CN106040251A - 一种溶胶‑凝胶一步法低温合成纯相Bi25FeO40/ZnO光催化剂的制备方法 - Google Patents
一种溶胶‑凝胶一步法低温合成纯相Bi25FeO40/ZnO光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种溶胶‑凝胶一步法低温合成纯相Bi25FeO40/ZnO光催化剂的制备方法，并将该催化剂用于在模拟太阳光下低浓度苯酚水溶液的降解反应。该催化剂利用溶胶‑凝胶法制备，以甘氨酸为络合剂，将Fe(NO3)3·9H2O、Bi(NO3)3·5H2O和Zn(NO3)2·6H2O反应络合，在空气气氛下500℃焙烧3h，形成半导体催化剂。各原料的物质的量之比为Fe∶Bi∶Zn＝1∶1∶4，络合剂甘氨酸与总金属离子的摩尔比为1∶2。本发明的特点是采用以甘氨酸为络合剂的溶胶‑凝胶一步法制备，并在较低的温度下合成了纯相Bi25FeO40/ZnO光催化剂。该制备方法操作简便，成本低廉，用于低浓度苯酚水溶液降解具有较高的催化活性和较好的结构稳定性。
Description
技术领域
本发明涉及一种溶胶-凝胶一步法低温合成纯相Bi25FeO40/ZnO光催化剂的制备方法，属无机非金属材料及半导体光催化材料的制备工艺技术领域，并将其应用于在模拟太阳光下降解低浓度有机污染物——苯酚的降解。
背景技术
在大多数煤化工产品的生产中，如煤炭气化、液化、焦化以及焦油加工等过程中均会产生大量含酚废水，苯酚及酚类化合物废水由于具有生物致畸、致癌的高毒性和强刺激性，被列为优先处理的污染物之一，但是苯酚本身非常难降解。对于苯酚及含酚类废水的处理，传统方法包括萃取法、膜分离法、生物处理、化学氧化或电化学催化氧化或多或少有一些缺点：能耗大，不完全降解，低矿化，或造成二次污染的可能性很高。而新兴的光催化氧化技术以其强氧化能力、高选择性、快速反应、反应条件温和、能耗低、能矿化绝大多数有机物及可以利用太阳光作为反应光源等突出优势在降解有机物、水体微污染处理中具有其他传统水处理工艺所无法比拟的优势，近年来在难降解污染物的处理方面得到了广泛的研究，在工业废水的处理及生活污水的深度治理和新能源的开发利用等方面展示了广阔的应用前景。
光催化氧化反应以半导体为催化剂，传统的半导体光催化剂有ZnS、TiO2、ZnO、CdS、SnO2和Fe3O4等，但是ZnS、ZnO、SnO2、CdS和Fe3O4等的光腐蚀现象时常发生，严重降低了催化活性，而TiO2半导体光催化氧化技术引起具有效率高、能耗低、操作简便、反应条件温和、适用范围广、可减少二次污染等突出优点，而TiO2催化剂本身无毒、廉价、高效、性能稳定而成为科研工作者的研究热点。但TiO2只能吸收波长小于387nm的紫外光(小于4％)，在可见光照射下没有光催化活性，而人造紫外光源又有耗电大、设备昂贵、稳定性差等缺陷，因此在对TiO2光催化剂改性的同时，研制新的光催化剂使得它能够吸收太阳光中大部分的可见光，利用空气中的氧作为氧化剂，有效地降解有毒污染物成为光催化领域关键的科学难题。
在现有研究中，尚未有关于Bi25FeO40/ZnO光催化剂的报道，而对于Bi25FeO40的合成，大多数是采用水热法合成，水热法时间比较长，制备样品重复性差，且受水热条件的影响很难制得纯相的催化剂成品。目前，以甘氨酸为络合剂，采用溶胶-凝胶一步法制备纯相Bi25FeO40/ZnO光催化剂，该法操作简单，容易放大，制备样品重复性好，且用于光催化降解苯酚的研究尚未见报道。故本专利提供一种纯相Bi25FeO40/ZnO光催化剂的较低温度的制备方法，用于光催化降解低浓度苯酚的反应，并能够促进苯酚溶液降解，提高苯酚降解率。
发明内容
本发明要解决的技术问题是提供一种溶胶-凝胶一步法低温合成纯相Bi25FeO40/ZnO光催化剂的制备方法，该催化剂利用溶胶-凝胶一步法制备，以甘氨酸为络合剂，将含有Bi、Fe和Zn离子的原溶液在一定温度下反应络合，形成半导体催化剂，并将该催化剂应用于模拟太阳光下降解低浓度苯酚废水的反应，使得低浓度苯酚在模拟太阳光下实现完全降解。
本发明涉及一种光催化降解苯酚的光催化剂Bi25FeO40/ZnO的制备方法，属无机非金属材料及半导体光催化材料的制备工艺技术领域。本发明主要采用Fe(NO3)3·9H2O、Bi(NO3)3·5H2O、Zn(NO3)2·6H2O为原料，按照物质的量之比为Fe∶Bi∶Zn＝1∶1∶4准确称取各药品，置于烧杯中，加入去离子水，在70℃水浴下搅拌使其完全溶解，再加入为金属离子总量的1/2倍物质的量的甘氨酸，使其充分络合，保持70℃恒温水浴磁力搅拌，蒸发得到粘稠状胶体。将所得胶体在烘箱内100℃空气气氛下干燥12h得干凝胶，然后在马弗炉中500℃焙烧3h，制得样品。
本发明的催化剂在模拟太阳光下降解低浓度苯酚有较好的催化效果。具体实验操作采用自组装光化学反应器考察催化剂的可见光光催化活性(CEL-LAX500，BeijingAuLightLtd.Co.)其中，可见光光源改用金属卤化物灯(300W，主波长420-630nm，光通量7500lm)，光源距离石英管10cm。基本的反应条件为：在室温条件下，以苯酚水溶液(20mg/L)为目标降解物考察其在可见光下的降解，催化剂用量为1g/L，电磁剧烈搅拌，且光照反应过程中容器底部鼓入一定量的空气(240mL/min)。实验时，称取30mg已制备好的光催化剂分散到包含30mL苯酚溶液(20mg/L)的石英管中，先将悬浮液在暗反应下搅拌30min，使苯酚和催化剂表面之间建立吸附-脱附平衡。然后用300W金属卤化物灯照射(加紫外滤波片)，每隔1小时定时取样(约3mL)，可见光总光照5h，反应结束后溶液离心分离15min(5000r/min)，然后用UV-7504PC型紫外-可见分光光度计测试其上清液在苯酚最大吸收波长(λmax＝270nm)处的吸光度。通过下式来计算苯酚的降解率，用(其中，η为光催化降解效率，C0为吸附-脱附平衡后苯酚水溶液的吸光度，Ct为光照过程中苯酚水溶液的吸光度)。另外，采用德国Bruker公司的D8ADVANCE型粉末X-射线衍射仪测试催化剂的物相组成，该仪器的工作参数如下：辐射源为CuKα(λ＝0.15406nm)，工作电压为36kV，电流为20mA，扫描范围10°～80°，扫描速度2°/min。
本发明所选用Bi、Fe、Zn物质的量之为1∶1∶4，采用的络合剂甘氨酸与总金属离子的摩尔比为1∶2。
本发明的优点是：采用溶胶-凝胶一步法，在较低温度下制备出了纯相的Bi25FeO40/ZnO光催化剂，其在可见光区有响应，作为光催化降解苯酚催化剂有着较好的催化活性和稳定性。且催化剂制备方法简单，条件温和，成本低廉。
本发明的实质性特征是：
1.采用甘氨酸为络合剂，通过溶胶-凝胶一步法制备出的Bi25FeO40/ZnO光催化剂中，无杂相产生。
2.采用甘氨酸为络合剂，通过溶胶-凝胶一步法制备出的催化剂为纯相Bi25FeO40/ZnO光催化剂，该催化剂用于在模拟太阳光下催化降解苯酚反应，在可见光下反应五小时后，苯酚降解率达到88.1％，COD去除率达到72.31％，说明低浓度苯酚在纯相Bi25FeO40/ZnO光催化剂催化下基本实现完全降解。
附图说明
图1是本发明中采用甘氨酸为络合剂，通过溶胶-凝胶一步法制备的纯相Bi25FeO40/ZnO催化剂的XRD图谱；图2是采用甘氨酸为络合剂，通过溶胶-凝胶一步法制备的Bi25FeO40/ZnO催化剂在模拟太阳光下催化降解苯酚活性测试图。
具体实施方式
现将本发明的具体实施例叙述于后。
实施例一：本实施例中的制备过程和步骤如下所述：
(1)准确称取2.0200g Fe(NO3)3·9H2O、2.4254g Bi(NO3)3·5H2O及5.9498g Zn(NO3)2·6H2O置于烧杯中，加入100mL去离子水，搅拌使其完全溶解。(2)再加入1.1261g甘氨酸，保持70℃恒温水浴磁力搅拌使其充分络合，蒸发得到粘稠状胶体。(3)将所得胶体在100℃普通烘箱内空气气氛下干燥12 h得干凝胶，然后在马弗炉中500℃焙烧3h，制得纯相Bi25FeO40/ZnO光催化剂样品。
制得的催化剂按照下面的方法进行催化活性的测试：
称取30mg已制备好的光催化剂分散到包含30mL苯酚溶液(20mg/L)的石英管中，先将悬浮液在暗反应下搅拌30min，使苯酚和催化剂表面之间建立吸附-脱附平衡。然后用300W金属卤化物灯照射(加紫外滤波片)，每隔1小时定时取样(约3mL)，可见光总光照5h，反应结束后溶液离心分离15min(5000r/min)，然后用UV-7504PC型紫外-可见分光光度计测试其上清液在苯酚最大吸收波长(λmax＝270nm)处的吸光度。
XRD及光催化性能测试结果
将本发明所制的Bi25FeO40/ZnO光催化剂样品进行表征和光催化性能测试。
1、XRD测试表征结构
测试结果如图1所示，图1为本发明所制的Bi25FeO40/ZnO光催化剂样品的XRD图。从图1中可以看出，所制得的Bi25FeO40/ZnO样品为纯相，没有杂相产生。
2、光催化性能测试表征模拟太阳光下降解苯酚的性能
测试结果见图2，图2为本发明所制的Bi25FeO40/ZnO光催化剂样品的光催化降解苯酚的曲线图。从图2可以看出，光催化反应5h后，Bi25FeO40/ZnO催化剂在在模拟太阳光下的降解效率为88.1％，而没有加催化剂的苯酚溶液在光照5h后几乎没有降解。
Claims (1)
1.一种光催化降解苯酚的Bi25FeO40/ZnO光催化剂的制备方法，该催化剂采用溶胶-凝胶一步法制备，其特征在于具有以下的过程和步骤：以甘氨酸为络合剂，甘氨酸与金属离子总量的摩尔比为1∶2，准确称取2.4254g Bi(NO3)3·5H2O、2.0200g Fe(NO3)3·9H2O和5.9498gZn(NO3)2·6H2O于烧杯中，同时向烧杯中加入100ml去离子水，磁力搅拌使其完全溶解，再加入1.1261g甘氨酸作为络合剂，然后将上述混合溶液在70℃恒温水浴磁力搅拌下蒸发得到粘稠状胶体，将所得到的胶体在100℃普通烘箱内空气气氛下干燥12h，制得干凝胶，然后在马弗炉中500℃焙烧3h，最终得到纯相的Bi25FeO40/ZnO催化剂样品，并将该催化剂应用于模拟太阳光下降解低浓度苯酚废水的反应。
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