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徐桂转,陈炳霖,张少浩,王冬祥,李凯.超低酸催化纤维素一锅法制取糠醛工艺优化[J].农业工程学报,2018,34(19):225-231.DOI:10.11975/j.issn.1002-6819.2018.19.029
超低酸催化纤维素一锅法制取糠醛工艺优化
投稿时间:2018-06-08  修订日期:2018-09-04
中文关键词:  纤维素  酸度  生物燃料  超低酸  5-乙氧基甲基糠醛  一锅法
基金项目:河南省基础与前沿技术研究项目(162300410007)
作者单位
徐桂转 1.河南农业大学机电工程学院郑州 4500022.农业部农村可再生能源新材料与装备重点试验室郑州 450002 
陈炳霖 1.河南农业大学机电工程学院郑州 4500022.农业部农村可再生能源新材料与装备重点试验室郑州 450002 
张少浩 1.河南农业大学机电工程学院郑州 4500022.农业部农村可再生能源新材料与装备重点试验室郑州 450002 
王冬祥 1.河南农业大学机电工程学院郑州 450002 
李凯 1.河南农业大学机电工程学院郑州 450002 
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中文摘要:5-乙氧基甲基糠醛(5-ethoxymethylfurfural,EMF)是一种新型液体生物燃料,具有较高的能量密度和优良的燃烧性能,被视为未来潜在的燃料替代物。该文利用酸质量为乙醇质量0.1%的硫酸催化纤维素与乙醇在高压反应釜中一锅法制取EMF。首先进行单因素试验,然后利用响应面Box-Behnken模型研究不同影响因素对超低酸催化纤维素制取EMF收率的影响,对EMF制取工艺条件进行优化。结果表明:在反应时间、反应温度和底物浓度3个影响因素中,反应时间对超低酸催化纤维素一锅法制取EMF收率影响最大。根据Box-Behnken模型获得最佳反应条件:反应温度200 ℃、反应时间75 min、底物浓度30 g/L进行试验验证,EMF实际平均收率为14.93%,与理论预测值相对误差为2.03%,说明该模型具有较好的预测性。该研究首次提出以超低酸催化纤维素直接制取EMF,并优化了超低酸催化纤维素制取EMF的工艺条件,可为成本低廉、产量丰富的纤维素生物质制取EMF提供借鉴和参考。
Xu Guizhuan,Chen Binglin,Zhang Shaohao,Wang Dongxiang,Li Kai.Process optimization on 5-ethoxymethylfurfural production from cellulose catalyzed by extremely low acid in one-pot reaction[J].Transactions of the Chinese Society of Agricultural Engineering (Transactions of the CSAE),2018,34(19):225-231.DOI:10.11975/j.issn.1002-6819.2018.19.029
Process optimization on 5-ethoxymethylfurfural production from cellulose catalyzed by extremely low acid in one-pot reaction
Author NameAffiliation
Xu Guizhuan 1. College of Mechanical and Electrical Engineering, Henan Agricultural University, Zhengzhou 450002, China
2. Key Laboratory of New Materials and Facilities for Rural Renewable Energy, Ministry of Agriculture, Zhengzhou 450002, China 
Chen Binglin 1. College of Mechanical and Electrical Engineering, Henan Agricultural University, Zhengzhou 450002, China
2. Key Laboratory of New Materials and Facilities for Rural Renewable Energy, Ministry of Agriculture, Zhengzhou 450002, China 
Zhang Shaohao 1. College of Mechanical and Electrical Engineering, Henan Agricultural University, Zhengzhou 450002, China
2. Key Laboratory of New Materials and Facilities for Rural Renewable Energy, Ministry of Agriculture, Zhengzhou 450002, China 
Wang Dongxiang 1. College of Mechanical and Electrical Engineering, Henan Agricultural University, Zhengzhou 450002, China
 
Li Kai 1. College of Mechanical and Electrical Engineering, Henan Agricultural University, Zhengzhou 450002, China
 
Key words:cellulose  acidity  biofuels  extremely low acid  5-ethoxymethylfurfural  one-pot reaction
Abstract: With the inevitable depletion of non-renewable petroleum resources and the rising environmental concerns, renewable biomass has been regarded as a potential resource for sustainable supply of biofuels. The development of simple, cheap and sustainable catalytic process for the production of biofuels has become a major target. Among the promising biofuels, EMF (5-ethoxymethylfurfural) has been considered as a new generation of biofuel or fuel additive due to its unique properties, such as its liquid characteristics under room temperature, non-toxicity, high lubricity, stable flashpoint and excellent flow properties under cold conditions. Recently, an increasing number of reports have been focused on the direct conversion of carbohydrates and platform chemicals such as 5-hydroxymethylfurfural (HMF), fructose, sucrose, or inulin into EMF catalyzed by different catalysts. However, from a point of view that raw materials are cheap and rich, it is more valuable to use cellulose or cellulosic biomass instead of model compounds, such as HMF and fructose, for the production of EMF. In the existing researches, cellulose was usually used as raw material to be converted into intermediate product HMF, 5-chloromethylfurfural (CMF) or 5-bromomethylfurfural (BMF), and so on, and then the target product EMF was obtained through the intermediate product. Using cheap and renewable cellulose as the raw material, and ethanol as the solvent, and combining the dehydration of cellulose to HMF, followed by the etherification of HMF to EMF in one-pot, is a more attractive reaction pathway. This one-pot reaction avoids the isolation and purification of HMF, which saves time, energy and solvent. The side reaction of process using extremely low sulfuric acid is slight, in which standard grade stainless steel facility can be used instead of high nickel alloy, which has a significant cost advantage in the equipment. In this paper, sulfuric acid with ultra low mass concentration (0.1% of the mass of ethanol) was used as catalyst to catalyze cellulose and ethanol to produce EMF in one-pot reaction. The effects of temperature, reaction time and substrate concentration on EMF yield were firstly studied and then the response surface methodology was used to design experiments to optimize the reaction conditions. The interactions of factors and the optimum reaction conditions were obtained. The results showed that the reaction temperature was the factor that mostly impacted the one-pot EMF production from cellulose and ethanol catalyzed by sulfuric acid with ultra low mass concentration. The maximum mean EMF yield of 14.93% was obtained under the optimum reaction conditions: reaction temperature of 200 ℃, reaction time of 75 min and substrate concentration of 30 g/L, with the prediction error of 2.03%, which showed that the model had a good fitting property. Compared to other studies, the study showed that EMF can be obtained directly from cellulose catalyzed by extremely low acid in one-pot reaction for the first time. The process conditions for producing EMF from cellulose catalyzed by extremely low acid in one-pot reaction had been optimized. This study can provide reference for the EMF one-pot production from much cheaper and abundant cellulosic biomass such as agricultural wastes catalyzed by sulfuric acid with extremely low concentration.
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