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In-Line Monitoring of Particle Size during Emulsion Polymerization under Different Operational Conditions using NIR Spectroscopy

机译：使用NIR光谱在线监测不同操作条件下乳液聚合过程中的粒径

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摘要

In the present work, the sensitivity of NIR spectroscopy toward the evolution of particle size was studied during emulsion homopolymerization of styrene (Sty) and emulsion copolymer-ization of vinyl acetate-butyl acrylate conducted in a semibatch stirred tank and a tubular pulsed sieve plate reactor, respectively. All NIR spectra were collected online with a trans-flectance probe immersed into the reaction medium. The spectral range used for the NIR monitoring was from 9 500 to 13 000 cm"1, where the absorbance of the chemical components present is minimal and the changes in the NIR spectrum can be ascribed to the effects of light scattering by the polymer particles. Off-line measurements of the average diameter of the polymer particles by DLS were used as reference values for the development of the multi variate NIR calibration models based on partial least squares. Results indicated that, in the spectral range studied, it is possible to monitor the evolution of the average size of the polymer particles during emulsion polymerization reactions. The inclusion of an additional spectral range, from 5 701 to 6 447 cm-1, containing information on absorbances ("chemical information") in the calibration models was also evaluated.
机译：在目前的工作中，研究了在半间歇搅拌釜和管状脉冲筛板反应器中进行的苯乙烯乳液均聚（Sty）和乙酸乙烯酯-丙烯酸丁酯的乳液共聚过程中，近红外光谱对粒度演变的敏感性。 ， 分别。所有NIR光谱都是通过浸入反应介质中的透反射探针在线收集的。用于NIR监测的光谱范围为9500至13000 cm-1，其中存在的化学成分的吸光度最小，并且NIR光谱的变化可归因于聚合物颗粒的光散射效应。通过偏最小二乘法离线测量聚合物颗粒的平均直径作为建立基于偏最小二乘的多元近红外校准模型的参考值，结果表明，在所研究的光谱范围内，有可能进行监测乳液聚合反应过程中聚合物颗粒平均尺寸的变化，还评估了校准模型中包含吸光度信息（“化学信息”）的附加光谱范围5 701至6 447 cm-1 。

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  • 来源
    《Macromolecular reaction engineering》 |2011年第4期|p.150-162|共13页
  • 作者

    Dennis LChicoma; Claudia Sayer; Reinaldo Giudici;

  • 作者单位

    Departamento de Engenharia Ouimica, Universidade de Sao Paulo, Escola Politecnica, Caixa Postal 61548, CEP 05424-970, Sao Paulo, SP, Brasil;

    Departamento de Engenharia Ouimica e de Alimentos,Universidade Federal de Santa Catarina, CTC, Caixa Postal 476,CEP 88040-970, Florianopolis, SC, Brasil;

    Departamento de Engenharia Ouimica, Universidade de Sao Paulo, Escola Politecnica, Caixa Postal 61548, CEP 05424-970, Sao Paulo, SP, Brasil;

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