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工业级丙二醇精制成医药级丙二醇的研究
Research on process for refining industrial grade 1,2-propanediol to pharmaceutical grade product
【摘要】 酯交换法生产碳酸二甲酯工艺中副产的1,2-丙二醇含有微量杂质并具有刺激性气味,达不到医药级标准。为了获得合格的医药级1,2-丙二醇,利用精馏实验筛选添加剂,确定80%水合肼为最佳添加剂,并从添加剂添加量、反应温度、反应时间、去离子水添加量和回流比这5个方面优化提纯脱味工艺。为获得品质更好的1,2-丙二醇,采用椰壳活性炭对原料进行前处理。结果表明,当实验条件为4%活性炭前处理、80%水合肼用量20 mg/L、反应温度70℃、反应时间60 min、去离子水添加量20%、绝对压力8 kPa、除水回流比1/3、精制回流比为1~3时,得到的1,2-丙二醇产品符合医药级标准,并且品质较高,在220、275 nm和350 nm处的紫外透光率分别为66.6%、94.5%和99.8%。
【Abstract】 Industrial grade 1,2-propanediol(PDO) product produced via the transesterification method contains trace impurities and exhibits an irritating odor, failing to meet pharmaceutical grade standard.In order to obtain qualified pharmaceutical grade PDO,this study employs rectification experiments to select various additives, and screen out 80% hydrazine hydrate as the optimal additive.The refining deodorization process is optimized across five parameters, including additive dosage, reaction temperature, reaction time, deionized water dosage, and reflux ratio.To obtain higher quality of PDO,the raw material(industrial grade PDO) is pre-treated by coconut shell-based activated carbon.The optimized conditions are obtained as follows: the industrial grade PDO is pre-treated by 4% activated carbon, the dosage of 80% hydrazine hydrate is 20 mg/L,reaction temperature is 70℃,reaction duration is 60 min, the dosage of deionized water is 20%,absolute pressure is 8 kPa, dehydration reflux ratio is 1/3,and purification reflux ratio ranging from 1 to 3.Under these conditions, the resulting PDO product meets pharmaceutical grade specifications with superior quality, its UV transmittance values at 220 nm, 275 nm, and 350 nm reach 66.6%,94.5%,and 99.8%,respectively.
【Key words】 transesterification method; 1,2-propanediol; additive; activated carbon; pharmaceutical grade;
- 【文献出处】 现代化工 ,Modern Chemical Industry , 编辑部邮箱 ,2025年S2期
- 【分类号】TQ223.162
- 【下载频次】11