CN106984348A - 一种偏钒酸银复合磷酸银光催化剂的制备方法 - Google Patents
一种偏钒酸银复合磷酸银光催化剂的制备方法 Download PDFInfo
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- RAVDHKVWJUPFPT-UHFFFAOYSA-N silver;oxido(dioxo)vanadium Chemical compound [Ag+].[O-][V](=O)=O RAVDHKVWJUPFPT-UHFFFAOYSA-N 0.000 title claims abstract description 38
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 150000001875 compounds Chemical class 0.000 title claims abstract description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000000084 colloidal system Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical class [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001961 silver nitrate Inorganic materials 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
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 6
- 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
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 6
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 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
- 239000010452 phosphate Substances 0.000 claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 6
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 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
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 1
- 230000004520 agglutination Effects 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
- 238000006555 catalytic reaction Methods 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
- XDBSEZHMWGHVIL-UHFFFAOYSA-M hydroxy(dioxo)vanadium Chemical compound O[V](=O)=O XDBSEZHMWGHVIL-UHFFFAOYSA-M 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
- 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
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 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
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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
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
- B01J27/198—Vanadium
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Abstract
本发明公开一种偏钒酸银复合磷酸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12mmol/L的硝酸银溶液，称取6.6～8mmol偏钒酸铵，在40～60℃水中，配置成10mmol/L的偏钒酸钠溶液；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，在搅拌过程中偏钒酸铵和硝酸银反应，生成偏钒酸银胶体；将偏钒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，再将该偏钒酸银胶体加入到60～80mL浓度为3～4mol/L的磷酸钠溶液中，浸泡2～4天，在偏钒酸银颗粒表面形成磷酸银纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种偏钒酸银复合磷酸银光催化剂。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
本发明涉及一种偏钒酸银复合磷酸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磷酸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。但由于磷酸银自身不稳定，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，提出一种偏钒酸银复合磷酸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12mmol/L的硝酸银溶液，称取6.6～8mmol偏钒酸铵，在40～60℃水中，配置成10mmol/L的偏钒酸钠溶液；
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，在搅拌过程中偏钒酸铵和硝酸银反应，生成偏钒酸银胶体；
3)将偏钒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，再将该偏钒酸银胶体加入到60～80mL浓度为3～4mol/L的磷酸钠溶液中，浸泡2～4天，在偏钒酸银颗粒表面形成磷酸银纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种偏钒酸银复合磷酸银光催化剂。
本发明的有益效果是：(1)本方法利用溶度积常数的差异，在偏钒酸银表面形成溶度积常数更小的磷酸银颗粒。
(2)偏钒酸银和磷酸银复合，协同作用，可以使偏钒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16mmol硝酸银，配置成12mmol/L的硝酸银溶液，称取8mmol偏钒酸铵，在60℃水中，配置成10mmol/L的偏钒酸钠溶液；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，在搅拌过程中偏钒酸铵和硝酸银反应，生成偏钒酸银胶体；将偏钒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，再将该偏钒酸银胶体加入到80mL浓度为4mol/L的磷酸钠溶液中，浸泡4天，在偏钒酸银颗粒表面形成磷酸银纳米颗粒，固液分离，去离子水洗涤固体3次，105℃烘干，制得一种偏钒酸银复合磷酸银光催化剂。
将得到的偏钒酸银复合磷酸银光催化剂0.3g加入到400mL浓度为40mg/L的酸性红废水中，在300w金卤灯照射下，反应30min，脱色率为94.9％，催化剂分离后可以重复利用。
实施例2
称取12mmol硝酸银，配置成12mmol/L的硝酸银溶液，称取6.6mmol偏钒酸铵，在40℃水中，配置成10mmol/L的偏钒酸钠溶液；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，在搅拌过程中偏钒酸铵和硝酸银反应，生成偏钒酸银胶体；将偏钒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，再将该偏钒酸银胶体加入到60mL浓度为3mol/L的磷酸钠溶液中，浸泡2天，在偏钒酸银颗粒表面形成磷酸银纳米颗粒，固液分离，去离子水洗涤固体2次，75℃烘干，制得一种偏钒酸银复合磷酸银光催化剂。
将得到的偏钒酸银复合磷酸银光催化剂0.3g加入到400mL浓度为40mg/L的金橙7废水中，在300w金卤灯照射下，反应30min，脱色率为95.7％，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，纯偏钒酸银的降解效率为57.1％，大大提高了其作用效果。
实施例3
称取15mmol硝酸银，配置成12mmol/L的硝酸银溶液，称取7mmol偏钒酸铵，在60℃水中，配置成10mmol/L的偏钒酸钠溶液；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，在搅拌过程中偏钒酸铵和硝酸银反应，生成偏钒酸银胶体；将偏钒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，再将该偏钒酸银胶体加入到80mL浓度为4mol/L的磷酸钠溶液中，浸泡4天，在偏钒酸银颗粒表面形成磷酸银纳米颗粒，固液分离，去离子水洗涤固体3次，105℃烘干，制得一种偏钒酸银复合磷酸银光催化剂。
将得到的偏钒酸银复合磷酸银光催化剂0.3g加入到400mL浓度为40mg/L的罗丹明B废水中，在300w金卤灯照射下，反应30min，脱色率为96.6％，催化剂分离后可以重复利用。
Claims (1)
1.一种偏钒酸银复合磷酸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12mmol/L的硝酸银溶液，称取6.6～8mmol偏钒酸铵，在40～60℃水中，配置成10mmol/L的偏钒酸钠溶液；
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，在搅拌过程中偏钒酸铵和硝酸银反应，生成偏钒酸银胶体；
3)将偏钒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，再将该偏钒酸银胶体加入到60～80mL浓度为3～4mol/L的磷酸钠溶液中，浸泡2～4天，在偏钒酸银颗粒表面形成磷酸银纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种偏钒酸银复合磷酸银光催化剂。
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