CN112337469A - 一种柱状多孔催化剂载体及其制备方法 - Google Patents
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Abstract
本发明属于催化剂载体制备领域,公开了一种柱状多孔催化剂载体及其制备方法。所述柱状多孔催化剂载体中的SiO2所占质量分数可达95%,多孔塑形剂所占质量分数可达50%,孔容积可达1.2ml/g,比表面积可达900㎡/g;Na2O所占质量分数≤0.15%,CaO、MgO及Fe2O3所占质量分数均≤0.03%,抗压强度可达120N。柱状多孔催化剂载体的制备方法包括配制组分A、配制组分B、混合组分A和组分B、造粒、老化、烘干等六个生产步骤。本发明柱状多孔催化剂载体的孔容积和比表面积大,抗压强度高,金属离子杂质含量低,可避免在负载或使用中颗粒破碎,有效避免使用过程中对反应体系和产物的污染,生产过程绿色环保,应用领域拓宽。
Description
技术领域
本发明属于催化剂载体制备领域,具体为一种柱状多孔催化剂载体及其制备方法。
背景技术
介孔二氧化硅主要化学分子式mSiO2·nH2O,其化学性质稳定、不燃烧、无毒无味、除氢氟酸和液碱外不与其他物质发生反应,主要用于医药行业的分离纯化、石油化工行业的催化剂和催化剂载体,工业上还用于干燥剂、液相中杂质吸附剂和气体分离等。
现有技术中介孔二氧化硅的制备方法主要有四种:溶胶凝胶法、沉淀法、气相法及硅脂水解法。应用工业规模化生产的为溶胶凝胶法、沉淀法和气相法,溶胶凝胶法和沉淀法均采用水玻璃泡花碱和硫酸为原料,经酸碱反应、凝胶陈化、水洗、烘干得到介孔二氧化硅。介孔二氧化硅产品为无定型和球型两种规格。无定型二氧化硅因强度不够易破碎,故其在负载反应和使用中有局限性。球型二氧化硅产品因液相改性时的吸附应力导致破碎,在负载后的使用中强度不够导致损耗增大,破碎的碎屑造成气阻增加降低反应效率,因而也具有局限性。因而,如何能保证载体二氧化硅孔结构又能提高强度使载体在催化剂负载时不破碎成为载体二氧化硅产品拓宽应用领域的工艺关键。
发明内容
针对上述问题,本发明提供一种柱状多孔催化剂载体及其制备方法。
一种柱状多孔催化剂载体,所述柱状多孔催化剂载体直径1-10mm,长度3-30mm,SiO2所占质量分数为50%-95%,多孔塑形剂所占质量分数为5%-50%,孔容积0.3-1.2ml/g,孔径2-20nm,比表面积250-900㎡/g。
所述柱状多孔催化剂载体Na2O所占质量分数≤0.15%,CaO所占质量分数≤0.03%,MgO所占质量分数≤0.03%,Fe2O3所占质量分数≤0.03%。
所述柱状多孔催化剂载体抗压强度≥50N。
所述柱状多孔催化剂载体抗压强度为80-120N。
一种柱状多孔催化剂载体的制备方法,其包括以下生产步骤:
(1)配制组分A:将介孔二氧化硅粉料40-90质量份及多孔塑形剂10-60质量份加入混料器中混合;混料器搅拌桨转速为5-200r/min,混料时间为5-100min;混合均匀后得到组分A;所述多孔塑形剂为膨润土、活性炭、硅藻土、淀粉、多孔分子筛中的一种或多种;
(2)配制组分B:将水70-95质量份、粘合剂5-25质量份及助剂0.5-5质量份加入混料器中混合;混料器搅拌桨转速为50-300r/min,混料时间为5-60min,溶液混合均匀后得到组分B;所述粘合剂为瓜尔胶、黄原胶、羧甲基纤维素钠、硅溶胶、聚丙烯酸酯共聚物中的一种或多种;所述助剂为十二烷基苯磺酸钠、聚乙二醇、聚乙烯醇、白油中的一种或多种;
(3)混合组分A和组分B:将生产步骤(1)得到的组分A和生产步骤(2)得到的组分B按照质量比1:0.2-1.5的比例加入到混料器中混合均匀;混料器搅拌桨转速为5-100r/min,混料时间为10-120min;
(4)造粒:将生产步骤(3)得到的物料经输送带输送到颗粒机料仓,颗粒机成型后物料成为直径1-10mm、长度3-30mm柱状规整颗粒;
(5)老化:将生产步骤(4)得到的柱状规整颗粒经传送带到老化槽进行老化,老化温度20-100℃,老化时间0.5-36h;
(6)烘干:将生产步骤(5)得到的柱状规整颗粒烘干,烘干温度60-200℃,烘干时间2-48h。
所述生产步骤(1)二氧化硅粉料粒径细于40目,多孔塑形剂粒径细于40目。
所述二氧化硅粉料粒径为60-400目,多孔塑形剂粒径为60-200目。
所述生产步骤(2)在组分B中,粘合剂质量浓度为0.5-30%、助剂质量浓度为0.5-10%。
所述生产步骤(4)颗粒机为平模颗粒机或环膜颗粒机。
所述生产步骤(6)柱状规整颗粒烘干后的固含量为70%-100%。
与现有技术相比,本发明主要具有以下有益技术效果:
1.柱状多孔催化剂载体具有大的孔容积和比表面积,便于催化剂的有效负载;抗压强度高,避免在负载或使用中颗粒破碎,解决了现有无定型和球型二氧化硅产品的强度不高易破碎、骨架强度低等难题,避免出现物料损耗大、小颗粒增大压阻降低反应效率等问题。
2.拓宽介孔二氧化硅载体应用领域,特别是在水相、强极性溶剂、回流、吸附、高温高压等负载条件的催化剂应用领域。
3.柱状多孔催化剂载体的金属离子杂质含量低,有效避免使用过程中对反应体系和产物的污染。
4.整个生产过程清洁无公害,无固体废弃物、废水、废气等有害物质排放,是一种绿色环保的生产制备方法。
5.该工艺以介孔二氧化硅、多孔塑形剂为原料,按比例均匀混合成组分A;采用水、粘合剂、助剂混合为组分B;组分A与组分B经混料器混合均匀后经颗粒机高温高压挤压成型,颗粒经老化、高温干燥活化并固定成型。该工艺步骤设计合理,劳动强度低,生产效率高,具有显著的经济效益,便于大规模生产应用。
6.注重老化工艺步骤,增强颗粒骨架强度,提高颗粒空隙度,有效防止直接烘干导致的破碎。
具体实施方式
下面通过实施例对本发明进行详细描述。
实施例1
一种柱状多孔催化剂载体,其直径10mm,长度30mm,SiO2所占质量分数为95%,多孔塑形剂所占质量分数为50%,孔容积1.2ml/g,孔径20nm,比表面积900㎡/g;Na2O所占质量分数为0.07%,CaO所占质量分数为0.015%,MgO所占质量分数为0.012%,Fe2O3所占质量分数为0.013%;抗压强度为120N。
实施例2
一种柱状多孔催化剂载体,其直径1mm,长度3mm,SiO2所占质量分数为50%,多孔塑形剂所占质量分数为5%,孔容积0.3ml/g,孔径2nm,比表面积250㎡/g;Na2O所占质量分数为0.15%,CaO所占质量分数为0.03%,MgO所占质量分数为0.03%,Fe2O3所占质量分数为0.03%;抗压强度为50N。
实施例3
取60-100目介孔二氧化硅粉料80kg与80-120目硅藻土10kg、60-80目活性炭粉10kg加入混料器中混合;混料器搅拌桨转速60r/min,混料时间40min,混合均匀后得到组分A;将80kg水、1kg瓜尔胶、5kg硅溶胶、0.5kg羧甲基纤维素钠、1kg聚乙二醇、1.5kg白油加入混料器中混合,混料器搅拌桨转速100r/min,混料时间30min,混合均匀后得到组分B;将组分A和组分B按照质量比1:0.6的比例加入到混料器中混合均匀,混料器搅拌桨转速60r/min,混料时间50min。物料经输送带输送到平模颗粒机成直径2.5mm、长度8mm规整颗粒;柱状颗粒在30℃下老化时间24h后烘干,干燥温度120℃、时间28h,颗粒水分质量分数为8.6%,孔容积为0.8ml/g,比表面积为350㎡/g,孔径为9.1nm,Na2O质量分数为0.12%,CaO质量分数为0.02%,MgO质量分数为0.015%,Fe2O3质量分数为0.018%,抗压强度为80N。
实施例4
取100-200目介孔二氧化硅粉料70kg与60-100目硅藻土15kg、100-200目膨润土粉10kg加入混料器中混合;混料器搅拌桨转速60r/min,混料时间30min,混合均匀后得到组分A;将90kg水、1kg黄原胶、4.5kg聚丙烯酸酯共聚物、1.5kg聚乙二醇、0.5kg聚乙烯醇加入混料器中混合,混料器搅拌桨转速70r/min,混料时间40min,混合均匀后得到组分B;将组分A和组分B按照质量比1:0.8的比例加入到混料器中混合均匀,混料器搅拌桨转速80r/min,混料时间70min。物料经输送带输送到平模颗粒机成直径3mm、长度10mm规整颗粒;柱状颗粒在25℃下老化时间12h后烘干,干燥温度100℃、时间36h,水分质量分数为6.5%,孔容积为0.72ml/g,比表面积为540㎡/g,孔径为5.3nm,Na2O质量分数为0.093%,CaO质量分数为0.018%,MgO质量分数为0.022%,Fe2O3质量分数为0.02%,抗压强度为105N。
实施例5
取200-400目介孔二氧化硅粉料75kg与100-200目活性炭15kg、100-200目多孔分子筛10kg加入混料器中混合;混料器搅拌桨转速40r/min,混料时间50min,混合均匀后得到组分A;将85kg水、10kg硅溶胶、1.5kg黄原胶、1.5kg十二烷基苯磺酸钠、1kg白油加入混料器中混合,混料器搅拌桨转速100r/min,混料时间30min,混合均匀后得到组分B;将组分A和组分B按照质量比1:0.6的比例加入到混料器中混合均匀,混料器搅拌桨转速60r/min,混料时间60min。物料经输送带输送到平模颗粒机成直径2mm、长度5mm规整颗粒;柱状颗粒在50℃下老化时间8h后烘干,干燥温度130℃、时间22h,水分质量分数为4.8%,孔容积为0.9ml/g,比表面积为360㎡/g,孔径为10nm,Na2O质量分数为0.085%,CaO质量分数为0.021%,MgO质量分数为0.02%,Fe2O3质量分数为0.016%,抗压强度为120N。
实施例6
取200-400目介孔二氧化硅粉料40kg与100-200目淀粉10kg加入混料器中混合;混料器搅拌桨转速5r/min,混料时间5min,混合均匀后得到组分A;将70kg水、5kg瓜尔胶、0.5kg十二烷基苯磺酸钠加入混料器中混合,混料器搅拌桨转速50r/min,混料时间5min,混合均匀后得到组分B;将组分A和组分B按照质量比1:0.2的比例加入到混料器中混合均匀,混料器搅拌桨转速5r/min,混料时间10min。物料经输送带输送到平模颗粒机成直径1mm、长度3mm规整颗粒;柱状颗粒在20℃下老化时间0.5h后烘干,干燥温度60℃、时间2h,水分质量分数为2.8%,孔容积为0.85ml/g,比表面积为350㎡/g,孔径为9.5nm,Na2O质量分数为0.08%,CaO质量分数为0.02%,MgO质量分数为0.02%,Fe2O3质量分数为0.015%,抗压强度为115N。
实施例7
取200-400目介孔二氧化硅粉料90kg与100-200目淀粉60kg加入混料器中混合;混料器搅拌桨转速200r/min,混料时间100min,混合均匀后得到组分A;将95kg水、25kg黄原胶、5kg聚乙二醇加入混料器中混合,混料器搅拌桨转速300r/min,混料时间60min,混合均匀后得到组分B;将组分A和组分B按照质量比1:1.5的比例加入到混料器中混合均匀,混料器搅拌桨转速100r/min,混料时间120min。物料经输送带输送到平模颗粒机成直径10mm、长度30mm规整颗粒;柱状颗粒在100℃下老化时间36h后烘干,干燥温度200℃、时间48h,水分质量分数为2.0%,孔容积为1.2ml/g,比表面积为900㎡/g,孔径为20nm,Na2O质量分数为0.07%,CaO质量分数为0.015%,MgO质量分数为0.012%,Fe2O3质量分数为0.013%,抗压强度为120N。
Claims (10)
1.一种柱状多孔催化剂载体,其特征在于,所述柱状多孔催化剂载体直径1-10mm,长度3-30mm,SiO2所占质量分数为50%-95%,多孔塑形剂所占质量分数为5%-50%,孔容积0.3-1.2ml/g,孔径2-20nm,比表面积250-900㎡/g。
2.根据权利要求1所述的一种柱状多孔催化剂载体,其特征在于,所述柱状多孔催化剂载体Na2O所占质量分数≤0.15%,CaO所占质量分数≤0.03%,MgO所占质量分数≤0.03%,Fe2O3所占质量分数≤0.03%。
3.根据权利要求1所述的一种柱状多孔催化剂载体,其特征在于,所述柱状多孔催化剂载体抗压强度≥50N。
4.根据权利要求3所述的一种柱状多孔催化剂载体,其特征在于,所述柱状多孔催化剂载体抗压强度为80-120N。
5.根据权利要求1-4任一所述的一种柱状多孔催化剂载体的制备方法,其特征在于,包括以下生产步骤:
(1)配制组分A:将介孔二氧化硅粉料40-90质量份及多孔塑形剂10-60质量份加入混料器中混合;混料器搅拌桨转速为5-200r/min,混料时间为5-100min;混合均匀后得到组分A;所述多孔塑形剂为膨润土、活性炭、硅藻土、淀粉、多孔分子筛中的一种或多种;
(2)配制组分B:将水70-95质量份、粘合剂5-25质量份及助剂0.5-5质量份加入混料器中混合;混料器搅拌桨转速为50-300r/min,混料时间为5-60min,溶液混合均匀后得到组分B;所述粘合剂为瓜尔胶、黄原胶、羧甲基纤维素钠、硅溶胶、聚丙烯酸酯共聚物中的一种或多种;所述助剂为十二烷基苯磺酸钠、聚乙二醇、聚乙烯醇、白油中的一种或多种;
(3)混合组分A和组分B:将生产步骤(1)得到的组分A和生产步骤(2)得到的组分B按照质量比1:0.2-1.5的比例加入到混料器中混合均匀;混料器搅拌桨转速为5-100r/min,混料时间为10-120min;
(4)造粒:将生产步骤(3)得到的物料经输送带输送到颗粒机料仓,颗粒机成型后物料成为直径1-10mm、长度3-30mm柱状规整颗粒;
(5)老化:将生产步骤(4)得到的柱状规整颗粒经传送带到老化槽进行老化,老化温度20-100℃,老化时间0.5-36h;
(6)烘干:将生产步骤(5)得到的柱状规整颗粒烘干,烘干温度60-200℃,烘干时间2-48h。
6.根据权利要求5所述的一种柱状多孔催化剂载体的制备方法,其特征在于,所述生产步骤(1)二氧化硅粉料粒径细于40目,多孔塑形剂粒径细于40目。
7.根据权利要求6所述的一种柱状多孔催化剂载体的制备方法,其特征在于,所述二氧化硅粉料粒径为60-400目,多孔塑形剂粒径为60-200目。
8.根据权利要求5所述的一种柱状多孔催化剂载体的制备方法,其特征在于,所述生产步骤(2)在组分B中,粘合剂质量浓度为0.5-30%、助剂质量浓度为0.5-10%。
9.根据权利要求5所述的一种柱状多孔催化剂载体的制备方法,其特征在于,所述生产步骤(4)颗粒机为平模颗粒机或环膜颗粒机。
10.根据权利要求5所述的一种柱状多孔催化剂载体的制备方法,其特征在于,所述生产步骤(6)柱状规整颗粒烘干后的固含量为70%-100%。
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