泡沫相相分离制备多孔聚合物微球连续化工艺

周强; 郝军正; 祝琳华; 王红; 司甜; 何艳萍; 孙彦琳

doi:10.11949/j.issn.0438-1157.20181012

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泡沫相相分离制备多孔聚合物微球连续化工艺

材料化学工程与纳米技术 | 更新时间：2026-07-24

- 泡沫相相分离制备多孔聚合物微球连续化工艺
- Foam phase preparation of porous poly(methyl methacrylate-co-butyl acrylate) microspheres in continuous process
- 化工学报 2019年70卷第3期页码：1208-1219
- 作者机构：
  
  1.昆明理工大学化学工程学院，云南昆明 650500
  2.昆明理工大学理学院，云南昆明 650500
- 作者简介：
  
  周强（1991—），男，硕士研究生，17667172353@163.com
  何艳萍（1985—），女，博士，讲师，grace.he1985@hotmail.com
- 基金信息：
  
  国家自然科学基金项目(21466016, 21577053);云南省科技厅面上项目(2016FB024)
- DOI：10.11949/j.issn.0438-1157.20181012
  中图分类号： TQ 31
- 收稿：2018-09-10，
  
  修回：2018-12-06，
  
  网络首发：2026-07-24，
  
  纸质出版：2019-03-05
- 稿件说明：
移动端阅览
周强, 郝军正, 祝琳华, 王红, 司甜, 何艳萍, 孙彦琳. 泡沫相相分离制备多孔聚合物微球连续化工艺[J]. 化工学报, 2019, 70(3): 1208-1219

ZHOU Qiang, HAO Junzheng, ZHU Linhua, WANG Hong, SI Tian, HE Yanping, SUN Yanlin. Foam phase preparation of porous poly(methyl methacrylate-co-butyl acrylate) microspheres in continuous process[J]. CIESC Journal, 2019, 70(3): 1208-1219
周强, 郝军正, 祝琳华, 王红, 司甜, 何艳萍, 孙彦琳. 泡沫相相分离制备多孔聚合物微球连续化工艺[J]. 化工学报, 2019, 70(3): 1208-1219 DOI： 10.11949/j.issn.0438-1157.20181012.

ZHOU Qiang, HAO Junzheng, ZHU Linhua, WANG Hong, SI Tian, HE Yanping, SUN Yanlin. Foam phase preparation of porous poly(methyl methacrylate-co-butyl acrylate) microspheres in continuous process[J]. CIESC Journal, 2019, 70(3): 1208-1219 DOI： 10.11949/j.issn.0438-1157.20181012.

摘要

采用在泡沫相进行溶剂挥发的方法，连续、高效制备聚甲基丙烯酸甲酯-丙烯酸丁酯[P(MMA-BA)]共聚物多孔微球。采用自制的连续化反应装置，在一定搅拌速率和反应温度下，向反应器连续加料，在出口处连续收集溢出的泡沫并进行消泡、分散，再经洗涤、过滤、干燥得到多孔聚合物微球。重点研究了油相进料速率、反应温度、搅拌速率、聚乙烯醇用量(PVA浓度)对平均泡沫溢出速率、微球收率、微球粒径以及多孔形态的影响规律。结果表明：在反应温度为45℃，搅拌速率为500 r/min，油相溶液进料速率为30 g/min，PVA浓度为1.0%(质量)，油相溶液中P(MMA-BA)∶二氯甲烷(DCM)∶正庚烷(HT)=10∶53∶6(质量比)的工艺条件下，聚合物微球的收率高达92%，平均粒径为130 μm，P(MMA-BA)微球球形饱满，呈多孔结构。

Abstract

Porous polymeric microspheres have been widely used since their characteristics in the structure. However

the reported methods are less efficient

especially no continuous process was reported to prepare porous polymeric microspheres. Therefore

there is a need to develop a time-saving method with high yield for producing porous polymeric microspheres. This paper reports a continuous process to prepare porous polymeric microspheres

via

the solvent evaporation method in foam phase

being efficient and of high yield. Preparation of porous poly(methyl methacrylate-

-butyl acrylate) [P(MMA-BA)

]

microspheres was carried out in a customized continuous reaction device. At a certain stirring rate and reaction temperature

the oil phase and the aqueous phase were pumped continuously into the reactor. Foam phase gradually generated and flowed out from the outlet of the reactor. Porous P(MMA-BA) microspheres were obtained after collecting the bubble phase followed by defoaming

washing

filtration and drying. The average foam flow rate

the microspheres’ yield

the average particle size and the pore structure were investigated as a function of the experimental conditions including the feed rate of the oil phase

the reaction temperature

the stirring rate and the concentration of PVA. The results showed that the reaction temperature was 45℃

the stirring rate was 500 r/min

the oil phase solution feed rate was 30 g/min

the PVA concentration was 1.0% (mass)

and the oil phase solution P (MMA-BA): DCM∶HT is 10∶53∶6 respectively

the yield of the porous P(MMA-BA) microspheres was up to 92% and the average particle size is 130 µm. The temperature and the residual amount of the aqueous phase left in the customized continuous reaction device are critical for the foam behavior and the yield of the porous P(MMA-BA) microspheres. This work validates that the customized continuous reaction device is capable to produce porous polymeric microspheres continuously

based on the method to prepar

e porous polymeric microspheres

via

solvent evaporation method in foam phase

with improved efficiency and yield. In addition

the method reported in this work is able to use continuously on an industrial scale potentially.

关键词

Keywords

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