CN110743575B - 一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法 - Google Patents
一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有吸附‑光催化协同效应的AgIn5S8/SnS2型可见光催化剂的合成方法,步骤如下:(1)将一定量的无机锡源、无机铟源和无机银源作为原料在持续搅拌下分散于去离子水中,室温下搅拌30分钟;(2)依次将硫代乙酰胺和柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;(3)将充分反应后的溶液转移至反应釜中,在150℃的温度下水热反应12小时,自然冷却到室温,经滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60℃下干燥24 h。本发明的固溶体催化剂能有效实现光生电子‑空穴对的高效分离、转移与迁移,具有较好的稳定性以及较强的可见光吸收;吸附效果好,对于污染物的降解具有显著作用。
Description
技术领域
本发明涉及一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法。该催化剂的吸附-光催化协同效应对于污染物的降解具有显著作用。
背景技术
当今社会正在高速发展,随之而来的工业化给这个有限且已经负担过重的
世界带来了巨大的压力,其中也括日益严重的水环境污染问题。这些废水中含难以降解的污染物如重金属、有机无机化合物和生物有机物等难以自然降解,会在环境中持续存在,在排放后很长时间内继续造成危害。因此,越来越多的学者将注意力转移至废水处理上,并设计、开发高效的技术来处理实际问题,以解决生态环境问题。
半导体的光催化技术是一种具有温和反应条件、简便制备工艺、低能量消耗、高反应速率的有前景的高级氧化技术,具有多种优点。近几年来,硫族化合物由于在可见吸收能力、化学稳定性、导电性能、抗光腐蚀等方面具有极为优秀的表现,从而引起研究学者们的关注。改良硫化物的光学性能对于利用光催化技术处理废水并缓解环境问题具有重大意义。
TiO2、GaN和ZnO等传统的光催化剂具有较宽的带隙,只在紫外光区域有光学活性,此外,由于光生电子、空穴的复合速率快,导致它们的量子效率很低,使材料在实际废水处理中的应用和发展就有很大的局限性。被后来的学者广泛研究的SnS2相对而言则具有优良的热稳定性和抗氧化性,并且不易在酸性或中性溶液中发生反应。其带隙值﹣2.2 eV,理论上可以用可见光激发进行光化学氧化还原反应,是一种高效的可见光催化剂。
然而,未经改良的纯SnS2材料的光学性能依旧很差,不能应用于实际问题中。本发明涉及一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备,能有效实现光生电子-空穴对的高效分离、转移与迁移,具有较好的稳定性以及较强的可见光吸收。除此之外,该催化剂同样具有很好的吸附效果。AgIn5S8/SnS2催化剂的吸附-光催化协同效应对于污染物的降解具有显著作用。
发明内容
本发明的目的在于针对现有光催化剂带隙能较大、仅在紫外光区相应、利用率差等缺点,提出一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂。这种光催化剂具有化学性质稳定、较强光吸收、高吸附-光催化降解污染物能力等优点。
本发明的目的通过以下技术方案实现。
一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于,具体步骤如下:
(1)将一定量的无机锡源、无机铟源和无机银源作为原料在持续磁力搅拌的条件下分散于60 mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2)依次将硫代乙酰胺和柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60 ℃下干燥24 h后即可得到AgIn5S8/SnS2固溶体催化剂。
进一步地,上述的具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述锡源为五水合氯化锡(SnCl4·5H2O)。
进一步地,上述的具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述铟源为四水合氯化铟(InCl3·4H2O)。
进一步地,上述的具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述银源为硝酸银(AgNO3)。
进一步地,上述的具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述锡源与铟源的摩尔比为200:9。
进一步地,上述的具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述AgNO3的质量可为0.01 g、0.02 g、0.03 g、0.04 g、0.05 g等。
所述光催化剂是用少量AgIn5S8掺杂SnS2来制备光催化剂。
本发明的有益效果是,本发明的具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法存在以下优点:
(1)本发明光催化剂的制备方法为水热反应,反应条件易达到,操作简易,能耗低,适用性广;
(2)本发明可以通过调控银源的用量,调控生成的固溶体催化剂AgIn5S8/SnS2,使其具有高的吸附能力和光降解能力;
(3)本发明制备的光催化剂的化学性质稳定,具有较高的吸附能力、可见光下较强的光吸收和光催化降解能力。
附图说明
图1为本发明的实施例1、实施例2和实施例5中通过调控银源含量而制备的AgIn5S8/SnS2固溶体催化剂的XRD图谱。其中,a:纯SnS2;b:纯AgIn5S8;c:(0.8%)AgIn5S8/SnS2。
图2为本发明的实施例1、例2和例5中所制备光催化剂的漫反射图及带隙能图谱。
图3为本发明的实施例1、例2和例5中所制备光催化剂的氮气吸附-脱附及孔径分布曲线图。
图4为本发明的实施例1、例2和例5中所制备的光催化剂的可见光下降解四环素的曲线图。
具体实施方式
以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1
(1)将3.5 g SnCl4·5H2O在持续磁力搅拌的条件下分散于60 mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2)依次将2.254 g(30 mmol)的硫代乙酰胺和1.921 g(10 mmol)柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60 ℃下干燥24 h。即可得到AgIn5S8/SnS2固溶体催化剂。
实施例2
(1)将0.05 g AgNO3、4.5 g InCl3·5H2O和0.45 g硫代乙酰胺在持续磁力搅拌的条件下分散于60mL去离子水中,室温下搅拌2 h,得到淡黄色混合溶液;
(2)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60℃下干燥24 h。即可得到AgIn5S8/SnS2固溶体催化剂。
实施例3
(1)将3.5 g SnCl4·5H2O、0.01 g AgNO3和0.15 g InCl3·5H2O在持续磁力搅拌的条件下分散于60 mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2)依次将2.254 g(30 mmol)的硫代乙酰胺和1.921 g(10 mmol)柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60 ℃下干燥24 h。即可得到AgIn5S8/SnS2固溶体催化剂。
实施例4
(1)将3.5 g SnCl4·5H2O、0.02 g AgNO3和0.15 g InCl3·5H2O在持续磁力搅拌的条件下分散于60mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2)依次将2.254 g(30 mmol)的硫代乙酰胺和1.921 g(10 mmol)柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60 ℃下干燥24 h。即可得到AgIn5S8/SnS2固溶体催化剂。
实施例5
(1)将3.5 g SnCl4·5H2O、0.03 g AgNO3和0.15 g InCl3·5H2O在持续磁力搅拌的条件下分散于60mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2)依次将2.254 g(30 mmol)的硫代乙酰胺和1.921 g(10 mmol)柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60 ℃下干燥24 h。即可得到AgIn5S8/SnS2固溶体催化剂。
实施例6
(1)将3.5 g SnCl4·5H2O、0.04 g AgNO3和0.15 g InCl3·5H2O在持续磁力搅拌的条件下分散于60mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2)依次将2.254 g(30 mmol)的硫代乙酰胺和1.921 g(10 mmol)柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60 ℃下干燥24 h。即可得到AgIn5S8/SnS2固溶体催化剂。
实施例7
(1)将3.5 g SnCl4·5H2O、0.05 g AgNO3和0.15 g InCl3·5H2O在持续磁力搅拌的条件下分散于60 mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2)依次将2.254 g(30 mmol)的硫代乙酰胺和1.921 g(10 mmol)柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3)将充分反应后的溶液转移至反应釜中,在150 ℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 m滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60 ℃下干燥24 h。即可得到AgIn5S8/SnS2固溶体催化剂。
图1为本发明的实施例1、实施例2和实施例5中通过调控银源含量而制备的AgIn5S8/SnS2固溶体催化剂的XRD图谱。其中曲线 a: 纯SnS2(银源含量为0 g);曲线b:纯AgIn5S8(锡源含量为0 g);曲线c: (0.8%)AgIn5S8/SnS2(银源含量为0.04 g)。对比样品的XRD图谱可知,(0.8%)AgIn5S8/SnS2的峰形和纯SnS2相似,表明成功合成SnS2,由于AgIn5S8含量极少,所以并没有明显表现出AgIn5S8的峰形,但是与纯SnS2的峰形比较,复合材料的峰形明显平缓,表明合成影响了复合材料的晶型结构。
图2为本发明的实施例1、实施例2和实施例5中所制备光催化剂的漫反射图及带隙能图谱。由图可知,纯SnS2和纯AgIn5S8对可见光的响应强度明显小于(0.8%)AgIn5S8/SnS2复合材料,这种合成方法拓宽了催化剂对可见光的响应,使其禁带宽度变小。
图3为本发明的实施例1、实施例2和实施例5中所制备光催化剂的氮气吸附-脱附及孔径分布曲线,由图可知,纯SnS2和纯AgIn5S8的比表面积分别为65.70 m2/g和20.49 m2/g,而(0.8%)AgIn5S8/SnS2复合材料的比面积为99.48 m2/g,远大于纯材料,这说明随着AgIn5S8的掺杂,材料表面和内部的结构发生变化,使材料具有更好的吸附性能和光催化性能。
图4为本发明的实施例1、实施例2和实施例5中所制备的光催化剂的可见光下降解四环素的曲线,由图可知, AgIn5S8的掺杂极大效率的提高了材料的吸附性能以及光催化活性。
以上仅就本发明的最佳实施例作了说明,但不能理解为是对权利要求的限制。本发明不仅局限于以上实施例,其具体结构允许有变化。凡在本发明独立权利要求的保护范围内所作的各种变化均在本发明保护范围内。
Claims (6)
1.一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于,具体步骤如下:
(1) 将一定量的无机锡源、无机铟源和无机银源作为原料在持续磁力搅拌的条件下分散于60 mL去离子水中,室温下搅拌30分钟,得到淡黄色混合溶液;
(2) 依次将硫代乙酰胺和柠檬酸缓慢加入上述混合溶液中,室温下磁力搅拌2 h;
(3) 将充分反应后的溶液转移至反应釜中,在150℃的温度下水热反应12小时,反应完毕后自然冷却到室温,经0.22 μm滤膜真空过滤,再用去离子水和无水乙醇多次洗涤,在60℃下干燥24 h后即可得到AgIn5S8/SnS2固溶体催化剂。
2.根据权利要求1所述的一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述锡源为五水合氯化锡 。
3.根据权利要求1所述的一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述铟源为四水合氯化铟。
4.根据权利要求1所述的一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述银源为硝酸银。
5.根据权利要求1所述的一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:锡源与铟源的摩尔比为200: 9。
6.根据权利要求4所述的一种具有吸附-光催化协同效应的AgIn5S8/SnS2固溶体催化剂的制备方法,其特征在于:所述硝酸银的质量为0.01 g、0.02 g、0.03 g、0.04 g或0.05 g。
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