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生物质化学工程 ›› 2019, Vol. 53 ›› Issue (2): 7-12.doi: 10.3969/j.issn.1673-5854.2019.02.002

• 研究报告 • 上一篇    下一篇

十一烯酸/马来酸酐共聚物的制备与表征

吴美婷1,张永贺2,金立维1,*()   

  1. 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:2018-01-26 出版日期:2019-03-30 发布日期:2019-04-09
  • 通讯作者: 金立维 E-mail:liwei-jin@163.com
  • 作者简介:吴美婷(1992—),女,山东德州人,硕士生,主要从事生物质高分子材料的研究
  • 基金资助:
    国家重点研发计划项目(2016YFD0600705)

Preparation and Characterization of Undecylenic Acid/Maleic Anhydride Copolymer

Meiting WU1,Yonghe ZHANG2,Liwei JIN1,*()   

  1. 1. Institute of Chemical Industry of Forestry 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. Research Institute of Forestry New Technology, CAF, Beijing 100091, China
  • Received:2018-01-26 Online:2019-03-30 Published:2019-04-09
  • Contact: Liwei JIN E-mail:liwei-jin@163.com
  • Supported by:
    国家重点研发计划项目(2016YFD0600705)

摘要:

以十一烯酸(UA)和马来酸酐(MAH)为原料,偶氮二异丁腈(AIBN)为引发剂,通过沉淀聚合的方法制备了十一烯酸/马来酸酐共聚物(UMA),研究了单体配比、引发剂用量及反应温度对共聚反应的影响,通过FT-IR、13C NMR、DSC分析和酸酐质量分数的测定对共聚物进行了表征。FT-IR和13C NMR结果表明:在实验条件下,十一烯酸(UA)与马来酸酐(MAH)发生了共聚反应。当反应温度为75 ℃、AIBN用量为0.75%时,随着MAH用量的增加,共聚物相对分子质量减小,得率和酸酐质量分数呈现先增大后略有减小的趋势,当UA与MAH的物质的量之比为40:60时共聚物的得率及酸酐质量分数均达到最大值,分别为61.78%和20.05%,与DSC曲线中玻璃化转变温度(Tg)的变化趋势基本一致,即当n(UA):n(MAH)为40:60,Tg达到最大值71.98 ℃。提高引发剂用量和反应温度有利于共聚反应的进行,但相对分子质量有所下降,因此可根据所需聚合物的性质来选择合适的反应条件。

关键词: 十一烯酸, 马来酸酐, 沉淀聚合, 共聚, 酸酐质量分数

Abstract:

Undecylenic acid/maleic anhydride copolymer(UMA) was prepared by precipitation polymerization method with undecylenic acid(UA) and maleic anhydride(MAH) as raw materials, azobisisobutyronitrile(AIBN) as initiator. The influences of monomer ratio, initiator dosage, and reaction temperature on polymerization were studied. The copolymer was characterized by FT-IR, 13C NMR, DSC and the mass fraction of anhydride of copolymer was measured. The results of FT-IR and 13C NMR showed that the copolymerization of UA and MAH successfully proceeded under the experimental conditions. When the reaction temperature was 75 ℃, the dosage of AIBN was 0.75%, with the increase of the amount of MAH, the molecular weight of copolymer decreased, the conversion rate and anhydride content incresed first and then declined slightly. When n(UA):n(MAH) was 40:60, the conversion rate and mass fraction of anhydride reached the maximum, 61.78% and 20.05%, respectively, which was basically consistent with the change of glass transition temperature(Tg) of DSC curves. Increasing the initiator dosage and reaction temperature was beneficial to the copolymerization but the molecular weight decreased, so the appropriate reaction conditions could be selected according to the properties of the desired polymer. When the n(UA):n(MAH) was 40:60, the Tg reached the maximum, 71.98 ℃.

Key words: undecylenic acid, maleic anhydride, precipitation polymerization, copolymerization, mass fraction of anhydride

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