CN106311293B - 一种硫代磷酸银/磷酸银催化剂的制备方法 - Google Patents
一种硫代磷酸银/磷酸银催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 23
- 239000004332 silver Substances 0.000 title claims abstract description 22
- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 20
- 229940019931 silver phosphate Drugs 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000010792 warming Methods 0.000 claims abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000004042 decolorization Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 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
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 238000009776 industrial production Methods 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
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开一种硫代磷酸银/磷酸银催化剂的制备方法,依次包括如下步骤:将磷酸银粉末置于管式炉中,通入H2S,以2~4℃/min的速度,升温到500~650℃后保持2~2.5h,停止加热后自然降温到室温,即可得到一种硫代磷酸银/磷酸银催化剂。表面部分磷酸银变成硫代磷酸银,形成异质结结构,增加催化剂的稳定性并拓展了催化剂对光的吸收范围。
Description
技术领域
本发明涉及环境污染控制新材料领域,尤其涉及一种硫代磷酸银/磷酸银催化剂的制备方法。
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。
然而,目前所报道的可见光光催化材料大多具有较高的光生载流子复合率和较差的可见光吸收,导致其量子效率较低。因此,开发新型高效可见光光催化材料,拓展半导体材料光谱响应范围以及促进光生电子和空穴有效分离,成为目前光催化材料研究领域急需解决的科学问题。
由于Ag3PO4在光催化反应过程中的稳定性较差以及成本较高,严重限制了其实际应用。因此,设计和制备具有高稳定性、低成本的Ag3PO4光催化材料成为目前急需开展的研究领域。
发明内容
本发明的目的是为克服现有技术中磷酸银光催化降解污染物过程中的不足,提供一种硫代磷酸银/磷酸银催化剂的制备方法。
为此,本发明提供了以下技术方案,一种硫代磷酸银/磷酸银催化剂的制备方法,依次包括如下步骤:
将磷酸银粉末置于管式炉中,通入H2S,以2~4℃/min的速度,升温到500~650℃后保持2~2.5h,停止加热后自然降温到室温,即可得到一种硫代磷酸银/磷酸银催化剂。
与未处理的磷酸银相比,本发明具有以下优越性:磷酸银经过H2S保护热处理后,表面部分磷酸银变成硫代磷酸银,形成异质结结构,增加催化剂的稳定性并拓展了催化剂对光的吸收范围。
具体实施方式
下面结合实施例来详细说明本发明,但本发明并不仅限于此。
实施例1
将磷酸银粉末置于管式炉中,通入H2S,以4℃/min的速度,升温到650℃后保持2h,停止加热后自然降温到室温,即可得到一种硫代磷酸银/磷酸银催化剂。
将制得的硫代磷酸银/磷酸银催化剂用于处理含酸性大红废水:0.5g硫代磷酸银/磷酸银催化剂加入到200mL浓度为40mg/L的酸性大红废水中,在300w金卤灯照射下,反应20min,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20min,脱色率为94.2%。同样质量的普通磷酸银颗粒在相同的条件下,30min时脱色率为91.5%。
实施例2
将磷酸银粉末置于管式炉中,通入H2S,以2℃/min的速度,升温到500℃后保持2.5h,停止加热后自然降温到室温,即可得到一种硫代磷酸银/磷酸银催化剂。
将制得的硫代磷酸银/磷酸银催化剂用于处理含亚甲基蓝废水:0.5g硫代磷酸银/磷酸银催化剂加入到200mL浓度为40mg/L的亚甲基蓝废水中,在300w金卤灯照射下,反应20min,脱色率为97.8%,催化剂分离重复利用5次后,同样条件下,反应20min,脱色率为93.6%。同样质量的普通磷酸银颗粒在相同的条件下,30min时脱色率为91.9%。
实施例3
将磷酸银粉末置于管式炉中,通入H2S,以2℃/min的速度,升温到650℃后保持2h,停止加热后自然降温到室温,即可得到一种硫代磷酸银/磷酸银催化剂。
将制得的硫代磷酸银/磷酸银催化剂用于处理含金橙II废水:0.5g硫代磷酸银/磷酸银催化剂加入到200mL浓度为40mg/L的金橙II废水中,在300w金卤灯照射下,反应20min,脱色率为99.2%,催化剂分离重复利用5次后,同样条件下,反应20min,脱色率为94.3%。同样质量的普通磷酸银颗粒在相同的条件下,30min时脱色率为90.5%。
Claims (1)
1.一种硫代磷酸银/磷酸银催化剂的制备方法,其特征在于:依次包括如下步骤:将磷酸银粉末置于管式炉中,通入H2S,以2~4℃/min的速度,升温到500~650℃后保持2~2.5h,停止加热后自然降温到室温,即可得到一种硫代磷酸银/磷酸银催化剂。
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10279818A (ja) * | 1997-04-07 | 1998-10-20 | Kenji Nakamura | 熱変色性を防止した銀含有樹脂組成物 |
CN102277157A (zh) * | 2011-05-30 | 2011-12-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | 近红外硫化银量子点、其制备方法及其应用 |
CN102824921A (zh) * | 2012-08-28 | 2012-12-19 | 湖南科技大学 | 一种Ag2S/Ag3PO4复合光催化剂的制备方法 |
CN103990476A (zh) * | 2014-06-04 | 2014-08-20 | 常州大学 | 一种硫掺杂磷酸银催化剂的制备方法 |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH10279818A (ja) * | 1997-04-07 | 1998-10-20 | Kenji Nakamura | 熱変色性を防止した銀含有樹脂組成物 |
CN102277157A (zh) * | 2011-05-30 | 2011-12-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | 近红外硫化银量子点、其制备方法及其应用 |
CN102824921A (zh) * | 2012-08-28 | 2012-12-19 | 湖南科技大学 | 一种Ag2S/Ag3PO4复合光催化剂的制备方法 |
CN103990476A (zh) * | 2014-06-04 | 2014-08-20 | 常州大学 | 一种硫掺杂磷酸银催化剂的制备方法 |
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