农作物秸秆加压液化制备乙酰丙酸乙酯及其分离初探

doi:10.3969/j.issn.0253-2417.2016.04.018

林产化学与工业 ›› 2016, Vol. 36 ›› Issue (4): 128-134.doi: 10.3969/j.issn.0253-2417.2016.04.018

农作物秸秆加压液化制备乙酰丙酸乙酯及其分离初探

关倩¹, 蒋剑春^1,2, 徐俊明^1,2, 王奎^1,2, 冯君锋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. 江苏强林生物能源材料有限公司, 江苏溧阳 213364

收稿日期:2015-07-17 出版日期:2016-08-25 发布日期:2016-09-01
通讯作者: 蒋剑春,男,研究员,博士,博士生导师,研究领域为生物质能源与炭材料;E-mail:bio-energy@163.com。 E-mail:bio-energy@163.com
作者简介:关倩(1986-),女,河南鹿邑人,博士生,主要从事生物质液化油的制备与精炼研究工作
基金资助:
“十二五”农村领域国家科技计划课题（2015BAD15B06）；国家自然科学基金优秀青年基金项目（31422013）

Preliminary Study on Pressurized Liquefaction of Three Crops Straw for Preparation of Ethyl Levulinate

GUAN Qian¹, JIANG Jian-chun^1,2, XU Jun-ming^1,2, WANG Kui^1,2, FENG Jun-feng¹

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 Qianglin Bio-energy and Bio-materials Co., Ltd., Liyang 213364, China

Received:2015-07-17 Online:2016-08-25 Published:2016-09-01

摘要/Abstract

摘要： 分别选取小麦、玉米和水稻等3种农作物的秸秆为原料，乙醇为溶剂，98%浓硫酸为催化剂，在反应压力2.25 MPa，反应温度200℃，催化剂用量5%，反应时间60 min和固液比1：15（质量比）的条件下，进行加压液化的初步研究，对液化产物进行分析，并分离得到液化产物中的乙酰丙酸乙酯（EL）。结果显示：同等液化条件下，所选原料中小麦秸秆的液化效果最好；FT-IR、TG-DTG和SEM分析表明液化过程中小麦秸秆组分的结构发生改变和降解，液化产物的主要组分为EL，在水相的乙酸乙酯萃取液中EL的GC含量为52.61%；在蒸馏分离的过程中，EL的纯度可达92.71%，回收率达89.93%。

关键词: 农作物秸秆, 加压液化, 乙酰丙酸乙酯, 蒸馏分离

Abstract: Three kinds of crops (wheat, corn and rice) straw were selected as raw materials for pressurized liquefaction. Ethanol and concentrated sulfuric acid (98%) were used as solvent and catalyst, respectively. The liquefaction was carried out under the conditions of reaction temperature 200℃, the dosage of catalyst 5%, the reaction time 60 min and the solid-liquid ratio 1:15. Products of liquefaction were analyzed, and ethyl levulinate (EL) was isolated from the liquefaction products. The results showed that under the same liquefaction conditions, wheat straw performed high liquefied performance. The structure of straw components was changed and degraded. Ethyl levulinate was the main component of liquefaction products. The purity and recovery rate of ethyl levulinate isolated by distillation were 92.71% and 89.93%, respectively.

Key words: crops straw, pressurized liquefaction, ethyl levulinate, distillation separation

中图分类号:

TQ35
TK6

关倩, 蒋剑春, 徐俊明, 王奎, 冯君锋. 农作物秸秆加压液化制备乙酰丙酸乙酯及其分离初探[J]. 林产化学与工业, 2016, 36(4): 128-134.

GUAN Qian, JIANG Jian-chun, XU Jun-ming, WANG Kui, FENG Jun-feng. Preliminary Study on Pressurized Liquefaction of Three Crops Straw for Preparation of Ethyl Levulinate[J]. Chemistry and Industry of Forest Products, 2016, 36(4): 128-134.

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农作物秸秆加压液化制备乙酰丙酸乙酯及其分离初探

Preliminary Study on Pressurized Liquefaction of Three Crops Straw for Preparation of Ethyl Levulinate

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