Zr、K改性费托合成铁基催化剂的研究
摘要
近年来,由于石油资源的不断消耗以及原油价格的起伏不定,费托(简称F-T)合成作为可将煤、天然气及生物质等含碳资源经合成气(主要为CO和H2)催化转化为清洁液体燃料及其它化学品的重要途径而备受关注。F-T合成作为重要的煤间接液化过程技术,其关键技术之一就是催化剂的研究与开发。在F-T合成催化剂中,铁基催化剂因其具有价格低廉、操作灵活及较高的水煤气变换(WGS)反应活性,适合于低氢碳比的煤基合成气的F-T合成。
本文选用Zr和K助剂为改性助剂,结合共沉淀、喷雾干燥及浸渍法等催化剂制备方法,同时采用N2物理吸附、X射线衍射(XRD)、程序升温还原(TPR)、程序升温脱附(TPD)和Mossbauer谱(MES)等表征方法着重研究Zr助剂添加方式、Zr和K助剂、Zr助剂添加量对铁基催化剂结构、还原碳化性能及F-T反应性能的影响,并在浆态床反应器中对催化剂进行CO消耗动力学研究,以期为F-T合成铁基催化剂的工业应用提供基础支持。
制备了由共沉淀与浸渍法添加Zr助剂的改性Fe/SiO2催化剂,并结合多种表征手段研究了Zr助剂的添加方式对催化剂Fe/SiO2的结构、还原和碳化行为、物相结构以及F-T合成反应性能的影响。N2物理吸附结果表明,Zr助剂的添加明显降低了催化剂比表面积和总孔体积,但提高了催化剂的平均孔径。H2-TPR和CO-TPR结果表明由于存在Fe和Zr的相互作用,Zr助剂的添加抑制了催化剂在H2和CO气氛中的还原。经还原和反应后催化剂Fe/SiO2均具有最高的铁碳化物含量,因而其初始反应活性最高,但催化剂失活较快。Zr助剂抑制了催化剂在还原和反应过程中活性相的形成,降低了催化剂的活性,但Zr助剂的添加明显提高了催化剂的稳定性,采用浸渍法制备的Zr助剂改性催化剂稳定性最佳。Zr助剂抑制了气态烃(CH4及C2-C4)的生成,明显提高了C5+选择性。
采用浸渍法引入助剂zr并制备Fe/SiO2、Fe/Zr/SiO2、Fe/K/SiO、Fe/Zr/K/SiO2系列催化剂,研究了Zr助剂、K助剂及Zr与K的协同作用对F-T合成铁基催化剂的结构、还原和碳化行为、体相结构以及F-T合成反应性能的影响。结果表明：Zr和K助剂降低了催化剂的比表面积。Fe和Zr间相互作用抑制了Fe/Zr/SiO2催化剂在H2和CO的还原或碳化；K助剂提高了CO的吸附并促进了催化剂在CO及原料气中的还原、碳化,但抑制了催化剂在H2中的还原和吸附；Zr、K助剂共存时,Zr和K助剂的协同效应进一步提高了对CO的吸附,还促进了催化剂在CO和原料气中的还原和碳化,从而使Fe/Zr/K/Si02催化剂具有最高的反应活性,此外,添加Zr和(或)K助剂明显提高了催化剂的稳定性。zr和(或)K助剂的添加抑制了气态烃(CH4、C2-C4)的生成,促进了链增长反应的进行。催化剂Fe/Zr/K/SiO2气态烃(CH4、C2-C4)选择性最低,C5+选择性最高。此外,烯烃选择性也随着Zr和(或)K助剂的添加而增大。单独添加Zr助剂后催化剂WGS反应活性基本不变,但添加K助剂催化剂的WGS反应活性则明显提高。
通过制备不同Zr助剂浸渍量的Fe/Zr/K/SiO2催化剂,研究Zr助剂含量对Fe/K/SiO2催化剂催化结构、还原和碳化行为、物相结构以及F-T合成反应性能的影响。结果表明,添加少量的Zr助剂提高催化剂比表面积,促进催化剂的还原和碳化,提高催化剂的反应活性,但继续增加Zr浸渍量则降低催化剂比表面积,抑制催化剂的还原和碳化,降低催化剂的活性同时加速催化剂的失活。随着助剂zr浸渍量的增加,轻烃(CH4,C2-C4)选择性先减小后增加,而重烃(C5+)选择性变化趋势恰恰相反。此外,烯烃选择性也随着Zr助剂浸渍量的增加而增加。少量Zr助剂对催化剂的WGS反应活性的影响不大,但随着Zr助剂浸渍量的增加催化剂的WGS反应活性明显下降。当n(Zr)：n(Fe)=0.01时,催化剂具有高的CO转化率和高的C5+选择性。
在温度为240-270℃、压力为1.0-2.0MPa、H2/CO=0.67、空速为0.3～1.ONL/(g-h)条件下对100Fe/1Zr/3K/12Si02(原子比)催化剂进行了F-T合成反应的CO消耗宏观动力学测定。采用Levenberg-Maquardit算法对动力学参数进行估值,筛选出最终的动力学模型为rCO=9.96×107×exp(-103.90×103/RT)PCOPH20.5/(1+0.87PCO)2,统计检验和相对误差分析显示该模型是适宜的,模型计算值与实验值吻合良好。
Due to the limited supplement and unpredictable price of crude oil, Fischer-Tropsch (F-T) synthesis converting syngas (mainly composed with CO and H2) derived from coal, natural gas or biomass to clean liquid fuels and other chemicals, has been renewedly attracted much attention in recent years. One of the key technologies for indirect coal liquefaction is to explore high performance catalysts for F-T synthesis. The iron-based catalysts are often used in commercial operations, due to their low cost, flexible operation and high water-gas-shift (WGS) activity, which helps to make up the deficit of H2 in the syngas from coal gasification.
Catalysts modified with Zr and K promoters in present study were prepared by a combination of coprecipitation. spry drying and impregnation techniques. The characterization technologies of N2-physisorption, X-ray diffraction (XRD), temperature-programming reduction (TPR), temperature-programming desorption (TPD) and Mossbauer effect spectroscopy (MES) were used to study the effects of incorporation manner of Zr, Zr and K promoters, different content of Zr addition on structure, reduction and carburization behaviors phase transformation and F-T synthesis performances of iron-based catalysts. The kinetics of CO consumption on selected catalytst was investigated in a stirred slurry autoclave. Works mentioned above can provide the basic support for industrial application of iron-based catalysts for F-T synthesis.
Zr modified catalysts were prepared by adding Zr to Fe/SiO2 using coprecipitation and impregation. The effects of incorporation manner of Zr on structure, reduction, carburization, phase transformation and catalytic performance were investigated. The result of N2-physicorption shows that Zr decreases the catalyst surface area and total pore volume significantly, but increases the average pore size of the catalyst. Results of H2-TPR and CO-TPR indicate that Zr inhibites the reduction of catalyst in the atmosphere of H2 and CO. After reduction and reaction, catalyst Fe/SiO2 has the highest content of iron carbides, thus it owns the highest initial activity but deactivates quickly. Though Zr inhibits the formation of active phases and decreases the activity, Zr improves the stability of the catalyst apparently. Zr modified catalyst by impregnation possesses the best stability. Zr suppresses the formation of gaseous hydrocarbons (CH4 and C2-C4), but enhances the C5+selectivity significantly.
Zr was added by impregnation and a series of catalysts (Fe/SiO2. Fe/Zr/SiO2, Fe/K/SiO2 and Fe/Zr/K/SiO2) were prepared in order to investigate the effects of Zr, K. the synergy effect of Zr and K on structure, reduction, carburization. phase transformation and catalytic performance. It is found that Zr and K decrease the surface area. The interaction between Zr and Fe suppresses the reduction or carbonization of Fe/Zr/SiO2 in H2 and CO. As an alkaline promoter, K enhances the adsorption of CO and promotes the reduction and carbonization in CO and feed gas. but obviously suppresses the adsorption and reduction in H2. When Zr and K coexit in catalyst, the synergy effect of Zr and K further enhances the adsorption of CO and facilitates the reduction and carbonization of the catalyst in CO and feed gas so that Fe/Zr/K/SiO2 has the highest activity. Zr and (or) K suppresses the formation of gaseous hydrocarbons (CH4 and C2-C4), but promotes the formation of heavy products to some extent. The selectivity to gaseous hydrocarbons (CH4 and C2-C4) reaches minimum on Fe/Zr/K/SiO2. In addition, the selectivity to olefin increases with the addition of Zr and K. Zr almost has no effect on WGS reaction activity, while K improves the WGS reaction activity significantly.
A group of Fe/Zr/K/SiO2 catalysts with different content of Zr were prepared for the purpose of study the Zr loading on structure, reduction, carburization, phase transformation and catalytic performance. The results show that small amount of Zr increases the BET surface area, promotes the reduction/carburization and improves the activity of the catalyst. While large amounts of Zr addition decreases the surface area, suppresses the reduction/carburization of the catalyst, decreases the activity and speeds up the catalyst deactivation. With the increasing Zr loading, the selectivity to gaseous hydrocarbons (CH4 and C2～C4) first decreases then increases, while the selectivity to C5+is on the contrary.In addition, the selectivity to olefin increases and the activity of WGS reaction decreases with the increasing Zr loading. The optimal catalyst with n(Zr):n(Fe)=0.01 has high CO conversion and high selectivity to C5+hydrocarbons.
The global kinetics of the Fischer-Tropsch synthesis on selected 100Fe/1Zr/3K/12SiO2 (in atomic ratio) catalyst was investigated in a 500mL stirred slurry autoclave. In the range of 240～270℃,1.0～2.2MPa.0.3～1.0NL/(g-h) and H2/CO=0.67. kinetic data were obtained under exclusion from effects of mass transfer. Parameters of rate constant, activation energy and adsorption coefficient are estimated by the Levenberg-Maquardit algorithm. The final kinetic model has the following rate expression: rco=9.96×10×exp(?)
The results of statistical tests and relative error analysis show that the final kinetic model is appropriate.
本文选用Zr和K助剂为改性助剂,结合共沉淀、喷雾干燥及浸渍法等催化剂制备方法,同时采用N2物理吸附、X射线衍射(XRD)、程序升温还原(TPR)、程序升温脱附(TPD)和Mossbauer谱(MES)等表征方法着重研究Zr助剂添加方式、Zr和K助剂、Zr助剂添加量对铁基催化剂结构、还原碳化性能及F-T反应性能的影响,并在浆态床反应器中对催化剂进行CO消耗动力学研究,以期为F-T合成铁基催化剂的工业应用提供基础支持。
制备了由共沉淀与浸渍法添加Zr助剂的改性Fe/SiO2催化剂,并结合多种表征手段研究了Zr助剂的添加方式对催化剂Fe/SiO2的结构、还原和碳化行为、物相结构以及F-T合成反应性能的影响。N2物理吸附结果表明,Zr助剂的添加明显降低了催化剂比表面积和总孔体积,但提高了催化剂的平均孔径。H2-TPR和CO-TPR结果表明由于存在Fe和Zr的相互作用,Zr助剂的添加抑制了催化剂在H2和CO气氛中的还原。经还原和反应后催化剂Fe/SiO2均具有最高的铁碳化物含量,因而其初始反应活性最高,但催化剂失活较快。Zr助剂抑制了催化剂在还原和反应过程中活性相的形成,降低了催化剂的活性,但Zr助剂的添加明显提高了催化剂的稳定性,采用浸渍法制备的Zr助剂改性催化剂稳定性最佳。Zr助剂抑制了气态烃(CH4及C2-C4)的生成,明显提高了C5+选择性。
采用浸渍法引入助剂zr并制备Fe/SiO2、Fe/Zr/SiO2、Fe/K/SiO、Fe/Zr/K/SiO2系列催化剂,研究了Zr助剂、K助剂及Zr与K的协同作用对F-T合成铁基催化剂的结构、还原和碳化行为、体相结构以及F-T合成反应性能的影响。结果表明：Zr和K助剂降低了催化剂的比表面积。Fe和Zr间相互作用抑制了Fe/Zr/SiO2催化剂在H2和CO的还原或碳化；K助剂提高了CO的吸附并促进了催化剂在CO及原料气中的还原、碳化,但抑制了催化剂在H2中的还原和吸附；Zr、K助剂共存时,Zr和K助剂的协同效应进一步提高了对CO的吸附,还促进了催化剂在CO和原料气中的还原和碳化,从而使Fe/Zr/K/Si02催化剂具有最高的反应活性,此外,添加Zr和(或)K助剂明显提高了催化剂的稳定性。zr和(或)K助剂的添加抑制了气态烃(CH4、C2-C4)的生成,促进了链增长反应的进行。催化剂Fe/Zr/K/SiO2气态烃(CH4、C2-C4)选择性最低,C5+选择性最高。此外,烯烃选择性也随着Zr和(或)K助剂的添加而增大。单独添加Zr助剂后催化剂WGS反应活性基本不变,但添加K助剂催化剂的WGS反应活性则明显提高。
通过制备不同Zr助剂浸渍量的Fe/Zr/K/SiO2催化剂,研究Zr助剂含量对Fe/K/SiO2催化剂催化结构、还原和碳化行为、物相结构以及F-T合成反应性能的影响。结果表明,添加少量的Zr助剂提高催化剂比表面积,促进催化剂的还原和碳化,提高催化剂的反应活性,但继续增加Zr浸渍量则降低催化剂比表面积,抑制催化剂的还原和碳化,降低催化剂的活性同时加速催化剂的失活。随着助剂zr浸渍量的增加,轻烃(CH4,C2-C4)选择性先减小后增加,而重烃(C5+)选择性变化趋势恰恰相反。此外,烯烃选择性也随着Zr助剂浸渍量的增加而增加。少量Zr助剂对催化剂的WGS反应活性的影响不大,但随着Zr助剂浸渍量的增加催化剂的WGS反应活性明显下降。当n(Zr)：n(Fe)=0.01时,催化剂具有高的CO转化率和高的C5+选择性。
在温度为240-270℃、压力为1.0-2.0MPa、H2/CO=0.67、空速为0.3～1.ONL/(g-h)条件下对100Fe/1Zr/3K/12Si02(原子比)催化剂进行了F-T合成反应的CO消耗宏观动力学测定。采用Levenberg-Maquardit算法对动力学参数进行估值,筛选出最终的动力学模型为rCO=9.96×107×exp(-103.90×103/RT)PCOPH20.5/(1+0.87PCO)2,统计检验和相对误差分析显示该模型是适宜的,模型计算值与实验值吻合良好。
Due to the limited supplement and unpredictable price of crude oil, Fischer-Tropsch (F-T) synthesis converting syngas (mainly composed with CO and H2) derived from coal, natural gas or biomass to clean liquid fuels and other chemicals, has been renewedly attracted much attention in recent years. One of the key technologies for indirect coal liquefaction is to explore high performance catalysts for F-T synthesis. The iron-based catalysts are often used in commercial operations, due to their low cost, flexible operation and high water-gas-shift (WGS) activity, which helps to make up the deficit of H2 in the syngas from coal gasification.
Catalysts modified with Zr and K promoters in present study were prepared by a combination of coprecipitation. spry drying and impregnation techniques. The characterization technologies of N2-physisorption, X-ray diffraction (XRD), temperature-programming reduction (TPR), temperature-programming desorption (TPD) and Mossbauer effect spectroscopy (MES) were used to study the effects of incorporation manner of Zr, Zr and K promoters, different content of Zr addition on structure, reduction and carburization behaviors phase transformation and F-T synthesis performances of iron-based catalysts. The kinetics of CO consumption on selected catalytst was investigated in a stirred slurry autoclave. Works mentioned above can provide the basic support for industrial application of iron-based catalysts for F-T synthesis.
Zr modified catalysts were prepared by adding Zr to Fe/SiO2 using coprecipitation and impregation. The effects of incorporation manner of Zr on structure, reduction, carburization, phase transformation and catalytic performance were investigated. The result of N2-physicorption shows that Zr decreases the catalyst surface area and total pore volume significantly, but increases the average pore size of the catalyst. Results of H2-TPR and CO-TPR indicate that Zr inhibites the reduction of catalyst in the atmosphere of H2 and CO. After reduction and reaction, catalyst Fe/SiO2 has the highest content of iron carbides, thus it owns the highest initial activity but deactivates quickly. Though Zr inhibits the formation of active phases and decreases the activity, Zr improves the stability of the catalyst apparently. Zr modified catalyst by impregnation possesses the best stability. Zr suppresses the formation of gaseous hydrocarbons (CH4 and C2-C4), but enhances the C5+selectivity significantly.
Zr was added by impregnation and a series of catalysts (Fe/SiO2. Fe/Zr/SiO2, Fe/K/SiO2 and Fe/Zr/K/SiO2) were prepared in order to investigate the effects of Zr, K. the synergy effect of Zr and K on structure, reduction, carburization. phase transformation and catalytic performance. It is found that Zr and K decrease the surface area. The interaction between Zr and Fe suppresses the reduction or carbonization of Fe/Zr/SiO2 in H2 and CO. As an alkaline promoter, K enhances the adsorption of CO and promotes the reduction and carbonization in CO and feed gas. but obviously suppresses the adsorption and reduction in H2. When Zr and K coexit in catalyst, the synergy effect of Zr and K further enhances the adsorption of CO and facilitates the reduction and carbonization of the catalyst in CO and feed gas so that Fe/Zr/K/SiO2 has the highest activity. Zr and (or) K suppresses the formation of gaseous hydrocarbons (CH4 and C2-C4), but promotes the formation of heavy products to some extent. The selectivity to gaseous hydrocarbons (CH4 and C2-C4) reaches minimum on Fe/Zr/K/SiO2. In addition, the selectivity to olefin increases with the addition of Zr and K. Zr almost has no effect on WGS reaction activity, while K improves the WGS reaction activity significantly.
A group of Fe/Zr/K/SiO2 catalysts with different content of Zr were prepared for the purpose of study the Zr loading on structure, reduction, carburization, phase transformation and catalytic performance. The results show that small amount of Zr increases the BET surface area, promotes the reduction/carburization and improves the activity of the catalyst. While large amounts of Zr addition decreases the surface area, suppresses the reduction/carburization of the catalyst, decreases the activity and speeds up the catalyst deactivation. With the increasing Zr loading, the selectivity to gaseous hydrocarbons (CH4 and C2～C4) first decreases then increases, while the selectivity to C5+is on the contrary.In addition, the selectivity to olefin increases and the activity of WGS reaction decreases with the increasing Zr loading. The optimal catalyst with n(Zr):n(Fe)=0.01 has high CO conversion and high selectivity to C5+hydrocarbons.
The global kinetics of the Fischer-Tropsch synthesis on selected 100Fe/1Zr/3K/12SiO2 (in atomic ratio) catalyst was investigated in a 500mL stirred slurry autoclave. In the range of 240～270℃,1.0～2.2MPa.0.3～1.0NL/(g-h) and H2/CO=0.67. kinetic data were obtained under exclusion from effects of mass transfer. Parameters of rate constant, activation energy and adsorption coefficient are estimated by the Levenberg-Maquardit algorithm. The final kinetic model has the following rate expression: rco=9.96×10×exp(?)
The results of statistical tests and relative error analysis show that the final kinetic model is appropriate.
引文
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