CN106984346A - 一种磷酸银复合磷酸铋光催化剂的制备方法 - Google Patents
一种磷酸银复合磷酸铋光催化剂的制备方法 Download PDFInfo
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- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 26
- LGUJZAHTSAGVMX-UHFFFAOYSA-N [Bi].P(O)(O)(O)=O Chemical compound [Bi].P(O)(O)(O)=O LGUJZAHTSAGVMX-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 150000001875 compounds Chemical class 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000000084 colloidal system Substances 0.000 claims abstract description 24
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 19
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 16
- 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
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 9
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 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
- 229910000397 disodium phosphate Inorganic materials 0.000 claims abstract description 6
- 235000019800 disodium phosphate Nutrition 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 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
- 239000002245 particle Substances 0.000 claims abstract description 6
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 4
- 238000004821 distillation Methods 0.000 claims abstract 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 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 1
- 230000002045 lasting effect Effects 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
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- 230000000694 effects Effects 0.000 description 5
- 238000004042 decolorization Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
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- 238000007146 photocatalysis Methods 0.000 description 3
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003426 co-catalyst Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- -1 Disodium hydrogen Chemical class 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 239000000463 material Substances 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
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229940100890 silver compound Drugs 0.000 description 1
- 150000003379 silver compounds Chemical class 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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- 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开一种磷酸银复合磷酸铋光催化剂的制备方法，具体步骤如下：称取硝酸银，配置成20mmol/L的硝酸银溶液，称取磷酸氢二钠，配置成20mmol/L的磷酸氢二钠溶液；将以上两种溶液在350～400转/分钟的转速下混合，形成黄绿色胶状物质，持续搅拌3～4h，在搅拌过程中磷酸氢二钠和硝酸银反应，生成磷酸银胶体；将磷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，再将该磷酸银胶体加入到60～80mL浓度为0.5～1mol/L的硝酸铋0～4℃溶液中，浸泡5～8天，在磷酸银颗粒表面形成磷酸铋纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种磷酸银复合磷酸铋光催化剂。磷酸银复合磷酸铋光催化剂，协同作用，可以提高磷酸银的稳定性并提高催化效果。
Description
技术领域
本发明涉及一种磷酸银复合磷酸铋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。
银化合物光催化剂具有吸收范围大等优点受到科学家们的广泛重视，而助催化剂的引入可以大大提高原催化剂的催化性能和稳定性，因此附载助催化剂也是提高催化剂性能的重要手段之一。
发明内容
本发明的目的在于针对现有技术的不足，提出一种磷酸银复合磷酸铋光催化剂的制备方法，该方法是在利用半导体材料性质差异，相互促进作用可以大大提高催化剂的稳定性和催化效率。
本发明采用的技术方案是采用如下步骤：
1)称取20～24mmol硝酸银，配置成20mmol/L的硝酸银溶液，称取6.6～8mmol磷酸氢二钠，配置成20mmol/L的磷酸氢二钠溶液；
2)将以上两种溶液在350～400转/分钟的转速下混合，形成黄绿色胶状物质，持续搅拌3～4h，在搅拌过程中磷酸氢二钠和硝酸银反应，生成磷酸银胶体；
3)将磷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，再将该磷酸银胶体加入到60～80mL浓度为0.5～1mol/L的硝酸铋0～4℃溶液中，浸泡5～8天，在磷酸银颗粒表面形成磷酸铋纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种磷酸银复合磷酸铋光催化剂。
本发明的有益效果是：(1)本方法利用溶度积常数的差异，在磷酸银表面形成溶度积常数更小的磷酸铋颗粒。
(2)磷酸银复合磷酸铋光催化剂，协同作用，可以提高磷酸银的稳定性并提高催化效果。
具体实施方式
实施例1
称取24mmol硝酸银，配置成20mmol/L的硝酸银溶液，称取8mmol磷酸氢二钠，配置成20mmol/L的磷酸氢二钠溶液；将以上两种溶液在400转/分钟的转速下混合，形成黄绿色胶状物质，持续搅拌4h，在搅拌过程中磷酸氢二钠和硝酸银反应，生成磷酸银胶体；将磷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，再将该磷酸银胶体加入到80mL浓度为1mol/L的硝酸铋4℃溶液中，浸泡8天，在磷酸银颗粒表面形成磷酸铋纳米颗粒，固液分离，去离子水洗涤固体3次，105℃烘干，制得一种磷酸银复合磷酸铋光催化剂。
将得到的磷酸银复合磷酸铋光催化剂0.3g加入到500mL浓度为40mg/L的酸性红废水中，在300w金卤灯照射下，反应20min，脱色率为98.1％，催化剂分离后可以重复利用。
实施例2
称取20mmol硝酸银，配置成20mmol/L的硝酸银溶液，称取6.6mmol磷酸氢二钠，配置成20mmol/L的磷酸氢二钠溶液；将以上两种溶液在350转/分钟的转速下混合，形成黄绿色胶状物质，持续搅拌3h，在搅拌过程中磷酸氢二钠和硝酸银反应，生成磷酸银胶体；将磷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，再将该磷酸银胶体加入到60mL浓度为0.5mol/L的硝酸铋0℃溶液中，浸泡5天，在磷酸银颗粒表面形成磷酸铋纳米颗粒，固液分离，去离子水洗涤固体2次，75℃烘干，制得一种磷酸银复合磷酸铋光催化剂。
将得到的磷酸银复合磷酸铋光催化剂0.3g加入到500mL浓度为40mg/L的金橙7废水中，在300w金卤灯照射下，反应20min，脱色率为98.1％，催化剂分离后在相同的条件下再重复利用四次，脱色率分别为97.9％、97.2％、96.9％、96.5％。
对于相同的废水的在相同的条件下，纯磷酸银的降解效率为85.1％。
实施例3
称取20mmol硝酸银，配置成20mmol/L的硝酸银溶液，称取7mmol磷酸氢二钠，配置成20mmol/L的磷酸氢二钠溶液；将以上两种溶液在400转/分钟的转速下混合，形成黄绿色胶状物质，持续搅拌4h，在搅拌过程中磷酸氢二钠和硝酸银反应，生成磷酸银胶体；将磷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，再将该磷酸银胶体加入到70mL浓度为0.8mol/L的硝酸铋2℃溶液中，浸泡7天，在磷酸银颗粒表面形成磷酸铋纳米颗粒，固液分离，去离子水洗涤固体3次，105℃烘干，制得一种磷酸银复合磷酸铋光催化剂。
将得到的磷酸银复合磷酸铋光催化剂0.3g加入到500mL浓度为30mg/L的玫瑰红B废水中，在300w金卤灯照射下，反应20min，脱色率为98.9％，催化剂分离后可以重复利用。
Claims (1)
1.一种磷酸银复合磷酸铋光催化剂的制备方法，其特征是依次包括如下步骤：
1)称取20～24mmol硝酸银，配置成20mmol/L的硝酸银溶液，称取6.6～8mmol磷酸氢二钠，配置成20mmol/L的磷酸氢二钠溶液；
2)将以上两种溶液在350～400转/分钟的转速下混合，形成黄绿色胶状物质，持续搅拌3～4h，在搅拌过程中磷酸氢二钠和硝酸银反应，生成磷酸银胶体；
3)将磷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，再将该磷酸银胶体加入到60～80mL浓度为0.5～1mol/L的硝酸铋0～4℃溶液中，浸泡5～8天，在磷酸银颗粒表面形成磷酸铋纳米颗粒，固液分离，去离子水洗涤固体2～3次，75～105℃烘干，制得一种磷酸银复合磷酸铋光催化剂。
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| CN111790419A (zh) * | 2020-08-10 | 2020-10-20 | 牡丹江师范学院 | 一种具有太阳光催化活性的磷酸银－碳酸氧铋光催化剂及其制备方法 |
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