CN107096555A - 一种碳酸钴复合磷酸钴光催化剂的制备方法 - Google Patents
一种碳酸钴复合磷酸钴光催化剂的制备方法 Download PDFInfo
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- 229910021446 cobalt carbonate Inorganic materials 0.000 title claims abstract description 43
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 title claims abstract description 43
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- REERVHLUKHFRQT-UHFFFAOYSA-N cobalt phosphoric acid Chemical compound [Co].P(O)(O)(O)=O REERVHLUKHFRQT-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 150000001875 compounds Chemical class 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000000084 colloidal system Substances 0.000 claims abstract description 24
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical class [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 18
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 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
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 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 7
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 7
- 239000011734 sodium Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 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
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 3
- 239000010452 phosphate Substances 0.000 claims abstract description 3
- 238000004821 distillation Methods 0.000 claims abstract 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 claims 1
- 150000001869 cobalt compounds Chemical class 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001699 photocatalysis Effects 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
- 241000220317 Rosa Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910000152 cobalt phosphate Inorganic materials 0.000 description 1
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 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
- 239000008187 granular material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 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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- 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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
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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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- 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
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明公开一种碳酸钴复合磷酸钴光催化剂的制备方法,具体步骤如下:称取12~16mmol硝酸钴,配置成12mmol/L的硝酸钴溶液,称取6.6~8mmol碳酸钠,配置成16mmol/L的碳酸钠溶液;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,在搅拌过程中碳酸钠和硝酸钴反应,生成碳酸钴胶体;将碳酸钴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,再将该碳酸钴胶体加入到60~80mL浓度为2~4mol/L的磷酸钠溶液中,浸泡2~4天,在碳酸钴颗粒表面形成磷酸钴纳米颗粒,固液分离,去离子水洗涤固体2~3次,75~105℃烘干,制得一种碳酸钴复合磷酸钴光催化剂。该方法是在碳酸钴表面形成催化剂,催化剂和载体紧密结合。
Description
技术领域
本发明涉及一种碳酸钴复合磷酸钴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。碳酸钴由于其本身特性的限制,在光催化降解方面,性能还有待提高。
发明内容
本发明的目的在于针对现有技术的不足,提出一种碳酸钴复合磷酸钴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硝酸钴,配置成12mmol/L的硝酸钴溶液,称取6.6~8mmol碳酸钠,配置成16mmol/L的碳酸钠溶液;
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,在搅拌过程中碳酸钠和硝酸钴反应,生成碳酸钴胶体;
3)将碳酸钴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,再将该碳酸钴胶体加入到60~80mL浓度为2~4mol/L的磷酸钠溶液中,浸泡2~4天,在碳酸钴颗粒表面形成磷酸钴纳米颗粒,固液分离,去离子水洗涤固体2~3次,75~105℃烘干,制得一种碳酸钴复合磷酸钴光催化剂。
本发明的有益效果是:(1)本方法利用溶度积常数的差异,在碳酸钴表面形成溶度积常数更小的磷酸钴颗粒。
(2)碳酸钴和磷酸钴复合,协同作用,可以使碳酸钴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硝酸钴,配置成12mmol/L的硝酸钴溶液,称取8mmol碳酸钠,配置成16mmol/L的碳酸钠溶液;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,在搅拌过程中碳酸钠和硝酸钴反应,生成碳酸钴胶体;将碳酸钴胶体置于半透膜袋内,用蒸馏水洗涤3次,去除掉游离离子,再将该碳酸钴胶体加入到60mL浓度为2mol/L的磷酸钠溶液中,浸泡2天,在碳酸钴颗粒表面形成磷酸钴纳米颗粒,固液分离,去离子水洗涤固体2次,75℃烘干,制得一种碳酸钴复合磷酸钴光催化剂。
将得到的碳酸钴复合磷酸钴光催化剂0.5g加入到300mL浓度为10mg/L的亚甲基蓝废水中,在300w金卤灯照射下,反应30min,脱色率为93.7%,催化剂分离后可以重复利用。
实施例2
称取12mmol硝酸钴,配置成12mmol/L的硝酸钴溶液,称取6.6mmol碳酸钠,配置成16mmol/L的碳酸钠溶液;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,在搅拌过程中碳酸钠和硝酸钴反应,生成碳酸钴胶体;将碳酸钴胶体置于半透膜袋内,用蒸馏水洗涤4次,去除掉游离离子,再将该碳酸钴胶体加入到80mL浓度为4mol/L的磷酸钠溶液中,浸泡4天,在碳酸钴颗粒表面形成磷酸钴纳米颗粒,固液分离,去离子水洗涤固体3次,105℃烘干,制得一种碳酸钴复合磷酸钴光催化剂。
将得到的碳酸钴复合磷酸钴光催化剂0.5g加入到300mL浓度为20mg/L的金橙7废水中,在300w金卤灯照射下,反应30min,脱色率为94.7%,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,纯碳酸钴的降解效率为62.9%,大大提高了其作用效果。
实施例3
称取14mmol硝酸钴,配置成12mmol/L的硝酸钴溶液,称取7mmol碳酸钠,配置成16mmol/L的碳酸钠溶液;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,在搅拌过程中碳酸钠和硝酸钴反应,生成碳酸钴胶体;将碳酸钴胶体置于半透膜袋内,用蒸馏水洗涤4次,去除掉游离离子,再将该碳酸钴胶体加入到70mL浓度为3mol/L的磷酸钠溶液中,浸泡3天,在碳酸钴颗粒表面形成磷酸钴纳米颗粒,固液分离,去离子水洗涤固体3次,95℃烘干,制得一种碳酸钴复合磷酸钴光催化剂。
将得到的碳酸钴复合磷酸钴光催化剂0.5g加入到300mL浓度为20mg/L的玫瑰红B废水中,在300w金卤灯照射下,反应30min,脱色率为96.1%,催化剂分离后可以重复利用。
Claims (1)
1.一种碳酸钴复合磷酸钴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硝酸钴,配置成12mmol/L的硝酸钴溶液,称取6.6~8mmol碳酸钠,配置成16mmol/L的碳酸钠溶液;
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,在搅拌过程中碳酸钠和硝酸钴反应,生成碳酸钴胶体;
3)将碳酸钴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,再将该碳酸钴胶体加入到60~80mL浓度为2~4mol/L的磷酸钠溶液中,浸泡2~4天,在碳酸钴颗粒表面形成磷酸钴纳米颗粒,固液分离,去离子水洗涤固体2~3次,75~105℃烘干,制得一种碳酸钴复合磷酸钴光催化剂。
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