CN107262125A - 一种银掺杂磷酸铟光催化剂的制备方法 - Google Patents
一种银掺杂磷酸铟光催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- UJXZVRRCKFUQKG-UHFFFAOYSA-K indium(3+);phosphate Chemical compound [In+3].[O-]P([O-])([O-])=O UJXZVRRCKFUQKG-UHFFFAOYSA-K 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004332 silver Substances 0.000 claims abstract description 14
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004254 Ammonium phosphate Substances 0.000 claims abstract description 8
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims abstract description 8
- 235000019289 ammonium phosphates Nutrition 0.000 claims abstract description 8
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000084 colloidal system Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052738 indium Inorganic materials 0.000 claims abstract description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 5
- -1 silver ions Chemical class 0.000 claims description 5
- 230000001699 photocatalysis Effects 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000007704 transition Effects 0.000 abstract description 3
- QAKNNONVLHYVFR-UHFFFAOYSA-N [In].OP(O)(O)=O Chemical compound [In].OP(O)(O)=O QAKNNONVLHYVFR-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 4
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 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 1
- 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 1
- 239000003905 agrochemical Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process 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
- 239000000975 dye Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 150000003254 radicals Chemical class 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
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- 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
- 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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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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- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开一种银掺杂磷酸铟光催化剂的制备方法,包括以下步骤:在300~400r/s的转速搅拌下,向磷酸铵溶液中滴加硝酸铟溶液和银氨溶液,滴加完成后继续以相同的转速搅拌15~30min,形成胶体后,加入15~20mmol乙二醇,再搅拌40~50min,最后将整个体系离心分离,用蒸馏水洗涤固体3~4次,真空烘干,即制得银掺杂磷酸铟光催化剂。本发明将银和磷酸铟掺杂,有利于光生电子的跃迁,避免复合,提高催化效率。
Description
技术领域
本发明属于水处理领域,涉及一种银掺杂磷酸铟光催化剂的制备方法,尤其涉及一种用于处理有机废水的光催化材料及其制备方法。
背景技术
当前,伴随工业技术的飞速发展,人类赖以生存的水资源均受到不同程度的污染,水资源污染已经成为世界各国面临的亟待解决的问题。水中的污染物,特别是有毒有机污染物的存在,不仅造成环境污染、生态破坏,而且严重危害人类健康。这些有机污染物包括多环芳烃、多氯联苯、农药、环境干扰素、染料等。
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。掺杂催化剂有利于电子跃迁,在催化剂表面形成自由基而提高催化效率。而提高光催化效果是一项无止境的工作。
发明内容
本发明的目的是为克服现有技术的不足,提供一种银掺杂磷酸铟光催化剂的制备方法。
为解决上述技术问题,本发明采用以下技术方案:
一种银掺杂磷酸铟光催化剂的制备方法,包括如下步骤:
(1)在300-400r/s的转速搅拌下,向磷酸铵溶液中同时滴加硝酸铟溶液和银氨溶液,滴加完成后继续在300-500r/s的转速下搅拌15-30min;
(2)形成胶体,加入15-20mmol乙二醇,再在300-400r/s的转速下搅拌40-50min,最后将整个体系离心分离;
(3)用蒸馏水洗涤固体3-4次,在103-105℃下真空烘干,即制得银掺杂磷酸铟光催化剂。
优选地,步骤(1)中磷酸铵溶液的浓度为0.2-0.4mol/L,体积为20-40mL。
优选地,步骤(1)中硝酸铟溶液的浓度为0.2-0.4mol/L,体积为20-40mL。
优选地,步骤(1)中的银氨溶液滴加量为1-10mL,银离子浓度为0.1-0.3mol/L。
本发明将银和磷酸铟掺杂,有利于光生电子的跃迁,避免复合,有利于提高催化效率。
具体实施方式
实施例1
一种银掺杂磷酸铟光催化剂的制备方法,在400r/s的转速搅拌下,向浓度为0.4mol/L,体积为40mL的磷酸铵溶液中同时滴加浓度为0.4mol/L,体积为40mL的硝酸铟溶液和银离子浓度为0.3mol/L,体积为1mL的银氨溶液,滴加完成后继续在400r/s的转速下搅拌15min,形成胶体后加入20mmol乙二醇,再在400r/s的转速下搅拌40min,最后将整个体系离心分离,用蒸馏水洗涤固体4次,在105℃下真空烘干,即制得银掺杂磷酸铟光催化剂。
取1g银掺杂磷酸铟光催化剂加入到装有80mL浓度为40mg/L的酸性大红溶液中,在120wLED灯照射下,反应60min,脱色率为95.4%。相同质量的磷酸铟在相同的条件下的脱色率仅为65.4%。相比之下,本实施例降解速度有很明显的提高。
实施例2
一种银掺杂磷酸铟光催化剂的制备方法,在350r/s的转速搅拌下,向浓度为0.3mol/L,体积为30mL的磷酸铵溶液中同时滴加浓度为0.3mol/L,体积为30mL的硝酸铟溶液和银离子浓度为0.2mol/L,体积为5mL的银氨溶液,滴加完成后继续在350r/s的转速下搅拌20min,形成胶体后加入18mmol乙二醇,再在350r/s的转速下搅拌45min,最后将整个体系离心分离,用蒸馏水洗涤固体3次,在104℃下真空烘干,即制得银掺杂磷酸铟光催化剂。
取1g银掺杂磷酸铟光催化剂加入到装有80mL浓度为40mg/L的亚甲基蓝溶液中,在120wLED灯照射下,反应60min,脱色率为97.4%。
实施例3
一种银掺杂磷酸铟光催化剂的制备方法,在300r/s的转速搅拌下,向浓度为0.2mol/L,体积为20mL的磷酸铵溶液中同时滴加浓度为0.2mol/L,体积为20mL的硝酸铟溶液和银离子浓度为0.1mol/L,体积为10mL的银氨溶液,滴加完成后继续在300r/s的转速下搅拌30min,形成胶体后加入15mmol乙二醇,再在350r/s的转速下搅拌50min,最后将整个体系离心分离,用蒸馏水洗涤固体3次,在103℃下真空烘干,即制得银掺杂磷酸铟光催化剂。
取1g银掺杂磷酸铟光催化剂加入到装有80mL浓度为40mg/L的罗丹明B溶液中,在120wLED灯照射下,反应60min,脱色率为95.2%。
Claims (4)
1.一种银掺杂磷酸铟光催化剂的制备方法,其特征在于,包括如下步骤:
(1)在300-400r/s的转速搅拌下,向磷酸铵溶液中同时滴加硝酸铟溶液和银氨溶液,滴加完成后继续在300-500r/s的转速下搅拌15-30min;
(2)形成胶体,加入15-20mmol乙二醇,再在300-400r/s的转速下搅拌40-50min,最后将整个体系离心分离;
(3)用蒸馏水洗涤固体3-4次,在103-105℃下真空烘干,即制得银掺杂磷酸铟光催化剂。
2.根据权利要求1所述的银掺杂磷酸铟光催化剂的制备方法,其特征在于,步骤(1)中磷酸铵溶液的浓度为0.2-0.4mol/L,体积为20-40mL。
3.根据权利要求1所述的银掺杂磷酸铟光催化剂的制备方法,其特征在于,步骤(1)中硝酸铟溶液的浓度为0.2-0.4mol/L,体积为20-40mL。
4.根据权利要求1所述的银掺杂磷酸铟光催化剂的制备方法,其特征在于,步骤(1)中的银氨溶液滴加量为1-10mL,银离子浓度为0.1-0.3mol/L。
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