氢等离子体法制备金属磷化物及其加氢脱硫催化性能研究
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摘要
过渡金属磷化物作为一类新型半导体材料可广泛应用于光电、磁、催化等领域。金属磷化物作为催化剂常采用程序升温还原法制备,但该法制备温度高,磷物种易损失,且高温制备容易导致催化剂颗粒烧结。本论文用氢等离子体还原法(PR)制备了一系列过渡金属磷化物,考察并优化了磷化镍(Ni2P)、磷化钻(CoP)、磷化钼(MoP)和磷化钨(WP)的制备条件；采用典型含硫化合物二苯并噻吩(DBT)和4,6二甲基二苯并噻吩(4,6-DMDBT),考察了金属磷化物的加氢脱硫催化反应性能；采用XRD、CO化学吸附、TPR、HRTEM、SEM、ICP-AES等对金属磷化物的结构进行了表征,初步研究了氢等离子体还原法制备过渡金属磷化物的反应机理。
论文系统考察了电压、放电时间、金属与磷的原子比(M/P)及加入贵金属对体相Ni2P, CoP, MoP和WP制备的影响。结果表明,提高电压和增加还原时间有利于提高所制备的金属磷化物的晶化程度；当金属磷化物存在一种晶型(如WP和MoP)时,氧化物前体中M/P影响其晶化程度；当存在多种晶型时,M/P比决定了金属磷化物的晶体结构；PR法可以按化学计量比制备金属磷化物,而不需要在其前体引入过量的磷；少量引入贵金属(如Ru)可进一步缓和制备条件；采用PR法可制备磷化镓(GaP)、磷化铟(InP)、磷化铁(Fe2P)等重要半导体材料。
采用PR法和传统程序升温还原法制备了体相Ni2P、CoP、MoP和WP,比较了不同方法制备的体相磷化物在DBT加氢脱硫反应中的催化性能；研究了制备条件和钝化方法对磷化物晶化度和加氢脱硫催化反应的影响规律。发现PR法制备的催化剂比传统程序升温法制备的活性高；PR法制备的体相磷化物活性顺序为CoP>Ni2P>MoP≈WP。
研究发现CoP在四种金属磷化物中制备条件最为苛刻,且易于形成加氢脱硫活性很低的Co2P相,因而采用传统程序升温还原法制备的CoP催化剂在加氢脱硫反应中表现出最低的活性。当在氧化物前体中引入少量Ru时,可以在较温和条件下制备出高结晶度、高活性CoP催化剂。反应评价结果表明,Ru的引入主要促进了CoP的形成,改善了晶粒的分散,但没有明显改变催化反应过程和活性中心本质。
用PR法制备了MCM-41担载的WP、MoP和Ni2P催化剂,以DBT和4,6-DMDBT的十氢萘溶液为模拟油考察了其加氢脱硫反应性能。对混合物料HDS活性顺序为：WP>MoP>Ni2P, WP和MoP以加氢脱硫路径为主,Ni2P以直接脱硫路径为主。若将WP/MCM-41与Ni2P/MCM-41机械混合,则可以同时高效脱除DBT和4,6-DMDBT。此外,比较了不同方法制备的Ni-W-P在加氢脱硫反应中的催化活性,其活性顺序顺序为：先硫化后还原法>PR法>先混合后还原法(MR)>>共浸渍法。共浸渍法制备的Ni-W-P活性低的主要原因是有杂晶生成。
Transition metal phosphides are attractive candidates for high-performance catalytic, electronic, and magnetic applications. A variety of methods can be used to synthesize bulk metal phosphides. Amoung them, temperature programmed reduction (TPR) of metal phosphates at high temperature was generally feasible for the preparation of supported transition-metal phosphides for using as hydrotreating or hydrogenation catalysts, but the particles were always aggregated, and phosphorus loss occured at high reduction temperature. In this paper, we describe a new strategy for synthesizing metal phosphides (Ni2P, CoP, MoP and WP) that using nonthermal hydrogen plasma as the reduction medium instead of the H2 used in the TPR method, and the HDS acitivity of DBT and 4,6-DMDBT was evaluated. XRD, CO chemisorption, TPR, HRTEM, SEM, ICP-AES techniques were used to characterize the structures of the metal phosphides. The mechanism of phosphide preparation with PR method was also speculated.
Bulk metal phosphides were prepared with PR method, the effect of voltage, reduction time, M/P ratio and doping of noble metal on the phosphide phase formation were investigated. The results told that under higher voltage, longer reduction time, the phosphides were better crystallized. For MoP and WP, the M/P ratio influenced the crystallization, while for Ni2P and CoP, it determined phase of the phosphide. The reduciton voltage of oxidic precursors could be lower down by co-impregnation of Ru; InP, GaP, Fe2P were also be prepared by hydrogen plasma method (PR).
Transition metal phosphides (Ni2P, CoP, MoP, WP) were prepared by TPR and PR method, the HDS performance was also compared. The influence of the M/P ratio, voltage and passivation method on the HDS performances of the phosphides prepared with PR method was examined. The results indicated that catalysts prepared by PR method showed higher DBT HDS activity then TPR method. And the activity of phosphides prepared by PR method was in the following order:CoP>Ni2P>MoP≈WP。
CoP was more difficult to be prepared then MoP, N12P and WP, and Co2P which owned low HDS activity could easily formed, so the activity of CoP prepared by TPR method showed lower HDS activity. Better crystallised and high HDS performance CoP could be prepared with lower reduction voltage by doping oxidic CoP with Ru, the particle size of CoP was smaller and CoP phase was not changed.
The phosphides catalysts:MoP/MCM-41, WP/MCM-41 and Ni2P/MCM-41, were prepared by four methods. The HDS activity was in the following order:WP>MoP>Ni2P, WP and MoP mainly through direct hydrodesulfurization path, while direct hydrodesulfurization mainly happened on Ni2P. The mechanically mixed of them were evaluated in simultaneously HDS of DBT and 4,6-DMDBT. The results showed that there was synergistic effect between WP+Ni2P/MCM-41 which exhibited best performance; the hydrodesulfurization activity was in the following order:SR>PR>MR>>IP.
论文系统考察了电压、放电时间、金属与磷的原子比(M/P)及加入贵金属对体相Ni2P, CoP, MoP和WP制备的影响。结果表明,提高电压和增加还原时间有利于提高所制备的金属磷化物的晶化程度；当金属磷化物存在一种晶型(如WP和MoP)时,氧化物前体中M/P影响其晶化程度；当存在多种晶型时,M/P比决定了金属磷化物的晶体结构；PR法可以按化学计量比制备金属磷化物,而不需要在其前体引入过量的磷；少量引入贵金属(如Ru)可进一步缓和制备条件；采用PR法可制备磷化镓(GaP)、磷化铟(InP)、磷化铁(Fe2P)等重要半导体材料。
采用PR法和传统程序升温还原法制备了体相Ni2P、CoP、MoP和WP,比较了不同方法制备的体相磷化物在DBT加氢脱硫反应中的催化性能；研究了制备条件和钝化方法对磷化物晶化度和加氢脱硫催化反应的影响规律。发现PR法制备的催化剂比传统程序升温法制备的活性高；PR法制备的体相磷化物活性顺序为CoP>Ni2P>MoP≈WP。
研究发现CoP在四种金属磷化物中制备条件最为苛刻,且易于形成加氢脱硫活性很低的Co2P相,因而采用传统程序升温还原法制备的CoP催化剂在加氢脱硫反应中表现出最低的活性。当在氧化物前体中引入少量Ru时,可以在较温和条件下制备出高结晶度、高活性CoP催化剂。反应评价结果表明,Ru的引入主要促进了CoP的形成,改善了晶粒的分散,但没有明显改变催化反应过程和活性中心本质。
用PR法制备了MCM-41担载的WP、MoP和Ni2P催化剂,以DBT和4,6-DMDBT的十氢萘溶液为模拟油考察了其加氢脱硫反应性能。对混合物料HDS活性顺序为：WP>MoP>Ni2P, WP和MoP以加氢脱硫路径为主,Ni2P以直接脱硫路径为主。若将WP/MCM-41与Ni2P/MCM-41机械混合,则可以同时高效脱除DBT和4,6-DMDBT。此外,比较了不同方法制备的Ni-W-P在加氢脱硫反应中的催化活性,其活性顺序顺序为：先硫化后还原法>PR法>先混合后还原法(MR)>>共浸渍法。共浸渍法制备的Ni-W-P活性低的主要原因是有杂晶生成。
Transition metal phosphides are attractive candidates for high-performance catalytic, electronic, and magnetic applications. A variety of methods can be used to synthesize bulk metal phosphides. Amoung them, temperature programmed reduction (TPR) of metal phosphates at high temperature was generally feasible for the preparation of supported transition-metal phosphides for using as hydrotreating or hydrogenation catalysts, but the particles were always aggregated, and phosphorus loss occured at high reduction temperature. In this paper, we describe a new strategy for synthesizing metal phosphides (Ni2P, CoP, MoP and WP) that using nonthermal hydrogen plasma as the reduction medium instead of the H2 used in the TPR method, and the HDS acitivity of DBT and 4,6-DMDBT was evaluated. XRD, CO chemisorption, TPR, HRTEM, SEM, ICP-AES techniques were used to characterize the structures of the metal phosphides. The mechanism of phosphide preparation with PR method was also speculated.
Bulk metal phosphides were prepared with PR method, the effect of voltage, reduction time, M/P ratio and doping of noble metal on the phosphide phase formation were investigated. The results told that under higher voltage, longer reduction time, the phosphides were better crystallized. For MoP and WP, the M/P ratio influenced the crystallization, while for Ni2P and CoP, it determined phase of the phosphide. The reduciton voltage of oxidic precursors could be lower down by co-impregnation of Ru; InP, GaP, Fe2P were also be prepared by hydrogen plasma method (PR).
Transition metal phosphides (Ni2P, CoP, MoP, WP) were prepared by TPR and PR method, the HDS performance was also compared. The influence of the M/P ratio, voltage and passivation method on the HDS performances of the phosphides prepared with PR method was examined. The results indicated that catalysts prepared by PR method showed higher DBT HDS activity then TPR method. And the activity of phosphides prepared by PR method was in the following order:CoP>Ni2P>MoP≈WP。
CoP was more difficult to be prepared then MoP, N12P and WP, and Co2P which owned low HDS activity could easily formed, so the activity of CoP prepared by TPR method showed lower HDS activity. Better crystallised and high HDS performance CoP could be prepared with lower reduction voltage by doping oxidic CoP with Ru, the particle size of CoP was smaller and CoP phase was not changed.
The phosphides catalysts:MoP/MCM-41, WP/MCM-41 and Ni2P/MCM-41, were prepared by four methods. The HDS activity was in the following order:WP>MoP>Ni2P, WP and MoP mainly through direct hydrodesulfurization path, while direct hydrodesulfurization mainly happened on Ni2P. The mechanically mixed of them were evaluated in simultaneously HDS of DBT and 4,6-DMDBT. The results showed that there was synergistic effect between WP+Ni2P/MCM-41 which exhibited best performance; the hydrodesulfurization activity was in the following order:SR>PR>MR>>IP.
引文
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