CN108722482A - 一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法 - Google Patents
一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法。包括以下步骤:(1)将碳纳米管置于浓硝酸中加热回流处理6~12h,冷却后,用水洗涤至中性并干燥;(2)将聚苯胺和预处理后的碳纳米管加入到N,N‑二甲基甲酰胺(DMF)溶液中,超声处理2~5h;(3)将AgNO3溶液逐滴加入上述混合溶液中,避光搅拌6~20h;(4)将Na2HPO4·12H2O溶液逐滴加入步骤(3)得到的溶液中,避光搅拌1~6h,用水和乙醇洗涤数次,离心分离得到固体部分,真空干燥后制得掺杂碳纳米管和聚苯胺的磷酸银复合光催化剂。本发明制备工艺简单,制备的材料具备环保、经济、优异的可见光催化性能以及重复利用性高等优点。
Description
技术领域
本发明属于半导体材料光催化应用、环保技术领域,具体涉及用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法。
背景技术
近几十年来,光催化技术因其可直接利用太阳能降解有机污染物,成为环境修复中最有前途的技术之一。然而大多数半导体光催化剂在可见光区域的光催化活性仍不理想,这阻碍了光催化技术的进一步发展和应用。因此研究和开发高效可见光光催化剂是解决这一技术瓶颈的关键。在众多具有可见光活性的催化剂中,磷酸银(Ag3PO4)表现出优异的有机污染物降解能力。Ag3PO4独特的能带位置使其价带中的光生空穴具备强氧化能力,可以直接氧化和降解污染物。但是Ag3PO4的光腐蚀较为严重,这严重阻碍了它的推广应用。光腐蚀的根本原因是光生电子-空穴对的复合过程远快于捕获-转移的过程。使得Ag+被光生电子还原成银单质,滞留的光生空穴对Ag3PO4本身产生氧化,这使得Ag3PO4晶体被破坏,光催化活性降低,重复利用性变差。
本发明针对Ag3PO4光生电子-空穴对分离效率低的缺点,通过碳纳米管和聚苯胺的协同作用对磷酸银进行改性,进一步提高Ag3PO4的光催化活性和重复利用性。利用MWCNTs良好的光电性能,将其作为光生电子的捕获中心和导体,使光生电子沿其纵向迁移至催化剂表面,使其与氧气和水反应分别生成超氧自由基和羟基自由基,通过自由基氧化降解污染物。同时利用PANI的共轭π结构和独特的导电性,将其作为光生空穴的载体,将光生空穴通过其HOMO轨道迅速迁移至催化剂表面,直接氧化降解有机污染物。通过碳纳米管和聚苯胺各自的优异特性,达到光生电子-空穴快速分离的效果,从而提高催化剂的光催化活性和重复利用性。
发明内容
本发明提供一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,制备方法简单、易操作,制备得到的光催化材料抗光腐蚀性强,同时具有高效的可见光催化活性,可高效降解有机污染物。
一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,包括以下步骤:
步骤1)将碳纳米管置于浓硝酸中加热回流处理6~12h,冷却后,用水洗涤至中性并干燥;
步骤2)将聚苯胺和预处理后的碳纳米管加入到N,N-二甲基甲酰胺(DMF)溶液中,超声处理2~5h;
步骤3)将AgNO3溶液逐滴加入上述混合溶液中,避光搅拌6~20h;
步骤4)将Na2HPO4·12H2O溶液逐滴加入步骤(3)得到的溶液中,避光搅拌1~6h,用水和乙醇洗涤数次,离心分离得到固体部分,真空干燥后制得掺杂碳纳米管和聚苯胺的磷酸银复合光催化剂。
进一步,步骤1)所述的碳纳米管优选为多壁碳纳米管(MWCNTs),直径为10~50nm,长度为10~30μm。
优选的,步骤1)所述的浓硝酸处理为将MWCNTs与浓HNO3以2~4g/L的固液比于110~130℃条件下进行边搅拌边回流处理,处理时间为6~12h;回流结束后用超纯水洗涤至中性,并于55~75℃真空干燥。
优选的,步骤2)所述的聚苯胺为导电型聚苯胺(PANI),MWCNTs与DMF溶液的固液比为0.02~0.15g/L;PANI与DMF溶液的固液比为0.4~2g/L。
优选的,步骤3)所述AgNO3与MWCNTs的质量比为1300:1~170:1;AgNO3与PANI的质量比为30:1~120:1。
进一步,步骤4)所述Na2HPO4·12H2O与AgNO3的摩尔比为1:3,真空干燥温度为50~60℃。
与现有技术相比,本发明具有以下有益效果:
(1)本发明将MWCNTs、Ag3PO4和PANI三种材料复合,成功制备了一种新型的高效可见光催化剂Ag3PO4@MWCNTs@PANI。
(2)本发明中掺杂HNO3改性后的MWCNTs,其良好的光电性能和独特的一维结构,可有效捕获、转移光生电子,增加载流子的生命周期。
(3)本发明中掺杂的PANI,其独特的π共轭长链结构使其成为光生空穴的良好载体和导体,可进一步促进光生载流子的分离。
(4)本发明操作简单易行、绿色无污染。
附图说明
图1为一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法的工艺流程图。
图2为制备得到的复合光催化剂Ag3PO4@MWCNTs@PANI的XRD图。
图3为制备得到的复合光催化剂Ag3PO4@MWCNTs@PANI的紫外可见吸收图。
图4为制备得到的磷酸银复合光催化剂Ag3PO4@MWCNTs@PANI用于降解苯酚的液相色谱图。
具体实施方式
下面通过附图和实施例对本发明作进一步详细描述:
实施例1:
一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,步骤如下:
(1)称取1g多壁碳纳米管(MWCNTs)于350mL HNO3溶液中,在120℃条件下进行边搅拌边回流处理,处理时间为8h。回流结束后用超纯水洗涤至中性,并于70℃真空干燥。
(2)称取干燥得到的0.0012g MWCNTs和0.0377g PANI于40mL N,N-二甲基甲酰胺(DMF)中,超声处理3h。
(3)称取1.53g AgNO3溶解在30mL超纯水中,将溶液逐滴加入上述溶液中,持续避光搅拌12h;
(4)称取1.074gNa2HPO4·12H2O溶解在30mL超纯水中,并将该溶液逐滴加入步骤(3)得到的溶液中,避光搅拌6h。将该固液混合物进行离心分离,并用乙醇和超纯水洗涤3~5次,在55℃真空条件下干燥。得到MWCNTs负载量为0.1%的PANI负载量为3%的Ag3PO4@0.1%MWCNTs@3%PANI复合材料。
制备工艺流程图如图1所示。图2为复合材料的XRD图谱,所有的衍射峰均与Ag3PO4的标准卡片(JCPDS no.06-0505)相符。图3为复合催化剂的紫外可见吸收光谱,吸收边为520nm左右,但在300-800nm均有较强光吸收,表明该催化剂具有优异的光吸收性能。
实施例2:
将制备得到的复合光催化剂用于苯酚的降解,以评估其光催化活性。准确称取制备得到的材料50mg于100mL浓度为25mg/L的苯酚溶液中,超声1min后,在黑暗中搅拌反应30min,使其达到吸附平衡。之后,在300W氙灯(λ>420nm)照射条件下进行降解反应。将不同时间的反应溶液用高效液相色谱进行测定,结果如图4所示。由结果可知,优选的光催化在光照12min后苯酚可被完全降解。
Claims (6)
1.一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,包括以下步骤:
步骤1)将碳纳米管置于浓硝酸中加热回流处理6~12h,冷却后,用水洗涤至中性并干燥;
步骤2)将聚苯胺和预处理后的碳纳米管加入到N,N-二甲基甲酰胺(DMF)溶液中,超声处理2~5h;
步骤3)将AgNO3溶液逐滴加入上述混合溶液中,避光搅拌6~20h;
步骤4)将Na2HPO4·12H2O溶液逐滴加入步骤3)得到的溶液中,避光搅拌1~6h,用水和乙醇洗涤数次,离心分离得到固体部分,真空干燥后制得掺杂碳纳米管和聚苯胺的磷酸银复合光催化剂。
2.根据权利1所述的一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,其特征在于:步骤1)所述的碳纳米管为多壁碳纳米管(MWCNTs),直径为10~50nm,长度为10~30μm。
3.根据权利1所述的一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,其特征在于:步骤1)所述的浓硝酸处理为将MWCNTs与浓HNO3以2~4g/L的固液比于110~130℃条件下进行边搅拌边回流处理,处理时间为6~12h;回流结束后用超纯水洗涤至中性,并于55~75℃真空干燥。
4.根据权利1所述的一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,其特征在于:步骤2)所述的聚苯胺为导电型聚苯胺(PANI),MWCNTs与DMF溶液的固液比为0.02~0.15g/L;PANI与DMF溶液的固液比为0.4~2g/L。
5.根据权利1所述的一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,其特征在于:步骤3)所述AgNO3与MWCNTs的质量比为1300:1~170:1;AgNO3与PANI的质量比为30:1~120:1。
6.根据权利1所述的一种利用碳纳米管和聚苯胺共改性磷酸银复合光催化剂的制备方法,其特征在于:步骤4)所述Na2HPO4·12H2O与AgNO3的摩尔比为1:3,真空干燥温度为50~60℃。
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