松香基单体的RAFT聚合和表征

doi:10.3969/j.issn.0253-2417.2016.04.014

林产化学与工业 ›› 2016, Vol. 36 ›› Issue (4): 99-104.doi: 10.3969/j.issn.0253-2417.2016.04.014

松香基单体的RAFT聚合和表征

刘少锋¹, 王春鹏^1,2, 储富祥^1,2, 俞娟¹, 王基夫^1,2

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. 中国林业科学研究院林业新技术研究所, 北京 100091

收稿日期:2015-07-21 出版日期:2016-08-25 发布日期:2016-09-01
通讯作者: 王基夫,副研究员,硕士生导师,从事生物质材料功能化研究;E-mail:wjf118@126.com。 E-mail:wjf118@126.com
作者简介:刘少锋(1990-),男,河北石家庄人,硕士生,主要从事生物质材料研究工作
基金资助:
江苏省自然科学基金资助项目（BK20131070）

RAFT Polymerization and Characterization of Rosin Derived Monomer

LIU Shao-feng¹, WANG Chun-peng^1,2, CHU Fu-xiang^1,2, YU-Juan¹, WANG Ji-fu^1,2

1. Institute of Chemical Industry of Forestry Products, CAF;National Engineering Lab. for Biomass Chemical Utilization;Key and Lab. of Forest Chemical Engineering, SFA;Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China;
2. Research Institute of Forestry New Technology, CAF, Beijing 100091, China

Received:2015-07-21 Online:2016-08-25 Published:2016-09-01

摘要/Abstract

摘要： 以松香为原料，依次进行酰氯化和酯化反应合成松香基混合单体，并采用FT-IR、GC-MS、¹³C NMR 对其结构进行表征；然后将该松香基混合单体、可逆加成-断裂链转移（RAFT）试剂二硫代苯甲酸异丙苯酯（CDB）和引发剂偶氮二异丁腈（AIBN）按物质的量比100：1：0.1进行RAFT聚合反应。为了进一步研究松香基单体的RAFT聚合过程，以高纯度的脱氢枞酸基单体进行了RAFT聚合反应。结果表明：脱氢枞酸基单体在松香基混合单体中GC含量为14.3%，在RAFT聚合中显示了很好的聚合结构可控性，聚合物的多分散系数（PDI）为1.28；而松香基混合单体基聚合物的PDI相对较高，PDI为1.85，但仍属于可控范围。所合成的松香基RAFT聚合物同时也是一种新型大分子RAFT试剂，可以作为下一步RAFT活性聚合的RAFT试剂。TGA分析表明：松香基RAFT聚合物显示了很好的热稳定性，质量损失为10%的温度和最大分解温度分别为250和350℃。

关键词: 松香, 松香基单体, 可逆加成-断裂链转移(RAFT)聚合, 松香基大分子RAFT试剂

Abstract: Rosin derived monomer blend was synthesized by chloridization and esterification in turn, and characterized by FT-IR, GC/MS and ¹³C NMR, respectively. Rosin derived monomer blend, reversible addition-fragmentation chain transfer (RAFT) agent CDB and initiator AIBN with molar ratio of 100:1:0.1 were then used to perform RAFT polymerization. In order to further investigate the RAFT polymerization of rosin derived monomer blend, high purity dehydroabietic acid was also employed to perform RAFT polymerization. The results showed that dehydroabietic acid derived monomer accounted for 14.3% in rosin derived monomer, and the RAFT polymerization of dehydroabietic acid derived monomer was well controlled and achieved a well-defined dehydroabietic acid based polymer with polydispersity index (PDI) of 1.28. And PDI of rosin derived monomer based polymer was 1.85 which was relative higher than that of dehydroabietic acid based polymer. However, its polymer structure was still regarded well-defined. The rosin based polymer obtained by RAFT polymerization was also a novel Marco-RAFT agent, which could be used as RAFT agent for next step RAFT polymerization with purpose of polymer chain extension. Additionally, the synthesized rosin based polymers were all demonstrated with good thermal stability, temperature of the mass loss at 10% and maximum decomposing temperature was 250℃ and 350℃, respectively.

Key words: rosin, rosin based monomer, reversible addition-fragmentation chain transfer (RAFT) polymerization, rosin based macro-RAFT agent

中图分类号:

TQ351

刘少锋, 王春鹏, 储富祥, 俞娟, 王基夫. 松香基单体的RAFT聚合和表征[J]. 林产化学与工业, 2016, 36(4): 99-104.

LIU Shao-feng, WANG Chun-peng, CHU Fu-xiang, YU-Juan, WANG Ji-fu. RAFT Polymerization and Characterization of Rosin Derived Monomer[J]. Chemistry and Industry of Forest Products, 2016, 36(4): 99-104.

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松香基单体的RAFT聚合和表征

RAFT Polymerization and Characterization of Rosin Derived Monomer

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