CN107522233A - 一种硫代钼酸锰催化剂的制备方法 - Google Patents
一种硫代钼酸锰催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 20
- -1 thio molybdic acid Chemical compound 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000011572 manganese Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 230000002045 lasting effect Effects 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 5
- 229910021380 Manganese Chloride Inorganic materials 0.000 abstract description 5
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 229910052748 manganese Inorganic materials 0.000 abstract description 5
- 235000002867 manganese chloride Nutrition 0.000 abstract description 5
- 239000011565 manganese chloride Substances 0.000 abstract description 5
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract description 4
- 239000000356 contaminant Substances 0.000 abstract description 3
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 abstract description 2
- 125000000446 sulfanediyl group Chemical group *S* 0.000 abstract description 2
- 238000004042 decolorization Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000000694 effects Effects 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
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- SCVJRXQHFJXZFZ-KVQBGUIXSA-N 2-amino-9-[(2r,4s,5r)-4-hydroxy-5-(hydroxymethyl)oxolan-2-yl]-3h-purine-6-thione Chemical compound C1=2NC(N)=NC(=S)C=2N=CN1[C@H]1C[C@H](O)[C@@H](CO)O1 SCVJRXQHFJXZFZ-KVQBGUIXSA-N 0.000 description 1
- 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 1
- 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 1
- 238000012271 agricultural production Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002086 nanomaterial Substances 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
- 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
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/006—Compounds containing, besides manganese, two or more other elements, with the exception of oxygen or hydrogen
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
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- 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
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- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
本发明公开了一种硫代钼酸锰催化剂的制备方法，步骤如下：将5~10 g二氯化锰加入到50~100 mL水中配制成溶液，再向该溶液中加入3~4 g钼酸钠，60~70℃水浴中搅拌10～50分钟，持续搅拌中，25℃和常压条件下缓慢通入0.5~6 L硫化氢气体，继续搅拌10~20分钟后，将溶液转移至水热反应器中，180~260℃下，反应5~10 h，过滤得到固体，用蒸馏水洗涤3~5遍，80℃烘干，即得到一种硫代钼酸锰催化剂。利用通入的硫化氢和钼酸根反应，但不完全反应，可以获得不同形态的硫代钼酸锰材料，提高污染物降解效率。
Description
技术领域
本发明涉及环境污染控制新材料领域，尤其涉及一种硫代钼酸锰催化剂的制备方法。
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。
钼酸锰纳米材料是一种重要的功能材料,在发光材料、微波材料、磁性器件、传感器件、催化剂等领域有很广阔的应用市场。硫代钼酸锰具有独特的结构，但单独使用钼酸锰作为光催化剂效果较差，并且无法得到相应的降解效率。
发明内容
本发明的目的是为克服现有技术的不足，提供一种硫代钼酸锰催化剂的制备方法。
本发明采用的技术方案是依次包括如下步骤：将5~10 g二氯化锰加入到50~100mL水中配制成溶液，再向该溶液中加入3~4 g钼酸钠，60~70℃水浴中搅拌10～50分钟，持续搅拌中，25℃和常压条件下缓慢通入0.5~6 L硫化氢气体，继续搅拌10~20分钟后，将溶液转移至水热反应器中，180~260℃下，反应5~10 h，过滤得到固体，用蒸馏水洗涤3~5遍，80℃烘干，即得到一种硫代钼酸锰催化剂。
本发明的优点是：利用通入的硫化氢和钼酸根反应，但不完全反应，可以获得不同形态的硫代钼酸锰材料，提高污染物降解效率。
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10 g二氯化锰加入到100 mL水中配制成溶液，再向该溶液中加入4 g钼酸钠，60~70℃水浴中搅拌50分钟，持续搅拌中，25℃和常压条件下缓慢通入6 L硫化氢气体，继续搅拌20分钟后，将溶液转移至水热反应器中，260℃下，反应10 h，过滤得到固体，用蒸馏水洗涤5遍，80℃烘干，即得到一种硫代钼酸锰催化剂。
0.5 g硫代钼酸锰催化剂加入到100 mL 浓度为25 mg/L 的亚甲基蓝废水中，在120 W的LED灯照射下，反应90 min，脱色率为96.7%，催化剂分离重复利用5次后，同样条件下，反应90 min，脱色率为92.5%。
实施例2
将5 g二氯化锰加入到50 mL水中配制成溶液，再向该溶液中加入3 g钼酸钠，60℃水浴中搅拌10分钟，持续搅拌中，25℃和常压条件下缓慢通入0.5 L硫化氢气体，继续搅拌10分钟后，将溶液转移至水热反应器中，180℃下，反应5 h，过滤得到固体，用蒸馏水洗涤3遍，80℃烘干，即得到一种硫代钼酸锰催化剂。
0.5 g硫代钼酸锰催化剂加入到100 mL 浓度为25 mg/L 的酸性大红废水中，在120 W的LED灯照射下，反应90 min，脱色率为96.7%，催化剂分离重复利用5次后，同样条件下，反应90 min，脱色率为92.8%。
实施例3
将8 g二氯化锰加入到60 mL水中配制成溶液，再向该溶液中加入4 g钼酸钠，70℃水浴中搅拌50分钟，持续搅拌中，25℃和常压条件下缓慢通入3 L硫化氢气体，继续搅拌20分钟后，将溶液转移至水热反应器中，200℃下，反应10 h，过滤得到固体，用蒸馏水洗涤4遍，80℃烘干，即得到一种硫代钼酸锰催化剂。
0.5 g硫代钼酸锰催化剂加入到100 mL 浓度为25 mg/L 的罗丹明B废水中，在120W的LED灯照射下，反应90 min，脱色率为96.9%，催化剂分离重复利用5次后，同样条件下，反应90 min，脱色率为91.5%。
Claims (1)
1.一种硫代钼酸锰催化剂的制备方法，其特征是依次包括如下步骤：将5~10 g二氯化锰加入到50~100 mL水中配制成溶液，再向该溶液中加入3~4 g钼酸钠，60~70℃水浴中搅拌10～50分钟，持续搅拌中，25℃和常压条件下缓慢通入0.5~6 L硫化氢气体，继续搅拌10~20分钟后，将溶液转移至水热反应器中，180~260℃下，反应5~10 h，过滤得到固体，用蒸馏水洗涤3~5遍，80℃烘干，即得到一种硫代钼酸锰催化剂。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616857A (zh) * | 2012-01-16 | 2012-08-01 | 渤海大学 | 一种钼酸锰微晶的制备方法 |
| JP2013256434A (ja) * | 2012-05-14 | 2013-12-26 | Univ Of Yamanashi | 金属酸窒化物の製造法 |
| CN106887346A (zh) * | 2017-03-07 | 2017-06-23 | 信阳师范学院 | 一种钼酸锰多孔纳米管的静电纺丝制备方法及钼酸锰多孔纳米管 |
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- 2017-09-24 CN CN201710870903.9A patent/CN107522233A/zh active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616857A (zh) * | 2012-01-16 | 2012-08-01 | 渤海大学 | 一种钼酸锰微晶的制备方法 |
| JP2013256434A (ja) * | 2012-05-14 | 2013-12-26 | Univ Of Yamanashi | 金属酸窒化物の製造法 |
| CN106887346A (zh) * | 2017-03-07 | 2017-06-23 | 信阳师范学院 | 一种钼酸锰多孔纳米管的静电纺丝制备方法及钼酸锰多孔纳米管 |
Non-Patent Citations (1)
| Title |
|---|
| 魏长平 等: "四硫代钼酸按与四硫代钨酸铵合成方法改进的研究", 《吉林工学院学报》 * |
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