乙醇酸合成工艺的研究论文.pdf

分类号: 密级: U D C: 编号: 河北工业大学硕士学位论文乙醇酸的合成工艺研究论文作者: 高雪莉学生类别:全日制学科门类: 工学学科专业:化学工艺指导教师: 刘雁职称:副教授万方数据 Dissertation Submitted to Hebei University of Technology for The Master Degree of Applied Chemistry STUDY ON THE SYNTHESIS OFTHE GLYCOLIC ACID by Gao Xueli Supervisor: Prof. Liu Yan April2014 万方数据万方数据河北工业大学硕士学位论文 I 摘要乙醇酸是一种重要的有机合成中间体和化工产品,广泛的应用于有机合成、化学清洗、电镀、纺织、皮革、灭菌等领域,因此,对乙醇酸的合成工艺研究具有深远意义。本文综述了乙醇酸的合成方法,通过理论分析与研究,选定了氯乙酸水解法和甲醛羰基化法两种合成路线。氯乙酸水解法以氯乙酸为原料在碱性条件下水解制得乙醇酸;甲醛羰基化法以多聚甲醛和一氧化碳为原料,以浓硫酸为反应介质,氧化亚铜为催化剂,经高压反应制得乙醇酸。研究结果表明:由氯乙酸水解法制备乙醇酸,反应温度为100℃,氯乙酸与氢氧化钠的摩尔比为1:,滴加的氢氧化钠的质量分数为45%,反应7小时,收率为93%, %;由多聚甲醛羰基化制备乙醇酸,,反应温度60℃,:1,多聚甲醛与氧化亚铜的摩尔比为50:1,反应时间为 3h,搅拌转速为150r/min,%。对乙醇酸稀溶液进行精制,实验得出最佳条件为:在真空度为20mmHg下进行减压蒸馏脱除水份,控制塔釜温度为80℃时停止蒸馏,得到质量分数约为70%的乙醇酸浓溶液。对乙醇酸浓溶液进行结晶,实验得出最佳条件为:℃/min,搅拌转速为60r/min,晶种的加入温度为30℃,得到的乙醇酸晶体在真空度为20mmHg %以上的乙醇酸晶体,收率为85%,熔点: ~℃。关键字:氯乙酸,多聚甲醛,一氧化碳,乙醇酸,结晶,Koch反应万方数据乙醇酸的合成工艺研究 II ABSTRACT Glycolic is a kind of important intermediates in organic synthesis and chemical products. It is widely used anic synthesis, chemical cleaning, electroplating, textile, leather, sterilization and other fields. This paper reviews the preparation of the glycolic acid. Analyze the correlated literature and design the route of the hydrolysis of chloroacetic acid and the carbonylation of formaldehyde. The hydrolysis of chloroacetic acid with chloroacetic acid as raw materials in alkaline water solution of glycolic acid; formaldehyde carbonylation with prarformaldehyde and carbon monoxide as raw materials, concentrated sulfuric acid as reaction medium, cuprous oxide as catalyst under the condition of high pressure, then obtained glycolic acid. The results show thatwith the method of chloroacetic acid to prepare glycolic acid, thereaction temperature is 100 ℃, the molar ratio of chloroacetic acid to sodium hydroxide is 1:1