NEW PREPARATION METHOD FOR HIGHLY DISPERSED METAL COMPOUNDS-CARBON BASED CATALYST BY CARBOTHERMAL REDUCTION METHOD

(1)利用金属离子交换金属在氮气中的碳热还原(MIER-CTR法)制备了纳米级超细金属化合物(铜、镍、铂、钛、钨、锌等)。(2)各种金属化合物(金属、氧化物、碳化物、氮化物、硫化物、硫化物等)。采用离子交换树脂、气球和热处理温度相结合的方法，在多孔炭基质中选择性地制备了多孔炭。在碳化过程中，分别在N_2、H_2-N_2和NH_3-H_2-N_2气流系统下，在炭基质中选择性地制备了W、金属、氧化物和氮化物。(3)碳化样品的孔径控制在4-7 nm左右。以离子树脂吸附Ni^&lt；2+&gt；，Co^&lt；2+&gt；或Fe^&lt；2+/3+&gt；为原料，经碳热还原反应合成。研究了它们的孔结构和气体吸附性能。(4)与常规浸渍法制备的催化剂相比，Mier-CTR法制备的碳基催化剂具有更高的活性和更长的寿命。特别是催化活化了分子氧，表现出了良好的催化活性。(5)MIER-CTR法制备的纳米硬质超细粒子(碳化物、氮化物和Fe、Mo、W的氧化物)-多孔碳基复合材料表现出弹性和残余磁化作用。将木屑浸渍到硝酸铜和硝酸锌的混合水溶液中，得到了高度分散的纳米级铜和氧化锌晶体颗粒。该炭化样品对CO_2加氢制甲醇具有较高的催化活性。

The results of this research project are as follows :(1) Nano scale ultra fine metal compounds (Cu, Ni, Pt, Ti, W,Zn and so on) implanted and highly dispersed in a porous carbon matrix were prepared by carbothermal reduction of metal ion exchanged metal (MIER-CTR method) in a stream of N_2.(2) The various metal compounds (metal, oxide, carbide, nitride, sulfide, phosfide etc.) were selectively prepared in the porous carbon matrix by the combination of ion exchange resin, gas atmonsphere- and temperature of heat treatment. Such W,metal, oxide, and nitride were selectively prepared in the carbon matrix under N_2, H_2-N_2 and NH_3-H_2-N_2 gas stream systems at the carbonization, respectively.(3) The pore size controlled carbonized samples (their pore diameter was about 4-7nm.) were synthesized by the carbothermal reduction from the ion resins on which Ni^<2+>, Co^<2+>, or Fe^<2+/3+> were adsorbed. Their pore structure and gas adsorption property were investigated.(4) The carbon-based catalysts prepared by the MIER-CTR method were more active and had more long-life time than the catalysts synthesized by the conventional impregnated method. Especially, they had the catalytically activated the molecular oxygen to show the excellent catalytic activities for the selective oxidation of benzene and olefins in liquid phase.(5) Nano size hard ultra fine particle (carbide, nitride and oxide of Fe, Mo and W) - porous carbon matrix composites prepared by the MIER-CTR showed elastics property and also had ressidual magnetization.It was found that saw dust also applicable to our MIER-CTR method. The sawdust impregnated to mixed aqueous solution of Cu (NO_3) _2 and Zn (NO_3)_2. gave the nano level Cu and ZnO crystal particle dispersed highly in the carbon matrix. This carbonized sample showed higher catalytic activity to produce methanol by hydrogenation of CO_2.