ZrO_2助剂对Ni/SiO_2气凝胶催化性能的影响
摘要
多相催化剂工业化应用以来,助催化剂一直是备受关注的热点问题,现在商品化的催化剂,一般都包含了多种助催化剂以提高催化剂的活性、选择性、寿命等。实践证明,通常情况下,酸催化和催化加氢反应中,助剂的效应是非常重要甚至是必不可少的。
本论文研究了引入ZrO_2助剂对Ni/SiO_2气凝胶催化顺酐加氢性能的影响规律。
ZrO_2是具有氧化还原性和酸碱性的两性氧化物,在催化领域ZrO_2有广泛的应用,作为助催化剂可对主催化剂产生各种调控效应,已有的研究表明,ZrO_2作为助催化剂可以明显提高催化剂的热稳定性、表面酸性及活性组分的分散度等。
气凝胶是经由溶胶-凝胶(sol-gel)过程和超临界流体干燥技术制备的高比表面、高孔隙率的新型催化材料,SiO_2气凝胶是一种优异的催化剂载体,具有化学惰性、高比表面积、高孔隙率和好的热稳定性,SiO_2负载的镍基催化剂具有活性高及价廉等优点,广泛应用于催化加氢反应。
本论文以气凝胶催化剂的制各方法为核心,利用溶胶-凝胶方法结合超临界流体干燥技术,制备了系列ZrO_2-SiO_2复合氧化物气凝胶,以该气凝胶为载体,浸渍法制备了负载型Ni/ZrO_2-SiO_2催化剂,考察了不同镍、锆含量对催化剂顺酐加氢催化性能的影响;并与一步溶胶-凝胶法制备的Ni-ZrO_2-SiO_2气凝胶催化剂,以及镍、锆混合溶液共浸渍单组分SiO_2气凝胶载体制备的Ni-ZrO_2/SiO_2催化剂进行了比较;采用N_2-物理吸附、FT-IR、XRD、TPR、NH_3-TPD、吡啶吸附红外光谱及CO吸附与加氢原位红外光谱等方法对制备的催化剂进行了结构和理化性质表征,探索ZrO_2助剂对催化剂结构和理化性质的影响规律,阐明引起催化性能差别的结构及理化性质原因。
本论文的工作主要分为两部分内容:一、催化剂的制备和顺酐催化加氢性能评价(第三、四章);二、催化剂的结构表征分析(第五、六、七章)。
一、采用溶胶-凝胶法结合超临界流体干燥技术制备了不同ZrO_2含量的ZrO_2-SiO_2复合氧化物气凝胶,浸渍法负载镍制备了系列Ni/ZrO_2-SiO_2催化剂,考察不同锆、镍含量对顺酐加氢活性和γ-丁内酯(GBL)选择性的影响;同时与单组分SiO_2气凝胶为载体浸渍镍、锆混合溶液的Ni-ZrO_2/SiO_2催化剂,以及镍、锆、硅前驱物一步共胶法制备的Ni-ZrO_2-SiO_2催化剂进行了比较。
二、采用N_2-物理吸附、FT-IR、XRD、TPR、NH_3-TPD、吡啶吸附红外光谱及CO吸附与加氢原位红外光谱等方法表征了催化剂的结构及表面性质,阐明造成催化性能差别的结构及理化性质原因。
催化活性评价表明,以溶胶-凝胶结合超临界流体干燥技术制备的ZrO_2-SiO_2复合氧化物气凝胶为载体,浸渍法制备的Ni/ZrO_2-SiO_2系列催化剂:ZrO_2助剂对GBL选择性的影响与Ni含量密切相关,当Ni含量低于13wt%时,引入ZrO_2助剂,GBL的选择性几乎没有变化;当Ni含量达到30wt%时,1wt%的ZrO_2就可使30Ni/ZrO_2-SiO_2催化剂的GBL选择性从0.7%提高到12.9%,ZrO_2含量为5wt%时,GBL选择性达到最大值,为15.1%。
单组分SiO_2气凝胶为载体浸渍镍、锆混合溶液制备的Ni-ZrO_2/SiO_2系列催化剂,在Ni含量低于40 wt%以下时,引入ZrO_2助剂对GBL选择性没有影响,只有当Ni含量达到50wt%时,GBL选择性从1.8%提高到13.07%;而镍、锆、硅前驱物一步共胶法制备的Ni-ZrO_2-SiO_2系列催化剂与共胶法制备的Ni-SiO_2催化剂对比,引入ZrO_2降低了催化剂对GBL的选择性,特别是当Ni含量为30 wt%时,使GBL的选择性从12.2%降低到了0.4%。
对催化剂的结构分析表明:
①共胶法制备的30Ni-SiO_2具有较高的比表面积和较大的孔容,这可能是其催化活性较高的主要原因。其余四种催化剂比表面和孔结构参数相近,特别是30Ni/ZrO_2-SiO_2和30Ni/SiO_2。可以推测,除30Ni-SiO_2外,孔结构不是各催化剂活性差别的主要原因。
②红外光谱、XRD和TPR等研究表明:锆的引入,一方面形成了Zr—O—Si键,降低了NiO与载体之间的相互作用,使NiO的可还原度增加,特别是30Ni-Zr/Si催化剂,表面形成的Zr—O—Si键可能阻断了部分形成Ni—O—Si键的位点,使得NiO与载体间的相互作用减弱明显,耗氢量最大;另一方面,对于30Ni/Zr-Si催化剂,锆在载体中的引入可能在催化剂表面增加了Ni与载体的作用位点。
③表面酸性研究表明:ZrO_2助剂明显增加了催化剂的表面酸量,并新增了B酸位,且表面ZrO_2含量越多酸性越强;同时,较多的Si-O-Zr键会增加中强度酸区的酸密度。
④MA、SAH和GBL表面吸附红外光谱研究表明:ZrO_2助剂明显提高了催化剂30Ni/Zr-Si和30Ni-Zr-Si与MA和SAH的相互作用,也可以说是结构适应性,增加了对反应物的吸附量;但对30Ni-Zr/Si催化剂的结构适应性没有提高,而且还有降低的趋势。
⑤CO吸附及加氢的原位红外光谱研究表明:ZrO_2助剂的引入明显提高了30Ni/Zr-Si催化剂表面活性组分的分散度,催化剂表面活性位分布密集,活性位之间相互作用密切;30Ni-Si催化剂发达的孔隙结构和高的比表面积使其具有了较高的CO吸附力和加氢活性;30Ni-Zr/Si催化剂单一的Ni晶体组成、弱的活性组分与载体之间的相互作用,使其对CO的吸附极弱;30Ni-Zr-Si催化剂则主要由于低的还原镍含量,使其没有足够的吸附CO活性位点,导致了其对CO弱的吸附力和加氢活性。
综合催化剂评价与表征结果可以得出,在顺酐液相加氢反应中,获得较高GBL选择性的主要因素是:较高的表面酸性、活性组分的高分散度及与载体之间合适的相互作用。
ZrO_2助剂的引入:①增加了气凝胶催化剂的表面酸性,新增了B酸位;②降低了NiO与载体之间的相互作用,提高了催化剂的可还原度,增加了催化剂表面活性组分含量;③提高了活性组分在催化剂表面的分散度,使表面活性位点分布密集,活性位之间相互作用密切。
ZrO_2助剂的不同引入方式对其作用有明显影响,只有ZrO_2-SiO_2复合气凝胶为载体浸渍法制各的Ni/ZrO_2-SiO_2催化剂能明显体现出ZrO_2助剂促进性能。而镍、锆混合溶液共浸渍单组分SiO_2气凝胶载体制备的Ni-ZrO_2/SiO_2催化剂,其活性组分与载体之间的相互作用被降低太多,形成了不利于催化反应的结构;一步共胶法引入ZrO_2助剂则造成了催化剂微孔结构的破坏和比表面积的大幅下降,同样是不利的结构。
总之,ZrO_2助剂调变了催化剂的表面酸性和活性组分的分散度及与载体间的相互作用,较好地调控了顺酐液相加氢GBL的选择性。
Promoters have been studied extensively since heterogeneous catalysts have been used industrially.Commercial catalysts tend to involve multiple promoters to enhance the activity,selectivity,lifetime and structural integrity. Generally,in acid catalysis and hydrogenation reactions,promoter effects can be dramatic and unexpected.
In this paper,the promotion effect of ZrO_2 in Ni/SiO_2 aerogel catalyst is investigated systematically.
ZrO_2 has received considerable attention as a promoter due to chemical inertness,higher thermal stability and a special combination of surface properties,namely the preservation of both acidic and basic sites,on the one hand,and reducing and oxidizing properties,on the other.It is reported: introduction of a small amount of zirconium into the support leads to a significant increase of the dispersion of supported metal oxide species, especially,on silica.
Silica aerogel is an excellent catalytic support due to its desirable characteristics,such as inertness,high specific surface area,pronounced mesoporosity,and good thermal stability.Among the silica-supported catalysts,Ni/SiO_2 has been investigated widely.
In this paper,ZrO_2 promoted Ni/SiO_2 catalysts were prepared via three different routes:(ⅰ) impregnation ZrO_2-SiO_2 composite aerogels with a aqueous solution of Ni(NO_3)_2,catalyst code Ni/Zr-Si;(ⅱ) impregnation SiO_2 aerogels with a mixed aqueous solution of Ni(NO_3)_2 and ZrO(NO_3)_2·2H_2O, catalyst code Ni-Zr/Si;(ⅲ) one-pot sol-gel procedure from precursors Ni(NO_3)_2/ZrO(NO_3)_2·2H_2O/Si(OC_2H_5)_4,catalyst code Ni-Zr-Si.For comparison,non-promoted catalysts Ni/Si and Ni-Si also prepared respectively by impregnation Ni(NO_3)_2 with silica aerogel and by one-pot sol-gel process of Ni(NO_3)_2/Si(OC_2H_5)_4.
The above prepared catalysts were characterized by X-ray diffraction (XRD),temperature programmed reduction(TPR),ammonia temperature-programmed desorption(NH_3-TPD),N_2 adsorption-desorption isotherms and Fourier transform infrared(FTIR).The Liquid-phase hydrogenation of maleic anhydride(MA) was evaluated over these catalysts. And the adsorptions of MA,SAH and GBL on these catalysts surfaces were also investigated by FT-IR.
The results revealed that the different preparation routes result in a difference among the obtained catalysts,concerning the crystal structure and composition,surface acidity,mixed level of each component,texture,and catalytic selectivity.
The main results and conclusions are summarized below:
1.Comparing to 30Ni/Si the promoted catalyst 30Ni/Zr-Si has higher activity and selectivity to GBL,which is due to increased surface acidity and the decreased interaction between NiO and SiO_2 and the Ni coverage that was induced by ZrO_2 promoter.
2.The 30Ni-Zr/Si catalyst has lower activity and selectivity than that of 30Ni/Zr-Si.The most possible reason is about the decreased interaction between NiO and SiO_2 that was induced by ZrO_2,and the poor structural suitability between the SAH and the catalyst.
3.The catalyst 30Ni-Zr-Si also has lower activity and selectivity.The main reason is that the content of Ni is too low to increase the GBL selectivity.
4.The main reason for the higher activity and selectivity of 30Ni-Si catalyst is the higher S_(BET) and pore volume over the other four catalysts.
本论文研究了引入ZrO_2助剂对Ni/SiO_2气凝胶催化顺酐加氢性能的影响规律。
ZrO_2是具有氧化还原性和酸碱性的两性氧化物,在催化领域ZrO_2有广泛的应用,作为助催化剂可对主催化剂产生各种调控效应,已有的研究表明,ZrO_2作为助催化剂可以明显提高催化剂的热稳定性、表面酸性及活性组分的分散度等。
气凝胶是经由溶胶-凝胶(sol-gel)过程和超临界流体干燥技术制备的高比表面、高孔隙率的新型催化材料,SiO_2气凝胶是一种优异的催化剂载体,具有化学惰性、高比表面积、高孔隙率和好的热稳定性,SiO_2负载的镍基催化剂具有活性高及价廉等优点,广泛应用于催化加氢反应。
本论文以气凝胶催化剂的制各方法为核心,利用溶胶-凝胶方法结合超临界流体干燥技术,制备了系列ZrO_2-SiO_2复合氧化物气凝胶,以该气凝胶为载体,浸渍法制备了负载型Ni/ZrO_2-SiO_2催化剂,考察了不同镍、锆含量对催化剂顺酐加氢催化性能的影响;并与一步溶胶-凝胶法制备的Ni-ZrO_2-SiO_2气凝胶催化剂,以及镍、锆混合溶液共浸渍单组分SiO_2气凝胶载体制备的Ni-ZrO_2/SiO_2催化剂进行了比较;采用N_2-物理吸附、FT-IR、XRD、TPR、NH_3-TPD、吡啶吸附红外光谱及CO吸附与加氢原位红外光谱等方法对制备的催化剂进行了结构和理化性质表征,探索ZrO_2助剂对催化剂结构和理化性质的影响规律,阐明引起催化性能差别的结构及理化性质原因。
本论文的工作主要分为两部分内容:一、催化剂的制备和顺酐催化加氢性能评价(第三、四章);二、催化剂的结构表征分析(第五、六、七章)。
一、采用溶胶-凝胶法结合超临界流体干燥技术制备了不同ZrO_2含量的ZrO_2-SiO_2复合氧化物气凝胶,浸渍法负载镍制备了系列Ni/ZrO_2-SiO_2催化剂,考察不同锆、镍含量对顺酐加氢活性和γ-丁内酯(GBL)选择性的影响;同时与单组分SiO_2气凝胶为载体浸渍镍、锆混合溶液的Ni-ZrO_2/SiO_2催化剂,以及镍、锆、硅前驱物一步共胶法制备的Ni-ZrO_2-SiO_2催化剂进行了比较。
二、采用N_2-物理吸附、FT-IR、XRD、TPR、NH_3-TPD、吡啶吸附红外光谱及CO吸附与加氢原位红外光谱等方法表征了催化剂的结构及表面性质,阐明造成催化性能差别的结构及理化性质原因。
催化活性评价表明,以溶胶-凝胶结合超临界流体干燥技术制备的ZrO_2-SiO_2复合氧化物气凝胶为载体,浸渍法制备的Ni/ZrO_2-SiO_2系列催化剂:ZrO_2助剂对GBL选择性的影响与Ni含量密切相关,当Ni含量低于13wt%时,引入ZrO_2助剂,GBL的选择性几乎没有变化;当Ni含量达到30wt%时,1wt%的ZrO_2就可使30Ni/ZrO_2-SiO_2催化剂的GBL选择性从0.7%提高到12.9%,ZrO_2含量为5wt%时,GBL选择性达到最大值,为15.1%。
单组分SiO_2气凝胶为载体浸渍镍、锆混合溶液制备的Ni-ZrO_2/SiO_2系列催化剂,在Ni含量低于40 wt%以下时,引入ZrO_2助剂对GBL选择性没有影响,只有当Ni含量达到50wt%时,GBL选择性从1.8%提高到13.07%;而镍、锆、硅前驱物一步共胶法制备的Ni-ZrO_2-SiO_2系列催化剂与共胶法制备的Ni-SiO_2催化剂对比,引入ZrO_2降低了催化剂对GBL的选择性,特别是当Ni含量为30 wt%时,使GBL的选择性从12.2%降低到了0.4%。
对催化剂的结构分析表明:
①共胶法制备的30Ni-SiO_2具有较高的比表面积和较大的孔容,这可能是其催化活性较高的主要原因。其余四种催化剂比表面和孔结构参数相近,特别是30Ni/ZrO_2-SiO_2和30Ni/SiO_2。可以推测,除30Ni-SiO_2外,孔结构不是各催化剂活性差别的主要原因。
②红外光谱、XRD和TPR等研究表明:锆的引入,一方面形成了Zr—O—Si键,降低了NiO与载体之间的相互作用,使NiO的可还原度增加,特别是30Ni-Zr/Si催化剂,表面形成的Zr—O—Si键可能阻断了部分形成Ni—O—Si键的位点,使得NiO与载体间的相互作用减弱明显,耗氢量最大;另一方面,对于30Ni/Zr-Si催化剂,锆在载体中的引入可能在催化剂表面增加了Ni与载体的作用位点。
③表面酸性研究表明:ZrO_2助剂明显增加了催化剂的表面酸量,并新增了B酸位,且表面ZrO_2含量越多酸性越强;同时,较多的Si-O-Zr键会增加中强度酸区的酸密度。
④MA、SAH和GBL表面吸附红外光谱研究表明:ZrO_2助剂明显提高了催化剂30Ni/Zr-Si和30Ni-Zr-Si与MA和SAH的相互作用,也可以说是结构适应性,增加了对反应物的吸附量;但对30Ni-Zr/Si催化剂的结构适应性没有提高,而且还有降低的趋势。
⑤CO吸附及加氢的原位红外光谱研究表明:ZrO_2助剂的引入明显提高了30Ni/Zr-Si催化剂表面活性组分的分散度,催化剂表面活性位分布密集,活性位之间相互作用密切;30Ni-Si催化剂发达的孔隙结构和高的比表面积使其具有了较高的CO吸附力和加氢活性;30Ni-Zr/Si催化剂单一的Ni晶体组成、弱的活性组分与载体之间的相互作用,使其对CO的吸附极弱;30Ni-Zr-Si催化剂则主要由于低的还原镍含量,使其没有足够的吸附CO活性位点,导致了其对CO弱的吸附力和加氢活性。
综合催化剂评价与表征结果可以得出,在顺酐液相加氢反应中,获得较高GBL选择性的主要因素是:较高的表面酸性、活性组分的高分散度及与载体之间合适的相互作用。
ZrO_2助剂的引入:①增加了气凝胶催化剂的表面酸性,新增了B酸位;②降低了NiO与载体之间的相互作用,提高了催化剂的可还原度,增加了催化剂表面活性组分含量;③提高了活性组分在催化剂表面的分散度,使表面活性位点分布密集,活性位之间相互作用密切。
ZrO_2助剂的不同引入方式对其作用有明显影响,只有ZrO_2-SiO_2复合气凝胶为载体浸渍法制各的Ni/ZrO_2-SiO_2催化剂能明显体现出ZrO_2助剂促进性能。而镍、锆混合溶液共浸渍单组分SiO_2气凝胶载体制备的Ni-ZrO_2/SiO_2催化剂,其活性组分与载体之间的相互作用被降低太多,形成了不利于催化反应的结构;一步共胶法引入ZrO_2助剂则造成了催化剂微孔结构的破坏和比表面积的大幅下降,同样是不利的结构。
总之,ZrO_2助剂调变了催化剂的表面酸性和活性组分的分散度及与载体间的相互作用,较好地调控了顺酐液相加氢GBL的选择性。
Promoters have been studied extensively since heterogeneous catalysts have been used industrially.Commercial catalysts tend to involve multiple promoters to enhance the activity,selectivity,lifetime and structural integrity. Generally,in acid catalysis and hydrogenation reactions,promoter effects can be dramatic and unexpected.
In this paper,the promotion effect of ZrO_2 in Ni/SiO_2 aerogel catalyst is investigated systematically.
ZrO_2 has received considerable attention as a promoter due to chemical inertness,higher thermal stability and a special combination of surface properties,namely the preservation of both acidic and basic sites,on the one hand,and reducing and oxidizing properties,on the other.It is reported: introduction of a small amount of zirconium into the support leads to a significant increase of the dispersion of supported metal oxide species, especially,on silica.
Silica aerogel is an excellent catalytic support due to its desirable characteristics,such as inertness,high specific surface area,pronounced mesoporosity,and good thermal stability.Among the silica-supported catalysts,Ni/SiO_2 has been investigated widely.
In this paper,ZrO_2 promoted Ni/SiO_2 catalysts were prepared via three different routes:(ⅰ) impregnation ZrO_2-SiO_2 composite aerogels with a aqueous solution of Ni(NO_3)_2,catalyst code Ni/Zr-Si;(ⅱ) impregnation SiO_2 aerogels with a mixed aqueous solution of Ni(NO_3)_2 and ZrO(NO_3)_2·2H_2O, catalyst code Ni-Zr/Si;(ⅲ) one-pot sol-gel procedure from precursors Ni(NO_3)_2/ZrO(NO_3)_2·2H_2O/Si(OC_2H_5)_4,catalyst code Ni-Zr-Si.For comparison,non-promoted catalysts Ni/Si and Ni-Si also prepared respectively by impregnation Ni(NO_3)_2 with silica aerogel and by one-pot sol-gel process of Ni(NO_3)_2/Si(OC_2H_5)_4.
The above prepared catalysts were characterized by X-ray diffraction (XRD),temperature programmed reduction(TPR),ammonia temperature-programmed desorption(NH_3-TPD),N_2 adsorption-desorption isotherms and Fourier transform infrared(FTIR).The Liquid-phase hydrogenation of maleic anhydride(MA) was evaluated over these catalysts. And the adsorptions of MA,SAH and GBL on these catalysts surfaces were also investigated by FT-IR.
The results revealed that the different preparation routes result in a difference among the obtained catalysts,concerning the crystal structure and composition,surface acidity,mixed level of each component,texture,and catalytic selectivity.
The main results and conclusions are summarized below:
1.Comparing to 30Ni/Si the promoted catalyst 30Ni/Zr-Si has higher activity and selectivity to GBL,which is due to increased surface acidity and the decreased interaction between NiO and SiO_2 and the Ni coverage that was induced by ZrO_2 promoter.
2.The 30Ni-Zr/Si catalyst has lower activity and selectivity than that of 30Ni/Zr-Si.The most possible reason is about the decreased interaction between NiO and SiO_2 that was induced by ZrO_2,and the poor structural suitability between the SAH and the catalyst.
3.The catalyst 30Ni-Zr-Si also has lower activity and selectivity.The main reason is that the content of Ni is too low to increase the GBL selectivity.
4.The main reason for the higher activity and selectivity of 30Ni-Si catalyst is the higher S_(BET) and pore volume over the other four catalysts.
引文
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