CN107442140A - 一种二硫化钼负载铁锰氧化物催化剂的制备方法 - Google Patents
一种二硫化钼负载铁锰氧化物催化剂的制备方法 Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- WQHONKDTTOGZPR-UHFFFAOYSA-N [O-2].[O-2].[Mn+2].[Fe+2] Chemical compound [O-2].[O-2].[Mn+2].[Fe+2] WQHONKDTTOGZPR-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 8
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 239000011572 manganese Substances 0.000 claims abstract description 7
- XTFPYEOBVLWDDP-UHFFFAOYSA-N CCO.CC(N)=S Chemical compound CCO.CC(N)=S XTFPYEOBVLWDDP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 239000000356 contaminant Substances 0.000 abstract description 3
- 238000004042 decolorization Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052961 molybdenite Inorganic materials 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- YYYARFHFWYKNLF-UHFFFAOYSA-N 4-[(2,4-dimethylphenyl)diazenyl]-3-hydroxynaphthalene-2,7-disulfonic acid Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C(S(O)(=O)=O)=CC2=CC(S(O)(=O)=O)=CC=C12 YYYARFHFWYKNLF-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 238000000034 method Methods 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- -1 under nanoscale Chemical class 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
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Abstract
本发明公开了一种二硫化钼负载铁锰氧化物催化剂的制备方法，步骤如下：将10~15 g钼酸铵加入到50~100 mL浓度为1~5 mg/L的硫代乙酰胺乙醇溶液中，60~70℃水浴中搅拌5～30分钟，再加入硝酸亚铁10~50 mmol和硝酸锰20~100 mmol，其中Fe/Mn=1∶2（摩尔比），加入适量NaOH溶液至pH为10～11，沉淀完全，置于水热反应器中，180~200℃下，反应5~10 h，过滤得到固体，洗涤至中性，80℃烘干，500~650℃焙烧2 h，即得到一种二硫化钼负载铁锰氧化物催化剂。铁锰相互复合形成具有异质结结构的化合物，并且，二硫化钼的负载，可以帮助铁锰氧化物分散，并相互促进，提高污染物降解速度。
Description
技术领域
本发明涉及环境污染控制新材料领域，尤其涉及一种二硫化钼负载铁锰氧化物催化剂的制备方法。
背景技术
随着科技的发展，来自工农业生产中产生的毒害有机污染物严重威胁着环境和人类的健康，寻求一种新型高效的环境治理技术具有重要的意义。光催化技术因其节能、高效、污染物降解彻底、无二次污染优点，目前已成为一种具有重要应用前景的新兴环境治理技术。近年来，新型高效的可见光光催化剂的研制成为光催化技术中的一个重要研究内容，其中具有表面等离子共振效应的光催化材料，因其独特的表面物理化学性质和高效的可见光光催化性能，成为研究的热点之一。但纳米颗粒物容易团聚，团聚后表面积大大减小，效果减弱。
二硫化钼是一种由钼和硫两种元素组成的化合物，化学式为MoS2。这种化合物属于过渡金属二硫族化合物，它有银黑色光泽，在自然界中以辉钼矿的形式存在，辉钼矿是最常见的含钼元素矿石。二硫化钼晶体通常情况下以粉末形式存在，它不溶于稀酸也不易被氧化。从外表上来看，二硫化钼和石墨很像，以其低摩擦系数和高坚固性常被用作固体润滑剂。块状二硫化钼固体是一种和硅类似的抗磁性间接带隙半导体，能带间隙为1.23eV。
铁和锰是自然界中常见的金属元素。铁、锰金属氧化物的应用是当前矿物学研究的一个主要方面，矿物-水界面反应对环境中物质的循环和元素的地球化学过程起着十分重要的作用。在沉积环境中，带有表面电荷、含有变价元素的天然铁锰氧化物是典型的潜在氧化剂，能与还原性的有机化合物发生反应，从而减轻对动植物的毒害。但在水处理方面，铁锰氧化物具有广泛的应用前景。特别是纳米尺度下的铁锰氧化物，可以提高降解速度。
发明内容
本发明的目的是为克服现有技术的不足，提供一种二硫化钼负载铁锰氧化物催化剂的制备方法。
本发明采用的技术方案是依次包括如下步骤：将10~15 g钼酸铵加入到50~100 mL浓度为1~5 mg/L的硫代乙酰胺乙醇溶液中，60~70℃水浴中搅拌5～30分钟，再加入硝酸亚铁10~50 mmol和硝酸锰20~100 mmol，其中Fe/Mn= 1∶2（摩尔比），加入适量NaOH溶液至pH为10～11，沉淀完全，置于水热反应器中，180~200℃下，反应5~10 h，过滤得到固体，洗涤至中性，80℃烘干，500~650℃焙烧2 h，即得到一种二硫化钼负载铁锰氧化物催化剂。
本发明的优点是：1. 铁锰相互复合形成具有异质结结构的化合物。2. 二硫化钼的负载，可以帮助铁锰氧化物分散，并相互促进，提高污染物降解速度。
具体实施方式
以下进一步提供本发明的3个实施例：
实施例1
将15 g钼酸铵加入到100 mL浓度为5 mg/L的硫代乙酰胺乙醇溶液中，60℃水浴中搅拌30分钟，再加入硝酸亚铁50 mmol和硝酸锰100 mmol，其中Fe/Mn= 1∶2（摩尔比），加入适量NaOH溶液至pH为11，沉淀完全，置于水热反应器中， 200℃下，反应10 h，过滤得到固体，洗涤至中性，80℃烘干，500℃焙烧2 h，即得到一种二硫化钼负载铁锰氧化物催化剂。
将制得的二硫化钼负载铁锰氧化物催化剂用于处理含亚甲基蓝废水： 0.5 g二硫化钼负载铁锰氧化物催化剂加入到200 mL 浓度为55 mg/L 的亚甲基蓝废水中，在120 W的LED灯照射下，反应100 min，脱色率为95.2%，催化剂分离重复利用5次后，同样条件下，反应100min，脱色率为92.1%。
实施例2
将10 g钼酸铵加入到50 mL浓度为1mg/L的硫代乙酰胺乙醇溶液中，60℃水浴中搅拌5分钟，再加入硝酸亚铁10 mmol和硝酸锰20 mmol，其中Fe/Mn= 1∶2（摩尔比），加入适量NaOH溶液至pH为10，沉淀完全，置于水热反应器中，180℃下，反应5 h，过滤得到固体，洗涤至中性，80℃烘干，650℃焙烧2 h，即得到一种二硫化钼负载铁锰氧化物催化剂。
将制得的二硫化钼负载铁锰氧化物催化剂用于处理含酸性大红废水： 0.5 g二硫化钼负载铁锰氧化物催化剂加入到300 mL 浓度为55 mg/L 的酸性大红废水中，在120 W的LED灯照射下，反应100 min，脱色率为94.7%，催化剂分离重复利用5次后，同样条件下，反应100min，脱色率为93.7%。
实施例3
将12 g钼酸铵加入到80 mL浓度为4 mg/L的硫代乙酰胺乙醇溶液中，70℃水浴中搅拌20分钟，再加入硝酸亚铁50 mmol和硝酸锰100 mmol，其中Fe/Mn= 1∶2（摩尔比），加入适量NaOH溶液至pH为10，沉淀完全，置于水热反应器中，180℃下，反应80 h，过滤得到固体，洗涤至中性，80℃烘干，650℃焙烧2 h，即得到一种二硫化钼负载铁锰氧化物催化剂。
将制得的二硫化钼负载铁锰氧化物催化剂用于处理含罗丹明B废水：0.5 g二硫化钼负载铁锰氧化物催化剂加入到300 mL 浓度为55 mg/L 的罗丹明B废水中，在120 W的LED灯照射下，反应100 min，脱色率为96.2%，催化剂分离重复利用5次后，同样条件下，反应100min，脱色率为91.9%。
Claims (1)
1.一种二硫化钼负载铁锰氧化物催化剂的制备方法，其特征是依次包括如下步骤： 将10~15 g钼酸铵加入到50~100 mL浓度为1~5 mg/L的硫代乙酰胺乙醇溶液中，60~70℃水浴中搅拌5～30分钟，再加入硝酸亚铁10~50 mmol和硝酸锰20~100 mmol，其中Fe/Mn= 1∶2（摩尔比），加入适量NaOH溶液至pH为10～11，沉淀完全，置于水热反应器中，180~200℃下，反应5~10 h，过滤得到固体，洗涤至中性，80℃烘干，500~650℃焙烧2 h，即得到一种二硫化钼负载铁锰氧化物催化剂。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142112A (zh) * | 2020-09-28 | 2020-12-29 | 湖北富邦科技股份有限公司 | 一种铁锰硫三元微米材料及其制备方法和应用 |
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