【作者】 刘学苏；

【导师】 李广学；

【作者基本信息】 安徽理工大学 ， 应用化学， 2006， 硕士

【摘要】 论文对我国造纸行业的副产物木质素磺酸钠进行了催化氧化制取香兰素的研究。对原料物质木质素磺酸钠进行了分析,利用元素分析仪分析了原料物质的元素组成,用傅立叶变换红外光谱仪考查了该物质的结构和官能团。在0.1L高压反应釜中进行木质素磺酸钠的催化氧化反应,利用正交实验考察了反应温度、反应时间、碱液浓度、木质素的浓度以及反应初始压力五个因素对反应的影响,得到了最佳的反应工艺条件。根据实验结果研究了该反应的宏观动力学,由曲线拟合法得出140℃时反应的宏观反应速率方程。 （1）由元素分析可知,原料物质主要由碳、氢、氧、硫组成,分子式可表示为C₉H_10.4O_3.6S_0.4。由红外光谱分析可知该物质含有大量的甲氧基、羟基、愈创木基和紫丁香基结构。 （2）用正交实验考察了五个因素对反应的影响,由极差分析得到了木质素磺酸钠催化氧化制取香兰素的最佳工艺条件为:反应时间70min,反应温度140℃,氢氧化钠浓度2.0mol·L^-1,初始压力0.8MPa,反应物浓度30g·L^-1。最佳工艺条件下,香兰素的收率可达7.2%。 （3）由曲线拟合法得出140℃反应的宏观反应速率方程如下:r=1.6665×10^-12t⁷-4.6614×10^-10t⁶+4.9869×10^-8t⁵-2.5474×10^-6t⁴+6.3473×10^-5t³-7.5057×10^-4t²+5.317×10^-3t-0.009881由分析可知产物香兰素的浓度变化较大,反应的最佳结束点在65min左右。更多还原

【Abstract】 Lignosulfonate obtained from black liquor of papermaking industry was investigated to prepare vanillin through catalytic oxidation process. the element composition、 structure、 functional group of raw material were analyzed by element analysis and FTIR. The experiments were carried out in a 0.1L autoclave .CuSO₄ was used as the catalyst. These reactions investigated the effects of reaction temperature, reaction time, the initial pressure of O₂, the contents of NaOH, the proportion of lignosulfonate by orthogonal testing , then got the optimal reaction condition. Finally the macrokinetics of the reaction was investigated.（1 ）The element analysis showed that lignosulfonate was composed of C、H、O、 S and the formula could express as C₉H_10.4O_3.6S_0.4 .The FTIR spectrum showed there were a lot of groups such as methoxy group、 hydroxy group、 guaiacyl group、 syringyl group.（2）The optimal reaction condition was as follows: reaction time 70min, reaction temperature 140℃, concentration of NaOH 2.0 mol.L^-1, initial pressure 0.8MPa,. concentration of raw material 30 g.L^-1 , the best yield of vanillin from oxygenation of lignosulfonate was about 7.2%.（3）The macroreaction rate equation was obtained by curve fitting, the concentration of vanillin changed in a extensive range. The optimal ending point was about 65min.更多还原