从麦草碱法制浆黑液中提取木质素,精制后,以苯乙酮为木质素的模型化合物,对催化剂组成及溶剂进行了考察.在此基础上,以NaBH4/I2为催化剂,无水乙醇为溶剂,对木质素进行加氢还原裂解反应研究.考察了温度和时间对木质素催化加氢效果的影响,采用红外光谱(FTIR)、元素分析及凝胶渗透色谱分析(GPC),表征木质素反应前后结构的变化.凝胶渗透色谱分析表明,加氢还原后木质素的分子量明显降低.采用自动电位滴定法测定反应前后木质素中总羟基含量,反应后木质素中总羟基含量为10.19%.得到了NaBH4/I2催化木质素加氢还原反应的最优条件:以1,2-二氯乙烷和乙醇(2∶1,v/v)作溶剂,m(NaBH4)∶m(I2)=1∶1,温度175℃,反应时间15 h.
We studied the reactivity of an osmium vinyl complex containing a coordinated hydroxyl group OsC12（PPh3）2[CH=C（PPh3）- CHPh（OH）] （1） toward bidentate ligand 1,4-bis（diphenylphosphino）butane （DPPB）, acid ligand （CO）, base （Cs2CO3） and heat. Two osmium vinyl complexes OsC12（dppb）[CH=C（PPh3）CHPh（OH）] （2） and OsCI2（CO）2（PPh3）[CH=C（PPh3）CHPh（OH）] （3）, as well as two relatively rare phosphonium-containing osmafuran complexes Os（q2-OCOO）（PPha）z[CHC（PPha）CPhO] （4） and OsClz（PPh3）z[CHC（PPh3）CPhO] （5）, were obtained in high yields from these reactions. All products were characterized by NMR spectroscopy, elemental analysis, and their structures were further confirmed by single crystal X-ray diffraction.
LIU BinZHAO QianYiWANG HuiJuanZENG BiRongCAO XiaoYuXIA HaiPing
