摘要
现有的人工采样分析方法如折光指数法、色谱法等操作复杂,存在时间上的滞后和人为误差,无法实时评估聚酯生产中的酯化反应过程,确定反应的清晰点。为此,该文搭建了以1064 nm为激光波长的在线拉曼分析系统,对对苯二甲酸(PTA)和1,3-丙二醇(PDO)生成聚对苯二甲酸丙二醇酯(PTT)的酯化反应过程进行光谱连续采集和处理。利用主成分分析法提取光谱信息,并结合酯化反应原理,利用位于1604 cm^-1附近的苯环基团和位于1720 cm^-1处的芳酯基团的拉曼特征峰面积比,建立了一种用于确定清晰点的定性分析方法。结果表明:拉曼光谱分析法可以准确反映聚酯过程酯化反应中的清晰点,且具有实时性好、操作方便、分析速度快的优势,可为聚酯生产的工艺控制和产品品质控制提供参考。
Current manual sampling and analysis methods,such as refractive index measurement,chromatography,etc.,have complex operations,time lags and human errors.Therefore,they cannot be used to evaluate the esterification process in polyester production in real time and determine the clear point of the reaction.In this article,an online Raman analysis system with 1064 nm as the laser wavelength was set up to collect continuously the spectra of the esterification reaction between terephthalic acid(PTA)and 1,3-propanediol(PDO)to create poly(tri-methylene terephthalate)(PTT),while using Savitzky-Golay algorithm to make baseline correction on the collected spectra.The principal component analysis was used to extract the spectral information.Based on the principle of esterification process,a qualitative analysis method was established to determine the clear point by using the area ratio for Raman characteristic peaks of benzene-loop located near 1604 cm^-1 and ester group located at 1720 cm^-1.Results showed that the developed Raman spectroscopy could accurately reflect the clear point in the esterification process of polyester prodction,With the advantages of good real-time performance,simple operation and rapid analysis,it provides a reference for the process control and product quality control of polyester production.
作者
陈怡帆
戴连奎
朱欢银
顾雪萍
CHEN Yi-fan;DAI Lian-kui;ZHU Huan-yin;GU Xue-ping(State Key Lab of Industrial Control Technology,Zhejiang University,Hangzhou310027,China;State Key Lab of Chemical Engineering,Zhejiang University,Hangzhou310027,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第4期434-440,共7页
Journal of Instrumental Analysis
基金
国家自然科学基金资助项目(U1609213)
国家重点研发计划项目(2017YFB0309401)。
关键词
拉曼光谱
聚酯纤维
在线检测
定性分析
荧光抑制
Raman spectroscopy
polyester
online detection
qualitative analysis
fluorescence suppression
