CN107961801B - 一种可见光响应的TiO2-AgBr催化剂的制备方法及其应用 - Google Patents
一种可见光响应的TiO2-AgBr催化剂的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种可见光响应的TiO2‑AgBr光催化剂的制备方法及其应用，属于纳米催化剂技术领域。本发明方法是由吡啶和溴代正丁烷在一定条件下制备得到的1‑丁基‑3‑甲基咪唑溴盐([BMIM]Br)。制备方法是称取一定量的吡啶和溴代正丁烷，循环回流一段时间，冷却得到的白色固体即1‑丁基‑3‑甲基咪唑溴盐([BMIM]Br)作为前躯体在制备光催化剂TiO2‑AgBr具有极高的催化活性。本发明方法所采用的工艺简单，对设备要求低，制备的光催化剂在可见光照射下降解染料、农药及酚类具有很高的降解率，光催化剂可重复使用，具有优异的可见光响应性能。
Description
技术领域
本发明涉及纳米催化技术领域，尤其涉及一种可见光响应的 TiO2-AgBr催化剂的制备方法及其应用。
背景技术
近几十年来，作为一种重要的无机材料，TiO2已经应用到大部分的光催化剂领域，但是其禁带宽度较大，只对紫外光起作用，由于其回收产量低和可见光利用缺乏，这就阻碍了它的实际应用。为了处理这些问题，通过金属、非金属掺杂，金属与非金属共掺杂，半导体复合及染料光敏化等技术来增强光催化效率和可见光对TiO2的利用降解效果。其中AgBr作为一种广泛的光敏材料，具有极强的可见光响应，能够与TiO2形成异质结构，抑制电子-空穴对复合，进而提高TiO2在可见光的催化性能。
中国专利CN201510026558.1公开了一种可见光响应的 AgBr/TiO2催化剂的制备方法，以钛酸酯、无水乙醇、CTAB、硝酸银、去离子水为原料，先将钛酸酯与无水乙醇混合，再将CTAB与硝酸银的混合水溶液滴加到钛酸酯溶液中。混合均匀后进行水热反应。将水热反应得到的产物分别用去离子水于乙醇离心洗涤后干燥，最后焙烧，得到AgBr/TiO2催化剂。本发明所采用的工艺简单，对设备要求较低，制备的二氧化钛光催化剂在可见光条件下表现出较强的催化活性。
中国专利CN201110338137.4公开了一直利用类微乳体系合成 AgBr-TiO2纳米异质结构光催化剂的方法，它涉及合成AgBr-TiO2纳米异质结构光催化剂的方法。它解决了现有的AgBr-TiO2纳米异质结构光催化剂的有效复合程度较差的技术问题。方法：先用TiO2纳米粒子、蒸馏水、十六烷基三甲基溴化铵和甲苯制备类微乳液；再用 AgNO3、乙醇胺和蒸馏水制备混合溶液；然后将混合溶液逐滴滴入到类微乳液中，避光搅拌，再经破乳、过滤或离心后得到沉淀，沉淀洗涤干燥后，得到光催化剂。本发明首次利用类微乳体系化学沉淀法合成了稳定的有效复合的AgBr-TiO2纳米异质结构光催化剂，其在可见光、紫外光下都有优异的光催化性能，可用于环境治理及新能源开发领域。
但是上述制备TiO2-AgBr催化剂的方法过程复杂，不易于大规模生产，并且生产过程不够清洁环保。
随着农药广泛应用于农业控制各种有害生物破坏农作物，世界各地使用700种农药之多，其中有600种不再使用，农药对农业生产的益处是不可否认的，尽管如此，少量的残留物可能会持续存在于食物，空气，水和土壤中，各种研究者证实了残留农药危及生命，致病性，致畸性和致癌性等毒性作用并可能引起很多食品安全问题。本方法提供了一种清洁环保且工艺简单的光催化剂。
发明内容
本发明专利的目的是提供一种工艺简单，对设备要求低，且对降解染料、农药及酚类具有优异催化性能的TiO2-AgBr光催化剂的制备方法。本发明方法是由离子液体作为溴源和稳定剂，水热直接制备得到光催化剂TiO2-AgBr，进行了光催化性能实验。
本发明采取的技术方案是：
本发明的可见光响应的TiO2-AgBr催化剂的制备方法具体步骤如下：
称取离子液体[BMIM]Br加水溶解，逐滴加入AgNO3和钛酸四丁酯的水溶液；滴加结束后再搅拌，移至高压反应釜中，水热反应，反应结束后自然冷却至室温，然后洗涤离心，干燥得到TiO2-AgBr光催化剂。
所述的离子液体[BMIM]Br的制备方法如下：准确称取N-甲基咪唑和溴代正丁烷(摩尔比1:1)，油浴加热，循环回流，结束冷却至室温；最后将所制备的离子液体即溴化1-丁基-3-甲基咪唑([BMIM]Br)，密封储存于干燥器中备用。
AgNO3和钛酸四丁酯的水溶液(浓度分别在50,14mol/L)；所述 AgNO3与钛酸四丁酯的摩尔比(3～4):1；AgNO3与离子液体的摩尔比1:(1～1.5)。
滴加结束后再搅拌20min。
所述的水热反应温度为120～160℃；水热时间为12～24h。
所述干燥是在真空60℃干燥6～10h。
本发明还要求保护所述的光催化剂TiO2-AgBr在催化领域的应用，以及在抗生素、染料或农药残留物降解方面的应用。
本发明的积极效果如下：
按照本发明方法制备得到的TiO2-AgBr光催化剂，工艺简单，设备要求低，在可见光有强烈吸收，与AgBr结合后，更加提高光催化剂的活性和催化性能，可在染料污染物的降解和水光解方面有很好的应用前景。
附图说明
图1是催化剂的循环利用示意图。
具体实施方式
下面的实施例是对本发明的进一步详细描述。
实施例1
(1)离子液体的制备
准确称取0.1mol的N-甲基咪唑和等摩尔的溴代正丁烷于三口烧瓶中，油浴加热，磁力搅拌，并维持80℃，2h，冷却即为制得的离子液体1-丁基-3-甲基咪唑溴盐([BMIM]Br)。
(2)TiO2-AgBr的制备
准确称取1.7g左右AgNO3和3.0g左右的钛酸四正丁酯混合均匀后，逐滴加入至溶有20ml水的离子液体(准确称取2.8g左右)中，滴加结束后，继续搅拌10min直至搅拌均匀。最后将这些物质转移到反应釜中，水热温度120～160℃，恒温反应12～24h，再经乙醇和水离心洗涤各两至三次，然后放入60℃烘箱内干燥即得TiO2-AgBr 催化剂。
(3)TiO2-AgBr降解性能实验
以甲基橙(MO)、对硝基苯酚(PNP)和吡虫啉(IMI)为例，对该三种的类型污染物进行降解，数据列于表1，并且对催化剂离心回收后再利用，均进行了5次循环回收，三种有机污染物的降解率均未有明显降低。
表1：TiO2-AgBr对不同类型有机物降解性能研究
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (8)
1.一种可见光响应的TiO2-AgBr催化剂的制备方法，其特征在于：所述方法的具体步骤如下：
称取离子液体[BMIM]Br加水溶解，逐滴加入AgNO3和钛酸四丁酯的水溶液；滴加结束后再搅拌，移至高压反应釜中，水热反应，反应结束后自然冷却至室温，然后洗涤离心，干燥得到TiO2-AgBr光催化剂。
2.如权利要求1所述的可见光响应的TiO2-AgBr催化剂的制备方法，其特征在于：所述的离子液体[BMIM]Br的制备方法如下：准确称取N-甲基咪唑和溴代正丁烷，摩尔比1:1，油浴加热，循环回流，结束冷却至室温；最后将所制备的离子液体即溴化1-丁基-3-甲基咪唑([BMIM]Br)，密封储存于干燥器中备用。
3.如权利要求1所述的可见光响应的TiO2-AgBr催化剂的制备方法，其特征在于：AgNO3和钛酸四丁酯的水溶液，浓度分别为50mol/L和14mol/L；所述AgNO3与钛酸四丁酯的摩尔比(3～4):1；AgNO3与离子液体的摩尔比1:(1～1.5)。
4.如权利要求1所述的可见光响应的TiO2-AgBr催化剂的制备方法，其特征在于：滴加结束后再搅拌20min。
5.如权利要求1所述的可见光响应的TiO2-AgBr催化剂的制备方法，其特征在于：所述的水热反应温度为120～160℃；水热时间为12～24h。
6.如权利要求1所述的可见光响应的TiO2-AgBr催化剂的制备方法，其特征在于：所述干燥是在真空60℃干燥6～10h。
7.如权利要求1-6任一项所述的方法制备的TiO2-AgBr在催化领域的应用。
8.如权利要求1-6任一项所述的方法制备的TiO2-AgBr在染料、酚类或农药残留领域的降解方面的应用。
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