲 烷做为溶剂、在加料初期加入催化剂、通过选用向苯酚水悬浮体中同步滴 加 BTC 二氯甲烷溶液和 30 ％NaOH 水溶液的加料方式、加强搅拌及控制 釜温不超过 30 ℃，可使产品的收率高达 98.5%( 以苯酚计) 比较合理的小试 工艺。在小试研究的基础上，通过物料、热量衡算，及通过反应器的冷模 试验，再结合工程放大的相关知识，对年产 500 吨/ 年的 DPC 进行中试工 艺设计。通过试生产检验中试设计效果，对不合理的地方进一步完善，使 中试装置在试生产中产品质量基本满足 PC 生产要求，产品收率高达（以 苯酚计）98.38% ，（以BTC 计）98.36% 。 关键词: 碳酸二苯酯；三光气；中试；工艺设计；试生产 III The Study of Technology and Engineering Scale-up for Synthesis of Diphenyl Carbonate from Triphosgene Abstract Diphenyl Carbonate is an important chemicals, it can be used to synthesize many important pharmaceuticals, pesticides and other organic compounds. Bis(trichlormethyl)carbonate compared with phosgene gas is more safety and environment-friendly. In this work, the time of adding the catalyst, solvent choice, mixing methods, and product purification and the yield on the quality of the product were investigated in the laboratory. The optimized conditions were: methylene chloride used as the solvent, adding the catalyst in the early feeding,the feeding method is through the use of water to phenol in the suspension simultaneously dropping BTC 30% NaOH solution, enhance mixing and control of reactor temperature does not exceed 30 ℃. The yield of product can be as high as 98.5% (in terms of phenol )and it is more reasonable scale craft. On the basis of the small trial, through the materials, energy accounting, and by reactive device cold model experiments, combined with engineeri