CN106179342A - 一种快速制备Ag3VO4纳米晶光催化剂的方法 - Google Patents
一种快速制备Ag3VO4纳米晶光催化剂的方法 Download PDFInfo
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Abstract
一种快速合成Ag3VO4纳米光催化剂的方法,Ag3VO4纳米光催化剂采用沉淀辅助微波水热法合成,其制备方法包括:将硝酸银加入到蛋白质和浓度为0.1~0.3mol/L的五氧化二钒混合溶液中,用氨水溶液调节pH值至3~12后,在80~120℃下热处理0.5~2h。所得到的沉淀物过滤后分别用蒸馏水和无水乙醇洗涤,并在40~80℃的真空干燥箱中干燥,得到的钒酸银粉末为单晶结构,化学组成均一,纯度较高,具有较大的比表面积,提高了材料的光催化性能。
Description
技术领域
本发明涉及半导体纳米材料制备和应用,属无机材料制备领域,具体涉及一种快速制备Ag3VO4纳米晶光催化剂的方法。
背景技术
V位于第三周期第五副族,属于过渡金属元素。钒元素的3d轨道的能量相比于其他第一过渡系金属元素其能量较低,导致含钒元素的半导体材料的导带能级较低,也就是说含钒元素的半导体材料在光催化领域会有一个较为合适的能带结构,是一类潜在的光催化剂备选材料。
目前,国内外提出的由水热法、微波水热法等方法制备的钒酸银的形貌包括:颗粒状、方块状、纤维状等。中国发明公告专利第201310257173.7号公开了一种钒酸银纳米纤维光催化剂及其制备方法,采用静电纺丝法制备,但对水分等要求高,技术难度大。第201210531539.0号公开了一种棒状钒酸银纳米光催化剂及其制备方法,采用双注沉淀法制备棒状钒酸银微晶,但技术难度大,且对所制备的产品保存条件要求高。CTAB-assistedhydrothermal synthesis of silver vanadates and their photocatalyticcharacterization.Chao-Ming Huang等人采用CTAB作为表面活性剂的水热结合热处理方式制备得到Ag3VO4与Ag4V2O7的混合相,其产品纯度不高,且尺寸较大。
目前特殊形貌的钒酸银的制备方法还很少,因此对特殊形貌的钒酸银的研究具有重大意义。
发明内容
本发明针对上述现有技术的不足,目的在于提出一种快速制备Ag3VO4纳米晶光催化剂的方法,该方法操作简单,反应条件温和,耗时短,且制备钒酸银产品纯度高,形貌和尺寸均一。
为了实现上述目的,本发明采用以下技术方案:
一种快速制备Ag3VO4纳米晶光催化剂的方法,包括以下步骤:
(1)将蛋白质加入到五氧化二钒水溶液中,搅拌均匀,得到混合溶液A;
(2)将硝酸银溶液滴加到混合溶液A中,搅拌下反应1~2h,得到混合溶液B;
(3)调节混合溶液B的pH值至3~12,然后在温度为80~120℃,功率为200~400W下进行微波水热反应0.5~2h后,将反应液过滤得到沉淀,沉淀经洗涤、干燥,得到颗粒状的Ag3VO4纳米晶光催化剂。
本发明进一步的改进在于,步骤(1)所述的五氧化二钒水溶液的浓度为0.1~0.3mol/L;蛋白质和五氧化二钒水溶液的用量比为(0.01~0.04)g:(20~60)mL。
本发明进一步的改进在于,步骤(1)所述的搅拌是在40~100℃下进行的,搅拌时间为1~2h。
本发明进一步的改进在于,步骤(2)所述的硝酸银溶液的浓度为0.1~0.4mol/L,硝酸银和五氧化二钒水溶液的用量比为(10~60)mL:(20~60)mL。
本发明进一步的改进在于,步骤(3)所述是采用0.1~0.3mol/L的氨水调节混合溶液B的pH值。
本发明进一步的改进在于,步骤(3)中调节混合溶液B的pH值至3~12后搅拌1~3h,再进行微波水热反应。
本发明进一步的改进在于,步骤(3)所述的微波水热反应是在微波反应釜中进行。
本发明进一步的改进在于,步骤(3)所述的洗涤是将沉淀分别用去离子水和乙醇洗涤。
本发明进一步的改进在于,步骤(3)所述的干燥是在40~80℃下进行。
与现有技术相比,本发明具有以下有益效果:
(1)本发明所采用的沉淀辅助微波水热方法以V2O5作为钒源,硝酸银溶液滴加到混合溶液A中,搅拌下进行反应,生成沉淀状前驱体;以AgNO3作为银源,蛋白质作为表面活性剂,调节溶液的pH值后再在80~120℃下进行微波水热反应,制得光催化性能良好的Ag3VO4。
(2)由于蛋白质具有快速吸附到界面的能力,所以当其达到界面后可迅速伸展和取向,可作为较为理想的表面活性剂,促进Ag3VO4纳米晶光催化剂的生成。
(3)本发明所述的沉淀辅助微波水热过程,操作简单,流程短,条件温和,产品质量稳定,易于实现工业化。
(4)本发明制得的钒酸银粉末为单晶结构,化学组成均一,纯度较高,所制备钒酸银的颗粒直径为30~60nm,具有较大的比表面积,提高了材料的光催化性能。将0.05g该粉体投入50mL罗丹明B溶液(罗丹明B浓度10mg/L)中,在可见光照射条件下,反应200min后罗丹明B的降解率可达75%以上。
附图说明
图1为本发明在实施例1条件下制备的钒酸银的X射线衍射图谱。
图2为本发明在实施例1条件下制备的钒酸银的扫描电子显微镜图,其中,图(a)为未添加蛋白质所制备光催化剂的扫描图,图(b)为蛋白质改性所制备光催化剂的扫描图。
图3为本发明在实施例1条件下制备的钒酸银的在可见光照射下对罗丹明B的降解图。
具体实施方式
下面结合附图以及具体实施例对本发明做进一步详细描述:
实施例1
(1)将0.01g蛋白质加入到20mL 0.1mol/L的五氧化二钒(V2O5)水溶液中,90℃下磁力搅拌2h,冷却到室温,得到混合溶液A。
(2)将60mL 0.3mol/L的硝酸银(AgNO3)溶液滴加到混合溶液A中,磁力搅拌2h,得到混合溶液B。
(3)采用0.1mol/L氨水调节混合溶液B的pH值至12后磁力搅拌3h,在温度为80℃,功率为400W下微波水热反应120min,反应结束后,将反应液过滤得到沉淀,所得到的沉淀物过滤后分别用蒸馏水和乙醇离心洗涤,并在70℃的烘箱中干燥,得到Ag3VO4纳米晶光催化剂。
参见图1,从图1可以看出,可以清晰的看到本发明制备的Ag3VO4为纯相单晶结构;
参见图2,从图2(a)和图2(b)可以看出,所制备钒酸银的颗粒直径为30~60nm;
参见图3,从图3可以看出,将0.05g该粉体投入50mL罗丹明B溶液(罗丹明B浓度10mg/L)中,在可见光照射条件下,反应200min后罗丹明B的降解率可达75%以上。
实施例2
(1)将0.02g蛋白质加入到20mL 0.1mol/L的五氧化二钒(V2O5)水溶液中,80℃下磁力搅拌2h,冷却到室温,得到混合溶液A。
(2)采用0.2mol/L氨水将60mL 0.3mol/L的硝酸银(AgNO3)溶液滴加到混合溶液A中,磁力搅拌2h,得到混合溶液B。
(3)调节混合溶液B的pH值至9后磁力搅拌3h,在温度为95℃,功率为350W下微波水热反应90min,反应结束后,将反应液过滤得到沉淀,所得到的沉淀物过滤后分别用蒸馏水和乙醇离心洗涤,并在70℃的烘箱中干燥,得到Ag3VO4纳米晶光催化剂。
实施例3
(1)将0.03g蛋白质加入到20mL 0.1mol/L的五氧化二钒(V2O5)水溶液中,70℃下磁力搅拌2h,冷却到室温,得到混合溶液A。
(2)将60mL 0.3mol/L的硝酸银(AgNO3)溶液滴加到混合溶液A中,磁力搅拌2h,得到混合溶液B。
(3)采用0.3mol/L氨水调节混合溶液B的pH值至6后磁力搅拌3h,在温度为105℃,功率为300W下微波水热反应60min,反应结束后,将反应液过滤得到沉淀,所得到的沉淀物过滤后分别用蒸馏水和乙醇离心洗涤,并在70℃的烘箱中干燥,得到Ag3VO4纳米晶光催化剂。
实施例4
(1)将0.04g蛋白质加入到20mL 0.1mol/L的五氧化二钒(V2O5)水溶液中,60℃下磁力搅拌2h,冷却到室温,得到混合溶液A。
(2)将60mL 0.3mol/L的硝酸银(AgNO3)溶液滴加到混合溶液A中,磁力搅拌2h,得到混合溶液B。
(3)采用0.1mol/L氨水调节混合溶液B的pH值至3后磁力搅拌3h,在温度为120℃,功率为250W下微波水热反应30min,反应结束后,将反应液过滤得到沉淀,所得到的沉淀物过滤后分别用蒸馏水和乙醇离心洗涤,并在70℃的烘箱中干燥,得到Ag3VO4纳米晶光催化剂。
实施例5
(1)将蛋白质加入到五氧化二钒水溶液中,在40℃下搅拌2h,得到混合溶液A;其中,所述的五氧化二钒水溶液的浓度为0.1mol/L;蛋白质和五氧化二钒水溶液的用量比为0.01g:60mL。
(2)将0.1mol/L的硝酸银溶液滴加到混合溶液A中,搅拌下反应1h,得到混合溶液B;其中,硝酸银和五氧化二钒水溶液的用量比为30mL:60mL。
(3)采用0.1mol/L的氨水调节混合溶液B的pH值至7后搅拌1h,然后在温度为90℃,功率为200W下在微波反应釜中进行微波水热反应40min后,将反应液过滤得到沉淀,沉淀分别用去离子水和乙醇洗涤洗涤、在40℃下干燥,得到颗粒状的Ag3VO4纳米晶光催化剂。
实施例6
(1)将蛋白质加入到五氧化二钒水溶液中,在100℃下搅拌1h,得到混合溶液A;其中,所述的五氧化二钒水溶液的浓度为0.3mol/L;蛋白质和五氧化二钒水溶液的用量比为0.04g:40mL。
(2)将0.4mol/L的硝酸银溶液滴加到混合溶液A中,搅拌下反应1.5h,得到混合溶液B;其中,硝酸银和五氧化二钒水溶液的用量比为10mL:40mL。
(3)采用0.1mol/L的氨水调节混合溶液B的pH值至10后搅拌2h,然后在温度为110℃,功率为400W下在微波反应釜中进行微波水热反应10min后,将反应液过滤得到沉淀,沉淀分别用去离子水和乙醇洗涤洗涤、在80℃下干燥,得到颗粒状的Ag3VO4纳米晶光催化剂。
与申请公开号为CN 103285861 A的专利在可见光下对甲苯的去除率相比,性能有显著提高。本发明得到的钒酸银粉末为单晶结构,化学组成均一,纯度较高,具有较大的比表面积,提高了材料的光催化性能。
Claims (9)
1.一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,包括以下步骤:
(1)将蛋白质加入到五氧化二钒水溶液中,搅拌均匀,得到混合溶液A;
(2)将硝酸银溶液滴加到混合溶液A中,搅拌下反应1~2h,得到混合溶液B;
(3)调节混合溶液B的pH值至3~12,然后在温度为80~120℃,功率为200~400W下进行微波水热反应0.5~2h后,将反应液过滤得到沉淀,沉淀经洗涤、干燥,得到颗粒状的Ag3VO4纳米晶光催化剂。
2.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(1)所述的五氧化二钒水溶液的浓度为0.1~0.3mol/L;蛋白质和五氧化二钒水溶液的用量比为(0.01~0.04)g:(20~60)mL。
3.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(1)所述的搅拌是在40~100℃下进行的,搅拌时间为1~2h。
4.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(2)所述的硝酸银溶液的浓度为0.1~0.4mol/L,硝酸银和五氧化二钒水溶液的用量比为(10~60)mL:(20~60)mL。
5.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(3)所述是采用0.1~0.3mol/L的氨水调节混合溶液B的pH值。
6.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(3)中调节混合溶液B的pH值至3~12后搅拌1~3h,再进行微波水热反应。
7.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(3)所述的微波水热反应是在微波反应釜中进行。
8.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(3)所述的洗涤是将沉淀分别用去离子水和乙醇洗涤。
9.根据权利要求1所述的一种快速制备Ag3VO4纳米晶光催化剂的方法,其特征在于,步骤(3)所述的干燥是在40~80℃下进行。
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