CN108273488A - 一种纳米片状二氧化铈/多孔炭复合材料的制备方法 - Google Patents
一种纳米片状二氧化铈/多孔炭复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米片状二氧化铈/多孔炭复合材料的制备方法,属于纳米材料和多相催化材料制备领域。该方法采用腐植酸、硝酸铈为原料,二甲基甲酰胺(DMF)溶液为溶剂,以氢氧化钠为还原剂,利用简单的溶剂热反应,通过改变反应的温度和时间可以明显调节负载在活性炭表面二氧化铈纳米粒子的分布和形貌。本发明操作简单,原料价廉易得,所制备的纳米片状二氧化铈能在高温下显示出优异分散性负载在多孔炭上。该纳米片状二氧化铈/多孔炭复合材料在水处理、热催化、电化学领域具有极大的应用潜力。
Description
技术领域
本发明属于纳米材料和多相催化材料制备领域,具体涉及一种片状二氧化铈/多孔炭复合材料的制备方法。
背景技术
二氧化铈作为重要的稀土金属氧化物之一,良好的氧化还原性以及环境友好性使得其在气体净化、催化剂、荧光材料、储氢材料等诸多领域中得到广泛的应用。当前研究发现,不同形貌的纳米二氧化铈,如纳米棒、纳米线、纳米片、纳米粒子等,由于独特的纳米效应则显示出更为优异的催化性能[(a)C.Pan,D.Zhang,L.Shi,J.Fang,Eur.J.Inorg.Chem.,2008,15:2429-2436.(b)KS.Lin,S.Chowdhury,Int.J.Mol.Sci.,2010,11(9):3226-3251.(c)K.Sudarshan,SK.Sharma,R.Gupta,SK.Gupta,FN.Sayed,PK.Pujari,Mater.Chem.Phys.,2017,200:99-106]。而单纯的纳米金属氧化物非常容易聚集从而降低其催化活性表面积,影响其催化活性,因此需要引入较大比表面的载体,实现纳米粒子的高分散,同时也可以减少纳米金属氧化物活性组分的用量,节约催化剂成本。
腐植酸作为高分子羟基羧酸组成的复杂混合物,其制备方法简单,材料价格低廉。结构中大量活性官能团的存在,如羟基、羧基、羰基、氨基等,使得其具有酸性、亲水性、界面活性、阳离子交换能力、络合能力及吸附分散能力。多芳香环层状结构和丰富的官能团本身可以为金属纳米粒子的负载提供大量活性位,使得腐植酸极易与无机金属粒子结合。并且,由于其具有非均相的多孔结构,拥有和活性炭相同数量级的空隙大小和较大的比表面积(330~340m2/g),一些研究中利用腐植酸的吸附特性,以其直接为催化剂和固体吸附剂来进行烟气的处理。同时,研究还发现通过进一步改性以及碳化处理可以将腐植酸转变为具有纳米片构成的三维交联结构多孔炭,可以看做纳米片状的多层类石墨烯结构以及多孔结构的结合,这种独特的结构使得其可以提供更高的比表面积和多级的孔径分布[(d)RF.Zhao,HD.Liu,SF.Ye,YS.Xie,Y.Chen,Ind.Eng.Chem.Res.,2006,45:7120-7125.(e).W.Shi,H.Fan,S.Ai,L.Zhu,RSC.Adv.,2015,5:32183-32190.(f)Z.Qiao,M.Chen,C.Wang,Y.Yuan,Bioresource.Technol.,2014,163:386-389.]。因此,以腐植酸基多孔炭为载体,可以进一步改善催化剂活性组分的分散性,提供更多的活性比表面积。所以,选择一种合适方法来制备具有高性能、独特纳米结构的二氧化铈/多孔炭复合材料,在热催化领域具有很大的应用潜力。
发明内容
针对产业化需求和上述技术难题,本发明的目的是提供一种高分散纳米片状二氧化铈/活性炭复合材料的简便制备方法,以期达到降低投资和运行成本,制备出的纳米片状二氧化铈能在高温下显示出优异分散性负载在多孔炭上。
本发明从实用的角度出发设计方案,采用腐植酸、硝酸铈为原料二甲基甲酰胺(DMF)溶液为溶剂,以氢氧化钠为还原剂,通过简单溶剂热法制备高分散纳米片状二氧化铈/多孔炭复合材料,具体步骤如下:
(1)将腐植酸和硝酸铈溶解于水和DMF形成的混合溶液中,室温下混合均匀;所述硝酸铈与腐植酸的质量比为4~5:1。
(2)将步骤(1)的混合溶液倒入反应器,置于水浴,搅拌回流,在升温条件下将氢氧化钠缓慢加入,反应0.2~2小时;水浴反应温度控制在10~70℃;所述氢氧化钠与腐植酸的质量比为1~20:1;
(3)将步骤(2)反应后的产物移入水热反应釜中升温至80~180℃,反应8~30小时,将所得沉淀物洗涤、干燥、煅烧得到纳米片状二氧化铈/多孔炭复合材料。
进一步的,所述水和DMF形成的混合溶液中,DMF:H2O=1:1(体积比)。
与现有技术相比,本发明具有以下技术效果:
1、利用腐植酸为载体,通过简单的溶剂热合成法可制备出具有独特纳米结构的片状二氧化铈/多孔炭复合材料;通过改变反应的温度和时间可以明显调节负载在活性炭表面二氧化铈纳米粒子的分布和形貌。
2、所制备的纳米片状二氧化铈能在高温下显示出优异分散性负载在多孔炭上,在水处理、热催化、电化学领域具有极大的应用潜力。
附图说明
图1为本发明实施例3所得产物的扫描电镜图;
由图可见:大小为80~450纳米的片状二氧化铈均匀负载在多孔炭载体表面,形成纳米片状二氧化铈/多孔炭复合材料。
图2为所得产物的XRD图(其中:a为本发明实施例3所得产物的XRD图;b为标准的CeO2XRD衍射图);
由图可见:图2a显示出相对应的CeO2XRD特征衍射峰,表示多孔炭载体上CeO2的存在。
具体实施方式
下面给出本发明的几个具体实施例,以对本发明进行更加详细的说明。所得到的产物的形貌通过透射电镜(SEM)观察,其物相组分通过X射线粉末衍射(XRD)鉴定。
实施例1
取0.434g硝酸铈加入到80ml DMF和水混合溶剂(DMF:H2O=1:1)中,超声分散0.5小时形成混合溶液1,将混合溶液1倒入250ml三颈烧瓶中搅拌,水浴回流。水浴温度升至50℃时缓慢加入0.4g NaOH,继续升温至70℃保持1小时,然后将混合溶液分为两份移至两个100ml水热釜中,升温至140℃,维持140℃下反应24h后,将所得沉淀物用蒸馏水洗涤,于60℃干燥24h,得到二氧化铈纳米材料。
实施例2
取100mg腐植酸和0.434g硝酸铈加入到80ml DMF和水混合溶剂(DMF:H2O=1:1)中,超声分散0.5小时形成混合溶液1,将混合溶液1倒入250ml三颈烧瓶中搅拌,水浴回流。水浴温度升至50℃时缓慢加入0.4g NaOH,继续升温至70℃保持1小时,然后将混合溶液分为两份移至两个100ml水热釜中,升温至140℃,维持140℃下反应24h后,将所得沉淀物用蒸馏水洗涤,于60℃干燥24h,然后在氩气气氛下,600℃煅烧2h后得到二氧化铈/多孔炭复合材料。
实施例3
取100mg腐植酸和0.434g硝酸铈加入到80ml DMF和水混合溶剂(DMF:H2O=1:1)中,超声分散0.5小时形成混合溶液1,将混合溶液1倒入250ml三颈烧瓶中搅拌,水浴回流。水浴温度升至50℃时缓慢加入0.4g NaOH,继续升温至70℃保持1小时,然后将混合溶液分为两份移至两个100ml水热釜中,升温至160℃,维持160℃下反应24h后,将所得沉淀物用蒸馏水洗涤,于60℃干燥24h,然后在氩气气氛下,600℃煅烧2h后得到二氧化铈/多孔炭复合材料。
实施例4
取100mg腐植酸和0.434g硝酸铈加入到80ml DMF和水混合溶剂(DMF:H2O=1:1)中,超声分散0.5小时形成混合溶液1,将混合溶液1倒入250ml三颈烧瓶中搅拌,水浴回流。水浴温度升至50℃时缓慢加入0.4g NaOH,继续升温至70℃保持1小时,然后将混合溶液分为两份移至两个100ml水热釜中,升温至180℃,维持180℃下反应24h后,将所得沉淀物用蒸馏水洗涤,于60℃干燥24h,然后在氩气气氛下,600℃煅烧2h后得到二氧化铈/多孔炭复合材料。
实施例5
取100mg腐植酸和0.434g硝酸铈加入到80ml DMF和水混合溶剂(DMF:H2O=1:1)中,超声分散0.5小时形成混合溶液1,将混合溶液1倒入250ml三颈烧瓶中搅拌,水浴回流。水浴温度升至50℃时缓慢加入0.4g NaOH,继续升温至70℃保持1小时,然后将混合溶液分为两份移至两个100ml水热釜中,升温至160℃,维持160℃下反应10h后,将所得沉淀物用蒸馏水洗涤,于60℃干燥24h,然后在氩气气氛下,600℃煅烧2h后得到二氧化铈/多孔炭复合材料。
Claims (2)
1.一种纳米片状二氧化铈/多孔炭复合材料的制备方法,其特征在于包括如下步骤:
(1)将腐植酸和硝酸铈溶解于水和DMF形成的混合溶液中,室温下混合均匀;
所述硝酸铈与腐植酸的质量比为4~5:1;
(2)将步骤(1)的混合溶液倒入反应器,置于水浴,搅拌回流,在升温条件下将氢氧化钠缓慢加入,反应0.5小时;水浴反应温度控制在50℃;
所述氢氧化钠与腐植酸的质量比为4:1;
(3)将步骤(2)反应后的产物移入水热反应釜中升温至140~180℃,反应10~30小时,将所得沉淀物洗涤、干燥、煅烧得到纳米片状二氧化铈/多孔炭复合材料。
2.如权利要求1所述的纳米片状二氧化铈/多孔炭复合材料的制备方法,其特征在于,所述水和DMF形成的混合溶液中,DMF与水的体积比为1:1。
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