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叶酸结晶基础数据测定与结晶过程研究
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摘要
叶酸是一种重要的维生素。市场需求量不断上涨,但其生产过程中三废多,产品质量不高,技术落后等问题困扰着叶酸的生产。结晶作为叶酸生产的最后一步精制过程,是保证产品质量的关键环节。因此叶酸结晶过程基础数据和工艺的研究对实际生产具有重要意义。
     晶习对产品下游处理(比如过滤、洗涤和干燥)以及最终产品的质量影响很大,是晶体产品质量考察的一个重要指标。本文应用显微镜观察晶体的晶习,并由结晶方法对叶酸晶习的影响进行实验研究,选用碱结晶路线制备晶形完整的叶状晶体产品。
     结晶热力学是决定结晶收率与操作方案的基本依据。本文测定了纯水中不同温度下叶酸溶解度数据,并观察盐类对溶解度的影响。同时用静态法与激光法测定不同pH下水溶液中不同温度下叶酸溶解度与超溶解度,并对介稳区数据进行曲线拟合。实验还测定了叶酸溶液如粘度、密度、电离平衡常数.、诱导期等基础物性常数,为结晶过程设计提供基本参数和依据。根据一次成核理论利用诱导期数据估算了叶酸的表面张力和表面熵因子数据,进而推断叶酸晶体生长模式为连续生长模式。
     以质量(晶形、CSD)和收率为目标,本文较系统地考察了盐酸浓度、反应结晶温度、初始浓度、过滤等操作条件对结晶过程的影响,从而确定优化操作条件。
Folate (folic acid) is an important basic vitamin, whose demand is rising. But more waste, poor product quality, technical backwardness and other problems hinder folic acid production.Crystallization as the final step in the production of folic acid refining process, is a key step to ensure product quality. The data and process of folic acid crystallization were studied in this paper.
     Crystal habit is an important issue in crystal quality, because it has main impact on the downstream processings(such as filtering, washing and drying) and the quality of the final product. The crystal habit were observed under microscope. And the effects of the crystal methods on crystal habit were studied. Alkali recrystallization method is selected to get ideal leafy crystal products.
     Crystallization thermodynamics is the fundamental basis for operating and determining the yield of crystallization. The solubilities of folic acid at different temperatures in pure water were measured and researched the impact of salts on them. Then the solubilities and supersolubilities of folic acid in different pH aqueous solutions at different temperatures were studied by the static method and the laser method. The fitting curves of the metastable zone data is established. Other basic physical constants of folic acid are also measured such as viscosity, density, and dissociation constants, which are the basis data for crystallizer design. According to the nucleation theory using the induction period data to estimate the surface tension and surface entropy factor data, inferred that folic acid crystal growth model was continuous growth mode. According to the nucleation theory, the interfacial tension and entropy factor were estimated by the induction period data, and then inferred folic acid crystal growth model was continuous growth mechanism.
     The operating conditions, including acid addition rate, acid concentration, crystallization temperature, initial concentration, and filtration, were optimized by examing the quality (crystal form, CSD) and yield goals.
引文
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