CN107774260A - 可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法 - Google Patents
可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法,属于光催化材料制备领域。本发明方法采用二次溶剂热工艺:首先,凹凸棒粘土为载体、Fe(NO3)3·9H2O为铁源,二乙二醇为溶剂,恒温反应数小时,磁性分离,乙醇洗涤,干燥,得到可磁分离的Fe3O4/凹凸棒粘土复合材料;然后以Fe3O4/凹凸棒粘土复合材料为载体,氟钛酸铵为钛源,去离子水为溶剂,加入适量尿素,恒温反应数小时,磁性分离,水洗,干燥,得到可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料。本发明无需高温煅烧,具有操作简便、安全性高以及环境无污染等优点。所制备的吸附光催化材料比表面积大,分散性好,在磁场作用下易于分离,解决纳米光催化材料回收困难问题。
Description
技术领域
本发明属于光催化材料制备领域,涉及一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法。
背景技术
在人类面临的众多环境问题中,污水中生物难降解的有机污染物的处理是一个难题。此类污染物由于难以用生物方法去除,而排放到环境中会对环境产生很大的危害作用,所以人们一直寻求新的方法来处理这个问题。高级氧化技术是基于在反应过程中形成具有强氧化能力的自由基尤其是羟基自由基对污染物进行分解,由于自由基的氧化能力非常强,可以将各种有机物无选择性氧化分解,所以高级氧化技术特别适合于处理含有难降解有机物的废水。
作为高级氧化技术的一种,光催化方法是利用能量大于或等于半导体禁带宽度的光源照射半导体,致使价带上的电子跃迁到导带,在价带上产生空穴(h+),导带上产生电子(e-),其中空穴可以与吸附在颗粒表面的羟基(OH-)和水分子(H2O)反应成·OH,·OH可以氧化有机物将其降解为CO2和H2O等无机小分子。在诸多可作为光催化剂的半导体材料中,TiO2(锐钛矿型)以其带隙能适中、对污染物的吸附能力强、光催化活性高,且无毒、稳定、价廉,兼有自洁、除臭、灭菌等独特的优点而得到广泛的研究和应用,成为具有应用前景的绿色环保型催化剂之一。
单纯的TiO2光催化方法在有机废水的处理应用中虽然达到了一定的效果,但由于TiO2在水溶液中易团聚失活,且难以回收和循环利用等弊端使其应用受到严重限制。因此,制备比表面积大,分散性好,易回收,可循环使用的TiO2光催化剂成为目前光催化领域的一个热点。
大量研究表明,将TiO2负载到具有磁性的吸附性载体上是行之有效的方法:一方面,作为载体的吸附剂通过吸附和表面富集,在TiO2周围形成浓度较高的污染物氛围,为TiO2提供了高浓度有机污染物的光催化反应环境,增加了TiO2与污染物的碰撞几率,有助于提高污染物光催化降解反应的速度;另一方面,通过外磁场作用使光催化剂从体系中快速富集回收,实现循环利用。
发明内容
发明目的:针对现有技术所存在的问题和不足,本发明旨在提供一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法。该方法具有操作简便,安全性较高,对环境无污染等优点,制备的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料比表面积大、分散性好、在磁场作用下易于分离,解决纳米光催化材料回收困难问题,为基于TiO2的复合光催化材料开辟了新的发展前景。
技术方案:一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法,包括以下步骤:
1)制备酸改性凹凸棒粘土
取2g凹凸棒粘土加入到50mL浓度为1~5mol/L的盐酸溶液中,在80~110℃油浴中,以转速300~700r/min搅拌回流2~6h;离心水洗至pH为中性,所得固体在105℃下鼓风干燥,研磨过200目筛,备用;
2)制备Fe3O4/凹凸棒粘土复合材料
取0.79g Fe(NO3)3·9H2O溶于到65mL二乙二醇中,然后加入0.5g上述Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浊液转移至100mL内衬为聚四氟乙烯的高压反应釜中,密封后置于180~240℃的电热鼓风干燥箱中陈化12~24h,自然冷却至室温,用磁铁收集固体产物,用乙醇洗涤5-6次后,于60℃下干燥8~12h即得Fe3O4/凹凸棒粘土复合材料;
3)制备TiO2/Fe3O4/凹凸棒粘土吸附光催化材料
取0.97g尿素溶于65mL蒸馏水中,然后加入0.13~0.39g氟钛酸铵,搅拌溶解,继而加入0.5g上述制备Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浮液转移至100mL高压反应釜中,密封后置于120~180℃鼓风干燥箱中陈化24~72h,自然冷却至室温,用磁铁收集固体产物,用蒸馏水和乙醇交替洗涤,于60℃下干燥8~12h即得TiO2/Fe3O4/凹凸棒粘土吸附光催化材料。
有益效果:本发明和现有的技术相比,成功地合成了可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料,该制备方法具有操作简便、安全性高以及环境无污染等优点,所制备的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料比表面积大、分散性好、在磁场作用下易于分离,解决纳米光催化材料回收困难问题,为基于TiO2的复合光催化材料开辟了新的发展前景。
附图说明
图1为酸改性凹凸棒粘土(a),Fe3O4/凹凸棒粘土复合材料(b),TiO2/Fe3O4/凹凸棒粘土磁性光催化剂(c)的X衍射(XRD)图。
图2为TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的吸附等温曲线图和孔径分布图(插图)。
图3为TiO2/Fe3O4/凹凸棒粘土磁性光催化剂的场发射扫描电镜(FESEM)照片。
图4为Fe3O4/凹凸棒粘土复合材料(a),TiO2/Fe3O4/凹凸棒粘土磁性光催化剂(b)的振动样品磁强计(VSM)图。
具体实施方式
下面结合具体实施例对本发明进行详细阐述。
具体实施例1:
一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法,包括以下步骤:
1)制备酸改性凹凸棒粘土
取2g凹凸棒粘土加入到50mL浓度为1~5mol/L的盐酸溶液中,在80~110℃油浴中,以转速300~700r/min搅拌回流2~6h;离心水洗至pH为中性,所得固体在105℃下鼓风干燥,研磨过200目筛,备用;
2)制备Fe3O4/凹凸棒粘土复合材料
取0.79g Fe(NO3)3·9H2O溶于到65mL二乙二醇中,然后加入0.5g上述Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浊液转移至100mL内衬为聚四氟乙烯的高压反应釜中,密封后置于180~240℃的电热鼓风干燥箱中陈化12~24h,自然冷却至室温,用磁铁收集固体产物,用乙醇洗涤5-6次后,于60℃下干燥8~12h即得Fe3O4/凹凸棒粘土复合材料;
3)制备TiO2/Fe3O4/凹凸棒粘土吸附光催化材料
取0.97g尿素溶于65mL蒸馏水中,然后加入0.13g氟钛酸铵,搅拌溶解,继而加入0.5g上述制备Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浮液转移至100mL高压反应釜中,密封后置于120~180℃鼓风干燥箱中陈化24~72h,自然冷却至室温,用磁铁收集固体产物,用蒸馏水和乙醇交替洗涤,于60℃下干燥8~12h即得TiO2/Fe3O4/凹凸棒粘土吸附光催化材料。
具体实施例2:
一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法,包括以下步骤:
1)制备酸改性凹凸棒粘土
取2g凹凸棒粘土加入到50mL浓度为1~5mol/L的盐酸溶液中,在80~110℃油浴中,以转速300~700r/min搅拌回流2~6h;离心水洗至pH为中性,所得固体在105℃下鼓风干燥,研磨过200目筛,备用;
2)制备Fe3O4/凹凸棒粘土复合材料
取0.79g Fe(NO3)3·9H2O溶于到65mL二乙二醇中,然后加入0.5g上述Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浊液转移至100mL内衬为聚四氟乙烯的高压反应釜中,密封后置于180~240℃的电热鼓风干燥箱中陈化12~24h,自然冷却至室温,用磁铁收集固体产物,用乙醇洗涤5-6次后,于60℃下干燥8~12h即得Fe3O4/凹凸棒粘土复合材料;
3)制备TiO2/Fe3O4/凹凸棒粘土吸附光催化材料
取0.97g尿素溶于65mL蒸馏水中,然后加入0.26g氟钛酸铵,搅拌溶解,继而加入0.5g上述制备Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浮液转移至100mL高压反应釜中,密封后置于120~180℃鼓风干燥箱中陈化24~72h,自然冷却至室温,用磁铁收集固体产物,用蒸馏水和乙醇交替洗涤,于60℃下干燥8~12h即得TiO2/Fe3O4/凹凸棒粘土吸附光催化材料。
具体实施例3:
一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法,包括以下步骤:
1)制备酸改性凹凸棒粘土
取2g凹凸棒粘土加入到50mL浓度为1~5mol/L的盐酸溶液中,在80~110℃油浴中,以转速300~700r/min搅拌回流2~6h;离心水洗至pH为中性,所得固体在105℃下鼓风干燥,研磨过200目筛,备用;
2)制备Fe3O4/凹凸棒粘土复合材料
取0.79g Fe(NO3)3·9H2O溶于到65mL二乙二醇中,然后加入0.5g上述Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浊液转移至100mL内衬为聚四氟乙烯的高压反应釜中,密封后置于180~240℃的电热鼓风干燥箱中陈化12~24h,自然冷却至室温,用磁铁收集固体产物,用乙醇洗涤5-6次后,于60℃下干燥8~12h即得Fe3O4/凹凸棒粘土复合材料;
3)制备TiO2/Fe3O4/凹凸棒粘土吸附光催化材料
取0.97g尿素溶于65mL蒸馏水中,然后加入0.39g氟钛酸铵,搅拌溶解,继而加入0.5g上述制备Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浮液转移至100mL高压反应釜中,密封后置于120~180℃鼓风干燥箱中陈化24~72h,自然冷却至室温,用磁铁收集固体产物,用蒸馏水和乙醇交替洗涤,于60℃下干燥8~12h即得TiO2/Fe3O4/凹凸棒粘土吸附光催化材料。
实验结果
实施例2制备出的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的X射线衍射测试结果如图1中谱线c所示。谱线c中既有TiO2的衍射峰,且峰型尖锐、强度大,也有Fe3O4的衍射峰,一方面说明样品中作为主要有效活性组分的TiO2晶型形成较好,另一方面说明在制备TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的过程中没有改变Fe3O4的结构,同时也说明该发明方法成功制备了TiO2/Fe3O4/凹凸棒粘土吸附光催化材料。
实施例2制备出的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的吸附等温曲线如图2所示。TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的氮气吸附和脱附等温线属于IV型吸附特性和H3型回滞环。回滞环都在中等的相对压力时开始出现,说明TiO2/Fe3O4/凹凸棒粘土吸附光催化材料存在一定量的介孔,且大多是由集聚颗粒构成的不规则的狭缝孔。在相对压力接近1的区域,等温线都有最后的上升的拖尾,结合图2插图孔径分布曲线可知,TiO2/Fe3O4/凹凸棒粘土吸附光催化材料孔径分布较广,具有介孔和大孔孔径。基于BJH方法对脱附曲线的分析,TiO2/Fe3O4/凹凸棒粘土吸附光催化材料孔径为15.89nm,孔体积为0.55cm3/g。基于BET的分析方法,TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的比表面积为130.87m2/g。
实施例2制备出的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的场发射扫描电镜照片如图3所示,TiO2纳米粒子均匀负载于棒状的磁性凹凸棒粘土表面,有效解决TiO2在水溶液中易团聚失活问题。
实施例2制备出的TiO2/Fe3O4/凹凸棒粘土可磁分离光催化剂的磁性参数测试结果如图4中曲线b所示,其饱和磁化强度为14.40emu/g,说明该复合物在室温下呈现超顺磁性。降解后的悬浮液中,催化剂被牢牢吸附在磁铁上,说明磁性能良好,易于回收再利用。
Claims (1)
1.一种可磁分离的TiO2/Fe3O4/凹凸棒粘土吸附光催化材料的制备方法,其特征在于,该方法包括以下步骤:
1)制备酸改性凹凸棒粘土
取2g凹凸棒粘土加入到50mL浓度为1~5mol/L的盐酸溶液中,在80~110℃油浴中,以转速300~700r/min搅拌回流2~6h;离心水洗至pH为中性,所得固体在105℃下鼓风干燥,研磨过200目筛,备用;
2)制备Fe3O4/凹凸棒粘土复合材料
取0.79g Fe(NO3)3·9H2O溶于到65mL二乙二醇中,然后加入0.5g上述Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浊液转移至100mL内衬为聚四氟乙烯的高压反应釜中,密封后置于180~240℃的电热鼓风干燥箱中陈化12~24h,自然冷却至室温,用磁铁收集固体产物,用乙醇洗涤5-6次后,于60℃下干燥8~12h即得Fe3O4/凹凸棒粘土复合材料;
3)制备TiO2/Fe3O4/凹凸棒粘土吸附光催化材料
取0.97g尿素溶于65mL蒸馏水中,然后加入0.13~0.39g氟钛酸铵,搅拌溶解,继而加入0.5g上述制备Fe3O4/凹凸棒粘土复合材料,超声波处理15~60min,分散均匀,将上述悬浮液转移至100mL高压反应釜中,密封后置于120~180℃鼓风干燥箱中陈化24~72h,自然冷却至室温,用磁铁收集固体产物,用蒸馏水和乙醇交替洗涤,于60℃下干燥8~12h即得TiO2/Fe3O4/凹凸棒粘土吸附光催化材料。
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