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微波辐射下丙烯海松酸烯丙酯的合成、表征及UV固化反应

卢言菊 赵振东 古研 王婧 徐士超

林产化学与工业2017,Vol.37Issue(6):49-55,7.
林产化学与工业2017,Vol.37Issue(6):49-55,7.DOI:10.3969/j.issn.0253-2417.2017.06.007

微波辐射下丙烯海松酸烯丙酯的合成、表征及UV固化反应

Microwave Irradiation Synthesis, Characterization and UV-curing Reaction of Allyl Acrylpimarate

卢言菊 1赵振东 2古研 3王婧 4徐士超1

作者信息

  • 1. 中国林业科学研究院林产化学工业研究所
  • 2. 生物质化学利用国家工程实验室
  • 3. 国家林业局林产化学工程重点开放性实验室
  • 4. 江苏省生物质能源与材料重点实验室,江苏南京210042 中国林业科学研究院林业新技术研究所,北京100091
  • 折叠

摘要

Abstract

A new polymerized monomer with two allyl groups was synthesized by Diels-Alder reaction, which could introduce the characteristic fused ring structure of rosin acids to the polymers. Allyl acrylpimarate was synthesized by using sodium acrylpimaric rosinate and allyl chloride as raw materials with molar ratio of 1:2, 5% cetyltrimethyl ammonium bromide as catalyst, 0. 02%hydroquinol as polymerization inhibitor and N, N-dimethylformamide as solvent under microwave irradiation. Under the reaction conditions of microwave energy 400 W, reaction time 2. 5 h, reaction temperature 50 ℃, the yield of allyl acrylpimarate( AA) was 72. 9%. The structure of the product was characterized by gas chromatography, gas chromatography mass spectrometry, infrared spectrum, and nuclear magnetic resonance spectra. The IR spectra showed that the characteristic absorption peak of C—C on AA addition appeared at 1686 and 1648 cm-1 . The GC content of AA was determined as 98. 6% by gas chromatography. Mass spectrometry and nuclear magnetic resonance spectra were used to verify the correctness of the structure of AA. The UV curing reaction of AA was studied. The results of infrared spectroscopy showed that the polymerization monomer was a free radical polymerization reaction. The surface curing time of AA decreased with the increasing of photo initiator dosage, decreasing of illumination distance and increasing of illumination intesity. TG and DSC analysis results showed that the UV curing product had good thermal stability with the initial decomposition temperature of 292. 9℃ and initial glass transition temperature of 49. 6 ℃.

关键词

微波辐射/丙烯海松酸/丙烯海松酸烯丙酯/UV固化反应/表干时间

Key words

microwave irradiation/acrylpimaric acid/allyl acrylpimarate/UV curing reaction/surface drying time

分类

化学化工

引用本文复制引用

卢言菊,赵振东,古研,王婧,徐士超..微波辐射下丙烯海松酸烯丙酯的合成、表征及UV固化反应[J].林产化学与工业,2017,37(6):49-55,7.

基金项目

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( CAFYBB2017QA018 ) ( CAFYBB2017QA018 )

国家自然科学基金资助项目(31370575) (31370575)

林产化学与工业

OA北大核心CSCDCSTPCD

0253-2417

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