分散聚合法制备单分散松香基聚合物微球

doi:10.3969/j.issn.0253-2417.2019.02.006

林产化学与工业 ›› 2019, Vol. 39 ›› Issue (2): 39-45.doi: 10.3969/j.issn.0253-2417.2019.02.006

分散聚合法制备单分散松香基聚合物微球

程增会^1,²(),张代晖¹,王基夫¹,王春鹏¹,储富祥^1,*(),许凤²

1. 中国林业科学研究院林产化学工业研究所；生物质化学利用国家工程实验室；国家林业局林产化学工程重点开放性实验室；江苏省生物质能源与材料重点实验室，江苏南京 210042
2. 北京林业大学材料科学与技术学院，北京 100083

收稿日期:2018-12-27 出版日期:2019-04-25 发布日期:2019-05-08
通讯作者: 储富祥 E-mail:chengzenghuia@163.com;chufuxiang@caf.ac.cn
作者简介:程增会(1986—)，女，山东潍坊人，博士生，研究方向为生物质高分子材料；E-mail：chengzenghuia@163.com
基金资助:
中国林科院中央级公益性科研院所基本科研业务费专项资金(CAFYBB2017ZF003)

Preparation of Monodisperse Rosin-based Polymer Microspheres by Dispersion Polymerization

Zenghui CHENG^1,²(),Daihui ZHANG¹,Jifu WANG¹,Chunpeng WANG¹,Fuxiang CHU^1,*(),Feng XU²

1. Institute of Chemical Industry of Forest Products, CAF; National Engineering Lab. for Biomass Chemical Utilization; Key and Open Lab. of Forest Chemical Engineering, SFA; Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China
2. College of Materials Science and Technology, Beijing Forestry University, Beijing 100083, China

Received:2018-12-27 Online:2019-04-25 Published:2019-05-08
Contact: Fuxiang CHU E-mail:chengzenghuia@163.com;chufuxiang@caf.ac.cn
Supported by:
中国林科院中央级公益性科研院所基本科研业务费专项资金(CAFYBB2017ZF003)

摘要/Abstract

摘要：

以新型的脱氢枞酸(2-甲基丙烯酰氧基异丙醇基)酯(DAGMA)为单体，聚乙烯吡咯烷酮(PVP)为分散稳定剂，偶氮二异丁腈(AIBN)为引发剂，异丙醇/水为反应分散介质，采用分散聚合法制备了单分散的聚脱氢枞酸(甲基丙烯酰氧基-β-羟基丙基)酯(PDAGMA)微球。研究了分散剂用量、单体质量分数、反应温度对PDAGMA聚合物微球粒径大小及分布的影响，并用交联剂进行交联，初步探索了其吸附性能。采用FT-IR、¹H NMR、GPC、SEM和TGA对聚合物微球的结构及微球的形貌和尺寸进行表征。研究结果表明：DAGMA单体在醇/水介质中能够发生聚合反应，且GPC测得聚合物的相对分子质量约为55 000；聚合物微球粒径随着PVP用量的增大而减小，随着单体质量分数增大聚合物微球平均粒径先减小后增大，并且反应温度升高粒径增大，分散聚合得到的聚合物微球PDI最低为1.014，粒径为1.37 μm；交联后松香基聚合物热稳定性提高，并且对芦丁的吸附量为12.3 mg/g。

关键词: 分散聚合, 松香, 聚合物微球

Abstract:

A new type of monodisperse microspheres consisted of poly (2-methacryloyloxyisopropanol ester of dehydroabietic acid) PDAGMA was prepared via dispersion polymerization in the presence of isopropyl alcohol/H₂O, using 2-methacryloyloxyisopropanol ester of dehydroabietic acid (DAGMA) as a monomer, polyvinylpyrrolidone(PVP) as stabilizer, 2, 2′-azobis (2-methylpropionitrile) (AIBN) as an initiator. The influences of PVP content, monomer concentration and reaction temperature on the particle size and distribution of microspheres were investigated. Then, these microspheres were crosslined and bed used as an adsorption material. And the rutin adsorption performance was also investigated. FT-IR, ¹H NMR, GPC and SEM were applied to characterize the structure, morphology and size of the microspheres, respectively. The results showed that the DAGMA monomer could polymerized in the alcohol/water medium. GPC analysis showed that the relative molecular weight of the polymer was about 55 000. The average diameter of the polymer microsphere was found to decrease with the increase of the amount of PVP. The polymer microsphere particle size decreased frist and then increased as the monomer concentration increased, as the reaction temperature increased, the polymer microsphere particle size also increased. By the optimize the polymerization techmology, monodispersed microspheres with particle size 1.37 μm and PDI 1.014 were obtained. Specially, the cross-linked rosin polymer microspheres exhibited an improved thermal stability and the adsorption capacity of rutin was 12.3 mg/g.

Key words: dispersion polymerization, rosin, polymer microspheres

中图分类号:

TQ35
O631.5

程增会,张代晖,王基夫,王春鹏,储富祥,许凤. 分散聚合法制备单分散松香基聚合物微球[J]. 林产化学与工业, 2019, 39(2): 39-45.

Zenghui CHENG,Daihui ZHANG,Jifu WANG,Chunpeng WANG,Fuxiang CHU,Feng XU. Preparation of Monodisperse Rosin-based Polymer Microspheres by Dispersion Polymerization[J]. Chemistry and Industry of Forest Products, 2019, 39(2): 39-45.

图/表 11

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项目 items		D_n/μm	D_w/μm	PDI
PVP用量 PVP dosage	20%	1.628	2.743	1.685
	30%	1.600	1.771	1.107
	40%	1.368	1.402	1.025
单体用量 monomer dosage	2%	4.700	7.318	1.557
	5%	1.368	1.402	1.025
	10%	1.370	1.389	1.014
	20%	2.001	2.073	1.036
反应温度 temperature	60 ℃	1.353	1.377	1.018
	70 ℃	1.368	1.402	1.025
	80 ℃	4.643	6.393	1.377
交联剂 cross-linking	0	1.368	1.402	1.025
交联剂 cross-linking	1%	2.08	2.162	1.039

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分散聚合法制备单分散松香基聚合物微球

Preparation of Monodisperse Rosin-based Polymer Microspheres by Dispersion Polymerization

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