为了提高碱木质素的反应活性,探讨了高压条件下,以Pd/C为催化剂,氢气对碱木质素的加氢反应。研究结果表明:在催化剂的负载量3%、用量10%,温度100%,时间4h,氢气压力3MPa的条件下,反应后碱木质素的总羟基、醇羟基和酚羟基含量分别为15.69%、11.45%、4.24%,较反应前分别提高了158.1%、310.4%、28.9%。^1H-NMR分析显示,代表羰基和羧基的质子吸收减少,而代表酚羟基和醇羟基的质子吸收增加。GPC分析表明,碱木质素结构单元间的缩合减少,质均分子质量和数均分子质量在反应后都有所下降,碱木质素的多分散性增大。元素分析显示,C和H的含量在反应后都有所增加,而O含量降低,表明碱木质素发生了还原反应。
To improve the reactivity of alkali lignin, hydrogenation modification reaction with H2 and catalyzed by Pd/C catalyst at the high pressure was carried out. Results showed that: at the condition of 3% loading of Pd, 10% of catalyst dosage, temperature of 100℃, time of 4 h, H2 pressure of 3 MPa, the contents of total hydroxyl, phenolic hydroxyl and alcoholic hydroxyl of alkali lignin are 15.69% , 4.24% and 11.45%, with an increase of 158. 1% , 28. 9% and 310.4% respectively. ^1H-NMR analysis showed that protons absorptions belonging to carbonyl and carboxyl decrease, while that belonging to phenolic hydroxyl and alcoholic hydroxyl increase. GPC analysis indicated that the condensation of lignin structure unit reduces, and both weight average and number average molecular weight decrease, so the polydispersity of alkali lignin increases. EA analysis showed that both of the contents of C and H increase, while that of O decreases, indicating that alkali lignin suffers deoxidization reaction.