CN107497454A - 一种硫代钨酸锰催化剂的制备方法 - Google Patents
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- 239000002253 acid Substances 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 20
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- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011572 manganese Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
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- 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
- 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
- 235000002867 manganese chloride Nutrition 0.000 abstract description 5
- 239000011565 manganese chloride Substances 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 239000000356 contaminant Substances 0.000 abstract description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052748 manganese Inorganic materials 0.000 abstract description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004042 decolorization Methods 0.000 description 6
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- 150000007513 acids Chemical class 0.000 description 3
- CRLHSBRULQUYOK-UHFFFAOYSA-N dioxido(dioxo)tungsten;manganese(2+) Chemical compound [Mn+2].[O-][W]([O-])(=O)=O CRLHSBRULQUYOK-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 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
- ZXOKVTWPEIAYAB-UHFFFAOYSA-N dioxido(oxo)tungsten Chemical group [O-][W]([O-])=O ZXOKVTWPEIAYAB-UHFFFAOYSA-N 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
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000013307 optical fiber 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
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- 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
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- 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
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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
- 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
- C02F2101/34—Organic compounds containing oxygen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/40—Organic compounds containing sulfur
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
本发明公开了一种硫代钨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钨酸钠，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1~4 L硫化氢气体，继续搅拌5~10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，即得到一种硫代钨酸锰催化剂。本发明的优点是：利用利用通入的硫化氢和钨酸根反应，但不完全反应，可以获得不同形态的硫代钨酸锰材料，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，尤其涉及一种硫代钨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。
钨酸锰是一种具有钨锰铁矿结构的重要的功能材料，在光致发光、光纤、多铁材料、光催化剂、闪烁体、湿度传感器及磁性材料等方面有着广泛的应用前景。硫代钨酸锰具有独特的结构，但单独使用钨酸锰作为光催化剂效果很差，并且无法得到相应的降解速度。
发明内容
本发明的目的是为克服现有技术的不足，提供一种硫代钨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钨酸钠，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1~4 L硫化氢气体，继续搅拌5~10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，即得到一种硫代钨酸锰催化剂。
本发明的优点是：利用利用通入的硫化氢和钨酸根反应，但不完全反应，可以获得不同形态的硫代钨酸锰材料，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钨酸钠，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1~4 L硫化氢气体，继续搅拌5~10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，即得到一种硫代钨酸锰催化剂。
0.5 g硫代钨酸锰催化剂加入到200 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95.2%，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91.4%。
实施例2
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钨酸钠，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1~4 L硫化氢气体，继续搅拌5~10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，即得到一种硫代钨酸锰催化剂。
0.5 g硫代钨酸锰催化剂加入到300 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96.4%，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91.9%。
实施例3
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钨酸钠，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1~4 L硫化氢气体，继续搅拌5~10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，即得到一种硫代钨酸锰催化剂。
0.5 g硫代钨酸锰催化剂加入到300 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95.6%，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%。
Claims (1)
1.一种硫代钨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钨酸钠，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1~4 L硫化氢气体，继续搅拌5~10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，即得到一种硫代钨酸锰催化剂。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113023784A (zh) * | 2021-01-08 | 2021-06-25 | 深圳万物创新集团有限公司 | 一种硫钨酸锰三元纳米材料及工作电极和过氧化氢探测器 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113023784A (zh) * | 2021-01-08 | 2021-06-25 | 深圳万物创新集团有限公司 | 一种硫钨酸锰三元纳米材料及工作电极和过氧化氢探测器 |
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Application publication date: 20171222 |