摘要
对氯乙酸氨解法合成甘氨酸工艺进行了改进和优化。试验分为2步进行,先在氯乙酸的甲醇溶液中通入氨气,反应制取氯乙酸铵;再在氯乙酸铵的甲醇溶液中加入适量催化剂乌洛托品,在适宜条件下通氨反应,得到产品甘氨酸。试验考察了第二步反应中的主要影响因素,优化条件为通氨时间120 min,反应温度60℃,n(氯乙酸铵)∶n(甲醇)=1∶7.5,保温时间为45 min。在母液套用条件下,第二步反应的单步收率可达99.35%,经2步合成后甘氨酸收率可达97.72%。
The synthesis technology of glycin by using ammonolysis method of chloroacetic acid were impreved and optimized. Glycin was synthesized through a two-step process. At first, ammonium monochloreacetate was prepared through pumping ammonia gas in methanol liquor of chloroacetic acid. Then appropriate amount of urotrepine was added as the catalyst and the product glycin was obtained from through pumping ammonia gas under suitable conditions. The main factors affecting the yield of the second step were investigated. Based on the experimental results, the optimal reaction conditions were as follows: ammonization time of 120 min, reaction temperature of 60 ℃ n(ammonium menochloroacetic acid) : n(methanol) = 1:7.5, holding time of 45 min. Under these conditions of mother liquor, the yield of the second step was up to 99.35%. After these two steps, the yield of glycin could reach 97.72%.
出处
《安徽农业科学》
CAS
北大核心
2009年第13期5828-5829,5837,共3页
Journal of Anhui Agricultural Sciences
关键词
甘氨酸
氯乙酸氨解法
母液回用
工艺优化
Glycine
Ammonolysis method of chloroactic acid
Mother liquor reclamation
Technology optimization