CN113694888B - 铌改性有机层状双氧化物/氧化石墨烯纳米复合材料作为co2吸附剂的制备方法和应用 - Google Patents
铌改性有机层状双氧化物/氧化石墨烯纳米复合材料作为co2吸附剂的制备方法和应用 Download PDFInfo
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Abstract
本发明提供了铌改性有机层状双氧化物/氧化石墨烯纳米复合材料作为CO2吸附剂的制备方法和应用。首先制备具有良好结构的插层长碳链有机阴离子硬脂酸盐的有机层状双氢氧化物,通过原位法与氧化石墨烯(GO)进行复合,得到有机层状双氢氧化物/氧化石墨烯纳米复合材料,然后通过浸渍法将草酸铌(C10H5NbO20)负载于上述复合材料上,最终通过煅烧活化得到铌改性有机层状双氧化物/氧化石墨烯复合材料作为高温CO2吸附剂。本发明在宽的温度(200℃~300℃)范围内,对CO2(浓度为5vol.%~25vol.%)和N2(浓度为75vol.%~95vol.%)的混合气体具有较高的吸附能力,本发明吸附剂具有较高的比表面积和较好的热稳定性。
Description
技术领域
本发明涉及一种用于吸附二氧化碳的铌改性有机层状双氧化物/氧化石墨烯纳米复合吸附剂的制备方法及其在高温条件下吸附CO2的应用。
背景技术
众所周知,全球变暖的一个主要原因之一就是温室气体CO2的排放。近些年来,人们越来越多的关注CO2 capture,utilization,and storage(CCUS)技术。其中吸附增强水煤气变换(SEWGS)被认为是一种很有前景的燃烧前CO2捕集技术,该技术是WGS反应和CO2吸附的结合,反应过程如等式1所示。通过反应过程中吸附或者去除CO2,促使反应向右侧进行,从而使该反应更加完全并且获得更多的H2能源。在实际的工业应用中吸附剂扮演着重要的角色,所以需要寻找一个高性能与再生性能良好的吸附剂。SEWGS反应通常发生在200~400℃的环境下,常见的物理吸附剂(如:活性炭,沸石等)在高温下吸附性能非常差;而常见的化学吸附剂(如胺基固体吸附剂,金属氧化物等)有着动力学,再生性能差等的缺点。因此,需要我们致力于寻找一个合适的吸附剂。
水滑石,又称为层状双氢氧化物(LDH)。其通式为:其在200-400℃下具有良好的吸附性能,并且具有良好的动力学和再生性能。此外,在H2O和SO2存在的情况下LDH依然保持着良好的吸附性能。近些年来LDH衍生的氧化物已经被众多学者证明其可以良好的应用与SEWGS反应中。已经有很多文献报道了关于LDH及其衍生物的CO2吸附性能。适当的高温煅烧可以使LDH形成表面具有更多碱性位点的层状双氧化物(LDO)纳米复合材料,从而可以提高其吸附容量。较大尺寸的阴离子An-可能会导致LDH前体中较大的层间距,从而使CO2分子更容易扩散到层间区域与活性中心相互作用。石墨烯是一种平面二维纳米材料,它被认为是当今世界上最薄的无带隙材料,这使它成为环境应用的绝佳候选材料。结合之前的研究,需要对LDH材料进一步的改性来改善其性能。在结构上,GO的2D片状形态与LDH非常的相容,GO的存在可以增强LDH的颗粒分散性。本专利,我们首次报道了通过沉淀法分别制备了硬脂酸插层的LDH(简称LDH-stearate)和GO/LDH-stearate复合材料,并通过浸渍法负载少量铌。通过一系列表征研究其结构和CO2吸附性能。本项目的实施得到:国家自然科学基金项目(编号:21277008;20777005);北京自然科学基金(编号:8082008);国家重点研发计划(No.2017YFC0209905)的资助,也是这些项目的研究内容。
发明内容
本发明的目的是提供一种有机层状双氧化物/氧化石墨烯纳米复合吸附剂的制备及其用于高温的CO2吸附。硬脂酸的插层使LDH产生更多的表面碱性位点,同时煅烧后所得的混合金属氧化物的结晶度较低,并且所形成的准非晶结构比LDH更稳定。带正电荷LDH沉淀到带负电荷GO上的过程中,相互之间的静电相互作用以逐层方式驱动异质结构的纳米复合材料进行自组装,GO的加入后复合材料分散性和稳定性均得到提高。复合材料的比表面积为:445m2/g。所提供的吸附剂可在较高的反应温度(200℃~300℃)下,对CO2具有较高的吸附量。其中,6GO/LDO-Stearate具有着最高的吸附容量(0.83mmol/g),比未改性的LDO(0.35mmol/g)高2倍以上。表征结果证明,复合材料吸附性能提高的关键因素是比表面积和碱性位点提高。此吸附剂制备工艺简单,原材料在自然界广泛存在。
本发明提供一种用于高温CO2吸附的有机层状双氧化物/氧化石墨烯纳米复合吸附剂的制备方法:
(1)将一定量的GO(10~100mg)分别溶解于100ml去离子水中,室温下搅拌0.5h,并将上述混合液于超声处理3~6h,得到分散均匀的GO。加入一定量的Mg(NO3)2·6H2O和Al(NO3)3·9H2O,保持[Mg2+]/[Al3+](摩尔比)=2~3,将0.2mol/L的硬脂酸混合于上述混合液中,保持硬脂酸阴离子C17H35COO-:Mg2++Al3+=1~3,将1.2~4mol/L的NaOH溶液,以1~10mL/min的速度滴加到上述溶液中调节pH,通过pH仪将溶液的pH维持在10±0.1,将上述溶液于60~80℃水浴搅拌6~12h。抽滤洗涤至pH=7,将所得固体于100~120℃干燥、研磨并过80目筛子,所得样品为xGO/LDH-Stearate,其中x为复合材料中GO含量的质量比。通过浸渍法将草酸铌(C10H5NbO20)负载于xGO-LDH-Stearate上。首先将一定量C10H5NbO20溶解于过量乙醇中,接着加入上述xGO-LDH-Stearate,其中C10H5NbO20:xGO-LDH-Stearate=0.01~0.2,将上述悬浮液搅拌2~10h,将其转移至60℃条件下真空烘干。获得的样品被称为yNb/xGO-LDH-Stearate,y是复合材料中C10H5NbO20负载量的质量百分比。在进行CO2吸附之前,将上述的吸附剂进行煅烧活化。取适量的样品于管式炉中,在300~500℃和50mL/min氮气气氛下煅烧2~6h。所得的样品被称为xGO-LDO-Stearate,yNb/xGO-LDO-Stearate。
(2)将一定量的吸附剂放置于热重仪器中,通入CO2(浓度为5vol.%~25vol.%)和N2(浓度为75vol.%~95vol.%)的混合气,反应温度为200℃~300℃,对混合气体进行吸附,通过质量变化检测吸附剂对CO2的附量。在上述条件下本吸附剂具有较高的吸附容量(0.35~0.83mmol/g)。
附图说明
图1为本发明制备的LDH、LDH-Stearate、6GO-LDH-Stearate、0.5Nb/6GO-LDH-Stearate、1Nb/6GO-LDH-Stearate、2Nb/6GO-LDH-Stearate吸附剂的XRD图。
图2为本发明制备的LDH、LDH-Stearate、6GO-LDH-Stearate、LDO、LDO-Stearate、6GO-LDO-Stearate吸附剂的透射电镜图。
图3为本发明制备的LDO、LDO-Stearate、6GO-LDO-Stearate、0.5Nb/6GO-LDO-Stearate、1Nb/6GO-LDO-Stearate、2Nb/6GO-LDO-Stearate吸附剂的N2-吸附/脱附图。
图4为本发明制备的LDO、LDO-Stearate、6GO/LDO-Stearate、0.5Nb/6GO-LDO-Stearate、1Nb/6GO-LDO-Stearate、2Nb/6GO-LDO-Stearate吸附剂在200℃吸附15%CO2混合气1小时的吸附图。
具体实施方式
吸附剂一般取5-30mg做实验。
实施例1
(1)将20mg的GO溶解于100ml去离子水中,室温下搅拌0.5h,并将上述混合液于超声处理3h,得到分散均匀的GO。加入一定量的Mg(NO3)2·6H2O和Al(NO3)3·9H2O,保持[Mg2+]/[Al3+](摩尔比)=2,将0.05mol的硬脂酸混合于上述120ml混合液中,[硬脂酸]/[Mg2+](摩尔比)=2,将1.2mol/L的NaOH溶液,以1mL/min的速度滴加到上述溶液中调节pH,通过pH仪将溶液的pH维持在10±0.1,将上述溶液于60℃水浴搅拌6h。抽滤洗涤至pH=7,将所得固体于100℃干燥、研磨并过80目筛子,所得样品为2GO-LDH-Stearate。通过浸渍法将草酸铌(C10H5NbO20)负载于2GO-LDH-Stearate上。首先将(0.01g)C10H5NbO20溶解于2ml乙醇中,接着加入2g上述2GO-LDH-Stearate,将上述悬浮液搅拌2h,将其转移至60℃条件下真空烘干。获得的样品被称为0.5Nb/2GO-LDH-Stearate,0.5是复合材料中C10H5NbO20负载量的质量百分比。在进行CO2吸附之前,将上述的吸附剂进行煅烧活化。取适量的样品于管式炉中,在300℃和50mL/min氮气气氛下煅烧2h。所得的样品被称为0.5Nb/2GO-LDO-Stearate。
(2)将吸附剂(10mg)放置于热重仪器中,通入CO2(浓度为15vol.%)和N2(浓度为85vol.%)的混合气,反应温度为200℃,对混合气体进行吸附,通过质量变化检测吸附剂对CO2的附量。在上述条件下本吸附剂具有较高的吸附容量。
实施例2
(1)将40mg的GO溶解于100ml去离子水中,室温下搅拌0.5h,并将上述混合液于超声处理4h,得到分散均匀的GO。加入一定量的Mg(NO3)2·6H2O和Al(NO3)3·9H2O,保持[Mg2+]/[Al3+](摩尔比)=2,将0.1mol的硬脂酸混合于上述120ml混合液中,[硬脂酸]/[Mg2+](摩尔比)=2,将2mol/L的NaOH溶液,以1mL/min的速度滴加到上述溶液中调节pH,通过pH仪将溶液的pH维持在10±0.1,将上述溶液于60℃水浴搅拌8h。抽滤洗涤至pH=7,将所得固体于100℃干燥、研磨并过80目筛子,所得样品为4GO-LDH-Stearate。通过浸渍法将草酸铌(C10H5NbO20)负载于4GO-LDH-Stearate上。首先将(0.02g)C10H5NbO20溶解于4ml乙醇中,接着加入2g上述4GO-LDH-Stearate,将上述悬浮液搅拌5h,将其转移至60℃条件下真空烘干。获得的样品被称为1Nb/4GO-LDH-Stearate,1是复合材料中C10H5NbO20负载量的质量百分比。在进行CO2吸附之前,将上述的吸附剂进行煅烧活化。取适量的样品于管式炉中,在300℃和50mL/min氮气气氛下煅烧6h。所得的样品被称为1Nb/4GO-LDO-Stearate。
(2)将一定量的吸附剂放置于热重仪器中,通入CO2(浓度为15vol.%)和N2(浓度为85vol.%)的混合气,反应温度为200℃,对混合气体进行吸附,通过质量变化检测吸附剂对CO2的附量。在上述条件下本吸附剂具有较高的吸附容量。
实施例3
(1)将60mg的GO溶解于100ml去离子水中,室温下搅拌0.5h,并将上述混合液于超声处理5h,得到分散均匀的GO。加入一定量的Mg(NO3)2·6H2O和Al(NO3)3·9H2O,保持[Mg2+]/[Al3+](摩尔比)=3,将0.15mol的硬脂酸混合于上述120ml混合液中,[硬脂酸]/[Mg2+](摩尔比)=2,将3mol/L的NaOH溶液,以1mL/min的速度滴加到上述溶液中调节pH,通过pH仪将溶液的pH维持在10±0.1,将上述溶液于80℃水浴搅拌10h。抽滤洗涤至pH=7,将所得固体于120℃干燥、研磨并过80目筛子,所得样品为6GO/LDH-Stearate。通过浸渍法将草酸铌(C10H5NbO20)负载于6GO-LDH-Stearate上。首先将(0.03g)C10H5NbO20溶解于5ml乙醇中,接着加入2g上述6GO-LDH-Stearate,将上述悬浮液搅拌5h,将其转移至60℃条件下真空烘干。获得的样品被称为1.5Nb/6GO-LDH-Stearate,1.5是复合材料中C10H5NbO20负载量的质量百分比。在进行CO2吸附之前,将上述的吸附剂进行煅烧活化。取适量的样品于管式炉中,在400℃和50mL/min氮气气氛下煅烧6h。所得的样品被称为1.5Nb/6GO-LDO-Stearate。
(2)将一定量的吸附剂放置于热重仪器中,通入CO2(浓度为15vol.%)和N2(浓度为85vol.%)的混合气,反应温度为200℃,对混合气体进行吸附,通过质量变化检测吸附剂对CO2的附量。在上述条件下本吸附剂具有较高的吸附容量。
实施例4
(1)将80mg的GO溶解于100ml去离子水中,室温下搅拌0.5h,并将上述混合液于超声处理6h,得到分散均匀的GO。加入一定量的Mg(NO3)2·6H2O和Al(NO3)3·9H2O,保持[Mg2+]/[Al3+](摩尔比)=3,将0.2mol的硬脂酸混合于上述120ml混合液中,[硬脂酸]/[Mg2+](摩尔比)=2,将4mol/L的NaOH溶液,以1mL/min的速度滴加到上述溶液中调节pH,通过pH仪将溶液的pH维持在10±0.1,将上述溶液于80℃水浴搅拌12h。抽滤洗涤至pH=7,将所得固体于120℃干燥、研磨并过80目筛子,所得样品为8GO-LDH-Stearate。通过浸渍法将草酸铌(C10H5NbO20)负载于8GO-LDH-Stearate上。首先将(0.04g)C10H5NbO20溶解于5ml乙醇中,接着加入2g上述8GO-LDH-Stearate,将上述悬浮液搅拌8h,将其转移至60℃条件下真空烘干。获得的样品被称为2Nb/8GO-LDH-Stearate,5是复合材料中C10H5NbO20负载量的质量百分比。在进行CO2吸附之前,将上述的吸附剂进行煅烧活化。取适量的样品于管式炉中,在400℃和50mL/min氮气气氛下煅烧6h。所得的样品被称为2Nb/8GO-LDO-Stearate。
(2)将一定量的吸附剂放置于热重仪器中,通入CO2(浓度为15vol.%)和N2(浓度为85vol.%)的混合气,反应温度为300℃,对混合气体进行吸附,通过质量变化检测吸附剂对CO2的附量。在上述条件下本吸附剂具有较高的吸附容量。
Claims (2)
1.铌改性有机层状双氧化物/氧化石墨烯纳米复合材料作为CO2吸附剂的制备方法,其特征在于,包括以下步骤:
将10~100 mg的GO分别溶解于100 ml去离子水中,室温下搅拌0.5 h,并将混合液于超声处理3~6 h,得到分散均匀的GO悬浮液;将Mg(NO3)2•6H2O和Al(NO3)3•9H2O固体加入50~200mL上述悬浮液中形成混合液,其中[Mg2+]/[Al3+]的摩尔比= 2~ 3;将0.05~0.2 mol的硬脂酸加入上述混合液中,其中[硬脂酸]/[Mg2+]的摩尔比=2~4;将1.2~4 mol/L的NaOH溶液,以1~10 mL/min的速度滴加到上述溶液中调节pH,通过pH仪将溶液的pH维持在10±0.1,将上述溶液于60~80℃水浴搅拌6~12 h;抽滤洗涤至pH = 7,将所得固体于100~120℃干燥、研磨并过80 目筛子,所得样品称为xGO-LDH-Stearate,其中x为复合材料中GO含量的质量比;通过浸渍法将草酸铌C10H5NbO20负载于xGO-LDH-Stearate上:首先将0.01~0.1 g C10H5NbO20溶解于2~10 ml乙醇中,再将上述1~5 g xGO-LDH-Stearate加入其中,形成悬浮液,其中[xGO-LDH-Stearate]/[C10H5NbO20]的质量比=50~200;将上述悬浮液搅拌2~10 h,转移至60℃条件下真空烘干;获得的样品被称为yNb/xGO-LDH-Stearate,y是复合材料中C10H5NbO20负载量的质量百分比;在进行CO2吸附之前,将yNb/xGO-LDH-Stearate进行煅烧活化;于管式炉中,在300~500℃和50 mL/min氮气气氛下煅烧2~6 h。
2.如权利要求1所述制备方法所制备的吸附剂在高温CO2吸附中的应用,其特征在于:将吸附剂放置于热重仪器中,通入浓度为5 vol.% ~ 25 vol.%的CO2和浓度为75 vol.% ~ 95vol.%的N2的混合气,对其进行吸附,通过质量变化检测吸附剂对CO2的吸附量,反应温度为200℃ ~ 300℃。
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