CN107469829A - 一种碳复合钨酸铁催化剂的制备方法 - Google Patents
一种碳复合钨酸铁催化剂的制备方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 25
- 239000002253 acid Substances 0.000 title claims abstract description 19
- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 15
- 150000001875 compounds Chemical class 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring 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 6
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims abstract description 5
- 238000003763 carbonization Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 150000007524 organic acids Chemical class 0.000 abstract description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 150000001722 carbon compounds Chemical class 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002351 wastewater Substances 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
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000002925 chemical effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- SSWAPIFTNSBXIS-UHFFFAOYSA-N dioxido(dioxo)tungsten;iron(2+) Chemical compound [Fe+2].[O-][W]([O-])(=O)=O SSWAPIFTNSBXIS-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 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
- 238000001556 precipitation Methods 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
- 238000003860 storage Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
-
- B01J35/39—
-
- 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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
Abstract
本发明公开了一种碳复合钨酸铁催化剂的制备方法,步骤如下:向100~200mL水中加入5~10g钨酸钠,搅拌,同时向其中缓慢滴加5~10g/L的柠檬酸溶液20~50mL,滴加完成后,再加入6~8g氯化铁粉末,搅拌4~5h,在室温下陈化24~48h,然后去除上清液,蒸馏水洗涤固体3~4次,105℃烘干,再置于马弗炉中,在氮气保护下,在350~550℃下煅烧2~5h,即得到一种碳复合钨酸铁催化剂。本发明的优点是:利用钨酸钠和柠檬酸生成有机酸络合物,再和铁反应,生成沉淀物,最后经过碳化,即得碳复合钨酸铁催化剂。催化效果有大大提高。
Description
技术领域
本发明涉及环境污染控制新材料领域,尤其涉及一种碳复合钨酸铁催化剂的制备方法。
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。
作为钨酸盐材料中的特殊组成成员,钨酸铁纳米材料因含有特殊过渡金属元素,且集量子效应和小尺寸效应等特殊物理化学效应于一体,而广泛应用于光学、磁学以及能量存储等重要功能领域。现阶段,钨酸铁在水处理领域应用还比较少见,主要是因为降解效率相对较低。
发明内容
本发明的目的是为克服现有技术的不足,提供一种碳复合钨酸铁催化剂的制备方法。
本发明采用的技术方案是依次包括如下步骤:
向100~200mL水中加入5~10g钨酸钠,搅拌,同时向其中缓慢滴加5~10g/L的柠檬酸溶液20~50mL,滴加完成后,再加入6~8g氯化铁粉末,搅拌4~5h,在室温下陈化24~48h,然后去除上清液,蒸馏水洗涤固体3~4次,105℃烘干,再置于马弗炉中,在氮气保护下,在350~550℃下煅烧2~5h,即得到一种碳复合钨酸铁催化剂。
本发明的优点是:利用钨酸钠和柠檬酸生成有机酸络合物,再和铁反应,生成沉淀物,最后经过碳化,即得碳复合钨酸铁催化剂。催化效果有大大提高。
具体实施方式
以下进一步提供本发明的3个实施例:
实施例1
向200mL水中加入10g钨酸钠,搅拌,同时向其中缓慢滴加10g/L的柠檬酸溶液50mL,滴加完成后,再加入8g氯化铁粉末,搅拌5h,在室温下陈化48h,然后去除上清液,蒸馏水洗涤固体4次,105℃烘干,再置于马弗炉中,在氮气保护下,在550℃下煅烧5h,即得到一种碳复合钨酸铁催化剂。
0.5g碳复合钨酸铁催化剂加入到100mL浓度为10mg/L的苯酚废水中,在120W的LED灯照射下,反应120min,降解率为97.2%。
实施例2
向100mL水中加入5g钨酸钠,搅拌,同时向其中缓慢滴加5g/L的柠檬酸溶液20mL,滴加完成后,再加入6g氯化铁粉末,搅拌4h,在室温下陈化24h,然后去除上清液,蒸馏水洗涤固体3次,105℃烘干,再置于马弗炉中,在氮气保护下,在350℃下煅烧2h,即得到一种碳复合钨酸铁催化剂。
0.5g碳复合钨酸铁催化剂加入到150mL浓度为25mg/L的亚甲基蓝废水中,在120W的LED灯照射下,反应120min,脱色率为95.6%。
实施例3
向150mL水中加入8g钨酸钠,搅拌,同时向其中缓慢滴加8g/L的柠檬酸溶液30mL,滴加完成后,再加入5g氯化铁粉末,搅拌5h,在室温下陈化48h,然后去除上清液,蒸馏水洗涤固体4次,105℃烘干,再置于马弗炉中,在氮气保护下,在550℃下煅烧4h,即得到一种碳复合钨酸铁催化剂。
0.5g碳复合钨酸铁催化剂加入到100mL浓度为30mg/L的罗丹明B废水中,在120W的LED灯照射下,反应120min,脱色率为94.7%。
Claims (1)
1.一种碳复合钨酸铁催化剂的制备方法,其特征是依次包括如下步骤:
向100~200mL水中加入5~10g钨酸钠,搅拌,同时向其中缓慢滴加5~10g/L的柠檬酸溶液20~50mL,滴加完成后,再加入6~8g氯化铁粉末,搅拌4~5h,在室温下陈化24~48h,然后去除上清液,蒸馏水洗涤固体3~4次,105℃烘干,再置于马弗炉中,在氮气保护下,在350~550℃下煅烧2~5h,即得到一种碳复合钨酸铁催化剂。
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CN110776016A (zh) * | 2019-09-29 | 2020-02-11 | 河北科技大学 | 用于超级电容器的电极材料钨酸钴的合成方法 |
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CN102336440A (zh) * | 2011-06-28 | 2012-02-01 | 福州大学 | 高纯度单斜相ZnWO4纳米颗粒的制备方法及其应用 |
CN102531062A (zh) * | 2012-03-02 | 2012-07-04 | 河北联合大学 | 一种厚度均匀的钨酸铁超薄纳米片的结构控制制备 |
CN102784624A (zh) * | 2012-07-23 | 2012-11-21 | 合肥工业大学 | 一种炭包覆磁性吸附材料的制备方法及其用途 |
CN105753060A (zh) * | 2016-05-06 | 2016-07-13 | 洛阳理工学院 | 一种纺锤形钨酸铁微米晶体的制备工艺 |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102336440A (zh) * | 2011-06-28 | 2012-02-01 | 福州大学 | 高纯度单斜相ZnWO4纳米颗粒的制备方法及其应用 |
CN102531062A (zh) * | 2012-03-02 | 2012-07-04 | 河北联合大学 | 一种厚度均匀的钨酸铁超薄纳米片的结构控制制备 |
CN102784624A (zh) * | 2012-07-23 | 2012-11-21 | 合肥工业大学 | 一种炭包覆磁性吸附材料的制备方法及其用途 |
CN105753060A (zh) * | 2016-05-06 | 2016-07-13 | 洛阳理工学院 | 一种纺锤形钨酸铁微米晶体的制备工艺 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110776016A (zh) * | 2019-09-29 | 2020-02-11 | 河北科技大学 | 用于超级电容器的电极材料钨酸钴的合成方法 |
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