CN108786824A - Si柱撑粘土负载高分散Co3O4-CeO2催化剂的制备方法及应用 - Google Patents
Si柱撑粘土负载高分散Co3O4-CeO2催化剂的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种Si柱撑粘土(SPC)负载高分散Co3O4‑CeO2催化剂的制备方法，包括两个步骤，一是SPC的制备，二是Co‑Ce/SPC的制备。本发明利用SPC为载体，通过沉积‑沉淀法合成高分散复合纳米Co3O4‑CeO2催化剂，并将其用于甲苯催化燃烧，该催化剂表现出优异的催化活性及稳定性。另外合成的SPC与蒙脱土相比，其层间距和比表面积均变大。以其为载体，制备的Co3O4‑CeO2纳米晶催化剂，活性组分颗粒小，分散均匀，催化降解甲苯的活性高，稳定性良好，是一种有良好应用前景的性能优异的降解VOC的催化材料。
Description
技术领域
本发明涉及一种化学催化剂制备工艺技术领域，特别是一种Si柱撑粘土负载高分散Co3O4-CeO2催化剂的制备方法及应用，主要用于甲苯催化燃烧。
背景技术
Si柱撑粘土(SPC)具有大比表面积和丰富的孔结构，近年来已引起了广泛的关注。现有文献中，关于SPC多是探讨其合成方法以及对其结构和性能进行表征，或是在SPC的框架中掺杂其他物质进行改性，然后应用于以下几个方面：催化氧化脱硫、催化植物沥青裂解、异丙苯的催化裂解、催化苯氢化反应、催化苯酚羟基化反应、消除水溶液中有毒的金属离子Cr(VI)、用于可控药物释放及目标定位、催化无水叔丁基环己烯、环己烯选择性氧化等。
已有的研究中，并未发现将SPC应用于甲苯催化降解方面的报道。并且，现有的过渡金属催化剂用于甲苯催化燃烧的活性较低，因此亟需一种高活性的催化剂。
发明内容
本发明的目的是为了解决上述现有技术的不足而提供一种SPC负载高分散Co3O4-CeO2催化剂的制备方法及应用，该催化剂的活性组分分散好、同时可将其用于甲苯高效催化燃烧。
为了实现上述目的，本发明所设计的一种SPC负载高分散Co3O4-CeO2催化剂的制备方法，包括以下两个步骤：
(1)SPC的制备
将Aladdin公司的KSF无机级蒙脱土(MMT)加水，首先制备成悬浊液A，另取十二烷基二甲基苄基氯化铵阳离子表面活性剂和十二烷基硫酸钠阴离子表面活性剂溶解到乙醇中，再加入正硅酸乙酯，搅拌0.5h后得到清澈溶液B，然后将清澈溶液B慢慢滴入到悬浊液A中，搅拌0.5h，用氨水溶液调节pH至10，在25℃下搅拌2h，过滤，90℃干燥，得到样品前驱体，然后在马弗炉中空气氛围下以10℃/min的速率程序升温至550℃煅烧3h，得到稳定的SPC；
所述MMT：十二烷基二甲基苄基氯化铵阳离子表面活性剂：十二烷基硫酸钠阴离子表面活性剂：正硅酸乙酯：乙醇：水的摩尔比为1:2:0.4:30:1.2:250。
(2)Co-Ce/SPC的制备
将1.0g SPC分散在100mL去离子水中，加入1.0mol/L Co(NO3)2溶液和1.0mol/L的Ce(NO3)3·6H2O溶液，得到的混合物在25℃下充分搅拌1h，再逐滴加入1.0mol/L的氨水，调节混合物的pH至9.0，搅拌12h，离心、洗涤，70℃干燥12h，然后在马弗炉中500℃煅烧2h，得到Co-Ce/SPC催化剂，其中Co占总质量的10％，Ce占总质量的5％。
一种SPC负载高分散Co3O4-CeO2催化剂的应用在于上述Co3O4-CeO2催化剂可用于甲苯催化燃烧。
由于SPC具有大比表面积和丰富的孔结构，不仅可使大分子有机物出入这些通道或在其内孔被吸附，而且将其作为催化剂载体，可使活性组分有极高的分散度，从而提高催化燃烧甲苯的活性。本专利利用SPC为载体，通过沉积-沉淀法合成高分散复合纳米Co3O4-CeO2催化剂，并将其用于甲苯催化燃烧，该催化剂表现出优异的催化活性及耐久性。
本发明得到的一种SPC负载高分散Co3O4-CeO2催化剂的制备方法，以其为载体，制备的Co3O4-CeO2纳米晶催化剂，活性组分颗粒小，分散均匀，催化燃烧甲苯的活性高，耐久性良好，是一种有良好应用前景的性能优异的降解VOC的催化剂。
附图说明
图1是SPC负载Co-Ce催化剂用于甲苯催化燃烧的活性图；
图2是SPC负载Co-Ce催化剂的耐久性测试图；
图3是MMT和SPC的小角X射线衍射图；
图4是10％Co-5％Ce/SPC催化剂的高分辨透射电镜图。
具体实施方式
下面结合附图和实施例对本发明进一步说明。
本实施例提供的一种Si柱撑粘土负载高分散Co3O4-CeO2催化剂的制备方法，包括以下两个步骤：
(1)SPC的制备
取MMT加30mL水，首先制备成悬浊液A。另取十二烷基二甲基苄基氯化铵阳离子表面活性剂和十二烷基硫酸钠阴离子表面活性剂，溶解到乙醇中，再加入正硅酸乙酯，搅拌0.5h得到清澈溶液B。然后将清澈溶液B慢慢滴入到悬浊液A中，搅拌0.5h。用氨水溶液调节pH至10，在25℃下搅拌2h，过滤，90℃干燥，得到样品前驱体。然后在马弗炉中空气氛围下以10℃/min的速率程序升温至550℃煅烧3h，得到稳定的SPC。其中，蒙脱土：十二烷基二甲基苄基氯化铵：十二烷基硫酸钠：正硅酸乙酯：乙醇：水(摩尔比)＝1:2:0.4:30:1.2:250。
(2)Co-Ce/SPC的制备
将1.0g SPC分散在100mL去离子水中，加入1.0mol/L的Co(NO3)2溶液和1.0mol/L的Ce(NO3)3·6H2O溶液。得到的混合物在25℃下充分搅拌1h。再逐滴加入1.0mol/L的氨水，调节混合物的pH至9.0，搅拌12h，离心、洗涤，70℃干燥12h。在马弗炉中500℃煅烧2h，得到10％Co-5％Ce/SPC。
下面对制得的SPC负载高分散Co3O4-CeO2催化剂进行测试，其中图1是SPC负载Co-Ce催化剂用于甲苯催化降解的活性图，活性评价实验在WFS-3010(天津，先权)反应装置上进行，空速为20000h-1，甲苯浓度为1000ppm。利用在线气相色谱(Shimadzu,GC-14C,Japan)，使用氢火焰离子化检测器(FID)检测进入色谱的有机物浓度。色谱工作条件如下：汽化室温度120℃，柱温80℃。采用N2000在线色谱工作站记录分析数据。图1表明，10％Co-5％Ce/SPC在200℃使甲苯的转化率达到98.6％。
图2是SPC负载Co-Ce催化剂的耐久性测试图，耐久性实验的测试条件与活性评价实验相同。图2表明，10％Co-5％Ce/SPC在190℃下连续反应1000h，甲苯的转化率仅从96％降低到90％，具有非常良好的稳定性，而且能够有效地抵抗含氯的VOC及H2O的影响。
图3是两种载体的小角X射线衍射图，该实验在X射线粉末衍射仪(PANalytical)上进行分析，实验条件如下：CuKα射线(40mA，40kV)，扫描速率为0.02°/s。利用Braggequation(2d001sinθ＝nλ)计算层间距。图3表明，柱撑使蒙脱土的层间距由0.96nm增加至2.61nm。
图4是10％Co-5％Ce/SPC催化剂的高分辨透射电镜图。样品的形貌利用JEOL-2010型透射电镜表征，工作电压为200kV。图4表明，在10％Co-5％Ce/SPC中，活性组分Co3O4和CeO2的颗粒直径在5-8nm，均匀分散在SPC表面。
表1是样品的比表面积、总孔体积，具体数据如下：
aBET specific surface area.
bTotalpore volume estimated atP/P0＝0.99.
样品的比表面积(SBET)、孔体积(Vp)利用TristarⅡ3020(MicromeriticsCompany，USA)全自动吸附仪表征。液氮温度(77K)下，利用N2吸附法测定SBET，利用Barrett-Joyner-Halenda(BJH)方法测定Vp。
从表1中可以看出，通过Si柱撑后，MMT的SBET由30m2/g增加到453m2/g，Vp由0.11cm3/g增加到0.77cm3/g。负载Co-Ce以后，SPC的SBET和Vp均减小(453m2/g减小到303m2/g，0.77cm3/g减小到0.30cm3/g)，说明部分负载组分进入了载体孔道，堵塞了一些孔。
以上所述实施例仅表达了本发明的一种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (2)
1.一种Si柱撑粘土负载高分散Co3O4-CeO2催化剂的制备方法，其特征在于，包括以下两个步骤：
(1)SPC的制备
将蒙脱土加水，首先制备成悬浊液A，另取十二烷基二甲基苄基氯化铵阳离子表面活性剂和十二烷基硫酸钠阴离子表面活性剂溶解到乙醇中，再加入正硅酸乙酯，搅拌0.5h后得到清澈溶液B，然后将清澈溶液B慢慢滴入到悬浊液A中，搅拌0.5h，用氨水溶液调节pH至10，在25℃下搅拌2h，过滤，90℃干燥，得到样品前驱体，然后在马弗炉中空气氛围下以10℃/min的速率程序升温至550℃煅烧3h，得到稳定的SPC；其中，蒙脱土：十二烷基二甲基苄基氯化铵阳离子表面活性剂：十二烷基硫酸钠阴离子表面活性剂：正硅酸乙酯：乙醇：水的摩尔比为1:2:0.4:30:1.2:250；
(2)Co-Ce/SPC的制备
将1.0g SPC分散在100mL去离子水中，加入1.0mol/L的Co(NO3)2溶液和1.0mol/L的Ce(NO3)3·6H2O溶液，得到的混合物在25℃下充分搅拌1h，再逐滴加入1.0mol/L的氨水，调节混合物的pH至9.0，搅拌12h，离心、洗涤，70℃干燥12h，然后在马弗炉中500℃煅烧2h，得到Co-Ce/SPC，其中Co占总质量的10％，Ce占总质量的5％。
2.一种如权利要求1所述的SPC负载高分散Co3O4-CeO2催化剂的应用，其特征在于：Co3O4-CeO2催化剂可用于甲苯催化燃烧。
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