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林产化学与工业 ›› 2013, Vol. 33 ›› Issue (4): 67-72.doi: 10.3969/j.issn.0253-2417.2013.04.013

• 1研究报告 • 上一篇    下一篇

甘油-甲醇复合溶剂液化杂木屑实验研究

杨中志, 蒋剑春, 徐俊明, 胡亿明   

  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
  • 收稿日期:2012-06-26 修回日期:1900-01-01 出版日期:2013-08-30 发布日期:2013-08-30
  • 通讯作者: 蒋剑春(1955- ),男,研究员,博士,主要从事生物质能源与活性炭方面的研究;E-mail:bio-energy@163.com。

Liquefaction of Sawdust Using Glycerin and Methanol Mixture as Solvents

YANG Zhong-zhi, JIANG Jian-chun, XU Jun-ming, HU Yi-ming   

  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
  • Received:2012-06-26 Revised:1900-01-01 Online:2013-08-30 Published:2013-08-30

摘要: 采用甘油-甲醇复合溶剂体系,利用高温高压下甲醇的亚/超临界效应,探索了反应时间、反应温度、催化剂种类及用量等条件对杂木屑液化效果的影响。研究结果表明:甲醇30g,甘油12g,草酸0.25g,粒径在0.28~0.90mm范围内的混合木屑6g,在290℃下反应40min,然后自然冷却至室温,即可获得很好的液化效果,木屑转化率为92.79%。采用GC-MS、FT-IR、GPC等技术手段测定了液化油的物质组成与基团结构,详细研究了水分含量、酸值、黏度等物理学性质。结果表明,液化油的物质构成较复杂,但主要是一些含氧衍生物,包括醇类、醚类、酯类和酚类化合物;液化油主要由小分子物质构成,相对分子质量分布在2 300以下。

关键词: 复合溶剂, 亚/超临界效应, 木屑, 液化

Abstract: The mixed sawdust was liquefied by glycerin and methanol as mixed solvents using a 1 L stainless steel high-pressure autovalve. This reaction was carried out at critical/supercritical effect of methanol in high temperature and pressure. The influence of reaction conditions such as reaction time, reaction temperature, catalyst types and dosage on liquefaction reactions was investigated. The results showed that the optimal liquefaction conditions of the mixed sawdust is methanol 30 g, glycerin 10 g, oxalic acid 0.25 g, mix sawdust 6 g(0.28-0.90 mm), at 290℃ with reaction time 40 min. Under this reaction conditions, the conversion of sawdust is up to 92.79%. Various analysis methods such as Gas chromatography-mass spectrometer(GC-MS), fourier transform infrared spectroscopy (FT-IR) and gel permeation chromatography(GPC) were used to analyze the composition and molecular structure of the liquefaction oil. Moisture, acid value, viscosity and other properties of the liquefied product were also studied. The analytical results showed that the liquefaction oil is complex compounds, which mainly contains oxygen derivatives such as alcohol, ether, ester and hydroxybenzene, etc. The liquefaction oil consists of low molecular weight components, i.e., which is below 2 300.

Key words: mix solvents, critical or supercritical effects, sawdust, liquefaction

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