近红外光谱检测技术在精细化工生产过程中的应用
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摘要
针对精细化学品D3生产过程中酸碱原料浓度检测和D2生产过程中粗品/精品快速检测鉴定需求,论述了近红外光谱检测的基本原理,给出了偏最小二乘定量建模和马氏距离分类判别等化学计量学算法,构建了Antaris II傅里叶变换近红外光谱检测系统。通过配制样品,采集光谱数据,并经求导、滤波和标准化数据处理,应用偏最小二乘法建立了D3生产过程HCl水溶液摩尔浓度、NaOH水溶液质量百分数和摩尔浓度的近红外光谱检测模型,应用马氏距离结合主元分析法建立了D2生产过程中粗品/精品判别分析模型,给出了详细的检测实验数据。生产现场样品检测结果表明,D3酸碱浓度的定量检测模型具有很高的检测精度,D2粗品/精品判别分析模型判别结果准确,可在相关精细化工生产过程中推广应用,提高生产过程检测鉴定效率。
According to the detection requirements of fine chemical production processes including D3 acidbase concentration and discriminant analysis of crude and fine D2,the detection technology of near infrared spectroscopy(NIR) was studied,the related spectral correction modeling algorithms including partial least squares(PLS) and Mahalanobis distance were presented,and the relevant testing system Antaris II Fourier transformer NIR analyzer was constructed. By collecting a large number of samples,testing with Antaris II near infrared spectrometer,and processing of the spectral data with derivation,filtering and standardization technique,the establishment of NIR calibration models for the molar concentration detection of HCl,the mass percentage and molar concentration detection of NaOH aqueous solution was completed using PLS,the discriminant analysis model of crude and fine D2 was built combining Mahalanobis distance and Principal Component Analysis(PCA),and detailed experimental detection results were achieved and presented in this paper. The NIR calibration models and discriminant analysis models were successfully used in D3 and D2 fine chemical production processes respectively,and the efficiency of detection of acid-base materials and identification of crude and fine D2 was much improved.
According to the detection requirements of fine chemical production processes including D3 acidbase concentration and discriminant analysis of crude and fine D2,the detection technology of near infrared spectroscopy(NIR) was studied,the related spectral correction modeling algorithms including partial least squares(PLS) and Mahalanobis distance were presented,and the relevant testing system Antaris II Fourier transformer NIR analyzer was constructed. By collecting a large number of samples,testing with Antaris II near infrared spectrometer,and processing of the spectral data with derivation,filtering and standardization technique,the establishment of NIR calibration models for the molar concentration detection of HCl,the mass percentage and molar concentration detection of NaOH aqueous solution was completed using PLS,the discriminant analysis model of crude and fine D2 was built combining Mahalanobis distance and Principal Component Analysis(PCA),and detailed experimental detection results were achieved and presented in this paper. The NIR calibration models and discriminant analysis models were successfully used in D3 and D2 fine chemical production processes respectively,and the efficiency of detection of acid-base materials and identification of crude and fine D2 was much improved.
引文
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2褚小立,张莉,燕泽程.现代过程分析技术交叉学科发展前沿与展望[M].北京:机械工业出版社,2016:1-131.
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4 Liu R H,Li L,Yin W P,and Xu D B.Near-infrared spectroscopy monitoring and control of the fluidized bed granulation and coating processes-A review[J].International Journal of Pharmaceutics.2017,530(1-2):308-315.
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7周昭露,李杰,黄生权.近红外光谱技术在中药质量控制应用中的化学计量学建模:综述和展望[J].化工进展,2016,35(6):1627-1645.
8邹志云,孟磊,常颖,郭宇晴,黄越,刘英莉,赵丹丹.精细化工过程非接触式检测技术的若干研究实例[J].计算机与应用化学,2017,34(9):649-654.
9 Wang W,Jiang H,and Liu G H.Qualitative Prediction of Yeast Growth Process Based on Near Infrared Spectroscopy[J].Chinese Journal of Analytical Chemistry.2017,45(8):1137-1141
10 Ling Z G,Yuuki Omura,Naruhito Hori,Tadahisa Iwata,and Akio Takemura.In-situ chemical structure analysis of aqueous vinyl polymer solution-isocyanate adhesive in post-cure process by using Fourier transform near infrared spectroscopy[J].International Journal of Adhesion and Adhesives.2018,81:56-64.
11淡图南,戴连奎.近红外光谱的甲醇汽油定量分析[J].计算机与应用化学,2011,28(3):329-332.
12 Lin H,Marjanovic O,Lennox B and Shamekh A.Application of Near-infrared Spectroscopy in Batch Process Control[J].IFAC Proceedings,2009,42(11):750-755.
13 David B?r,Heiko Debus,Sina Brzenczek and Wolfgang Fischer.Determining particle size and water content by near-infrared spectroscopy in the granulation of naproxen sodium[J].Journal of Pharmaceutical and Biomedical Analysis,2018,151:209-218.
14张小超,吴静珠,徐云.近红外光谱分析技术及其在现代农业中的应用[M].北京:电子工业出版社,2012:95-179.
15褚小立.化学计量学方法与分子光谱分析技术[M].北京:化学工业出版社,2011:259-307.
16 Jerry Workman and Lois Weyer.Practical guide and spectral atlas for interpretive near-infrared spectroscopy[M].Boca Raton:CRC Press,2012:1-309.
17 Andrea Stockl and Fabian Lichti.Near-infrared spectroscopy(NIRS)for a real time monitoring of the biogas process[J].Bioresource Technology,2018,247:1249-1252.
18李雪园,张红光,卢建刚,施英姿,陈金水.近红外光谱定量分析的模型转移新方法[J].计算机与应用化学,2018,1:27-36.
19 Julio C Machado Jr,Miguel A Faria,Isabel MFerreira and Ricardo N Pásco.Varietal discrimination of hop pellets by near and mid infrared spectroscopy[j].Talanta,2018,180:69-75.
20郭正飞,戴连奎.基于近红外谱形分析的中药提取过程终点判断[J].光谱实验室,2013,30(5):2418-2423.
21赛默飞世尔科技公司,Thermo Antaris近红外分析仪培训手册[M].2009:1-144.
22韩君,孙长海,方洪壮.近红外光谱结合反向区间偏最小二乘法检测药用辅料糊精[J].计算机与应用化学,2016,33(2):205-208.
2褚小立,张莉,燕泽程.现代过程分析技术交叉学科发展前沿与展望[M].北京:机械工业出版社,2016:1-131.
3 Freek van der Meer.Near-infrared laboratory spectroscopy of mineral chemistry:A review[J].International Journal of Applied Earth Observation and Geoinformation.2018,65:71-78.
4 Liu R H,Li L,Yin W P,and Xu D B.Near-infrared spectroscopy monitoring and control of the fluidized bed granulation and coating processes-A review[J].International Journal of Pharmaceutics.2017,530(1-2):308-315.
5褚小立,陆婉珍.近五年我国近红外光谱分析技术研究与应用进展[J].光谱学与光谱分析,2014,10:2595-2605.
6 Celio Pasquini.Near infrared spectroscopy:A mature analytical technique with new perspectives-Areview[J].Analytica Chimica Acta.2018,1026:8-36.
7周昭露,李杰,黄生权.近红外光谱技术在中药质量控制应用中的化学计量学建模:综述和展望[J].化工进展,2016,35(6):1627-1645.
8邹志云,孟磊,常颖,郭宇晴,黄越,刘英莉,赵丹丹.精细化工过程非接触式检测技术的若干研究实例[J].计算机与应用化学,2017,34(9):649-654.
9 Wang W,Jiang H,and Liu G H.Qualitative Prediction of Yeast Growth Process Based on Near Infrared Spectroscopy[J].Chinese Journal of Analytical Chemistry.2017,45(8):1137-1141
10 Ling Z G,Yuuki Omura,Naruhito Hori,Tadahisa Iwata,and Akio Takemura.In-situ chemical structure analysis of aqueous vinyl polymer solution-isocyanate adhesive in post-cure process by using Fourier transform near infrared spectroscopy[J].International Journal of Adhesion and Adhesives.2018,81:56-64.
11淡图南,戴连奎.近红外光谱的甲醇汽油定量分析[J].计算机与应用化学,2011,28(3):329-332.
12 Lin H,Marjanovic O,Lennox B and Shamekh A.Application of Near-infrared Spectroscopy in Batch Process Control[J].IFAC Proceedings,2009,42(11):750-755.
13 David B?r,Heiko Debus,Sina Brzenczek and Wolfgang Fischer.Determining particle size and water content by near-infrared spectroscopy in the granulation of naproxen sodium[J].Journal of Pharmaceutical and Biomedical Analysis,2018,151:209-218.
14张小超,吴静珠,徐云.近红外光谱分析技术及其在现代农业中的应用[M].北京:电子工业出版社,2012:95-179.
15褚小立.化学计量学方法与分子光谱分析技术[M].北京:化学工业出版社,2011:259-307.
16 Jerry Workman and Lois Weyer.Practical guide and spectral atlas for interpretive near-infrared spectroscopy[M].Boca Raton:CRC Press,2012:1-309.
17 Andrea Stockl and Fabian Lichti.Near-infrared spectroscopy(NIRS)for a real time monitoring of the biogas process[J].Bioresource Technology,2018,247:1249-1252.
18李雪园,张红光,卢建刚,施英姿,陈金水.近红外光谱定量分析的模型转移新方法[J].计算机与应用化学,2018,1:27-36.
19 Julio C Machado Jr,Miguel A Faria,Isabel MFerreira and Ricardo N Pásco.Varietal discrimination of hop pellets by near and mid infrared spectroscopy[j].Talanta,2018,180:69-75.
20郭正飞,戴连奎.基于近红外谱形分析的中药提取过程终点判断[J].光谱实验室,2013,30(5):2418-2423.
21赛默飞世尔科技公司,Thermo Antaris近红外分析仪培训手册[M].2009:1-144.
22韩君,孙长海,方洪壮.近红外光谱结合反向区间偏最小二乘法检测药用辅料糊精[J].计算机与应用化学,2016,33(2):205-208.