基于ATR-UV实时浓度检测的扑热息痛冷却结晶过程研究

doi:10.11949/j.issn.0438-1157.20150763

化工学报 ›› 2015, Vol. 66 ›› Issue (9): 3580-3587.DOI: 10.11949/j.issn.0438-1157.20150763

基于ATR-UV实时浓度检测的扑热息痛冷却结晶过程研究

关国强^1,2, 唐凯¹, 李红³, 卢帅涛¹, 江燕斌¹

1 华南理工大学化学与化工学院, 广东广州 510640;
2 传热强化与过程节能教育部重点实验室, 广东广州 510640;
3 广东肇庆星湖生物科技股份有限公司技术中心, 广东肇庆 526040

收稿日期:2015-06-01 修回日期:2015-06-22 出版日期:2015-09-05 发布日期:2015-09-05
通讯作者: 江燕斌
基金资助:
国家自然科学基金项目(21276091,91434126);教育部博士点基金项目(20120172110010)。

Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement

GUAN Guoqiang^1,2, TANG Kai¹, LI Hong³, LU Shuaitao¹, JIANG Yanbin¹

1 School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, Guangdong, China;
2 Key Laboratory of Enhanced Heat Transfer and Energy Conservation, Ministry of Education, South China University ofTechnology, Guangzhou 510640, Guangdong, China;
3 Star Lake Bioscience Co., Inc., Zhaoqing 526040, Guangdong, China

Received:2015-06-01 Revised:2015-06-22 Online:2015-09-05 Published:2015-09-05
Supported by:
supported by the National Natural Science Foundation of China (21276091, 91434126) and the Doctoral Fund of the Ministry of Education of China (20120172110010).

摘要/Abstract

摘要：

以无水乙醇-扑热息痛为模型物体系,对基于衰减全反射紫外光谱(ATR-UV)分析的结晶过程实时浓度检测进行了研究。采用偏最小二乘法进行结晶过程浓度关联,建立了ATR-UV实时浓度检测模型,该模型实时分析结果与重量法测量结果一致,均方根平均偏差为0.0075。通过ATR-UV实时浓度分析关联结晶过程的过饱和度变化,并结合聚焦光束反射测量技术分析了不同降温方式对结晶产品的影响。结果表明:相对于自然冷却和线性冷却温度控制方式,受控冷却过程能获得尺寸更大、分布更均一的晶体产品。

关键词: 扑热息痛, 结晶, 衰减全反射紫外光谱, 偏最小二乘法, 实时浓度, 粒度分布, 控制

Abstract:

Real-time concentration determination is critical in process analytical technology for advance quality control of crystallization. A novel approach is presented to correlate in-situ concentration of paracetamol in ethanol solution with the attenuated total reflection/ultraviolet (ATR-UV) spectrum by using the partial least squares method. The correlated concentrations are well consistent with the measurement of gravimetric method and the root-mean-square derivation is found to be 0.0075. Supersaturation correlation based on the developed ATR-UV in-situ concentration measurement, coupled with focused beam reflection measurement for monitoring the nucleation and growth during crystallization procedure, is utilized to investigate the effect of three cooling policies on cooling crystallization, i.e., natural cooling policy (NCP), linear cooling policy (LCP) and control cooling policy (CCP). The results show that the CCP has advantages over NCP and LCP in producing more crystals with the large and well-distributed crystal sizes.

Key words: paracetamol, crystallization, ATR-UV, partial least squares method, in-situ concentration, size distribution, control

中图分类号:

TQ420.6⁺1

关国强, 唐凯, 李红, 卢帅涛, 江燕斌. 基于ATR-UV实时浓度检测的扑热息痛冷却结晶过程研究[J]. 化工学报, 2015, 66(9): 3580-3587.

GUAN Guoqiang, TANG Kai, LI Hong, LU Shuaitao, JIANG Yanbin. Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement[J]. CIESC Journal, 2015, 66(9): 3580-3587.

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基于ATR-UV实时浓度检测的扑热息痛冷却结晶过程研究

Cooling crystallization of paracetamol in ethanol solution based on real-time ATR-UV measurement

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