以镁铝尖晶石为基础的酸碱一体化材料的研究
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摘要
近年来随着催化裂化(FCC)加工原油含硫量的提高和环保法规对污染物排放的严格限制,减少催化裂化再生烟气中SO2的排放问题受到关注,其中添加2%-3%的镁铝尖晶石体系的硫转移剂是最为廉价且有效的手段。但由于镁铝尖晶石的偏碱性,其裂化性能甚至低于常规FCC催化剂的惰性载体如高岭土等粘土类。随着原油含硫量的逐年增加,势必要求增加硫转移剂的添加量才能满足日益严格的环保要求,因而必然会对FCC主催化剂产生稀释作用,进而影响FCC反应的转化深度及产物分布。
因此,设想将镁铝尖晶石的碱性与分子筛的酸性结合制备以镁铝尖晶石为基础的酸碱一体化材料。这样可以在保证对主催化剂影响较小的情况下适当增加其添加量。本论文主要从两方面着手：一是将镁铝尖晶石与ZSM-5分子筛机械混合,制备既增产丙烯又可降低SO2排放的双功能助剂(以ZSM-5分子筛为活性组分,镁铝尖晶石为基质)；二是借鉴微介孔复合材料的合成方法,采用在镁铝尖晶石介孔结构中附着分子筛的初级或次级结构单元的方法,使得合成的酸碱双功能镁铝尖晶石材料具有较高的裂化性能和一定的脱硫性能。另外,镁铝尖晶石的脱硫活性与比表面关系密切,比表面越高,越有利于尖晶石的脱硫。因此本论文还对高比表面镁铝比尖晶石的合成进行了探索。
增产丙烯与烟气脱硫双功能助剂与酸碱双功能镁铝尖晶石材料的共同点是二者均将分子筛的酸性和镁铝尖晶石的碱性融合为一体,不同点在于前者添加至FCC主催化剂中是以牺牲汽油收率为代价使得丙烯和LPG收率提高,同时附加了脱硫功能；而后者可以在不影响主催化剂的裂化性能(尤其是汽油、柴油收率)的前提下适量提高添加量,保证较优的脱硫性能。
研究发现增产丙烯与烟气脱硫双功能助剂的瓶颈问题在于：镁铝尖晶石与ZSM-5在焙烧和水热处理过程中发生相互作用,使得ZSM-5的结构和酸性发生变化进而使得ZSM-5增产丙烯的效果降低；同时镁铝尖晶石本身较高的HTC值和焦炭选择性也是造成双功能助剂增产丙烯效果降低的原因之一。对ZSM-5分子筛进行La、P改性,可提高其水热稳定性和酸性,进而改善双功能助剂的增产丙烯性能。对镁铝尖晶石进行P改性、用氯化铵或盐酸溶液处理镁铝尖晶石等方法,可改变ZSM-5分子筛的酸性并降低镁铝尖晶石的氢转移活性,改善双功能助剂的增产丙烯性能,同时不同程度地提高脱硫性能。
将Y分子筛纳米簇溶液或ZSM-5分子筛母液和镁铝尖晶石混合后晶化,可以将分子筛的结构单元引入到尖晶石介孔结构中,使得尖晶石酸性和裂化重油性能大大提高,但脱硫性能明显降低；对含铈尖晶石采用ZSM-5分子筛母液在中性(pH=7)条件下改性,可以在保持氧化铈结构的同时引入分子筛的结构单元,使得裂化性能提高的同时保持较好的脱硫性能。
在镁铝尖晶石中引入二价过渡金属Cu、Co或三价过渡金属Fe、Cr时,可以不同程度地提高尖晶石的脱硫活性和还原再生性能,也可以提高对重油的转化率,但是裂化VGO过程中会明显增大尖晶石的非选择性氢转移活性。
对富镁或富铝的镁铝尖晶石采用适当的硝酸处理均可分别获得比表面高达301和311m2/g的较纯的镁铝尖晶石,但其水热稳定性均较差。
As the sulfur content in crude oil for fluid catalytic cracking (FCC) process is increased and the environmental legislation becomes more stringent, the removal of SOx from FCC units has been the subject of a considerable amount of attention over the past few years. To date, the least costly means is the addition of 2%～3% of sulfur-transfer agent which generally contains MgAl2O4. However, the stronger basic property for the spinel makes it to be less active for cracking hydrocarbons even compared with conventional inert matrices of FCC catalysts such as clays. Since the amount of sulfur-transfer agents required for effective SOx emission reduction is increased due to the increasing sulfur content in crude oil and the more stringent environmental regulations, there is no doubt that their dilution effect on FCC catalysts would be stronger.
Therefore, an assumption of preparing the MgAl2O4-based materials which combine the basic property of MgAl2O4 with acidic property of zeolites was put forward. In this way, the addition amount of spinel would be increased without much affecting the catalytic performance of the FCC base catalyst. This paper mainly focused on two aspects. One way is physically mixing MgAl2O4 with ZSM-5 zeolite in order to obtain the bifunctional additives for enhancing propylene yield and removing SO2 in FCC units. For the bifunctional additives, ZSM-5 zeolite was employed as the active component and MgAl2O4 applied as matrix.
The other method is to introduce the zeolitic building units into the mesopores of the spinel in light of the synthesis of meso-microporous zeolite. The obtained modified spinels with both basic and acidic sites would have much higher cracking ability compared to the parent spinel due to the improvement of Bronsted and Lewis acidity which can survive the severe hydrothermal treatment. Moreover, there would be still basic sites remained active for SO2 adsorption. Besides, the capacity of SO2 picking-up of MgAl2O4 is closely related to surface area. The increase in surface area can lead to the improvement in SO2 uptake capacity. So the synthesis of MgAl2O4 with high surface area was also explored in the paper.
The common point of the bifunctional additive for enhancing propylene yield and removing SO2 and the modified spinel with both basic and acidic sites is that both combine the acidic property for the zeolite and the basic property for the spinel into a single particle. But there is big difference between the two kinds of materials. When the bifunctional additive is added into the FCC base catalyst, the propylene and LPG yield increase at the cost of gasoline yield, and the function of removing SO2 is also attached. While the introduction of a larger amount of modified spinel into the FCC system would guarantee the effective SO2 removal on the condition that it affects little the catalytic property of FCC catalyst (especially gasoline and diesiel oil yileds).
As to the bifunctional additive for enhancing propylene yield and removing SO2, the bottleneck is that the existence of magnesium though in the form of stable spinel would interact with ZSM-5 during calcination and severe hydrothermal conditions, resulting in lower ZSM-5 activity. Moreover, the relatively higher HTC value and coke selectivity of MgAl2O4 also contribute to the lower ZSM-5 acitivity of the bifunctional additives for increasing propylene yield. However, the negative effect of Mg2+ could be counteracted by modification of ZSM-5 with both La and P, leading to the improvement of ZSM-5 hydrothermal stability and activity. On the other hand, modifying MgAl2O4 with P could not only inhibit the change in ZSM-5 acidity caused by the existence of MgAl2O4 but also largely decrease the hydrogen transfer activity of spinels, thereby boosting the ZSM-5 effectiveness in increasing propylene yield. And P doping also distinctly promoted the SO2 uptake capacity of bifunctional additives. What's more, pretreating MgAl2O4 with NH4Cl or HCl solutions or further exchanging bifunctional additives with amonium cations could also increase the ZSM-5 activity for increasing propylene yield and improve the DeSOx activity. The pretreatment of MgAl2O4 with NH4Cl or HCl solutions not only changed the ZSM-5 acidity and increased the weak acidic hydroxyl groups of additives, but also decreased the selective hydrogen transfer activity of spinels, which may both be responsible for the increase in ZSM-5 activity.
Concerning the modified spinel with both acidic and basic sites, the structural building units of zeolite can be introduced into the mesopore of the spinel by employing the nanocluster solutions of zeolite Y or ZSM-5 mother solution. Compared to the parent spinel, the acidity and cracking ability of spinel were greatly increased, but the DeSOx activity was obviously decreased. When modifying the Ce/MgAl2O4 with ZSM-5 mother solution under neutral condition (pH=7), the building units of zeolite could be introduced into the spinel with the preservation of the CeO2 phase, obtaining the modified Ce/MgAl2O4 with both improved cracking ability and well remained DeSOx activity.
The introduction of divalent transition metals Cu, Co or trivalent transition metals Fe, Cr into MgAl2O4 could improve the SO2 uptake capacity of the spinel and the reducibility of the sulfate formed during removal SO2 in different extents. Also it could increase the conversion of VGO cracking, but the non-selective hydrogen transfer activity (esp. coke selectivity) was evidently increased.
Suitable treatment of Mg- or Al-rich magnesium-aluminate spinel prepared under acidic conditions with HNO3 solutions could obtain spinels with high surface areas of 301 and 311 m2/g, respectively. But the obtained spinels revealed poor hydrothermal stability.
因此,设想将镁铝尖晶石的碱性与分子筛的酸性结合制备以镁铝尖晶石为基础的酸碱一体化材料。这样可以在保证对主催化剂影响较小的情况下适当增加其添加量。本论文主要从两方面着手：一是将镁铝尖晶石与ZSM-5分子筛机械混合,制备既增产丙烯又可降低SO2排放的双功能助剂(以ZSM-5分子筛为活性组分,镁铝尖晶石为基质)；二是借鉴微介孔复合材料的合成方法,采用在镁铝尖晶石介孔结构中附着分子筛的初级或次级结构单元的方法,使得合成的酸碱双功能镁铝尖晶石材料具有较高的裂化性能和一定的脱硫性能。另外,镁铝尖晶石的脱硫活性与比表面关系密切,比表面越高,越有利于尖晶石的脱硫。因此本论文还对高比表面镁铝比尖晶石的合成进行了探索。
增产丙烯与烟气脱硫双功能助剂与酸碱双功能镁铝尖晶石材料的共同点是二者均将分子筛的酸性和镁铝尖晶石的碱性融合为一体,不同点在于前者添加至FCC主催化剂中是以牺牲汽油收率为代价使得丙烯和LPG收率提高,同时附加了脱硫功能；而后者可以在不影响主催化剂的裂化性能(尤其是汽油、柴油收率)的前提下适量提高添加量,保证较优的脱硫性能。
研究发现增产丙烯与烟气脱硫双功能助剂的瓶颈问题在于：镁铝尖晶石与ZSM-5在焙烧和水热处理过程中发生相互作用,使得ZSM-5的结构和酸性发生变化进而使得ZSM-5增产丙烯的效果降低；同时镁铝尖晶石本身较高的HTC值和焦炭选择性也是造成双功能助剂增产丙烯效果降低的原因之一。对ZSM-5分子筛进行La、P改性,可提高其水热稳定性和酸性,进而改善双功能助剂的增产丙烯性能。对镁铝尖晶石进行P改性、用氯化铵或盐酸溶液处理镁铝尖晶石等方法,可改变ZSM-5分子筛的酸性并降低镁铝尖晶石的氢转移活性,改善双功能助剂的增产丙烯性能,同时不同程度地提高脱硫性能。
将Y分子筛纳米簇溶液或ZSM-5分子筛母液和镁铝尖晶石混合后晶化,可以将分子筛的结构单元引入到尖晶石介孔结构中,使得尖晶石酸性和裂化重油性能大大提高,但脱硫性能明显降低；对含铈尖晶石采用ZSM-5分子筛母液在中性(pH=7)条件下改性,可以在保持氧化铈结构的同时引入分子筛的结构单元,使得裂化性能提高的同时保持较好的脱硫性能。
在镁铝尖晶石中引入二价过渡金属Cu、Co或三价过渡金属Fe、Cr时,可以不同程度地提高尖晶石的脱硫活性和还原再生性能,也可以提高对重油的转化率,但是裂化VGO过程中会明显增大尖晶石的非选择性氢转移活性。
对富镁或富铝的镁铝尖晶石采用适当的硝酸处理均可分别获得比表面高达301和311m2/g的较纯的镁铝尖晶石,但其水热稳定性均较差。
As the sulfur content in crude oil for fluid catalytic cracking (FCC) process is increased and the environmental legislation becomes more stringent, the removal of SOx from FCC units has been the subject of a considerable amount of attention over the past few years. To date, the least costly means is the addition of 2%～3% of sulfur-transfer agent which generally contains MgAl2O4. However, the stronger basic property for the spinel makes it to be less active for cracking hydrocarbons even compared with conventional inert matrices of FCC catalysts such as clays. Since the amount of sulfur-transfer agents required for effective SOx emission reduction is increased due to the increasing sulfur content in crude oil and the more stringent environmental regulations, there is no doubt that their dilution effect on FCC catalysts would be stronger.
Therefore, an assumption of preparing the MgAl2O4-based materials which combine the basic property of MgAl2O4 with acidic property of zeolites was put forward. In this way, the addition amount of spinel would be increased without much affecting the catalytic performance of the FCC base catalyst. This paper mainly focused on two aspects. One way is physically mixing MgAl2O4 with ZSM-5 zeolite in order to obtain the bifunctional additives for enhancing propylene yield and removing SO2 in FCC units. For the bifunctional additives, ZSM-5 zeolite was employed as the active component and MgAl2O4 applied as matrix.
The other method is to introduce the zeolitic building units into the mesopores of the spinel in light of the synthesis of meso-microporous zeolite. The obtained modified spinels with both basic and acidic sites would have much higher cracking ability compared to the parent spinel due to the improvement of Bronsted and Lewis acidity which can survive the severe hydrothermal treatment. Moreover, there would be still basic sites remained active for SO2 adsorption. Besides, the capacity of SO2 picking-up of MgAl2O4 is closely related to surface area. The increase in surface area can lead to the improvement in SO2 uptake capacity. So the synthesis of MgAl2O4 with high surface area was also explored in the paper.
The common point of the bifunctional additive for enhancing propylene yield and removing SO2 and the modified spinel with both basic and acidic sites is that both combine the acidic property for the zeolite and the basic property for the spinel into a single particle. But there is big difference between the two kinds of materials. When the bifunctional additive is added into the FCC base catalyst, the propylene and LPG yield increase at the cost of gasoline yield, and the function of removing SO2 is also attached. While the introduction of a larger amount of modified spinel into the FCC system would guarantee the effective SO2 removal on the condition that it affects little the catalytic property of FCC catalyst (especially gasoline and diesiel oil yileds).
As to the bifunctional additive for enhancing propylene yield and removing SO2, the bottleneck is that the existence of magnesium though in the form of stable spinel would interact with ZSM-5 during calcination and severe hydrothermal conditions, resulting in lower ZSM-5 activity. Moreover, the relatively higher HTC value and coke selectivity of MgAl2O4 also contribute to the lower ZSM-5 acitivity of the bifunctional additives for increasing propylene yield. However, the negative effect of Mg2+ could be counteracted by modification of ZSM-5 with both La and P, leading to the improvement of ZSM-5 hydrothermal stability and activity. On the other hand, modifying MgAl2O4 with P could not only inhibit the change in ZSM-5 acidity caused by the existence of MgAl2O4 but also largely decrease the hydrogen transfer activity of spinels, thereby boosting the ZSM-5 effectiveness in increasing propylene yield. And P doping also distinctly promoted the SO2 uptake capacity of bifunctional additives. What's more, pretreating MgAl2O4 with NH4Cl or HCl solutions or further exchanging bifunctional additives with amonium cations could also increase the ZSM-5 activity for increasing propylene yield and improve the DeSOx activity. The pretreatment of MgAl2O4 with NH4Cl or HCl solutions not only changed the ZSM-5 acidity and increased the weak acidic hydroxyl groups of additives, but also decreased the selective hydrogen transfer activity of spinels, which may both be responsible for the increase in ZSM-5 activity.
Concerning the modified spinel with both acidic and basic sites, the structural building units of zeolite can be introduced into the mesopore of the spinel by employing the nanocluster solutions of zeolite Y or ZSM-5 mother solution. Compared to the parent spinel, the acidity and cracking ability of spinel were greatly increased, but the DeSOx activity was obviously decreased. When modifying the Ce/MgAl2O4 with ZSM-5 mother solution under neutral condition (pH=7), the building units of zeolite could be introduced into the spinel with the preservation of the CeO2 phase, obtaining the modified Ce/MgAl2O4 with both improved cracking ability and well remained DeSOx activity.
The introduction of divalent transition metals Cu, Co or trivalent transition metals Fe, Cr into MgAl2O4 could improve the SO2 uptake capacity of the spinel and the reducibility of the sulfate formed during removal SO2 in different extents. Also it could increase the conversion of VGO cracking, but the non-selective hydrogen transfer activity (esp. coke selectivity) was evidently increased.
Suitable treatment of Mg- or Al-rich magnesium-aluminate spinel prepared under acidic conditions with HNO3 solutions could obtain spinels with high surface areas of 301 and 311 m2/g, respectively. But the obtained spinels revealed poor hydrothermal stability.
引文
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