环氧脱水蓖麻油的制备工艺研究

doi:10.3969/j.issn.0253-2417.2015.04.007

林产化学与工业 ›› 2015, Vol. 35 ›› Issue (4): 41-47.doi: 10.3969/j.issn.0253-2417.2015.04.007

环氧脱水蓖麻油的制备工艺研究

黄旭娟¹, 刘鹤¹, 商士斌^1,2, 齐帆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:2014-05-28 出版日期:2015-08-25 发布日期:2015-08-29
通讯作者: 商士斌(1964—),男,研究员,博士生导师,研究领域为生物质资源的化学研究与利用;E-mail:shangsb@hotmail.com。 E-mail:shangsb@hotmail.com
作者简介:黄旭娟(1991—),女,江苏常熟人,硕士生,主要从事松脂化学利用的研究
基金资助:
国家自然科学基金资助项目(31200446);江苏省自然科学基金资助项目(BK2012063);中国林科院林业新技术所基本科研业务费专项资金(CAFINT2012C05)

Synthesis Process of Epoxidized Dehydrated Castor Oil

HUANG Xu-juan¹, LIU He¹, SHANG Shi-bin^1,2, QI Fan¹

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. Research Institute of Forestry New Technology, CAF, Beijing 100091, China

Received:2014-05-28 Online:2015-08-25 Published:2015-08-29

摘要/Abstract

摘要： 以蓖麻油(CTO)为原料,先制备脱水蓖麻油(DCO),再以磷酸为催化剂,过氧乙酸为氧化剂,进行环氧化反应制备环氧脱水蓖麻油(EDCO),通过单因素和正交试验优化不同条件对产品环氧值的影响。结果表明,制备EDCO较佳工艺条件为反应温度30 ℃、反应时间3.5 h、DCO与过氧乙酸物质的量之比5.5:1、磷酸用量0.5%,此条件下所得EDCO的环氧值达到4.82%。采用FT-IR和 ¹H NMR 表征了蓖麻油、脱水蓖麻油以及环氧脱水蓖麻油的化学结构,结果证实EDCO中C=C被环氧化后基本消失,生成了环氧键。通过黏度测定、热重分析(TG)等方法对产品的性能进行了分析,得到CTO黏度为1100.0 mPa·s,DCO黏度为299.5 mPa·s,EDCO黏度为1896.0 mPa·s;产品的热稳定性顺序为EDCO> DCO> CTO。

关键词: 过氧乙酸, 环氧化, 环氧脱水蓖麻油

Abstract: Dehydrated castor oil(DCO) was firstly prepared by using castor oil(CTO) as raw material via dehydration reaction, and epoxidized dehydrated castor oil(EDCO) was synthesized using phosphoric acid as catalyst and acetic acid peroxide as the oxidant by epoxidation reaction afterwards. The influences of different parameters on the epoxy value of EDCO were investigated through single factor and orthogonal experiments. The results indicated that the optimal preparation conditions of EDCO were 3.5 h reaction time, 30 ℃ reaction temperature, 5.5:1 molar ratio of peracetic acid to DCO and 0.5％ phosphoric acid dosage. The epoxy value of EDCO could be up to 4.82% under these conditions. In addition, the chemical structures of CTO, DCO, and EDCO were characterized by FT-IR and ¹H NMR . It was confirmed that the C=C double bonds in EDCO almost disappeared and the epoxy bonds were formed during the epoxidation. The properties of the products were also studied by viscosity measurement and thermogravimetric analysis(TG). Viscosity measurement showed that the viscosities of CTO, DCO, and EDCO were 1100.0, 299.5 and 1896.0 mPa·s, respectively. TG analysis demonstrated that the descending order of thermal stability of the products was EDCO> DCO> CTO.

Key words: peracetic acid, epoxidation, epoxidized dehydrated castor oil

中图分类号:

TQ35
TQ645

黄旭娟, 刘鹤, 商士斌, 齐帆. 环氧脱水蓖麻油的制备工艺研究[J]. 林产化学与工业, 2015, 35(4): 41-47.

HUANG Xu-juan, LIU He, SHANG Shi-bin, QI Fan. Synthesis Process of Epoxidized Dehydrated Castor Oil[J]. Chemistry and Industry of Forest Products, 2015, 35(4): 41-47.

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环氧脱水蓖麻油的制备工艺研究

Synthesis Process of Epoxidized Dehydrated Castor Oil

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