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林产化学与工业

林产化学与工业 ›› 2016, Vol. 36 ›› Issue (1): 42-48.doi: 10.3969/j.issn.0253-2417.2016.01.006

• 研究报告 • 上一篇    下一篇

水可分散型松香基聚酯多元醇的制备及耐热性研究

司红燕, 商士斌, 廖圣良, 王丹, 宋湛谦   

  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
  • 收稿日期:2014-12-23 出版日期:2016-02-25 发布日期:2016-03-18
  • 通讯作者: 宋湛谦,研究员,博士生导师,研究领域为天然产物化学;E-mail:songzq@hotmail.com。 E-mail:songzq@hotmail.com
  • 作者简介:司红燕(1987-),女,山东德州人,博士生,主要研究方向为生物质资源化学与利用
  • 基金资助:
    国家自然科学基金云南联合基金项目(U1202265)

Preparation and Heat Resistance of Water Dispersible Rosin-based Polyester Polyol

SI Hong-yan, SHANG Shi-bin, LIAO Sheng-liang, WANG Dan, SONG Zhan-qian   

  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
  • Received:2014-12-23 Online:2016-02-25 Published:2016-03-18

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摘要： 以马来海松酸(MPA)、新戊二醇(NPG)、三羟甲基丙烷(TMP)、间苯二甲酸(IPA)、己二酸(AA)、间苯二甲酸-5-磺酸钠(5-SSIPA)为原料,采用先分步熔融后溶剂回流法制得水可分散型松香基聚酯多元醇(WDRPP)。探讨了反应时间、催化剂用量、n(-OH):n(-COOH)和亲水单体用量对反应的影响,并利用傅里叶红外光谱(FT-IR)和13C NMR对产物进行了表征。利用热重分析(TG)研究了WDRPP的耐热性,并采用Coats-Redfem法对WDRPP的热分解动力学试验数据进行拟合分析,得到动力学参数。结果表明,当反应时间为5.5 h(熔融反应3 h,溶剂回流2.5 h),催化剂用量为0.10%,n(-OH):n(-COOH)为1.4:1,亲水单体用量为2.86%时,制备的WDRPP的热稳定性和WDRPP水分散体的稳定性最佳;WDRPP的最大失重速率温度(Tmax)为406.7℃、热解反应活化能为64.65 kJ/mol,且热分解动力学曲线线性良好(R2=0.9973),表明WDRPP热分解过程符合一级反应动力学规律;FT-IR和13C NMR的分析结果表明WDRPP制备成功。

关键词: 水可分散, 松香基聚酯多元醇, 耐热性, Coats-Redfem法

Abstract: Water dispersible rosin-based polyester polyol (WDRPP) was prepared through the method of first fractional melting reaction and then reflux, using maleopimaric anhydride (MPA), neopentyl glycol (NPG), trimethylolpropane (TMP), isophthalic acid (IPA), adipic acid (AA) and 5-sulfoiso-phtalic acid mono sodium salt (5-SSIPA) as raw materials.Effects of reaction time, the amount of catalyst, n(-OH):n(-COOH) and the amount of hydrophilic monomer on the reactions were investigated.The products were characterized by fourier transform infrared spectroscopy (FT-IR) and 13 C NMR.The heat resistance of WDRPP was studied using thermogravimetric analyzer (TG).The thermal degradation kinetic data were analyzed using Coats-Redfem method, and the kinetic parameters were obtained.The results showed that WDRPP with excellent thermostability and the WDRPP dispersion with good stability were obtained when reaction time was 5.5 h(melting reaction time of 3 h and reflux time of 2.5 h), the amount of catalyst was 0.10%, n(-OH):n(-COOH) was 1.4:1, and the amount of hydrophilic monomer was 2.86%, respectively.It was found that the temperature at maximum weight loss rate was 406.7℃, the reaction activation energy of pyrolysis was 64.65 kJ/mol, and the linear curves of thermal degradation kinetics fitted well (R2=0.997 3). This indicated that the thermal degradation process of WDRPP followed the law of first-order kinetic reaction.FT-IR and 13C NMR results demonstrated that WDRPP was prepared successfully.

Key words: water dispersible, rosin-based polyester polyol, heat resistance, Coats-Redfem method

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