首页|2-吡啶甲酸铬的工艺改进

2-吡啶甲酸铬的工艺改进

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以2-氰基吡啶为原料,经水解、中和、络合反应得到2-吡啶甲酸铬.通过对反应溶剂、络合pH值、络合温度进行改进,解决了2-吡啶甲酸铬晶体细小、流动性差等问题.水解反应使用乙醇溶解2-氰基吡啶,加入NaOH水溶液进行水解,使反应在均相中进行,反应时间由10 h缩短为1.5h.水解完毕调节pH值为8.9,易于络合反应的进行.络合温度控制在(50±2)℃,利于晶体的增长.按此工艺制得的2-吡啶甲酸铬纯度为99.8%,单杂0.04%,总杂0.12%,晶体颗粒均匀,流动性好,休止角为31°,更易于制剂过程中混合均匀.
Technology improvement of chromium 2-picolinate
With 2-cyanopyridine as raw material,through hydrolysis,neutralization and complexation reaction,chromium 2-picolinate is prepared.By improving the reaction solvent,the complexation pH and the complexation temperature,some problems of chromium 2-picolinate are solved,for example the crystal size is too small and the fluidity is poor.After 2-cyanopyridine is dissolved in ethanol,sodium hydroxide aqueous solution is added,and the hydrolysis reaction happens in homogeneous phase,and the reaction time is reduced from 10 h to 1.5 h.The pH value is adjusted to 8.9 after the hydrolysis reaction,which makes complexation reaction occur easily.Complexation temperature is set to(50±2)℃,which is in favor of crystal growing bigger.The purity of chromium 2-picolinate prepared by this method is 99.8%,the max impurity is 0.04%,the total impurity is 0.12%,the crystal particles are uniform,the fluidity is good,the angle of repose is 31°,and the method makes it easy to mix uniformly in the process of pharmaceutic preparation.

organic synthesis chemistrychromium 2-picolinatetechnology improvementfluidityangle of repose

张向彬、高金亮、郭永斌、鲁会杰、郑兰星、葛雅坤

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河北富格药业有限公司,河北石家庄 050700

有机合成化学 2-吡啶甲酸铬 工艺改进 流动性 休止角

2015

河北工业科技
河北科技大学

河北工业科技

CSTPCD
影响因子:0.694
ISSN:1008-1534
年,卷(期):2015.32(6)
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