化工学报 ›› 2019, Vol. 70 ›› Issue (3): 1208-1219.DOI: 10.11949/j.issn.0438-1157.20181012
周强1(),郝军正1,祝琳华1,王红2,司甜1,何艳萍1(),孙彦琳1
收稿日期:
2018-09-10
修回日期:
2018-12-06
出版日期:
2019-03-05
发布日期:
2019-03-05
通讯作者:
何艳萍
作者简介:
<named-content content-type="corresp-name">周强</named-content>(1991—),男,硕士研究生,<email>17667172353@163.com</email>|何艳萍(1985—),女,博士,讲师,<email>grace.he1985@hotmail.com</email>
基金资助:
Qiang ZHOU1(),Junzheng HAO1,Linhua ZHU1,Hong WANG2,Tian SI1,Yanping HE1(),Yanlin SUN1
Received:
2018-09-10
Revised:
2018-12-06
Online:
2019-03-05
Published:
2019-03-05
Contact:
Yanping HE
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。
中图分类号:
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.
Qiang ZHOU, Junzheng HAO, Linhua ZHU, Hong WANG, Tian SI, Yanping HE, Yanlin SUN. Foam phase preparation of porous poly(methyl methacrylate-co-butyl acrylate) microspheres in continuous process[J]. CIESC Journal, 2019, 70(3): 1208-1219.
Fm-oil phase/(g/min) | T/℃ | ωPVA/%(mass) | N/(r/min) |
---|---|---|---|
10 | 45 | 1.0 | 500 |
20 | 45 | 1.0 | 500 |
30 | 45 | 1.0 | 500 |
40 | 45 | 1.0 | 500 |
50 | 45 | 1.0 | 500 |
30 | 35 | 1.0 | 500 |
30 | 40 | 1.0 | 500 |
30 | 45 | 1.0 | 500 |
30 | 50 | 1.0 | 500 |
30 | 55 | 1.0 | 500 |
30 | 45 | 0.5 | 500 |
30 | 45 | 1.0 | 500 |
30 | 45 | 1.5 | 500 |
30 | 45 | 2.0 | 500 |
30 | 45 | 2.5 | 500 |
30 | 45 | 1.0 | 100 |
30 | 45 | 1.0 | 300 |
30 | 45 | 1.0 | 500 |
30 | 45 | 1.0 | 700 |
30 | 45 | 1.0 | 900 |
表1 多孔聚合物微球制备连续化工艺条件
Table 1 Preparative conditions of porous polymeric microspheres in continuous process
Fm-oil phase/(g/min) | T/℃ | ωPVA/%(mass) | N/(r/min) |
---|---|---|---|
10 | 45 | 1.0 | 500 |
20 | 45 | 1.0 | 500 |
30 | 45 | 1.0 | 500 |
40 | 45 | 1.0 | 500 |
50 | 45 | 1.0 | 500 |
30 | 35 | 1.0 | 500 |
30 | 40 | 1.0 | 500 |
30 | 45 | 1.0 | 500 |
30 | 50 | 1.0 | 500 |
30 | 55 | 1.0 | 500 |
30 | 45 | 0.5 | 500 |
30 | 45 | 1.0 | 500 |
30 | 45 | 1.5 | 500 |
30 | 45 | 2.0 | 500 |
30 | 45 | 2.5 | 500 |
30 | 45 | 1.0 | 100 |
30 | 45 | 1.0 | 300 |
30 | 45 | 1.0 | 500 |
30 | 45 | 1.0 | 700 |
30 | 45 | 1.0 | 900 |
图4 油相溶液进料速率(Fm-oil phase)对泡沫平均溢出速率(Fm-foam phase)和微球收率(Y)的影响
Fig.4 Effect of feed rate of oil phase (Fm-oil phase) on average foam flow rate (Fm-foam phase) and microspheres’ yield (Y)
图5 油相溶液进料速率对DCM进料速率(Fm-DCM)和连续相平均温度(Taverage)的影响
Fig.5 Effect of feed rate of oil phase on feed rate of DCM (Fm-DCM) and average temperature of continuous phase (Taverage)
图8 反应温度(T)对液体剩余量(V)和连续相平均温度(Taverage)的影响
Fig.8 Effect of temperature (T) on amount of residual liquid (V) and average temperature of continuous phase (Taverage)
图10 不同PVA质量分数0.5%(a),1.5%(b),2.5%(c)所得多孔微球的光学显微镜图片和PVA浓度对微球平均粒径的影响(d)
Fig.10 Optical microscope images of porous microspheres with different mass fraction of PVA[0.5%(a), 1.5%(b), 2.5%(c)], effect of concentration of PVA on average particle size of microspheres(d)
图11 PVA浓度对液体剩余量(V)和连续相平均温度(Taverage)的影响
Fig.11 Effect of concentration of PVA (ωPVA) on amount of residual liquid (V) and average temperature of continuous phase (Taverage)
图14 不同搅拌速率所得多孔微球的平均粒径(a)及粒径分布(b)
Fig.14 Average particle size (a) and particle size distribution (b) of porous microspheres with different stirring rates
图15 搅拌速率对连续相平均温度(Taverage)和液体剩余量(V)的影响
Fig.15 Effect of stirring rate on average temperature of continuous phase (Taverage) and amount of residual liquid (V)
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