Application of attenuated total reflectance-Fourier transform infrared (ATR-FTIR) technique in the monitoring and control of anti-solvent crystallization

被引：54

作者：

Yu, ZQ

Chow, PS

Tan, RBH

机构：

[1] Natl Univ Singapore, Dept Chem & Biomol Engn, Singapore 119260, Singapore

[2] Inst Chem & Engn Sci Ltd, Singapore 627833, Singapore

来源：

INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH | 2006年 / 45卷 / 01期

关键词：

D O I：

10.1021/ie050660i

中图分类号：

TQ [化学工业];

学科分类号：

0817 ;

摘要：

On-line attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy and focused-beam reflectance measurement (FBRM) were used to monitor and control anti-solvent crystallization of paracetamol from an acetone-water mixture, which was conducted isothermally in a 1-L crystallizer with a flat bottom. After analyzing the particle size distribution (PSD) and transient relative supersaturation data from constant anti-solvent addition rate experiments, a simple calculation method for the set point of anti-solvent addition rate, to maintain constant supersaturation via ATR-FTIR, was developed and implemented for feedback control of unseeded and seeded crystallization. The results of the controlled feeding rate experiments show that the particle size and PSD, as well as the total batch time, can be favorably manipulated simultaneously.

引用

页码：438 / 444

页数：7

共 28 条

[1]

Barrett P, 1999, PART PART SYST CHAR, V16, P207, DOI 10.1002/(SICI)1521-4117(199910)16:5<207::AID-PPSC207>3.0.CO

[2]

2-U

[3] Examination of the semi-batch crystallization of benzophenone from saturated methanol solution via aqueous antisolvent drowning-out as monitored in-process using ATR FTIR spectroscopy [J].