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采用微波辅助加热,在甲酸溶剂体系下(甲酸,分析纯)液相降解黑液木质素,获得以单酚类化合物为主的油1相和木质素部分降解并能溶于乙酸乙酯的大分子物质的油2相产物。实验研究加热温度(110~180℃)、反应时间(5~90 min)、微波功率(400~1000 W)和液固比(6~16 m L/g)对油相产率以及单酚类化合物分布特性的影响规律。当温度为160℃,反应时间为30 min时,微波功率为600 W,液固比为12 m L/g时油相总产率达到最大值,其中油1产率最高为9.69%,油2产率最高为54.39%。单酚类产物(以4-羟基-3-甲氧基苯基乙酮、4-羟基-3-甲氧基苯基丙酮和4-羟基-3,5-二甲氧基苯基乙酮为主)的分布受温度、时间、功率和液固比的影响较为明显。基于实验结论解析,对产物中主要的guaiacol(G)类和syringol(S)类化合物的形成机理做出推断。
Using microwave-assisted heating, the liquid lignin of black liquor was degraded in the formic acid solvent system (formic acid, analytical grade) to obtain a mixture of oil-based lignin and lignin partially degraded and dissolved in ethyl acetate Molecular 2-phase oil product. The effects of heating temperature (110-180 ℃), reaction time (5-90 min), microwave power (400-1000 W) and liquid-solid ratio (6-16 m L / g) Influence of compound distribution characteristics. When the temperature is 160 ℃, the reaction time is 30 min, the microwave power is 600 W and the liquid-solid ratio is 12 m L / g, the total oil yield reaches the maximum value, the highest oil yield is 9.69% The highest yield was 54.39%. The monophenolic products (prepared with 4-hydroxy-3-methoxyphenylethanone, 4-hydroxy-3-methoxyphenylacetone and 4-hydroxy-3,5-dimethoxyphenylethanone as Main) distribution by the temperature, time, power and liquid-solid ratio of the more obvious. Based on the experimental results, the formation mechanism of the main guaiacol (G) and syringol (S) compounds in the product was deduced.