CN107096549A - 一种钨酸银复合溴化银光催化剂的制备方法 - Google Patents
一种钨酸银复合溴化银光催化剂的制备方法 Download PDFInfo
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- 239000002253 acid Substances 0.000 title claims abstract description 45
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 42
- 239000004332 silver Substances 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- -1 compound silver bromide Chemical class 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000084 colloidal system Substances 0.000 claims abstract description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical class [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 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 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- 230000031709 bromination Effects 0.000 claims abstract description 6
- 238000005893 bromination reaction Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 claims abstract description 6
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 238000006731 degradation reaction Methods 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
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 241000220317 Rosa Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229940083025 silver preparation Drugs 0.000 description 1
- 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 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/132—Halogens; Compounds thereof 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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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J35/39—Photocatalytic properties
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Abstract
本发明公开一种钨酸银复合溴化银光催化剂的制备方法，具体步骤如下：称取12～16mmol硝酸银，配置成18mmol/L的硝酸银溶液，称取6.6～8mmol钨酸钠，配置成18mmol/L的钨酸钠溶液；将以上两种溶液在350～400转/分钟的转速下混合，形成胶状物质，持续搅拌3～4h，在搅拌过程中钨酸钠和硝酸银反应，生成钨酸银胶体；将钨酸银胶体置于半透膜袋内，用蒸馏水洗涤3～4次，去除掉游离离子，再将该钨酸银胶体加入到60～80mL浓度为3～4mol/L的溴化钠溶液中，浸泡2～4天，在钨酸银颗粒表面形成溴化银纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种钨酸银复合溴化银光催化剂。该方法是在载体表面形成催化剂，催化剂和载体紧密结合。
Description
技术领域
本发明涉及一种钨酸银复合溴化银光催化剂的制备方法，属于环境保护中污水处理技术领域。
背景技术
传统的水处理方法效率低、成本高、存在二次污染等问题，污水治理一直得不到好的解决。纳米技术的发展和应用很可能彻底解决这一难题。1972年开始发现TiO2氧化活性较高，化学稳定性好，对人体无毒害，成本低，无污染，应用范围广，因而最受重视，但是TiO2的禁带宽度较大(例如锐钛矿TiO2的禁带宽度Eg＝3.2eV)，仅能吸收紫外光区(波长小于387nm)的光，对太阳能的利用效率较低。
在污染物降解以及能源生产领域中，半导体光催化是最有前景的方法之一。当能量大于或等于半导体禁带宽度的光子照射在光催化剂表面上时就会产生电子-空穴对的分离，这是光催化反应的最初的基本步骤。为了寻找高效的光催化剂，大量研究工作都集中在研究光催化活性的影响因素上。2010年6月，物质材料研究机构研究人员发现溴化银具有光催化剂的效果，且光氧化效果是目前已知各种光催化剂的数十倍以上。但由于溴化银自身不稳定，在光催化中易自蚀，导致催化剂降解性能迅速降低。而提高光催化效果是一项无止境的工作。另外，由于纳米颗粒在处理废水后很难从废水中分离，因此需要将纳米颗粒负载在一些载体上。在其表面合成的材料是一种复合材料，可以有很好的光催化效果。
发明内容
本发明的目的在于针对现有技术的不足，提出一种钨酸银复合溴化银光催化剂的制备方法，该方法是在载体表面形成催化剂，催化剂和载体紧密结合。
本发明采用的技术方案是采用如下步骤：
1)称取12～16mmol硝酸银，配置成18mmol/L的硝酸银溶液，称取6.6～8mmol钨酸钠，配置成18mmol/L的钨酸钠溶液；
2)将以上两种溶液在350～400转/分钟的转速下混合，形成胶状物质，持续搅拌3～4h，在搅拌过程中钨酸钠和硝酸银反应，生成钨酸银胶体；
3)将钨酸银胶体置于半透膜袋内，用蒸馏水洗涤3～4次，去除掉游离离子，再将该钨酸银胶体加入到60～80mL浓度为3～4mol/L的溴化钠溶液中，浸泡2～4天，在钨酸银颗粒表面形成溴化银纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种钨酸银复合溴化银光催化剂。
本发明的有益效果是：(1)本方法利用溶度积常数的差异，在钨酸银表面形成溶度积常数更小的溴化银颗粒。
(2)钨酸银和溴化银复合，协同作用，可以使钨酸银在可见光下更好的发挥催化作用而能获得很好的催化效果。
具体实施方式
实施例1
称取12mmol硝酸银，配置成18mmol/L的硝酸银溶液，称取6.6mmol钨酸钠，配置成18mmol/L的钨酸钠溶液；将以上两种溶液在350转/分钟的转速下混合，形成胶状物质，持续搅拌3h，在搅拌过程中钨酸钠和硝酸银反应，生成钨酸银胶体；将钨酸银胶体置于半透膜袋内，用蒸馏水洗涤3次，去除掉游离离子，再将该钨酸银胶体加入到60mL浓度为3mol/L的溴化钠溶液中，浸泡2天，在钨酸银颗粒表面形成溴化银纳米颗粒，固液分离，去离子水洗涤固体2次，75℃烘干，制得一种钨酸银复合溴化银光催化剂。
将得到的钨酸银复合溴化银光催化剂0.5g加入到400mL浓度为30mg/L的酸性红废水中，在300w金卤灯照射下，反应30min，脱色率为96.2％，催化剂分离后可以重复利用。
实施例2
称取16mmol硝酸银，配置成18mmol/L的硝酸银溶液，称取8mmol钨酸钠，配置成18mmol/L的钨酸钠溶液；将以上两种溶液在400转/分钟的转速下混合，形成胶状物质，持续搅拌4h，在搅拌过程中钨酸钠和硝酸银反应，生成钨酸银胶体；将钨酸银胶体置于半透膜袋内，用蒸馏水洗涤4次，去除掉游离离子，再将该钨酸银胶体加入到80mL浓度为4mol/L的溴化钠溶液中，浸泡4天，在钨酸银颗粒表面形成溴化银纳米颗粒，固液分离，去离子水洗涤固体3次，105℃烘干，制得一种钨酸银复合溴化银光催化剂。
将得到的钨酸银复合溴化银光催化剂0.5g加入到400mL浓度为30mg/L的金橙7废水中，在300w金卤灯照射下，反应30min，脱色率为98.3％，催化剂分离后可以重复利用。对于相同的废水的在相同的条件下，纯钨酸银的降解效率为63.1％，大大提高了其作用效果。
实施例3
称取14mmol硝酸银，配置成18mmol/L的硝酸银溶液，称取7mmol钨酸钠，配置成18mmol/L的钨酸钠溶液；将以上两种溶液在400转/分钟的转速下混合，形成胶状物质，持续搅拌4h，在搅拌过程中钨酸钠和硝酸银反应，生成钨酸银胶体；将钨酸银胶体置于半透膜袋内，用蒸馏水洗涤4次，去除掉游离离子，再将该钨酸银胶体加入到60mL浓度为4mol/L的溴化钠溶液中，浸泡3天，在钨酸银颗粒表面形成溴化银纳米颗粒，固液分离，去离子水洗涤固体3次，105℃烘干，制得一种钨酸银复合溴化银光催化剂。
将得到的钨酸银复合溴化银光催化剂0.5g加入到400mL浓度为30mg/L的玫瑰红B废水中，在300w金卤灯照射下，反应30min，脱色率为97.5％，催化剂分离后可以重复利用。
Claims (1)
1.一种钨酸银复合溴化银光催化剂的制备方法，其特征是依次包括如下步骤：
1)称取12～16mmol硝酸银，配置成18mmol/L的硝酸银溶液，称取6.6～8mmol钨酸钠，配置成18mmol/L的钨酸钠溶液；
2)将以上两种溶液在350～400转/分钟的转速下混合，形成胶状物质，持续搅拌3～4h，在搅拌过程中钨酸钠和硝酸银反应，生成钨酸银胶体；
3)将钨酸银胶体置于半透膜袋内，用蒸馏水洗涤3～4次，去除掉游离离子，再将该钨酸银胶体加入到60～80mL浓度为3～4mol/L的溴化钠溶液中，浸泡2～4天，在钨酸银颗粒表面形成溴化银纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种钨酸银复合溴化银光催化剂。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110560100A (zh) * | 2019-08-16 | 2019-12-13 | 南京理工大学 | 一种Z-Scheme AgBr/Ag8W4O16光催化剂的合成方法 |
| CN110560101A (zh) * | 2019-08-16 | 2019-12-13 | 南京理工大学 | 一步合成Z-Scheme AgBr/β-Ag2WO4光催化剂的方法 |
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| CN110560100B (zh) * | 2019-08-16 | 2022-11-18 | 南京理工大学 | 一种Z-Scheme AgBr/Ag8W4O16光催化剂的合成方法 |
| CN110560101B (zh) * | 2019-08-16 | 2022-12-02 | 南京理工大学 | 一步合成Z-Scheme AgBr/β-Ag2WO4光催化剂的方法 |
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