CN114377688B - 一种高效烟气脱硝催化剂及其制备方法 - Google Patents
一种高效烟气脱硝催化剂及其制备方法 Download PDFInfo
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B01D—SEPARATION
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- B01D53/34—Chemical or biological purification of waste gases
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Abstract
本发明涉及一种烟气脱硝催化剂，利用常压加热条件下制备得到薄片状的B掺杂FeMnO3，纳米晶型ZnMn2O4均匀分散于纳米片上，具有较高的比表面积，利于NOx在材料表面的吸附，B元素掺杂不仅影响材料形貌，同时有利于材料电子的传递，原材料简单，制备工艺简单，成本低廉，在燃煤电厂烟气脱硝、汽车尾气处理有潜在的应用价值。
Description
技术领域
本发明属于烟气脱硝领域，尤其是一种烟气脱硝催化剂。
背景技术
近年来，随着汽车保有量的持续增加以及化石能源的燃烧，氮氧化物的排放量逐年递增。氮氧化物的排放对大气环境造成破坏，引发臭氧层空洞，酸雨和光化学烟雾等，严重威胁着人类身心健康。选择性催化还原法是利用催化剂在一定温度下将烟气中的含氮氧化物选择性还原为氮气，目前已经成为重要的脱硝技术之一，越来越受到研究者的关注。
专利文献CN105618032A公开了一种负载型锰基低温脱硝催化剂及其制备方法，该制备方法具体包括以下步骤：1)将铈盐或铁盐或钴盐和锰盐溶于水中形成金属盐溶液，将非离子表面活性剂、助表面活性剂和有机溶剂加入到金属盐溶液中，搅拌至澄清，得到微乳液；所述的水、非离子表面活性剂、助表面活性剂和有机溶剂的摩尔比例为1：0.03～0.6：0.1～1.2：1～5；2)将钛溶胶加入到所述的微乳液中，搅拌，然后用pH调节剂调节其pH值为8～11，加热，得到干凝胶；3)将所述的干凝胶研磨、煅烧，得到脱硝催化剂。专利文献CN112844404A公开了以TiO2纳米管为载体，并负载MnOx、CeO2、Fe2O3，以质量百分比计，各组分的质量含量为：MnOx：3.0-15％，CeO2：2.0-12％，Fe2O3：3.0-15％，TiO2纳米管：58-90％。专利文献CN104525211A公开了TiO2-CuO/CeO2负载型催化剂的方法，它是将一定量的钛酸丁酯和硝酸铜在冰水浴中混合均匀，然后加入一定量的CeO2继续搅拌得到悬浊液，最后经过油浴蒸干、干燥、焙烧制得TiO2-CuO/CeO2催化剂。但是，目前的脱硝催化剂整体脱硝性能不佳，难以满足工业化需求。
发明内容
本发明的目的在于提供一种高效廉价且具有优异脱硝性能的薄片催化剂及其制备方法。
一种高效的烟气脱硝催化材料，其特征在于，采用如下工艺制备：在100mL的去离子水中加入(2-8)mmol硝酸铁、(2-8)mmol硝酸锰以及(0.2-1)mmol的硼酸，搅拌10-20min混合均匀，随后加入10-20ml乙二醇的作为助溶剂以及30-80mg的聚乙二醇，将反应前驱体溶液加热回流，加热回流的温度为80-100℃，反应时间为4-5h，反应结束后自然冷却至室温，把将产物进行离心，并用乙醇和去离子水清洗三次，干燥；将得到的产物于400-500摄氏度条件下热处理2-3h，从而得到薄片结构的B掺杂FeMnO3；
(2)将薄片状的FeMnO3溶于100ml去离子水中，随后加入(0.5-1)mmol硝酸锰、(0.25-0.5)mmol硝酸锌和(0.5-1)mmol四丁基溴化铵，采用氨水调控pH为9-10，将混合液转入高压反应釜中，水热反应，将产物离心分离，并用去离子水和乙醇洗涤3次，于400-500摄氏度条件下热处理2-3h，得到薄片FeMnO3负载纳米晶型ZnMn2O4的复合材料。
优选的，水热反应温度为120-160摄氏度；
优选的，薄片结构的FeMnO3尺寸为2-3微米。
本发明有益的技术效果：
本发明综合调控实验条件制备得到薄片状的B掺杂FeMnO3，纳米晶型ZnMn2O4均匀分散于纳米片上，具有较高的比表面积，有助于NOx在材料表面的吸附，B元素掺杂不仅影响材料形貌，同时有利于材料电子的传递，原材料简单，制备工艺简单，成本低廉，在燃煤电厂烟气脱硝、汽车尾气处理有潜在的应用价值。
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)在100mL的去离子水中加入3mmol硝酸铁、3mmol硝酸锰以及0.2mmol的硼酸，搅拌12min混合均匀，随后加入10ml乙二醇的作为助溶剂以及30mg的聚乙二醇，将反应前驱体溶液加热回流，加热回流的温度为80℃，反应时间为4h，反应结束后自然冷却至室温，把将产物进行离心，并用乙醇和去离子水清洗三次，干燥；将得到的产物于400摄氏度条件下热处理2h，从而得到薄片结构的B掺杂FeMnO3；
(2)将薄片状的FeMnO3溶于100ml去离子水中，随后加入0.5mmol硝酸锰、0.25mmol硝酸锌和0.6mmol四丁基溴化铵，采用氨水调控pH为9，将混合液转入高压反应釜中，水热反应，水热温度为130摄氏度，水热时间为10h，将产物离心分离，并用去离子水和乙醇洗涤3次，于400摄氏度条件下热处理3h，得到薄片FeMnO3负载纳米晶型ZnMn2O4的复合材料。
对比例1
在100mL的去离子水中加入3mmol硝酸铁、3mmol硝酸锰以及0.2mmol的硼酸，搅拌12min混合均匀，随后加入10ml乙二醇的作为助溶剂以及30mg的聚乙二醇，将反应前驱体溶液加热回流，加热回流的温度为80℃，反应时间为4h，反应结束后自然冷却至室温，把将产物进行离心，并用乙醇和去离子水清洗三次，干燥；将得到的产物于400摄氏度条件下热处理2h，从而得到薄片结构的B掺杂FeMnO3；
对比例2
在100ml去离子水中加入0.5mmol硝酸锰、0.25mmol硝酸锌和0.6mmol四丁基溴化铵，采用氨水调控pH为9，将混合液转入高压反应釜中，水热反应，水热温度为130摄氏度，水热时间为10h，将产物离心分离，并用去离子水和乙醇洗涤3次，于400摄氏度条件下热处理3h，得到ZnMn2O4。
对比例3
(1)在100mL的去离子水中加入3mmol硝酸铁、3mmol硝酸锰，搅拌12min混合均匀，随后加入10ml乙二醇的作为助溶剂以及30mg的聚乙二醇，将反应前驱体溶液加热回流，加热回流的温度为80℃，反应时间为4h，反应结束后自然冷却至室温，把将产物进行离心，并用乙醇和去离子水清洗三次，干燥；将得到的产物于400摄氏度条件下热处理2h，从而得到薄片结构的FeMnO3；
(2)将薄片状的FeMnO3溶于100ml去离子水中，随后加入0.5mmol硝酸锰、0.25mmol硝酸锌和0.6mmol四丁基溴化铵，采用氨水调控pH为9，将混合液转入高压反应釜中，水热反应，水热温度为130摄氏度，水热时间为10h，将产物离心分离，并用去离子水和乙醇洗涤3次，于400摄氏度条件下热处理3h，得到薄片FeMnO3负载纳米晶型ZnMn2O4的复合材料。
将实施利1和对比例1-3中制得的催化材料放入固定床反应器中。随后于固定床反应器中通入模拟烟气，烟气成分为NO500ppm，NH3500ppm，O2 5％，氮气作为平衡气体，控制空速为6000L/h-1，测试不同温度下的脱硝率，结果如下表。
表1
| 实施例1 | 对比例1 | 对比例2 | 对比例3 | |
| 150℃ | 97.2％ | 90.4％ | 86.3％ | 92.1％ |
| 200℃ | 99.8％ | 93.6％ | 93.9％ | 96.4％ |
| 250℃ | 99.8％ | 98.1％ | 97.6％ | 98.3％ |
| 300℃ | 99.7％ | 98.1％ | 98.0％ | 98.6％ |
| 350℃ | 99.6％ | 94.8％ | 95.8％ | 94.6％ |
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。
Claims (3)
1.一种高效的烟气脱硝催化材料，其特征在于，采用如下工艺制备：在100mL的去离子水中加入(2-8)mmol硝酸铁、(2-8)mmol硝酸锰以及(0.2-1)mmol的硼酸，搅拌10-20min混合均匀，随后加入10-20ml乙二醇的作为助溶剂以及30-80mg的聚乙二醇，将反应前驱体溶液加热回流，加热回流的温度为80-100℃，反应时间为4-5h，反应结束后自然冷却至室温，把将产物进行离心，并用乙醇和去离子水清洗三次，干燥；将得到的产物于400-500摄氏度条件下热处理2-3h，从而得到薄片结构的B掺杂FeMnO3；
(2)将薄片状的B掺杂FeMnO3溶于100ml去离子水中，随后加入(0.5-1)mmol硝酸锰、(0.25-0.5)mmol硝酸锌和(0.5-1)mmol四丁基溴化铵，采用氨水调控pH为9-10，将混合液转入高压反应釜中，水热反应，将产物离心分离，并用去离子水和乙醇洗涤3次，于400-500摄氏度条件下热处理2-3h，得到薄片B掺杂FeMnO3负载纳米晶型ZnMn2O4的复合材料。
2.根据权利要求1所述的一种高效的烟气脱硝催化材料，水热反应温度为120-160摄氏度。
3.根据权利要求1所述的一种高效的烟气脱硝催化材料，薄片结构的B掺杂FeMnO3尺寸为2-3微米。
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