微晶纤维素复合溶剂醇解制备乙酰丙酸甲酯的研究  

Conversion of microcrystalline cellulose into methyl levulinate in mixed solvents

作　　者：贺小亮[1] 蒋剑春[1] 冯君锋 司展[1] 

机构地区：[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

出　　处：《现代化工》2014年第7期89-93,共5页Modern Chemical Industry

基　　金：林业公益性行业科研专项经费项目(201204801)

摘　　要：以微晶纤维素为原料,甘油-甲醇复合溶剂为液化剂,研究了不同催化剂、反应温度、催化剂用量、反应时间、甘油/甲醇质量比对微晶纤维素液化及乙酰丙酸甲酯得率的影响。实验的较佳工艺条件为:硫酸为催化剂,液化温度为200℃,硫酸用量为0.25 g,反应时间为30 min,甘油/甲醇质量比为10/50,该条件下液化转化率为93.7%,乙酰丙酸甲酯得率为25.05%。对液化产物进行GC-MS分析结果表明,反应温度为180℃时,液化产物中含有大量未反应的甘油和部分甲基糖苷;200℃时绝大部分甘油已反应,且此温度条件下乙酰丙酸甲酯的含量最高,达到26.838%;在220℃和240℃时,甘油完全反应,液化产物更加复杂。By using microcrystalline cellulose as raw material,mixed solvent of glycerin and methanol as liquid agent,the effects of different catalyst,reaction temperature,catalyst dosage,residence time and mass ratio of glycerin to methanol on microcrystalline cellulose liquefaction conversion and methyl levulinate（ MLA） yield are studied. The optimal conditions are as follows： sulfuric acid as catalyst,200℃ of reaction temperature,0. 25 g of sulfuric acid dosage,30 minutes of residence time,10 /50 of mass ratio of glycerin to methanol. The liquefaction conversion rate and MLA yield are 93. 7% and 25. 05%,respectively. It means that cellulose can be effectively liquefied and produce methyl levulinate.The gas chromatograph-mass spectrometer is used for analyzing the liquefaction products components. The analysis results of GC-MS on liquid show that when the reaction temperature is 180℃,there are a large amount unreacted glycerin and some methyl glucoside in the liquid product. When the temperature is 200℃,most of glycerins are reacted and the content of MLA can reach 26. 838% in the product. At 220℃ and 240℃,all of the glycerins are converted to other products,which makes the liquefaction products more complicated.

关 键 词：微晶纤维素 复合溶剂 醇解 乙酰丙酸甲酯 

分 类 号：TQ35[化学工程] TK6[动力工程及工程热物理—生物能]