精细化工氰化物原料替代技术及污染减排技术与示范

张光晋 闫瑞 王雪松 黄杰 吾满江

摘 要：该年度课题总体进展达到原任务书中规定的进度。替代有毒有害原料氢氰酸的MMA清洁生产技术方面，应用系统工程的原理与方法，确立催化反应过程的最优工艺技术参数；完成异丁烯选择氧化制备MMA的分离工艺设计及全流程的模拟，实现全系统能量-物质-环境的多目标优化和集成。提出优化的工艺流程，确定生产工艺与反应设备，并进行催化剂的公斤级生产及吨级放大生产、千吨级中试示范装置工程设计，提出千吨级工艺基础数据包，并完成了工程设计与装置建设。 替代剧毒铬酐氧化剂的16-DPA绿色工业制备技术方面，完成40吨/年16-DPA绿色生产示范线建设，并在示范线上优化了16-DPA光敏氧化绿色制备技术各项工艺参数，以薯蓣皂苷元计算，16-DPA总收率达到68%，纯度大于98%，实现预期年度目标。并在实验室尝试利用LED光源替代高压汞灯开展16-DPA的光敏氧化绿色制备，取得可喜进展。以季鏻盐类离子液体为催化剂的绝缘油清洁生产技术方面，目前已筛选出具有高催化剂和高稳定性的Lewis酸性季鏻盐类离子液体，并用于合成PEPE绝缘油。该离子液体催化剂可循环使用30余次而保持催化活性和选择性不变。同时建成了100吨/年的季鏻盐类离子液体生产线，为绝缘油PEPE的工业化催化剂来源提供了可靠来源。1 000吨/年的离子液体催化合成绝缘油PEPE生产装置已开工建设。

关键词：氢氰酸 铬 硫酸 清洁工艺 甲基丙烯酸甲酯 16-DPA PEPE

Abstract：The project runs well and reaches the main target of assignment book. In the first part， for the clean manufacture technology of MMA， the technology parameter in catalytic process was clarified by using theory of system engineering. The design of the separation technology in selection oxidation of isobutene and simulation of the full process were finished. The optimal technology process was proposed. The reaction facilities were defined. The production of the catalyst in kg scale was finished. The fundamental data pacage for technology in 1 000 t scale was provided. The design of the process and the construction of devices were finished. In the second part， for the green manufacture technology of 16-DPA， the construction of demonstration production line of 16-DPA in 40 T/year scale was finished. The manufacture parameters was optimized in the production line. The total yield of 16-DPA reached 68% and the purity reached 98%. In laboratory， we try to use LED as light sources to replace Hg lamp to produce 16-DPA， and the results are satisfied. In the third part， for the clean technology of insulating oil， the best ionic liquid was selected to synthesis of insulating oil. The ionic liquid can cycle for more than 30 times without changing of its activity. The production line for the ionic liquid in 100 T/year was constructed. And the catalysis synthesis of insulting oil PEPE in 1 000 T/year scale was began to constructed.

Key Words： Hydrocyanic acid； Chromium； Sulfuric acid； Clean process； Methyl methacrylate； 16-dehydropregnenolone acetate； Phenyl ethenyl ethane

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