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Study of Crystallization Process of D-p-Hydroxyphenylglycine

Author: LiTian
Tutor: QuYiXin
School: Beijing University of Chemical Technology
Course: Chemical Engineering and Technology
Keywords: Hydroxyphenylglycine Crystallization Solubility Hybrid model Vibration mode
CLC: TQ464.7
Type: Master's thesis
Year: 2011
Downloads: 88
Quote: 0
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Abstract


Hydroxyphenylglycine (DL-p-HPG) is an important pharmaceutical intermediates. D-hydroxyphenylglycine (Dp-HPG) is an important raw material for synthetic broad-spectrum antibiotic amoxicillin, cephalosporins cefadroxil, etc.. L-hydroxyphenylglycine (Lp-HPG) is the raw material for the treatment of heart drugs hydroxyphenylglycine. Dp-HPG obtained by enzymatic synthesis, the very low concentrations, in order to get a better product, the crystallization process of the Dp-HPG study. Including cell parameters of the crystal molecular configuration with nature, crystal thermodynamics, solid-liquid phase equilibria of binary mixed solvent, crystallization process. Determined by X-ray powder diffraction pattern of the Dp-HPG, the cell parameters to utilize JADE5.0 software analysis. Quantitative calculations, select the appropriate calculation method and basis set to optimize the geometry of the Dp-HPG calculate optimized molecular vibration frequency and bond length, and the calculated values ??are compared with the experimental values, found two good agreement, its resolving agent provides a theoretical basis. Crystallization thermodynamics is a basic research of the crystallization process. Lp-HPG solubility in ethanol, ethylene glycol, DMF, dimethylsulfoxide and water was measured by a laser method, and the data were fitted using Apelblat equation, the experimental and calculated values ??coincide. The laser method of cooling rate the 1K/10min.2K/10min and 3K/10min when, Dp-HPG in water metastable zone. Above data provides theoretical support for the crystallization process development, and optimization of the crystallization process of guiding significance. D - p-HPG and Lp-HPG solubility in water - ethanol mixtures based on crystallization thermodynamics. Both associated with temperature and solvent composition based on generalized solubility model and (CNIBS) / Redlich-Kister model two hybrid model. According to a p-value of the regression parameters obtained deleted entries, and thus not significantly simplified model. Further, in order without affecting the model accuracy under the premise of reducing the number of decimal digits of the parameter values, using the discrete planning methods to optimize the parameter values, the resulting model is not only simple, but also provide a solution for optimizing the model parameter values ??of other thermodynamic ideas. The models were tested by statistical standards, found that the hybrid model can well describe Dp-HPG and Lp-HPG solubility in water - ethanol mixed solution. Finally, to study the crystallization process of the Dp-HPG, by examining the evaporation rate, stirring speed, cooling rate, the amount of water crystallization end temperature on product yield, purity and particle size distribution to determine the better crystallization process operating parameters.

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CLC: > Industrial Technology > Chemical Industry > Pharmaceutical chemical industry > Drug production of biological products > Amino acids,peptides,proteins
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