为了探讨碱木质素在甲酸盐与Pd/C体系中的水热解聚特性,选取7种甲酸盐进行实验,得到最优的工艺条件如下:甲酸镍和Pd/C用量(相对于原料,以质量分数计)10%、反应时间30 min,反应温度325℃.在该条件下,解聚产物中的液相产物得率为56.24%,4种单酚总得率为12.14%.空白样以及添加了甲酸镍与Pd/C的液相产物的高分辨质谱、有机元素分析以及热重分析结果表明,甲酸镍和Pd/C的添加有利于木质素水热反应的脱氧过程,使产物向相对分子质量更小的方向移动.
In order to explore the depolymerization characteristics of alkali lignin in the hydrothermal system with formate and Pd/C,seven kinds of formates were selected to conduct experiments. The results show that optimal conditions are a nickel formate and Pd/C amount( with respect to raw material) of 10%,a reaction time of 30 min and a reaction temperature of 325 ℃,and under such conditions,the liquid product yield in depolymerization products is 56. 24% and the overall yield of four monophenols is 12. 14%. By comparing high resolution mass spectra,organic elements and thermogravimetric characteristics of the control sample with those of the sample with nickel formate and Pd/C,it is found that the addition of nickel formate and Pd/C is helpful in the deoxygenation process of hydrothermal reaction of lignin,and causes more products of smaller relative molecular mass to produce.