CN106964382A - 一种硫化锌复合磷酸银光催化剂的制备方法 - Google Patents
一种硫化锌复合磷酸银光催化剂的制备方法 Download PDFInfo
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 22
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 15
- 150000001875 compounds Chemical class 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000013049 sediment Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000084 colloidal system Substances 0.000 claims abstract description 15
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 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
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 5
- 235000009529 zinc sulphate Nutrition 0.000 claims abstract description 5
- 239000011686 zinc sulphate Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 claims description 5
- 235000013904 zinc acetate Nutrition 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 239000011734 sodium Substances 0.000 claims 1
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical group [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 abstract description 9
- -1 3~4h is stirred Substances 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000004073 vulcanization Methods 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 abstract 1
- 238000013019 agitation Methods 0.000 abstract 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 abstract 1
- 239000004246 zinc acetate Substances 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229910052946 acanthite 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
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 3
- 229940056910 silver sulfide Drugs 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 241000220317 Rosa Species 0.000 description 1
- AMHXQVUODFNFGR-UHFFFAOYSA-K [Ag+3].[O-]P([O-])([O-])=O Chemical group [Ag+3].[O-]P([O-])([O-])=O AMHXQVUODFNFGR-UHFFFAOYSA-K 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 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
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 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
- 239000004065 semiconductor Substances 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
- 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
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 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
- B01J27/16—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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开一种硫化锌复合磷酸银光催化剂的制备方法,具体步骤如下:将醋酸锌和硫代乙酰胺和十六烷基三甲基溴化铵加到去离子水中,搅拌至完全溶解,得到混合溶液,将混合溶液转移至水热釜并置于烘箱中恒温加热,待反应结束后取出水热釜,自然冷却至室温后弃掉上清液,收集沉淀物得到硫化锌粉末;将硝酸银溶液和磷酸氢二钠溶液在搅拌下混合,形成黄绿色胶状物质,生成磷酸银胶体;将得到的硫酸锌粉末加入到磷酸银胶体中,搅拌3~4h,沉淀分离,将沉淀物洗涤、烘干,即得一种硫化锌复合磷酸银光催化剂。磷酸银在纳米硫化锌表面形成复合结构,可以使磷酸银有效分布而不聚集,并在硫化锌表面形成更小的颗粒,提高催化活性。
Description
技术领域
本发明涉及一种硫化锌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。
发明内容
本发明的目的在于针对现有技术的不足,提出一种硫化锌复合磷酸银光催化剂的制备方法。
本发明采用的技术方案是采用如下步骤:
1)将1~5g醋酸锌和3~20g硫代乙酰胺和0.5~1.2g十六烷基三甲基溴化铵加到40~80mL去离子水中,搅拌至完全溶解,得到混合溶液,将混合溶液转移至水热釜并置于烘箱中105~140℃恒温加热24~36h,待反应结束后取出水热釜,自然冷却至室温后弃掉上清液,收集沉淀物;
2)将上述沉淀物分别用去离子水和无水乙醇洗涤各3~4次,将洗涤后的沉淀物在50~70℃下恒温干燥,得到硫化锌粉末;
3)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;
4)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;
5)将得到的硫酸锌粉末加入到磷酸银胶体中,搅拌3~4h,沉淀分离,用去离子水洗涤沉淀物4~5次,将洗涤后的沉淀物105℃下烘干,即得一种硫化锌复合磷酸银光催化剂。
本发明的有益效果是:(1)磷酸银在纳米硫化锌表面形成复合结构,可以使磷酸银有效分布而不聚集,并在硫化锌表面形成更小的颗粒,提高催化活性。
(2)磷酸银和硫化锌复合,协同作用,可以使硫化锌在可见光的作用下也能够发挥催化作用,而能获得很好的催化效果。
具体实施方式
实施例1
将5g醋酸锌和20g硫代乙酰胺和1.2g十六烷基三甲基溴化铵加到80mL去离子水中,搅拌至完全溶解,得到混合溶液,将混合溶液转移至水热釜并于烘箱中140℃恒温加热36h,待反应结束后取出水热釜,自然冷却至室温后弃掉上清液,收集沉淀物;将上述沉淀物分别用去离子水和无水乙醇洗涤各4次,将洗涤后的沉淀物在70℃恒温干燥,得到硫化锌粉末;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;将得到的硫酸锌粉末加入到该磷酸银胶体中,搅拌4h,沉淀分离,用去离子水洗涤沉淀物5次,将洗涤后的沉淀物105℃下烘干,即得一种硫化锌复合磷酸银光催化剂。
将得到的负载型磷酸银/硫化银复合光催化剂0.5g加入到500mL浓度为20mg/L的酸性红废水中,在300w金卤灯照射下,反应30min,脱色率为96.7%,催化剂分离后可以重复利用。
实施例2
将1g醋酸锌和3g硫代乙酰胺和0.5g十六烷基三甲基溴化铵加到40mL去离子水中,搅拌至完全溶解,得到混合溶液,将混合溶液转移至水热釜并于烘箱中105℃恒温加热24h,待反应结束后取出水热釜,自然冷却至室温后弃掉上清液,收集沉淀物;将上述沉淀物分别用去离子水和无水乙醇洗涤各3次,将洗涤后的沉淀物在50℃恒温干燥,得到硫化锌粉末;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;将得到的硫酸锌粉末加入到磷酸银胶体中,搅拌3h,沉淀分离,用去离子水洗涤沉淀物4次,将洗涤后的沉淀物105℃下烘干,即得一种硫化锌复合磷酸银光催化剂。
将得到的负载型磷酸银/硫化银复合光催化剂0.5g加入到500mL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97.5%,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,纯磷酸银的降解效率为91.4%,但由于是纯磷酸银,催化剂中银的消耗量很大,经济上消耗大。
实施例3
将3g醋酸锌和6g硫代乙酰胺和0.8g十六烷基三甲基溴化铵加到50mL去离子水中,搅拌至完全溶解,得到混合溶液,将混合溶液转移至水热釜并于烘箱中120℃恒温加热36h,待反应结束后取出水热釜,自然冷却至室温后弃掉上清液,收集沉淀物;将上述沉淀物分别用去离子水和无水乙醇洗涤各4次,将洗涤后的沉淀物在60℃恒温干燥,得到硫化锌粉末;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;将得到的硫酸锌粉末加入到磷酸银胶体中,搅拌4h,沉淀分离,用去离子水洗涤沉淀物4次,将洗涤后的沉淀物105℃下烘干,即得一种硫化锌复合磷酸银光催化剂。
将得到的负载型磷酸银/硫化银复合光催化剂0.5g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30min,脱色率为96.2%,催化剂分离后可以重复利用。
Claims (1)
1.一种硫化锌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)将1~5g醋酸锌和3~20g硫代乙酰胺和0.5~1.2g十六烷基三甲基溴化铵加到40~80mL去离子水中,搅拌至完全溶解,得到混合溶液,将混合溶液转移至水热釜并置于烘箱中105~140℃恒温加热24~36h,待反应结束后取出水热釜,自然冷却至室温后弃掉上清液,收集沉淀物;
2)将上述沉淀物分别用去离子水和无水乙醇洗涤各3~4次,将洗涤后的沉淀物在50~70℃下恒温干燥,得到硫化锌粉末;
3)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;
4)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;
5)将得到的硫酸锌粉末加入到磷酸银胶体中,搅拌3~4h,沉淀分离,用去离子水洗涤沉淀物4~5次,将洗涤后的沉淀物105℃下烘干,即得一种硫化锌复合磷酸银光催化剂。
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