CN111036245A - 一种TiO2-BiOCl复合光催化剂低温液相一步制备方法 - Google Patents
一种TiO2-BiOCl复合光催化剂低温液相一步制备方法 Download PDFInfo
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Abstract
一种TiO2‑BiOCl复合光催化剂低温液相一步制备方法，包括以下步骤；(1)将硫酸氧钛和硝酸铋溶解于去离子水中，得到透明硫酸氧钛和硝酸铋水溶液；(2)向步骤(1)中的硫酸氧钛和硝酸铋水溶液中加入无机碱液到pH值为8‑10，得到白色钛酸和氢氧化铋悬浮液；(3)用去离子水将步骤(2)中的白色钛酸和氢氧化铋悬浮液洗涤；(4)用过氧化氢将步骤(3)中的白色钛酸和氢氧化铋沉淀溶解，得到黄色透明的过氧化钛铋前驱体；(5)在搅拌条件下，向步骤(4)得到黄色透明的过氧化钛铋前驱体中加入氯盐，再加入水合肼溶液，经过滤、洗涤得到TiO2‑BiOCl复合光催化剂。本发明具有原料易得、易批量化化工生产的特点。
Description
技术领域
本发明涉及TiO2-BiOCl复合光催化剂技术领域，特别涉及一种TiO2-BiOCl复合光催化剂低温液相一步制备方法。
背景技术
TiO2因其具有化学稳定性好、光催化活性高、价廉易得、无毒等优点，被广泛用于光催化降解有机物和光解水制氢领域。但是TiO2光生载流子符合效率高，导致其光催化活性下降。为降低TiO2光生载流子率复合率,研究者通过各种方法和手段拓展其吸光域，如采用金属或非金属掺杂、贵金属沉积、染料敏化以及半导体复合等。半导体复合是提高半导体催化活性和效率最有效的手段之一，将两种能带结构相匹配的半导体进行复合可以有效促进光生电子-空穴对的分离，降低光生载流子的复合几率。BiOCl是V-VI-VII三元半导体化合物，也是BiOX(X＝Cl、Br、I)系列材料中被研究和应用最为广泛和深入的。由于BiOCl价带顶和导带底电位(3.59eV，0.19eV)均高于TiO2 (-0.29eV，2.91eV)，能带结构相互匹配。若能将BiOCl和TiO2形成异质复合结构，将可能使其光催化活性进一步提高。但是，具有光催化活性的晶态TiO2合成一般需要苛刻的物理条件，固相合成温度一般高于400℃；水热和溶剂热合成温度一般在200℃左右，但需要高压反应体系。TiO2的制备条件限制了其复合光催化剂的制备。因此，发展低温液相一步合成TiO2和BiOCl复合光催化剂，具有重要的实际意义。
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TiO2-BiOCl复合光催化剂低温液相一步制备方法，具有原料易得、易批量化化工生产的特点。
为了实现上述目的，本发明采用的技术方案是：
一种TiO2-BiOCl复合光催化剂低温液相一步制备方法，包括以下步骤；
(1)将硫酸氧钛和硝酸铋溶解于去离子水中，得到透明硫酸氧钛和硝酸铋水溶液；
(2)向步骤(1)中的硫酸氧钛和硝酸铋水溶液中加入无机碱液到pH值为8-10，得到白色钛酸和氢氧化铋悬浮液；
(3)用去离子水将步骤(2)中的白色钛酸和氢氧化铋悬浮液洗涤，洗涤后的废液电导率小于1000us/cm,得到白色钛酸和氢氧化铋沉淀；
(4)用过氧化氢将步骤(3)中的白色钛酸和氢氧化铋沉淀溶解，得到黄色透明的过氧化钛铋前驱体；
(5)在搅拌条件下，向步骤(4)得到黄色透明的过氧化钛铋前驱体中加入氯盐，机械搅拌10min，再加入水合肼溶液，然后在40-80℃搅拌反应60min,得到白色沉淀，经过滤、洗涤得到TiO2-BiOCl复合光催化剂。
所述的步骤(1)中硫酸氧钛和硝酸铋摩尔比为1:5-3:1。
所述的步骤(2)中无机碱液包括：氢氧化钠、氢氧化钾或氨水。
所述的步骤(4)中过氧化氢和钛酸沉淀质量比为：2-4：1。
所述的步骤(5)中氯盐包括氯化钠或氯化钾，所述的水合肼加入量与硫酸氧钛摩尔量相同，所述的铋离子和氯离子摩尔比1：1。
本发明的有益效果：
(1)本发明制备的TiO2-BiOCl复合光催化剂，TiO2纳米粒子原位生长在BiOCl表面，两者是以化学键合方式复合，有利于光生电子转移，提高复合光催化剂的活性。
(2)本发明的原料易得，制备方法简单、易操作，可重复性高，整个过程制备成本低。
附图说明
图1是实施例1所制备TiO2-BiOCl复合光催化剂的TEM照片。
图2是实施例1所制备TiO2-BiOCl复合光催化剂的选取电子衍射照片。
具体实施方式
下面结合附图对本发明作进一步详细说明。
实施例1：
取0.32g硫酸氧钛(0.002mol)和4.85g(0.01mol)五水硝酸铋溶于100ml去离子水中，机械搅拌条件下，向上述溶液中滴加氨水至pH为9，得到白色沉淀，用去离子水洗涤上述白色沉淀至废液的电导率为600us/cm，得到得到白色钛酸和氢氧化铋；向得到白色钛酸和氢氧化铋中加入0.928g过氧化氢(30w％)，机械搅拌20min后,加入 0.585g氯化钠，机械搅拌10min,然后加入0.196g水合肼(50％)溶液，然后在60℃搅拌反应60min,得到白色沉淀，经过滤、洗涤得到TiO2-BiOCl复合光催化剂。
如图1所示：从图中可以看出，所制备样品中TiO2纳米粒子生长在BiOCl纳米片表面上。其中，纳米TiO2粒子的颗粒尺寸大约在 30nm,颗粒尺寸分布均匀，BiOCl纳米片为无规则形状。
如图2所示：从选取电子衍射中可以看出，存在一套单晶衍射斑点和一套多晶衍射环。其中单晶衍射电子图样可以标定为四方相BiOCl(110)和(200)面，说明TiO2-BiOCl复合光催化剂中BiOCl纳米片为单晶结构。此外，SAED图谱中，通过测量多晶衍射环的晶面间距，其值分别对应锐钛矿相TiO2(101)，(004)，(200)和(105)晶面。
实施例2：
取4.8g硫酸氧钛(0.03mol)和4.85g(0.01mol)五水硝酸铋溶于100ml去离子水中，机械搅拌条件下，向上述溶液中滴加氨水至 pH为9，得到白色沉淀，用去离子水洗涤上述白色沉淀至废液的电导率为600us/cm，得到得到白色钛酸和氢氧化铋；向得到白色钛酸和氢氧化铋中加入13.92g过氧化氢(30w％)，机械搅拌20min后,加入 0.585g氯化钠，机械搅拌10min,然后加入2.94g水合肼(50％)溶液，然后在60℃搅拌反应60min,得到白色沉淀，经过滤、洗涤得到TiO2-BiOCl复合光催化剂。
实施例3：
取2.4g硫酸氧钛(0.015mol)和4.85g(0.01mol)五水硝酸铋溶于100ml去离子水中，机械搅拌条件下，向上述溶液中滴加氨水至 pH为9，得到白色沉淀，用去离子水洗涤上述白色沉淀至废液的电导率为600us/cm，得到得到白色钛酸和氢氧化铋；向得到白色钛酸和氢氧化铋中加入6.96g过氧化氢(30w％)，机械搅拌20min后,加入 0.585g氯化钠，机械搅拌10min,然后加入1.47g水合肼(50％)溶液，然后在60℃搅拌反应60min,得到白色沉淀，经过滤、洗涤得到TiO2-BiOCl复合光催化剂。
Claims (5)
1.一种TiO2-BiOCl复合光催化剂低温液相一步制备方法，其特征在于，包括以下步骤；
(1)将硫酸氧钛和硝酸铋溶解于去离子水中，得到透明硫酸氧钛和硝酸铋水溶液；
(2)向步骤(1)中的硫酸氧钛和硝酸铋水溶液中加入无机碱液到pH值为8-10，得到白色钛酸和氢氧化铋悬浮液；
(3)用去离子水将步骤(2)中的白色钛酸和氢氧化铋悬浮液洗涤，洗涤后的废液电导率小于1000us/cm,得到白色钛酸和氢氧化铋沉淀；
(4)用过氧化氢将步骤(3)中的白色钛酸和氢氧化铋沉淀溶解，得到黄色透明的过氧化钛铋前驱体；
(5)在搅拌条件下，向步骤(4)得到黄色透明的过氧化钛铋前驱体中加入氯盐，机械搅拌10min，再加入水合肼溶液，然后在40-80℃搅拌反应60min,得到白色沉淀，经过滤、洗涤得到TiO2-BiOCl复合光催化剂。
2.根据权利要求1所述的一种TiO2-BiOCl复合光催化剂低温液相一步制备方法，其特征在于，所述的步骤(1)中硫酸氧钛和硝酸铋摩尔比为1:5-3:1。
3.根据权利要求1所述的一种TiO2-BiOCl复合光催化剂低温液相一步制备方法，其特征在于，所述的步骤(2)中无机碱液包括：氢氧化钠、氢氧化钾或氨水。
4.根据权利要求1所述的一种TiO2-BiOCl复合光催化剂低温液相一步制备方法，其特征在于，所述的步骤(4)中过氧化氢和钛酸沉淀质量比为：2-4：1。
5.根据权利要求1所述的一种TiO2-BiOCl复合光催化剂低温液相一步制备方法，其特征在于，所述的步骤(5)中氯盐包括氯化钠或氯化钾，所述的水合肼加入量与硫酸氧钛摩尔量相同，所述的铋离子和氯离子摩尔比1：1。
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