CN108187695A - 一种二硫化钼负载铜钼氧化物催化剂的制备方法 - Google Patents
一种二硫化钼负载铜钼氧化物催化剂的制备方法 Download PDFInfo
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- molybdenum disulfide
- molybdenum
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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 18
- PVGRIQYJDHKRFC-UHFFFAOYSA-N copper;oxomolybdenum Chemical compound [Cu].[Mo]=O PVGRIQYJDHKRFC-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 8
- 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
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000004042 decolorization Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 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 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052961 molybdenite Inorganic materials 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 molybdenum disulfide Copper-molybdenum oxide Chemical compound 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 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
- 238000003933 environmental pollution control Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 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
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
本发明公开了一种二硫化钼负载铜钼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，2~5 g二氯化铜，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铜钼氧化物催化剂。本发明的优点是：1.二硫化钼和铜钼氧化物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，可以帮助铜钼氧化物分散，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铜钼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。
氧化钼能隙较小且光生电子空穴对的复合率较低，在阳光下有较好的光催化活性，但在废水处理方面仍有提高可能。氧化铜作为催化剂活性组分在催化各种氧化反应中具有很高的催化活性，但作为催化剂时，效能有待提高。
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铜钼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，2~5 g二氯化铜，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铜钼氧化物催化剂。
本发明的优点是：1. 二硫化钼和铜钼氧化物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，可以帮助铜钼氧化物分散，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，70℃水浴中搅拌30分钟，5 g二氯化铜，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， 650℃焙烧2 h，即得到一种二硫化钼负载铜钼氧化物催化剂。
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40 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98.4%，催化剂分离重复利用5次后，同样条件下，反应100 min，脱色率为92.8%。
实施例2
将10 g钼酸铵加入到50 mL浓度为1 mg/L的硫代乙酰胺乙醇溶液中，60℃水浴中搅拌5分钟，2 g二氯化铜，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，500℃焙烧2 h，即得到一种二硫化钼负载铜钼氧化物催化剂。
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40 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97.1%，催化剂分离重复利用5次后，同样条件下，反应100 min，脱色率为91.2%。
实施例3
将12 g钼酸铵加入到80 mL浓度为2 mg/L的硫代乙酰胺乙醇溶液中，70℃水浴中搅拌25分钟，3 g二氯化铜，加入适量NaOH溶液至pH为11，沉淀完全，置于水热反应器中，180℃下，反应10 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铜钼氧化物催化剂。
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40 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96.8%，催化剂分离重复利用5次后，同样条件下，反应100 min，脱色率为92.1%。
Claims (1)
1.一种二硫化钼负载铜钼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，2~5 g二氯化铜，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铜钼氧化物催化剂。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112439422A (zh) * | 2020-12-07 | 2021-03-05 | 岭南师范学院 | 一种Cu3Mo2O9/BiVO4纳米异质结构复合材料及其制备方法和应用 |
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| WO2005023416A1 (en) * | 2003-04-07 | 2005-03-17 | Board Of Regents, The University Of Texas System | Molybdenum sulfide/carbide catalysts |
| CN106732668A (zh) * | 2016-11-18 | 2017-05-31 | 中国计量大学 | 一种花状二硫化钼/氧化铜复合纳米材料的水热制备方法 |
| CN106904655A (zh) * | 2017-03-22 | 2017-06-30 | 陕西科技大学 | 一种钼酸铜纳米颗粒及其制备方法和应用 |
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- 2017-09-26 CN CN201710885177.8A patent/CN108187695A/zh active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005023416A1 (en) * | 2003-04-07 | 2005-03-17 | Board Of Regents, The University Of Texas System | Molybdenum sulfide/carbide catalysts |
| CN106732668A (zh) * | 2016-11-18 | 2017-05-31 | 中国计量大学 | 一种花状二硫化钼/氧化铜复合纳米材料的水热制备方法 |
| CN106904655A (zh) * | 2017-03-22 | 2017-06-30 | 陕西科技大学 | 一种钼酸铜纳米颗粒及其制备方法和应用 |
Non-Patent Citations (2)
| Title |
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| HONGLIN LI,ET AL: "High photocatalytic performance of a type-II α-MoO3@MoS2 heterojunction: from theory to experiment", 《PHYSICAL CHEMISTRY CHEMICAL PHYSICS》 * |
| JUAN XIA,ET AL: "Highly monodisperse Cu3Mo2O9 micropompons with excellent performance in photocatalysis, photocurrent response and lithium storage", 《RSC ADVANCES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112439422A (zh) * | 2020-12-07 | 2021-03-05 | 岭南师范学院 | 一种Cu3Mo2O9/BiVO4纳米异质结构复合材料及其制备方法和应用 |
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Application publication date: 20180622 |