CN111974428A - 一种Bi2O2CO3-Bi2WO6复合光催化剂制备方法 - Google Patents
一种Bi2O2CO3-Bi2WO6复合光催化剂制备方法 Download PDFInfo
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
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- AAQNGTNRWPXMPB-UHFFFAOYSA-N dipotassium;dioxido(dioxo)tungsten Chemical compound [K+].[K+].[O-][W]([O-])(=O)=O AAQNGTNRWPXMPB-UHFFFAOYSA-N 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
一种Bi2O2CO3‑Bi2WO6复合光催化剂制备方法,包括以下步骤;步骤1:将Bi(NO3)3·5H2O和钨酸盐依次加入甲醇溶液中,机械搅拌后,得到混合液所述Bi(NO3)3·5H2O与钨酸盐的摩尔比为1‑10:1;步骤2:将混合液在压强3Mpa以上、150‑200℃条件下保温3‑12小时进行反应;步骤3:反应完成后,自然冷却至室温,对产物进行离心,水洗,室温下干燥,即得到Bi2O2O3‑Bi2WO6复合光催化剂。本发明具有光量子效率高,可见光活性好的特点。
Description
技术领域
本发明涉及复合光催化剂的制备技术领域,特别涉及一种 Bi2O2CO3-Bi2WO6复合光催化剂制备方法。
背景技术
近年来,半导体光催化技术越来越得到研究者的重视,尤其是在世界环境污染如此严重的情况下,人们发现光催化可以降解大部分有机物。当有特定波长的光照射到催化剂上时,光生电子和空穴发生分离,光生电子和空穴分别于吸附在催化剂表面的目标污染物和氢氧根离子(或者水)发生反应,并分别生成超氧负离子和羟基自由基,超氧负离子和羟基自由基均具有超强的氧化性,可以参与光催化反应,将目标污染物降解,生成二氧化碳和水等无机小分子。其中,铋系半导体光催化材料具有良好的光催化活性,逐渐发展成为光催化领域的研究热点。
Bi2O2CO3半导体由[Bi2O2]2+层与CO32-层互相交错组成,是一种适用于紫外光照射驱动的有机污染物光催化去除的环境友好材料。然而,其具有较大的带隙能,且单体系中仍存在载流子复合速率较高的问题。构建半导体异质结构光催化材料是克服传统光催化剂固有缺陷的有效途径之一。Bi2WO6的光学带隙大约为2.0eV,是一种可用于可见光催化的窄带隙钙钛矿型半导体材料。Bi2WO6还具有成本低、稳定性好、无毒、光催化性能好、带隙窄等优点,是一种有前途的催化材料。专利CN 110152701 A:一种 Bi2O2CO3/Bi2WO6:Yb3+、Er3+光催化剂及其制备方法和应用,采用两步溶剂热法,以Bi(NO3)3·5H2O和Na2WO4·2H2O的混合溶液为前驱体,采用水热法结合煅烧法获得Bi2WO6:Yb3+、Er3+粉末;将 Bi2WO6:Yb3+、Er3+粉末加入到Bi2O2CO3的前驱体溶液中混合均匀,得到的悬浊液转移至聚四氟乙烯不锈钢反应釜中,置于烘箱中,再次溶剂热反应,自然冷却至室温,将所得沉淀用去离子水和无水乙醇分别漂洗,离心分离,于干燥箱内干燥,得 Bi2O2CO3/Bi2WO6:Yb3+、Er3+。该方法步骤繁琐,且需在550- 650℃高温焙烧,能耗均较高不利于工业化生产。
发明内容
为了克服上述现有技术的不足,本发明的目的在于提供一种 Bi2O2CO3-Bi2WO6复合光催化剂制备方法,具有光量子效率高,可见光活性好的特点。
为了实现上述目的,本发明采用的技术方案是:
一种Bi2O2CO3-Bi2WO6复合光催化剂制备方法,包括以下步骤;
步骤1:将Bi(NO3)3·5H2O和钨酸盐依次加入甲醇溶液中,机械搅拌后,得到混合液所述Bi(NO3)3·5H2O与钨酸盐的摩尔比为1-10: 1;
步骤2:将混合液在压强3Mpa以上、150-200℃条件下保温3- 12小时进行反应;
步骤3:反应完成后,自然冷却至室温,对产物进行离心,水洗,室温下干燥,即得到Bi2O2O3-Bi2WO6复合光催化剂。
所述钨酸盐包括钨酸钠、钨酸钾和钨酸铵。
所述步骤1中机械搅拌时间为0.5-1小时。
本发明的有益效果:
将宽禁带Bi2O2CO3与窄禁带Bi2WO6复合,一方面扩展了 Bi2O2CO3光响应范围,提高了其可见光利用率;另一方面有利于促进光生电子-空穴的分离,大幅增加了空穴和电子的数量,而电子可以与水分子反应,产生化学超氧自由基和羟基自由基,从而提高了光催化剂的光化学活性和降解效率。
改制备方法中甲醇即作为溶剂,同时为Bi2O2CO3提供碳源,避免了添加其它碳源,实现Bi2O2CO3-Bi2WO6复合光催化剂的一步合成,具有工艺简单、易于控制且成本低廉特点。
上述比例有利于制得分散性良好的产物,提高产物的光催化活性。
附图说明
图1是本发明Bi(NO3)3·5H2O和Na2WO4·2H2O摩尔比为5:1 Bi2O2O3-Bi2WO6复合光催化剂样品的TEM照片。
图2为不同Bi(NO3)3·5H2O和Na2WO4·2H2O摩尔比条件下所制备Bi2O2O3-Bi2WO6复合光催化剂样品的XRD照片。
具体实施方式
下面结合实施例对本发明作进一步详细说明。
具体实施例1(摩尔比10:1,图2a)
取2.425g Bi(NO3)3·5H2O和0.165g Na2WO4·2H2O加入到30 ml甲醇溶液中,机械搅拌1小时后转移到高压反应釜中,压强4Mpa;将高压反应釜放置于恒温干燥箱中,在200℃条件下反应6h;待反应釜自然冷却至室温后,产品经过过滤、洗涤,干燥等处理得到Bi2O2O3-Bi2WO6复合光催化剂。
具体实施例2(摩尔比5:1,图2b)
取2.425g Bi(NO3)3·5H2O和0.33g Na2WO4·2H2O加入到30 ml甲醇溶液中,机械搅拌1小时后转移到高压反应釜中,压强4Mpa;将高压反应釜放置于恒温干燥箱中,在200℃条件下反应6h;待反应釜自然冷却至室温后,产品经过过滤、洗涤,干燥等处理得到Bi2O2O3-Bi2WO6复合光催化剂。
具体实施例3(摩尔比5:3,图2c)
取2.425g Bi(NO3)3·5H2O和0.99g Na2WO4·2H2O加入到30 ml甲醇溶液中,机械搅拌1小时后转移到高压反应釜中,压强4 Mpa;将高压反应釜放置于恒温干燥箱中,在200℃条件下反应6 h;待反应釜自然冷却至室温后,产品经过过滤、洗涤,干燥等处理得到Bi2O2O3-Bi2WO6复合光催化剂。
具体实施例4(摩尔比1:1,图2d)
取2.425g Bi(NO3)3·5H2O和1.65g Na2WO4·2H2O加入到 30ml甲醇溶液中,机械搅拌1小时后转移到高压反应釜中,压强4 Mpa;将高压反应釜放置于恒温干燥箱中,在200℃条件下反应6 h;待反应釜自然冷却至室温后,产品经过过滤、洗涤,干燥等处理得到Bi2O2O3-Bi2WO6复合光催化剂。
如图1所示:所制得Bi2O2CO3-Bi2WO6复合光催化剂形貌为不规则片状,其中Bi2WO6纳米片附着在Bi2O2CO3纳米片表面。
如图2所示:采用实施例中的Bi(NO3)3·5H2O和Na2WO4·2H2O 摩尔配比均能得到Bi2O2CO3-Bi2WO6复合光催化剂,且原料中摩尔配比的改变可以调整产物中Bi2O2CO3和Bi2WO6的相对含量。
Claims (3)
1.一种Bi2O2CO3-Bi2WO6复合光催化剂制备方法,其特征在于,包括以下步骤;
步骤1:将Bi(NO3)3·5H2O和钨酸盐依次加入甲醇溶液中,机械搅拌后,得到混合液所述Bi(NO3)3·5H2O与钨酸盐的摩尔比为1-10:1;
步骤2:将混合液在压强3Mpa以上、150-200℃条件下保温3-12小时进行反应;
步骤3:反应完成后,自然冷却至室温,对产物进行离心,水洗,室温下干燥,即得到Bi2O2O3-Bi2WO6复合光催化剂。
2.根据权利要求1所述的一种Bi2O2CO3-Bi2WO6复合光催化剂制备方法,其特征在于,所述钨酸盐包括钨酸钠、钨酸钾和钨酸铵。
3.根据权利要求1所述的一种Bi2O2CO3-Bi2WO6复合光催化剂制备方法,其特征在于,所述步骤1中机械搅拌时间为0.5-1小时。
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