200720515059张光辉L-异亮氨酸结晶工艺研究.docVIP

二 〇 一 一 年 六 月 摘 要 L-异亮氨酸是人体必需的八种氨基酸之一，它在医药、食品和饲料行业具有非常重要的作用。目前，国内药用产品普遍存在着质量问题，如结晶产品粒度小、晶形差等问题。 本次实验对L-异亮氨酸结晶工艺进行了初步的研究。本次实验分别采用了冷却结晶法、真空蒸发结晶法、溶析结晶法。并分别考察了降温速率、搅拌速率、乙醇的滴加速率、养晶时间的长短对晶体产品质量的影响。 分析所得结晶产品的粒度分布及晶形，并结合重结晶收率，最终确定了制备L实验分别采用冷却法、溶析法、真空蒸发结晶法对L-苏氨酸进行重结晶。且利用检测显微-异亮氨酸产品的最优方法为冷却-溶析结晶方法。并且对L-异亮氨酸冷却-溶析结晶过程进行了实验优化，考察了各操作参数（乙醇滴加速率，降温速率，搅拌速率等）对结晶过程或最终产品粒度分布和晶体质量的影响，并确定了最优的结晶工艺操作参数为：降温速度率0.5℃，乙醇滴加速率为0.05ml/min，搅拌速率为200r/min，陈化时间为60min。 关键词：L-异亮氨酸； 粒度； 冷却-溶析结晶 Abstract L-isoleucine is one of the eight necessary amino acids to human beings. It has great importance in medication, food and forage industry. At present, there was a substantially increasing demand for L-isoleucine in pharmaceutical grade at the present time, but production status of L-isoleucine can not meet the needs of the domestic market. There are some problems about local L-isoleucine products for medicine, such as small crystal size and bad morphology. The experiments were conducted to select proper crystallization process from comparisons among the crystallization efficiency for L-isoleucine. The influence factors in L-isoleucine crystallization process were studied, in order to determine operating conditions. L-isoleucine was recrystallized by solvating out cooling, dissolve chromatography and vacuum evaporation crystallization method. Particle size and morphology were observed under electronic microscope, and the yield of the recrystallization was investigated. The crystallization process of solvating-out and cooling was determined. And the experiment process of L-isoleucine cooling - dissolve the crystallization was optimized. The effects of operational parameters such as agitation intensity, seed and adding rate of ethanol etc. on the CSD, yield and morphology were investigated systematically by experiment. The experimental optimum operational conditions for the crystallization of L-isoleucine were finally obtained, adding rate of ethanol at 0.05 mL/min, cooling rate at 0.5 ℃/min,