Mo-Ni_2P/SBA-15堇青石整体式催化剂加氢脱硫催化性能的研究
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摘要
近年来,随着世界各国对环保要求的提高,进一步激发和促进了石油加氢脱硫技术的发展。研究表明磷化镍在加氢脱硫反应过程中显示出优异的深度脱硫性能,被认为是新一代加氢脱硫催化剂。整体式催化剂以其床层压降底和内扩散阻力小等特点受到越来越广泛的关注。
经过前期的研究工作发现Ni2P/SBA-15颗粒催化剂和Ni2P/SBA-15/堇青石整体式催化剂具有优异的深度加氢脱硫性能。本文的研究思路考虑将将金属Mo作为助剂引入至Ni2P/SBA-15颗粒催化剂及Ni2P/SBA-15/堇青石整体式催化剂中,通过XRD、N2吸脱附等温线、SEM和XPS等分析手段对所得催化剂进行结构表征,最后采用二苯并噻吩的加氢脱硫模型反应评价催化剂的性能,考察助剂Mo对催化剂活性和稳定性的影响。
以介孔分子筛SBA-15为载体,采用浸渍法制备了不同Mo含量的Mo-Ni2P/SBA-15前驱体,通过程序升温还原法得到了Mo-Ni2P/SBA-15颗粒式催化剂(w(Mo)=0%,1.0%,3.0%,5.0%,7.0%,10.0%)。所得样品均保留有介孔结构；当w(Mo)≤7.0%时,活性相为Ni2P；当w(Mo)=10.0%时,活性相为Ni2P和MoNiP2的混合相；Mo-Ni2P/SBA-15 (w(Mo)=1.0%)具有最好的DBT加氢脱硫活性,在380℃时DBT的转化率已达99.0%。
将制备的Mo-Ni2P/SBA-15前驱体均匀涂敷至预处理过的堇青石上,通过程序升温还原制备得Mo-Ni2P/SBA-15/堇青石整体式催化剂(w(Mo)=0%,0.6%,1.8%,3.0%,4.2%,6.0%)。所的样品都具有介孔结构,活性相为Ni2P, Ni、Mo、P元素均可以检测到以过渡金属磷化物的Niδ+、Moδ+、Pδ-价态存在,w(Mo)=4.2%时催化剂活性最好,在380℃时DBT的转化率达99.0%以上,温度的上升可以提高产物CHB的选择性,380℃直接脱硫和预加氢脱硫机理均起着重要作用。
对Ni2P/SBA-15堇青石整体式催化剂进行不同DBT浓度下的稳定性实验发现,在w(DBT)=1.0%时催化剂对DBT的脱除效果最佳,转化率保持在86%,稳定性实验后样品的比表面积、孔容积有所增大,孔径为6nm的介孔结构分布增多,但Niδ+、Pδ-的流失使催化剂活性下降幅度较大。对Mo-Ni2P/SBA-15堇青石整体式催化剂进行w(DBT)=1.0%的加氢脱硫100h稳定性实验,DBT转化率保持在90%,样品的比表面积、孔容积和孔径变化不大,Niδ+、Moδ+、Pδ-流失不多,说明Mo-Ni2P/SBA-15堇青石整体式催化剂具有很好的加氢脱硫活性和稳定性。
Recently, the oil hydrodesulfurization(HDS) technology needs a high development with the improving of environmental requirements in the world. Nickel phosphides(Ni2P) as the active component in the hydrodesulfurization process which have showed excellent desulfurization performance is considered as new generation of HDS catalysts. As a new-type catalyst, monolithic catalysts have better mass transfer performance and lower pressure drop.
In previous research work, Ni2P/SBA-15 catalysts and Ni2P/SBA-15/cord monolithic catalysts had showed deep HDS activity, but the effect of promoters has not been studied. Therefore, in this paper, molybdenum was added into Ni2P/SBA-15 and Ni2P/SBA-15/cord monolithic catalyst as promoters. Then, the prepared catalysts were characterized by XRD, N2 adsorption-desorption isotherms, SEM and XPS. Finally, the catalytic performances of the catalysts were evaluated by HDS of dibenzothiophene (DBT).
A series of Mo-Ni2P/SBA-15 precursors that varied the Mo contents were prepared by co-impregnation method using mesoporous molecular sieve SBA-15 as support. Then, the Mo-Ni2P/SBA-15 catalysts were obtained by temperature-programmed carburization (TPC) method(w(Mo)=0%,1.0%, 3.0%,5.0%,7.0%,10.0%). All obtained samples had well mesoporous structure. When w(Mo)≤7.0%, the active phase was Ni2P; when w(Mo)=10.0%, the active phase were mixtures of Ni2P and MoNiP2. Mo-Ni2P/SBA-15(w(Mo)=1.0%) had the best DBT HDS activity at 380℃while the conversion had reached 99.0%.
Mo-Ni2P/SBA-15 precursors were coated to the pretreated cordierite and Mo-Ni2P/SBA-15/cordierite monolithic catalysts(w(Mo)=0%,0.6%,1.8%, 3.0%,4.2%,6.0%) were obtained by TPR. All the samples had mesoporous structures, the active phase was Ni2P. Ni, Mo, P elements were found to be Niδ+, Moδ+, Pδ- valence in the transition metal phosphides. When w(Mo)=4.2%, the DBT conversion was 99.0% at 380℃, the selectivity of CHB increased with the improving of temperature, DDS and HYD mechanism both played an important role.
In the stability tests of different DBT concentrations, the best DBT conversion remained at 86% when w(DBT)=1.0% on Ni2P/SBA-15 cordierite monolithic catalyst.After the experiment, the surface area and pore volume had increased, the pore size distribution of 6nm increased. Niδ+ and Pδ- of the catalyst decreased greatly. In the 100h stability test of Mo-Ni2P/SBA-15 cordierite monolithic catalyst for w(DBT)=1.0%, DBT conversion remained at 90%. The sample surface area, pore volume and pore diameter changing little and Niδ+, Moδ+ and Pδ- few loss indicated Mo-Ni2P/SBA-15 cordierite monolithic catalyst had excellent HDS activity and stability.
经过前期的研究工作发现Ni2P/SBA-15颗粒催化剂和Ni2P/SBA-15/堇青石整体式催化剂具有优异的深度加氢脱硫性能。本文的研究思路考虑将将金属Mo作为助剂引入至Ni2P/SBA-15颗粒催化剂及Ni2P/SBA-15/堇青石整体式催化剂中,通过XRD、N2吸脱附等温线、SEM和XPS等分析手段对所得催化剂进行结构表征,最后采用二苯并噻吩的加氢脱硫模型反应评价催化剂的性能,考察助剂Mo对催化剂活性和稳定性的影响。
以介孔分子筛SBA-15为载体,采用浸渍法制备了不同Mo含量的Mo-Ni2P/SBA-15前驱体,通过程序升温还原法得到了Mo-Ni2P/SBA-15颗粒式催化剂(w(Mo)=0%,1.0%,3.0%,5.0%,7.0%,10.0%)。所得样品均保留有介孔结构；当w(Mo)≤7.0%时,活性相为Ni2P；当w(Mo)=10.0%时,活性相为Ni2P和MoNiP2的混合相；Mo-Ni2P/SBA-15 (w(Mo)=1.0%)具有最好的DBT加氢脱硫活性,在380℃时DBT的转化率已达99.0%。
将制备的Mo-Ni2P/SBA-15前驱体均匀涂敷至预处理过的堇青石上,通过程序升温还原制备得Mo-Ni2P/SBA-15/堇青石整体式催化剂(w(Mo)=0%,0.6%,1.8%,3.0%,4.2%,6.0%)。所的样品都具有介孔结构,活性相为Ni2P, Ni、Mo、P元素均可以检测到以过渡金属磷化物的Niδ+、Moδ+、Pδ-价态存在,w(Mo)=4.2%时催化剂活性最好,在380℃时DBT的转化率达99.0%以上,温度的上升可以提高产物CHB的选择性,380℃直接脱硫和预加氢脱硫机理均起着重要作用。
对Ni2P/SBA-15堇青石整体式催化剂进行不同DBT浓度下的稳定性实验发现,在w(DBT)=1.0%时催化剂对DBT的脱除效果最佳,转化率保持在86%,稳定性实验后样品的比表面积、孔容积有所增大,孔径为6nm的介孔结构分布增多,但Niδ+、Pδ-的流失使催化剂活性下降幅度较大。对Mo-Ni2P/SBA-15堇青石整体式催化剂进行w(DBT)=1.0%的加氢脱硫100h稳定性实验,DBT转化率保持在90%,样品的比表面积、孔容积和孔径变化不大,Niδ+、Moδ+、Pδ-流失不多,说明Mo-Ni2P/SBA-15堇青石整体式催化剂具有很好的加氢脱硫活性和稳定性。
Recently, the oil hydrodesulfurization(HDS) technology needs a high development with the improving of environmental requirements in the world. Nickel phosphides(Ni2P) as the active component in the hydrodesulfurization process which have showed excellent desulfurization performance is considered as new generation of HDS catalysts. As a new-type catalyst, monolithic catalysts have better mass transfer performance and lower pressure drop.
In previous research work, Ni2P/SBA-15 catalysts and Ni2P/SBA-15/cord monolithic catalysts had showed deep HDS activity, but the effect of promoters has not been studied. Therefore, in this paper, molybdenum was added into Ni2P/SBA-15 and Ni2P/SBA-15/cord monolithic catalyst as promoters. Then, the prepared catalysts were characterized by XRD, N2 adsorption-desorption isotherms, SEM and XPS. Finally, the catalytic performances of the catalysts were evaluated by HDS of dibenzothiophene (DBT).
A series of Mo-Ni2P/SBA-15 precursors that varied the Mo contents were prepared by co-impregnation method using mesoporous molecular sieve SBA-15 as support. Then, the Mo-Ni2P/SBA-15 catalysts were obtained by temperature-programmed carburization (TPC) method(w(Mo)=0%,1.0%, 3.0%,5.0%,7.0%,10.0%). All obtained samples had well mesoporous structure. When w(Mo)≤7.0%, the active phase was Ni2P; when w(Mo)=10.0%, the active phase were mixtures of Ni2P and MoNiP2. Mo-Ni2P/SBA-15(w(Mo)=1.0%) had the best DBT HDS activity at 380℃while the conversion had reached 99.0%.
Mo-Ni2P/SBA-15 precursors were coated to the pretreated cordierite and Mo-Ni2P/SBA-15/cordierite monolithic catalysts(w(Mo)=0%,0.6%,1.8%, 3.0%,4.2%,6.0%) were obtained by TPR. All the samples had mesoporous structures, the active phase was Ni2P. Ni, Mo, P elements were found to be Niδ+, Moδ+, Pδ- valence in the transition metal phosphides. When w(Mo)=4.2%, the DBT conversion was 99.0% at 380℃, the selectivity of CHB increased with the improving of temperature, DDS and HYD mechanism both played an important role.
In the stability tests of different DBT concentrations, the best DBT conversion remained at 86% when w(DBT)=1.0% on Ni2P/SBA-15 cordierite monolithic catalyst.After the experiment, the surface area and pore volume had increased, the pore size distribution of 6nm increased. Niδ+ and Pδ- of the catalyst decreased greatly. In the 100h stability test of Mo-Ni2P/SBA-15 cordierite monolithic catalyst for w(DBT)=1.0%, DBT conversion remained at 90%. The sample surface area, pore volume and pore diameter changing little and Niδ+, Moδ+ and Pδ- few loss indicated Mo-Ni2P/SBA-15 cordierite monolithic catalyst had excellent HDS activity and stability.
引文
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