Demonstration of a Process for the Conversion of Kraft Lignin into Vanillin and Methyl Vanillate by Acidic Oxidation in Aqueous Methanol
Demonstration of a Process for the Conversion of Kraft Lignin into Vanillin and Methyl Vanillate by Acidic Oxidation in Aqueous Methanol
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DOI：
10.1021/ie901293p
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发表时间：
2010-01
影响因子：
4.2
通讯作者：
T. Voitl;P. Rohr
中科院分区：
文献类型：
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作者：
T. Voitl;P. Rohr
本文研究了以工业木质素为原料，在酸性条件下在甲醇水溶液中氧化制备香兰素和香兰素甲酯的工艺。进行了一系列连续运行，包括硫酸盐木质素氧化，单体提取和残余木质素过滤的步骤。以80 vol %的甲醇/水为溶剂，H3PMo12O40为均相催化剂，初始氧气为10 bar，在搅拌间歇式反应器中进行硫酸盐木质素的解聚（1 g /次）。采用氯仿萃取法回收单体产物，并采用气相色谱/质谱法（GC/MS）进行定量分析。通过过滤回收反应介质中残留的硫酸盐木质素。萃取和过滤后，含有均相催化剂的反应介质在下次运行中重复使用。所有量化产物（气相、萃取物和固体）的总和以及消耗的氧气量在…之后达到恒定水平。
In this work, a process for producing vanillin and methyl vanillate from an industrial kraft lignin by oxidation in aqueous methanol at acidic pH is proposed. A series of consecutive runs, comprising the steps of kraft lignin oxidation, monomer extraction, and filtration of residual lignin, were conducted. The depolymerization of kraft lignin (1 g per run) was carried out in a stirred batch reactor with 80 vol % methanol/water as the solvent, with H3PMo12O40 as a homogeneous catalyst, and with 10 bar of oxygen initially present. The monomeric products were recovered from the process by extraction with chloroform and quantified by gas chromatography/mass spectrometry (GC/MS). Residual kraft lignin was recovered from the reaction medium by filtration. After extraction and filtration, the reaction medium, containing the homogeneous catalyst, was reused in the next run. The sum of all quantified products (gas phase, extract, and solids), as well as the amount of consumed oxygen, reached constant levels after ...