木质素模型化合物的合成及木质素磺酸盐的氧化分解研究
发布时间：2018-08-24 12:00
【摘要】：由于受到化石燃料短缺和全球环境污染的制约,充分利用天然的可再生资源-木质素,已经成为广大科学工作者的研究热点。木质素是一种广阔的可再生的资源,能够可持续生产清洁燃料和基础有机化工原料。木质素氧化降解可以产生多种芳香族物质及常用的有机小分子化合物,可以为香料、医药和农药等行业提供原料。然而由于木质素复杂的分子结构等原因,导致对其基础研究不深入,应用研究也不全面,影响了木质素的本来具备的工业利用价值。因此研究低成本、绿色环保的高效催化剂和氧化剂,在温和的条件下催化氧化降解木质素成为如今的研究热点。本文介绍了木质素模型化合物愈创木基丙三醇-p-愈创木基醚的一种重要中间体4-(α-溴代乙酰基)-愈创木酚的合成过程。以愈创木酚为原料,详细全面探索了反应温度、反应时间、原料摩尔比、催化剂用量等对反应的影响。4-乙酰基愈创木酚的最优合成条件为：愈创木酚用量6.3 g,无水乙酸钠用量2.5 g,反应温度95℃,催化剂PPA0.5g,用量按其与底物的质量比(0.08：01)加入,反应时间90 min,得到4-乙酰基愈创木酚的产率为67.5%。4-(a-溴代乙酰基)-愈创木酚的最优合成条件为：溴化铜用量4.5 g(0.02mol),4-乙酰基愈创木酚用量2.0 g(0.012 mo1),反应温度75℃,溶剂乙酸乙酯和氯仿用量分别为40 ml,反应时间为100 min,得到4-(α-溴代乙酰基)-愈创木酚的产率为88.1%。在木质素磺酸钠的氧化降解过程中,使用了两类不同催化剂：无机盐催化剂(氯化锌、硫酸铜、硫酸钻)和新型咔咯类(咔咯钴、咔咯铁)催化剂。研究探索了常压条件下的各种反应条件对木质素磺酸盐的降解产物产率的影响。得到了一种较为理想的常压降解条件：在200 mL,1.5 mol/L的氢氧化钠溶液中充分溶解10.0 g木质素磺酸钠,再加入0.5 g硫酸铜作为催化剂,通入氧气量为20 mL/min(或过氧化氢体积25 mL),反应温度为30℃,反应时间40 mmin,此时木质素磺酸钠的降解率达到最大化。
[Abstract]:Due to the shortage of fossil fuels and the global environmental pollution, the utilization of lignin, a natural renewable resource, has become a hot research topic for many scientists. Lignin is a broad renewable resource, which can produce clean fuel and basic organic chemical raw materials. Lignin oxidative degradation can produce a variety of aromatic substances and commonly used organic small molecular compounds, and can be used as raw materials for spice, medicine and pesticide industries. However, because of the complex molecular structure of lignin, the basic research of lignin is not thorough and the applied research is not comprehensive, which affects the industrial utilization value of lignin. Therefore, the research on low cost, green and environmental efficient catalysts and oxidants, catalytic oxidation and degradation of lignin under mild conditions has become a hot research topic. In this paper, the synthesis process of 4- (伪 -bromoacetyl) guaiacol, an important intermediate of the lignin model compound, is described. The reaction temperature, reaction time and molar ratio of guaiacol were studied in detail. The optimum synthesis conditions of guaiacol were as follows: guaiacol 6.3 g, anhydrous sodium acetate 2.5 g, reaction temperature 95 鈩，
本文编号：2200763
[Abstract]:Due to the shortage of fossil fuels and the global environmental pollution, the utilization of lignin, a natural renewable resource, has become a hot research topic for many scientists. Lignin is a broad renewable resource, which can produce clean fuel and basic organic chemical raw materials. Lignin oxidative degradation can produce a variety of aromatic substances and commonly used organic small molecular compounds, and can be used as raw materials for spice, medicine and pesticide industries. However, because of the complex molecular structure of lignin, the basic research of lignin is not thorough and the applied research is not comprehensive, which affects the industrial utilization value of lignin. Therefore, the research on low cost, green and environmental efficient catalysts and oxidants, catalytic oxidation and degradation of lignin under mild conditions has become a hot research topic. In this paper, the synthesis process of 4- (伪 -bromoacetyl) guaiacol, an important intermediate of the lignin model compound, is described. The reaction temperature, reaction time and molar ratio of guaiacol were studied in detail. The optimum synthesis conditions of guaiacol were as follows: guaiacol 6.3 g, anhydrous sodium acetate 2.5 g, reaction temperature 95 鈩，
本文编号：2200763
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