CN107970912A - 一种阿尔法氧化铋/钒酸铋及制备方法 - Google Patents
一种阿尔法氧化铋/钒酸铋及制备方法 Download PDFInfo
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Abstract
本发明公开了一种阿尔法氧化铋/钒酸铋及制备方法。本发明制备方法步骤如下:先将硝酸铋加入去硝酸中,将偏钒酸铵加入到氢氧化钠溶液中,将两溶液混合调控pH值后,经过干燥、研磨和煅烧后得到钒酸铋,将获得的钒酸铋粉末与氯氧化铋粉末混合、分散后加入氢氧化钠溶液、搅拌、洗涤、烘干后得到一种阿尔法氧化铋/钒酸铋粉末。本发明通过使用氢氧化钠原位转变氯氧化铋后获得阿尔法氧化铋/钒酸铋中的阿尔法氧化铋。本发明具有两相组分之间的比例易于调控、生产成本低、工艺方法简便等优点。
Description
技术领域
本发明属于功能材料领域,涉及一种阿尔法氧化铋/钒酸铋及制备方法。
背景技术
近年来,随着全球工业化进程的迅速发展,环境污染问题日益突出。光催化技术以其直接利用太阳光来解决水体污染的优势,得到了越来越多的关注,光催化剂是这项技术的核心。阿尔法氧化铋和钒酸铋在光照条件下可以催化分解水和降解有机污染物,然而单独使用时存在光生载流子分离效率低、光催化性能差等问题。作为典型的制备案例,在Inorg. Chem. (2011, 50, 800–805)中报道了钒酸铋/氧化铋复合材料的制备方法,1mmol的硝酸铋加入到40毫升的混合溶剂(超纯水和乙二醇)。然后加入1mmol偏钒酸钠和3mmol的2 -乙基己基磺基琥珀酸。溶液被倒入一个50毫升容量、衬里为聚四氟乙烯的反应釜中,在160℃下保温18小时后冷却至室温,离心分离,并用超纯水和无水乙醇清洗三次,然后对产品进行真空下60℃干燥4小时,得到钒酸铋。将0.5毫摩尔所获得的钒酸铋粉末分散在40ml超纯水中。然后在溶液中加入5毫摩尔的NaOH。搅拌一段时间后,将溶液倒入不锈钢高压釜,在180℃保温12小时后,得到钒酸铋/氧化铋复合材料。可以看出现有技术的复杂性导致成本过高,不易实现工业化生产。本发明通过一种更为简单的方式实现阿尔法氧化铋/钒酸铋的复合,通过一种简便的方法生成第二相阿尔法氧化铋,达到提高钒酸铋基材料的光生载流子分离效率的目的,对开发有实用价值的钒酸铋光催化剂具有重要的意义。
发明内容
本发明的目的在于提供一种阿尔法氧化铋/钒酸铋高效光催化剂的制备方法,所述的阿尔法氧化铋/钒酸铋及制备方法,其特征在于,所述阿尔法氧化铋/钒酸铋中的钒酸铋结构为单斜相,阿尔法氧化铋也为单斜相结构。本发明具有两相组分之间的比例易于调控、生产成本低、工艺方法简便等优点。
本发明采用如下技术方案:
一种阿尔法氧化铋/钒酸铋及制备方法,包括以下步骤:
步骤1,将一定量的硝酸铋加入到硝酸中,搅拌至均匀,形成A液;
步骤2,将一定量的偏钒酸铵加入到氢氧化钠溶液中,得到B液;
步骤3,将B液加入到A液中,形成C液前驱体,其中硝酸铋与偏钒酸铵的摩尔比为1:1;
步骤4,用NaOH溶液调节C液前驱体的PH值为6.5~7,干燥、研磨、煅烧后得到钒酸铋;
步骤5,将氯氧化铋粉末与步骤4中得到的钒酸铋混合,加入去离子水后超声分散,然后将氢氧化钠溶液加入到上述体系中,其中钒酸铋与氯氧化铋摩尔比为1:(0~0.5),氯氧化铋与氢氧化钠摩尔比为1:(3~4),将沉淀使用乙醇和去离子水反复洗涤3次,干燥后得到阿尔法氧化铋/钒酸铋。
所述的阿尔法氧化铋/钒酸铋在光催化方面的应用。与现有技术相比,本发明具有以下有益效果:
(1)本发明采用溶胶法与原位化学转变法相结合制备了阿尔法氧化铋/钒酸铋复合光催化剂。本发明具有两相组分之间的比例易于调控、生产成本低、工艺方法简便等优点。
(2) 本发明比传统的物理混合或表面生成的方法更加有效提高钒酸铋与阿尔法氧化铋的有效接触面积,利于得到更加高效的阿尔法氧化铋/钒酸铋复合光催化剂。阿尔法氧化铋/钒酸铋在可见光照360min后脱色率可达92%,钒酸铋粉体在可见光照360min后的脱色率为35%,阿尔法氧化铋在可见光照射360min后脱色率为16%,阿尔法氧化铋/钒酸铋的脱色率较阿尔法氧化铋和钒酸铋有很大的提高。
附图说明
图1是本发明实施例1中制备的阿尔法氧化铋的XRD衍射图谱;
图2是本发明实施例2中制备的钒酸铋的XRD衍射图谱;
图3是本发明实施例3中制备的阿尔法氧化铋/钒酸铋的XRD衍射图谱;
图4是本发明实施例1~3中制备的阿尔法氧化铋、钒酸铋和阿尔法氧化铋/钒酸铋的光催化脱色率曲线。
具体实施方式:
下面结合附图和本发明优选的具体实施例对本发明做进一步描述,原料均为分析纯。
实施例1:
将一定量的氯氧化铋粉末加入到去离子水中后超声分散,然后将氢氧化钠溶液加入到上述体系中,其中氯氧化铋与氢氧化钠摩尔比为1:4,将沉淀使用乙醇和去离子水反复洗涤3次,干燥后得到阿尔法氧化铋。
实施例2:
步骤1,将一定量的柠檬酸加入到2 mol/L的硝酸中,然后加入一定量的Bi(NO3)3·5H2O,搅拌至均匀,其中Bi(NO3)3·5H2O和柠檬酸的摩尔比为1:2,并用氨水调节pH值到7;
步骤2,将一定量的NH4VO3溶于氢氧化钠溶液中,将步骤1中获得溶液加入到上述溶液中,用氨水调节pH值到7;
步骤3,将步骤2获得的溶液先在80℃下水浴,然后在135℃下干燥5小时,研磨后得到的粉末在500°C下煅烧4小时后得到钒酸铋。
实施例3:
步骤1,将一定量的柠檬酸加入到2 mol/L的硝酸中,然后加入一定量的Bi(NO3)3·5H2O,搅拌至均匀,其中Bi(NO3)3·5H2O和柠檬酸的摩尔比为1:2,并用氨水调节pH值到7;
步骤2,将一定量的NH4VO3溶于氢氧化钠溶液中,将步骤1中获得溶液加入到上述溶液中,用氨水调节pH值到7;
步骤3,将步骤2获得的溶液先在80℃下水浴,然后在135℃下干燥5小时,研磨后得到的粉末在500°C下煅烧4小时后得到钒酸铋;
步骤5,将氯氧化铋粉末与得到的钒酸铋混合,加入去离子水后超声分散,然后将氢氧化钠溶液加入到上述体系中,其中钒酸铋与氯氧化铋摩尔比为1:0.25,氯氧化铋与氢氧化钠摩尔比为1:4,将沉淀使用乙醇和去离子水反复洗涤3次,干燥后得到阿尔法氧化铋/钒酸铋。
应用例:
对实施列1~3中所制得的阿尔法氧化铋、钒酸铋和阿尔法氧化铋/钒酸铋进行光催化活性评价,具体操作步骤为:
称量实施例1~3中所制得的阿尔法氧化铋、钒酸铋和阿尔法氧化铋/钒酸铋分别取光催化剂100 mg,将其加入到罗丹明B染料溶液中(100mL,3.13×10-5mol·L-1),避光搅拌1h,待脱吸附达到平衡后打开500W氙灯光源,每隔30min检测一次染料的浓度,在给定时间内表征出所制备材料对罗丹明B的催化脱色情况。
以上所述内容仅为本发明构思下的基本说明,通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换,均应属本发明的保护范围。
Claims (7)
1.一种阿尔法氧化铋/钒酸铋及制备方法,其特征在于阿尔法氧化铋/钒酸铋中钒酸铋为单斜相结构,阿尔法氧化铋为单斜相结构,包括以下制备步骤:
步骤1,将一定量的硝酸铋加入到硝酸中,搅拌至均匀,形成A液;
步骤2,将一定量的偏钒酸铵加入到氢氧化钠溶液中,得到B液;
步骤3,将B液加入到A液中,形成C液前驱体,其中硝酸铋与偏钒酸铵的摩尔比为1:1;
步骤4,用NaOH溶液调节C液前驱体的PH值为6.5~7,干燥、研磨、煅烧后得到钒酸铋;
步骤5,将氯氧化铋粉末与步骤4中得到的钒酸铋混合,加入去离子水后超声分散,然后将氢氧化钠溶液加入到上述体系中,其中钒酸铋与氯氧化铋摩尔比为1:(0~0.5),氯氧化铋与氢氧化钠摩尔比为1:(3~4),将沉淀使用乙醇和去离子水反复洗涤3次,干燥后得到阿尔法氧化铋/钒酸铋。
2.所述步骤1中硝酸铋的浓度为25~40mmol/L。
3.所述步骤2中偏钒酸铵的浓度为25~40mmol/L。
4.所述步骤3中硝酸铋与偏钒酸铵的摩尔比为1:1。
5.所述步骤4中C液前驱体的PH值为6.5~7,煅烧温度为400~600℃,保温时间为3~5小时。
6.所述步骤5中钒酸铋与氯氧化铋摩尔比为1:(0~0.5),氢氧化钠浓度为0.5~1.5mol/L,氯氧化铋与氢氧化钠摩尔比为1:(3~4)。
7.所述的阿尔法氧化铋/钒酸铋在光催化方面的应用。
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