CN114054038B - 一种高效降解污水有机污染物的复合材料 - Google Patents
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Abstract
本发明涉及一种高效降解污水有机污染物的复合材料，采用如下工艺制备：(1)将一定摩尔比的硝酸铜和硝酸锰溶解在乙二醇溶剂中，接着加入醋酸铵、柠檬酸，超声混合均匀，将混合液转入高压反应釜中进行溶剂热反应，随后将产物进行热处理从而获得花状结构的CuMn2O4；(2)将步骤(1)制备得到的CuMn2O4加入去离子水中，随后加入Co盐、Ti盐、氨水和聚乙二醇‑400，搅拌条件下在100‑200摄氏度反应10‑20h，将产物继续进行热处理，得到花状结构的CuMn2O4负载纳米CoTiO3的复合材料。
Description
技术领域
本发明涉及环保领域，尤其涉及一种花状复合催化剂及其制备方法。
背景技术
近些年来，随着社会经济的不断发展，能源开发对环境产生不同程度的影响，环境问题日益严重，农药和染料等对水源的污染严重威胁人类身体健康。
光催化降解法是一种高效的降解有机污染物的方法，其可以将水体当中的有机污染物高效的分解成无害物质(如水和二氧化碳)，目前，常见的光催化剂有TiO2、ZnO、过渡金属硫化物等，但是单一的光催化材料的光生电子和空穴容易复合，并且比表面积不高、容易发生团聚，因此，开发成本低廉、结构稳定的高效催化剂是光催化技术应用的核心所在。
发明内容
针对现有技术中存在的问题，本发明的目的在于提供一种CuMn2O4/CoTiO3复合光催化剂，该催化剂制备工艺简单，可见光光催化活性高，且重复使用性良好。
一种高效降解污水有机污染物的复合材料，其特征在于，采用如下工艺制备：
(1)将一定摩尔比的硝酸铜和硝酸锰溶解在乙二醇溶剂中，接着加入醋酸铵、柠檬酸，超声混合均匀，将混合液转入高压反应釜中进行溶剂热反应，随后将产物进行热处理从而获得花状结构的CuMn2O4；
(2)将步骤(1)制备得到的CuMn2O4加入去离子水中，随后加入Co盐、Ti盐和氨水和聚乙二醇-400，搅拌条件下在100-200摄氏度反应10-20h，将产物继续进行热处理，得到花状结构的CuMn2O4负载纳米CoTiO3的复合材料。
硝酸铜和硝酸锰、醋酸铵和柠檬酸的摩尔比为1：2：(1-2)：(1-2)；
溶剂热的反应温度为180-200摄氏度，反应时间为10-20h；
步骤(1)-(2)的热处理温度为300-400摄氏度，热处理时间为30-60min；
Co盐、Ti盐为硝酸钴、钛酸四乙酯；加入氨水调节pH为8-9，硝酸钴、钛酸四乙酯摩尔比为1：1；硝酸钴和聚乙二醇-400的加入质量比为1：(0.2-0.8)。
有益效果：
本申请通过以乙二醇作为溶剂，在溶剂热反应中引入醋酸铵和柠檬酸，从而获得花状结构的CuMn2O4，其高比表面积结构容易捕获有机污染物，极大的增多了催化反应位点，将其作为载体负载纳米CoTiO3，聚乙二醇-400避免了晶粒的长大利于形成纳米结构，CuMn2O4和CoTiO3二者可形成异质结，CuMn2O4表面的光生电子可以转移到CoTiO3，增强了电子传输速率，抑制了光生电子与空穴的复合率，二者协同提高光催化降解有机物的效率，弥补了单一光催化材料的不足。
附图说明
图1为本申请制备得到的实施例1的复合材料的SEM图。
具体实施方式
实施例1
(1)将10mmol硝酸铜和20mmol硝酸锰溶解在80ml乙二醇溶剂中，接着加入10mmol醋酸铵、10mmol柠檬酸，100w的超声功率超声10min，将混合液转入高压反应釜中进行溶剂热反应，溶剂热温度为180摄氏度，反应温度为10h，随后将产物在350摄氏度下热处理1h从而获得花状结构的CuMn2O4；
(2)将步骤(1)制备得到的CuMn2O4加入50ml去离子水中，随后加入3mmol硝酸钴、钛酸四乙酯和聚乙二醇-400，硝酸钴和聚乙二醇-400的加入质量比为1：0.4，加入氨水调节pH为9，搅拌条件下在120摄氏度反应10h，将产物继续在350摄氏度下热处理1h，得到花状结构的CuMn2O4负载纳米CoTiO3的复合材料。
对比例1
将10mmol硝酸铜和20mmol硝酸锰溶解在80ml乙二醇溶剂中，接着加入10mmol醋酸铵、10mmol柠檬酸，100w的超声功率超声10min，将混合液转入高压反应釜中进行溶剂热反应，溶剂热温度为180摄氏度，反应温度为10h，随后将产物在350摄氏度下热处理1h从而获得花状结构的CuMn2O4。
对比例2
在50ml去离子水中依次加入3mmol硝酸钴、钛酸四乙酯和聚乙二醇-400，硝酸钴和聚乙二醇-400的加入质量比为1：0.4，加入氨水调节pH为9，搅拌条件下在120摄氏度反应10h，将产物继续在350摄氏度下热处理1h，得到CoTiO3材料。
将实施例1以及对比例1-2的光催化剂用于光催化降解实验。具体方法如下：
取15mg复合材料加入到10ml，浓度为3M的罗丹明B的水溶液中，在400w的氙灯照射下搅拌照射1、2h，随后检测罗丹明B降解后的浓度，并计算光降解效率。
| 光降解率 | 实施例1 | 对比例1 | 对比例2 |
| 1h后 | 87.5％ | 76.8％ | 30.9％ |
| 2h后 | 95.4％ | 84.1％ | 40.9％ |
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等同物限定。
Claims (2)
1.一种降解有机污染物的复合材料，其特征在于，采用如下工艺制备：
(1)将一定摩尔比的硝酸铜和硝酸锰溶解在乙二醇溶剂中，接着加入醋酸铵、柠檬酸，超声混合均匀，将混合液转入高压反应釜中进行溶剂热反应，随后将产物进行热处理从而获得花状结构的CuMn2O4；
(2)将步骤(1)制备得到的CuMn2O4加入去离子水中，随后加入Co盐、Ti盐和氨水、聚乙二醇-400，搅拌条件下在100-200摄氏度反应10-20h，将产物继续进行热处理，得到花状结构的CuMn2O4负载纳米CoTiO3的复合材料，硝酸铜和硝酸锰、醋酸铵和柠檬酸的摩尔比为1：2：(1-2)：(1-2)，溶剂热的反应温度为180-200摄氏度，反应时间为10-20h；步骤(1)-(2)的热处理温度为300-400摄氏度，热处理时间为30-60min。
2.根据权利要求1所述的一种降解有机污染物的复合材料，Co盐、Ti盐为硝酸钴、钛酸四乙酯；加入氨水调节pH为8-9，硝酸钴、钛酸四乙酯摩尔比为1：1；硝酸钴和聚乙二醇-400的加入质量比为1：(0.2-0.8)。
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| CN101623635A (zh) * | 2009-08-13 | 2010-01-13 | 湖南理工学院 | 一种可见光响应的复合光催化剂及制备方法 |
| CN110813298A (zh) * | 2019-11-06 | 2020-02-21 | 齐鲁工业大学 | 一种钛酸钴@氧化镍核壳光催化材料及其制备方法和应用 |
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| CN107572590A (zh) * | 2017-09-21 | 2018-01-12 | 柳州若思纳米材料科技有限公司 | 一种锰酸铜光催化剂的制备方法 |
| CN107557908B (zh) * | 2017-10-16 | 2019-08-27 | 济南大学 | 一种珠链状CuMn2O4/ZnO复合纤维的制备方法及所得产品 |
| CN113046778B (zh) * | 2021-03-05 | 2022-11-15 | 北京化工大学 | 一种氨刻蚀海胆状球形结构铜锰尖晶石材料及其制备方法和应用 |
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| CN101623635A (zh) * | 2009-08-13 | 2010-01-13 | 湖南理工学院 | 一种可见光响应的复合光催化剂及制备方法 |
| CN110813298A (zh) * | 2019-11-06 | 2020-02-21 | 齐鲁工业大学 | 一种钛酸钴@氧化镍核壳光催化材料及其制备方法和应用 |
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