羟基化木本油脂的合成及其结构表征

doi:10.3969/j.issn.0253-2417.2018.06.004

林产化学与工业 ›› 2018, Vol. 38 ›› Issue (6): 27-32.doi: 10.3969/j.issn.0253-2417.2018.06.004

羟基化木本油脂的合成及其结构表征

张飞^1,2, 胡云¹, 刘承果¹, 周永红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. 江苏警官学院, 江苏南京 210031

收稿日期:2018-07-18 出版日期:2018-12-25 发布日期:2018-12-27
通讯作者: 刘承果,副研究员,硕士生导师,研究领域为生物基光固化材料;E-mail:liuchengguo@icifp.cn。 E-mail:liuchengguo@icifp.cn
作者简介:张飞(1988-),男,江西抚州人,讲师,博士生,主要从事生物质材料开发利用工作
基金资助:
国家重点研发计划资助（2016YFD0600802）；江苏警官学院食品药品与环境犯罪检验技术创新团队项目（2018SJYTD03）

Synthesis and Characterization of Hydroxylated Woody Oil

ZHANG Fei^1,2, HU Yun¹, LIU Chengguo¹, ZHOU Yonghong¹

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. Jiangsu Police Institute, Nanjing 210031, China

Received:2018-07-18 Online:2018-12-25 Published:2018-12-27

摘要/Abstract

摘要： 以光皮树果油（WFO）和橡胶籽油（RSO）为原料，采用过氧乙酸法制备环氧化光皮树果油（EWFO）和环氧化橡胶籽油（ERSO），并以四氟硼酸为催化剂，乙二醇为羟基化试剂，对EWFO和ERSO进行羟基化改性制备羟基化光皮树果油（HWFO）和羟基化橡胶籽油（HRSO）。正交试验结果表明：EWFO的最佳制备工艺为WFO原料质量30 g，乙酸用量11 g，双氧水用量23 g，浓硫酸用量0.4 g，反应时间2 h，反应温度65℃，此条件下制备的EWFO的环氧值可达4.13%。以产物羟值为考察目标，对EWFO和ERSO羟基化条件进行优化，结果表明：m（乙二醇）：m（ERSO）=3：1，催化剂用量1%，90℃反应2 h的优化条件下，HRSO的羟值可达241.1 mg/g；催化剂用量1%，m（乙二醇）：m（EWFO）=2：1，100℃反应2 h的优化条件下，HWFO的羟值可达179.7 mg/g。FT-IR和¹H NMR分析结果表明：在上述实验条件下，环氧化和羟基化反应均顺利进行，得到了相应的环氧化木本油脂和羟基化木本油脂。

关键词: 光皮树果油, 橡胶籽油, 环氧化, 羟基化

Abstract: The epoxidized wilsoniana fruit oil (EWFO) and epoxidized rubber seed oil (ERSO) were prepared by peracetic acid method from wilsoniana oil (WFO) and rubber seed oil (RSO). The hydroxylation of EWFO and ERSO were carried out to obtain hydroxyl wilsoniana fruit oil (HWFO) and hydroxyl rubber seed oil (HRSO) using tetrafluoroborate as catalyst, and ethylene glycol as the hydroxyl reagent. The results of orthogonal test showed that the optimum preparation process of EWFO was as followed:the weight of WFO 30 g, the amount of acetic acid 11 g, the amount of hydrogen peroxide 23 g, the amount of concentrated sulfuric acid 0.4 g, the reaction time 2 h, the reaction temperature 65℃, and the epoxy value of the EWFO could reach 4.13%. The conditions of hydroxylation of EWFO and ERSO were potimized based on the hydroxy value of hydroxylation products. The results showed that the hydroxy value of the HRSO could reach 241.1 mg/g under the conditions of m(ethylene glycol):m(ERSO)=3:1, the amount of catalyst 1%,90℃ and 2 h; the hydroxy value of HWFO could reach 179.7 mg/g under the conditions of m(ethylene glycol):m(EWFO)=2:1, the amount of catalyst 1%, 100℃ and 2 h. FT-IR and ¹H NMR analyses indicated that the epoxidation and hydroxylation reactions were carried out successfully under the above experimental conditions, and the corresponding epoxy woody oil and hydroxyl woody oil were obtained.

Key words: wilsoniana fruit oil, rubber seed oil, epoxidation, hydroxylation

中图分类号:

TQ35

张飞, 胡云, 刘承果, 周永红. 羟基化木本油脂的合成及其结构表征[J]. 林产化学与工业, 2018, 38(6): 27-32.

ZHANG Fei, HU Yun, LIU Chengguo, ZHOU Yonghong. Synthesis and Characterization of Hydroxylated Woody Oil[J]. Chemistry and Industry of Forest Products, 2018, 38(6): 27-32.

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羟基化木本油脂的合成及其结构表征

Synthesis and Characterization of Hydroxylated Woody Oil

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