CN108786852A - 一种用于光芬顿反应材料的制备方法 - Google Patents
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 7
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 7
- -1 iron sulfide cadmium sulfide compound Chemical class 0.000 claims abstract description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 7
- 238000013019 agitation Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 abstract description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052980 cadmium sulfide Inorganic materials 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract description 2
- FRLJSGOEGLARCA-UHFFFAOYSA-N cadmium sulfide Chemical compound [S-2].[Cd+2] FRLJSGOEGLARCA-UHFFFAOYSA-N 0.000 abstract 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 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 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 229960004887 ferric hydroxide Drugs 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000009303 advanced oxidation process 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
- 238000001354 calcination Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 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
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2101/30—Organic compounds
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
本发明公开一种用于光芬顿反应材料的制备方法,依次包括如下步骤:在搅拌条件下,同时向浓度为0.5~2mol/L的氯化铁溶液中滴加浓度为0.5~1mol/L的氢氧化钠溶液、浓度为0.01~0.03mol/L的氯化镉和浓度为1~3mol/L的硫化钠溶液,保持Fe3+:OH‑:Cd2+:S2‑=8:4:1:14,沉淀分离,将固体用去离子水洗涤2~3次,105℃烘干;将得到的固体置于马弗炉中,在300~400℃下煅烧2~3h,制得硫化铁硫化镉复合物,即为一种用于光芬顿反应材料。该方法硫化铁和硫化镉复合有助于促进参与反应的Fe3+/Fe2+之间的循环,突破芬顿反应的速度控制步骤,使有机物降解速度大大加快。
Description
技术领域
本发明涉及环境污染控制领域,尤其涉及一种用于光芬顿反应材料的制备方法。
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。水体中含有大量的有机污染物,它们以毒性和使水中溶解氧减少的形式对生态系统产生影响,危害人体健康。
随着我国国民经济的快速发展,高浓度的有机废水对我国宝贵的水资源造成了威胁。然而利用现有的生物处理方法,对可生化性差、相对分子质量从几千到几万的物质处理较困难,而高级氧化法可将其直接矿化或通过氧化提高污染物的可生化性,同时还在环境类激素等微量有害化学物质的处理方面具有很大的优势,能够使绝大部分有机物完全矿化或分解,具有很好的应用前景。
传统的芬顿反应速度慢,主要原因是反应过程中二价铁离子和三价铁离子之间循环速度限制了整个芬顿反应过程。
发明内容
本发明的目的是为克服现有技术的不足,提供一种用于光芬顿反应材料的制备方法。
本发明采用的技术方案是依次包括如下步骤:
1)在搅拌条件下,同时向浓度为0.5~2mol/L的氯化铁溶液中滴加浓度为0.5~1mol/L的氢氧化钠溶液、浓度为0.01~0.03mol/L的氯化镉和浓度为1~3mol/L的硫化钠溶液,保持Fe3+:OH-:Cd2+:S2-=8:4:1:14,沉淀分离,将固体用去离子水洗涤2~3次,105℃烘干;
2)将得到的固体置于马弗炉中,在300~400℃下煅烧2~3h,制得硫化铁硫化镉复合物,即为一种用于光芬顿反应材料。
本发明的优点是:
(1)在氯化铁溶液中滴加少量氢氧化钠溶液,形成氢氧化铁胶体形成载体,同时滴加过量硫化钠和氯化镉形成硫化铁及硫化镉颗粒,硫化铁硫化镉颗粒附着在氢氧化铁胶体表面,经过煅烧后,形成均匀的复合物。
(2)硫化镉有助于硫化铁表面的芬顿反应进行,促进表面参与反应的Fe3+/Fe2+之间的循环,突破芬顿反应的速度控制步骤,使有机物降解速度大大加快。
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
在搅拌条件下,同时向浓度为2mol/L的氯化铁溶液中滴加浓度为1mol/L的氢氧化钠溶液、浓度为0.03mol/L的氯化镉和浓度为3mol/L的硫化钠溶液,保持Fe3+:OH-:Cd2+:S2-=8:4:1:14,沉淀分离,将固体用去离子水洗涤3次,105℃烘干;将得到的固体置于马弗炉中,在400℃下煅烧3h,制得硫化铁硫化镉复合物,即为一种用于光芬顿反应材料。
将制得的光芬顿反应材料加入到待处理的浓度为1mg/L的苯酚废水中,加入30μL质量浓度为30%的双氧水,在120W的LED灯照射下,搅拌100min,沉淀分离,去除率为96.2%,上清液可以排放。
实施例2
在搅拌条件下,同时向浓度为0.5mol/L的氯化铁溶液中滴加浓度为0.5mol/L的氢氧化钠溶液、浓度为0.01mol/L的氯化镉和浓度为1mol/L的硫化钠溶液,保持Fe3+:OH-:Cd2+:S2-=8:4:1:14,沉淀分离,将固体用去离子水洗涤2次,105℃烘干;将得到的固体置于马弗炉中,在300℃下煅烧2h,制得硫化铁硫化镉复合物,即为一种用于光芬顿反应材料。
将制得的光芬顿反应材料加入到待处理的浓度为10mg/L的亚甲基蓝废水中,加入30μL质量浓度为30%的双氧水,在120W的LED灯照射下,搅拌50min,沉淀分离,去除率为95.1%,上清液可以排放。
以市售的硫化铁为材料,将同样量的硫化铁,投入相同条件下的废水中,经过同样的反应时间,去除率只有56.8%。复合材料大大提高了降解速度。
实施例3
在搅拌条件下,同时向浓度为1mol/L的氯化铁溶液中滴加浓度为1mol/L的氢氧化钠溶液、浓度为0.02mol/L的氯化镉和浓度为2mol/L的硫化钠溶液,保持Fe3+:OH-:Cd2+:S2-=8:4:1:14,沉淀分离,将固体用去离子水洗涤3次,105℃烘干;将得到的固体置于马弗炉中,在400℃下煅烧3h,制得硫化铁硫化镉复合物,即为一种用于光芬顿反应材料。
将制得的光芬顿反应材料加入到待处理的浓度为10mg/L的亚甲基蓝废水中,加入30μL质量浓度为30%的双氧水,在120W的LED灯照射下,搅拌50min,沉淀分离,去除率为95.9%,上清液可以排放。
Claims (1)
1.一种用于光芬顿反应材料的制备方法,其特征是依次包括如下步骤:
1)在搅拌条件下,同时向浓度为0.5~2mol/L的氯化铁溶液中滴加浓度为0.5~1mol/L的氢氧化钠溶液、浓度为0.01~0.03mol/L的氯化镉和浓度为1~3mol/L的硫化钠溶液,保持Fe3+:OH-:Cd2+:S2-=8:4:1:14,沉淀分离,将固体用去离子水洗涤2~3次,105℃烘干;
2)将得到的固体置于马弗炉中,在300~400℃下煅烧2~3h,制得硫化铁硫化镉复合物,即为一种用于光芬顿反应材料。
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CN110773200A (zh) * | 2019-11-27 | 2020-02-11 | 绍兴文理学院 | 一种生物炭载硫化铁类芬顿催化剂的制备方法 |
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CN106238053A (zh) * | 2016-07-06 | 2016-12-21 | 华南理工大学 | 一种光芬顿催化剂Fe3O4/rGO/TiO2及其制备方法和应用 |
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CN107720930A (zh) * | 2017-11-20 | 2018-02-23 | 华东理工大学 | 一种含硫化物的工业废水处理用试剂及其反应方法 |
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CN104190422A (zh) * | 2014-09-22 | 2014-12-10 | 北京师范大学 | 一种异相光芬顿催化剂及其用途 |
CN105562036A (zh) * | 2015-12-15 | 2016-05-11 | 同济大学 | 一种铁硫多相类芬顿催化剂的制备方法及应用 |
CN106238053A (zh) * | 2016-07-06 | 2016-12-21 | 华南理工大学 | 一种光芬顿催化剂Fe3O4/rGO/TiO2及其制备方法和应用 |
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CN107720930A (zh) * | 2017-11-20 | 2018-02-23 | 华东理工大学 | 一种含硫化物的工业废水处理用试剂及其反应方法 |
Cited By (2)
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CN110773200A (zh) * | 2019-11-27 | 2020-02-11 | 绍兴文理学院 | 一种生物炭载硫化铁类芬顿催化剂的制备方法 |
CN110773200B (zh) * | 2019-11-27 | 2022-10-25 | 绍兴文理学院 | 一种生物炭载硫化铁类芬顿催化剂的制备方法 |
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