CN106513026A - 一种氧化铁/磷酸钇复合催化剂的制备方法 - Google Patents
一种氧化铁/磷酸钇复合催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 20
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 title claims abstract description 19
- UXBZSSBXGPYSIL-UHFFFAOYSA-K yttrium(iii) phosphate Chemical compound [Y+3].[O-]P([O-])([O-])=O UXBZSSBXGPYSIL-UHFFFAOYSA-K 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title abstract 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title abstract 3
- 238000003756 stirring Methods 0.000 claims abstract description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 229960004887 ferric hydroxide Drugs 0.000 claims abstract description 10
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 14
- 239000000084 colloidal system Substances 0.000 claims description 8
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 5
- 235000019800 disodium phosphate Nutrition 0.000 claims description 5
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- -1 stirs 6~8h Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims 1
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 3
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- 238000001782 photodegradation Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 230000015556 catabolic process Effects 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
- 239000002244 precipitate Substances 0.000 description 3
- 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 2
- 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 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- KWMKCPAIFULUBU-UHFFFAOYSA-N phosphoric acid yttrium Chemical compound [Y].P(O)(O)(O)=O KWMKCPAIFULUBU-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010409 thin film 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
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- 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
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
本发明公开一种氧化铁/磷酸钇复合催化剂的制备方法,依次包括如下步骤:将10mL浓度为0.1~0.5mol/L硝酸亚铁溶液置于温度为60~80℃水浴中,滴加浓度为40~80mmol/L的碳酸钠溶液5~8mL,搅拌4~6h,形成氢氧化铁胶体物质;在40~60℃水浴下,向5~10mL浓度为0.1~0.5mol/L的硝酸钇溶液中边搅拌边滴加10~15mL浓度为0.2~0.8mol/L磷酸氢二钠溶液,搅拌60~100min后,沉淀,加入氢氧化铁胶体物质,搅拌6~8h,固液分离,将固体用去离子水洗涤3~5遍,在105℃下烘干;将烘干得到的产品在400~600℃下煅烧5~8h,即可得到一种氧化铁/磷酸钇复合催化剂。所制得的催化剂有较好的晶体结构且有有较大的比表面积,稳定,光降解处理效率高。
Description
技术领域
本发明涉及环境污染控制新材料领域,尤其涉及一种氧化铁/磷酸钇复合催化剂的制备方法。
背景技术
随着科技的发展,来自工农业生产中产生的毒害有机污染物严重威胁着环境和人类的健康,寻求一种新型高效的环境治理技术具有重要的意义。光催化技术因其节能、高效、污染物降解彻底、无二次污染优点,目前已成为一种具有重要应用前景的新兴环境治理技术。近年来,新型高效的可见光光催化剂的研制成为光催化技术中的一个重要研究内容,其中具有表面等离子共振效应的光催化材料,因其独特的表面物理化学性质和高效的可见光光催化性能,成为研究的热点之一。
然而,目前所报道的可见光光催化材料大多具有较高的光生载流子复合率和较差的可见光吸收,导致其量子效率较低。因此,开发新型高效可见光光催化材料,拓展半导体材料光谱响应范围以及促进光生电子和空穴有效分离,成为目前光催化材料研究领域急需解决的科学问题。
发明内容
本发明的目的是为克服现有技术中光催化降解污染物过程中的不足,提供一种氧化铁/磷酸钇复合催化剂的制备方法。
为此,本发明提供了以下技术方案,一种氧化铁/磷酸钇复合催化剂的制备方法,依次包括如下步骤:
1)将10mL浓度为0.1~0.5mol/L硝酸亚铁溶液置于温度为60~80℃水浴中,滴加浓度为40~80mmol/L的碳酸钠溶液5~8mL,搅拌4~6h,形成氢氧化铁胶体物质;
2)在40~60℃水浴下,向5~10mL浓度为0.1~0.5mol/L的硝酸钇溶液中边搅拌边滴加10~15mL浓度为0.2~0.8mol/L磷酸氢二钠溶液,搅拌60~100min后,沉淀,加入氢氧化铁胶体物质,搅拌6~8h,固液分离,将固体用去离子水洗涤3~5遍,在105℃下烘干;
3)将烘干得到的产品在400~600℃下煅烧5~8h,即可得到一种氧化铁/磷酸钇复合催化剂。
本发明具有以下优越性:在该过程中利用铁氢氧化物形成的胶体物质在磷酸钇固体表面形成薄膜,形成均匀的复合体。经过煅烧后,形成铁的氧化物和磷酸钇复合,所制得的催化剂有较好的晶体结构且有较大的比表面积,稳定,光降解处理效率高。
具体实施方式
下面结合实施例来详细说明本发明,但本发明并不仅限于此。
实施例1
将10mL浓度为0.5mol/L硝酸亚铁溶液置于温度为80℃水浴中,滴加浓度为80mmol/L的碳酸钠溶液8mL,搅拌6h,形成氢氧化铁胶体物质;在60℃水浴下,向10mL浓度为0.5mol/L的硝酸钇溶液中边搅拌边滴加15mL浓度为0.8mol/L磷酸氢二钠溶液,搅拌100min后,沉淀,加入氢氧化铁胶体物质,搅拌8h,固液分离,将固体用去离子水洗涤5遍,在105℃下烘干;将烘干得到的产品在600℃下煅烧8h,即可得到一种氧化铁/磷酸钇复合催化剂。
将制得的氧化铁/磷酸钇复合催化剂用于处理含酸性大红废水:0.3g氧化铁/磷酸钇复合催化剂加入到50mL浓度为10mg/L的酸性大红废水中,在300w金卤灯照射下,反应1h,脱色率为92.1%。
实施例2
将10mL浓度为0.1mol/L硝酸亚铁溶液置于温度为60℃水浴中,滴加浓度为40mmol/L的碳酸钠溶液5mL,搅拌4h,形成氢氧化铁胶体物质;在40℃水浴下,向5mL浓度为0.1mol/L的硝酸钇溶液中边搅拌边滴加10mL浓度为0.2mol/L磷酸氢二钠溶液,搅拌60min后,沉淀,加入氢氧化铁胶体物质,搅拌6h,固液分离,将固体用去离子水洗涤3遍,在105℃下烘干;将烘干得到的产品在400℃下煅烧5h,即可得到一种氧化铁/磷酸钇复合催化剂。
将制得的氧化铁/磷酸钇复合催化剂用于处理含亚甲基蓝废水:0.3g氧化铁/磷酸钇复合催化剂加入到50mL浓度为10mg/L的亚甲基蓝废水中,在300w金卤灯照射下,反应1h,脱色率为93.1%。
实施例3
将10mL浓度为0.2mol/L硝酸亚铁溶液置于温度为80℃水浴中,滴加浓度为70mmol/L的碳酸钠溶液8mL,搅拌6h,形成氢氧化铁胶体物质;在60℃水浴下,向8mL浓度为0.4mol/L的硝酸钇溶液中边搅拌边滴加10mL浓度为0.2mol/L磷酸氢二钠溶液,搅拌60min后,沉淀,加入氢氧化铁胶体物质,搅拌8h,固液分离,将固体用去离子水洗涤5遍,在105℃下烘干;将烘干得到的产品在600℃下煅烧8h,即可得到一种氧化铁/磷酸钇复合催化剂。
将制得的氧化铁/磷酸钇复合催化剂用于处理含金橙II废水:0.3g氧化铁/磷酸钇复合催化剂加入到100mL浓度为10mg/L的金橙II废水中,在300w金卤灯照射下,反应1h,脱色率为93.5%。
Claims (1)
1.一种氧化铁/磷酸钇复合催化剂的制备方法,其特征在于:1)将10mL浓度为0.1~0.5mol/L硝酸亚铁溶液置于温度为60~80℃水浴中,滴加浓度为40~80mmol/L的碳酸钠溶液5~8mL,搅拌4~6h,形成氢氧化铁胶体物质;
2)在40~60℃水浴下,向5~10mL浓度为0.1~0.5mol/L的硝酸钇溶液中边搅拌边滴加10~15mL浓度为0.2~0.8mol/L磷酸氢二钠溶液,搅拌60~100min后,沉淀,加入氢氧化铁胶体物质,搅拌6~8h,固液分离,将固体用去离子水洗涤3~5遍,在105℃下烘干;
3)将烘干得到的产品在400~600℃下煅烧5~8h,即可得到一种氧化铁/磷酸钇复合催化剂。
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CN102941107A (zh) * | 2012-11-27 | 2013-02-27 | 武汉工程大学 | 用于光催化的磷酸银/二氧化钛复合材料及其制备方法 |
CN103480400A (zh) * | 2013-09-22 | 2014-01-01 | 江苏大学 | 一种磷酸银/氧化锌复合光催化材料及其制备方法 |
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CN103894216A (zh) * | 2014-03-27 | 2014-07-02 | 常州大学 | 一种磁性纳米磷酸银/二氧化钛复合光催化材料的制备方法 |
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CN102941107A (zh) * | 2012-11-27 | 2013-02-27 | 武汉工程大学 | 用于光催化的磷酸银/二氧化钛复合材料及其制备方法 |
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CN103553014A (zh) * | 2013-11-12 | 2014-02-05 | 青岛大学 | 一种磷酸钇纳米材料的制备方法 |
CN103894216A (zh) * | 2014-03-27 | 2014-07-02 | 常州大学 | 一种磁性纳米磷酸银/二氧化钛复合光催化材料的制备方法 |
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Title |
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