CN105749916B - 一种富勒醇/水铁矿光催化材料 - Google Patents
一种富勒醇/水铁矿光催化材料 Download PDFInfo
- Publication number
- CN105749916B CN105749916B CN201610097427.7A CN201610097427A CN105749916B CN 105749916 B CN105749916 B CN 105749916B CN 201610097427 A CN201610097427 A CN 201610097427A CN 105749916 B CN105749916 B CN 105749916B
- Authority
- CN
- China
- Prior art keywords
- fullerol
- ferrihydrite
- catalysis material
- solution
- sodium hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000463 material Substances 0.000 title claims abstract description 60
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 46
- 239000013049 sediment Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 11
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000015556 catabolic process Effects 0.000 claims abstract description 8
- 238000006731 degradation reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 3
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 33
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 11
- 239000012498 ultrapure water Substances 0.000 claims description 11
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 8
- 230000001699 photocatalysis Effects 0.000 claims description 7
- 238000007146 photocatalysis Methods 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 239000000356 contaminant Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 229910052742 iron Inorganic materials 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000005416 organic matter Substances 0.000 abstract description 5
- 238000004065 wastewater treatment Methods 0.000 abstract description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 13
- 239000002351 wastewater Substances 0.000 description 12
- 239000000975 dye Substances 0.000 description 10
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- 239000010865 sewage Substances 0.000 description 7
- 239000000987 azo dye Substances 0.000 description 6
- 230000005855 radiation Effects 0.000 description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 5
- 239000012901 Milli-Q water Substances 0.000 description 5
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229940032296 ferric chloride Drugs 0.000 description 5
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 5
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910001415 sodium ion Inorganic materials 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000006298 dechlorination reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 229910003472 fullerene Inorganic materials 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000005297 material degradation process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 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 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010893 paper waste Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
-
- 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
- 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
-
- 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
-
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
本发明公开了一种富勒醇/水铁矿光催化材料。其制备方法包括以下步骤：1)将三价铁化合物溶液和氢氧化钠溶液同时缓慢加入富勒醇溶液中，并维持pH为6.5～7.5，搅拌0.5～2 h后，分离出沉淀物，洗涤干净；2）将沉淀物干燥后研磨成粉末状，即得富勒醇/水铁矿光催化材料。本发明的富勒醇/水铁矿光催化材料，其催化降解有机物的效果要远远高于纯水铁矿。本发明方法制备得到的富勒醇/水铁矿光催化材料中水铁矿与富勒醇结合更牢固，有利于回收利用，重复使用次数高，可降低废水处理成本，是一个环保、经济的工艺技术；且本发明制备方法简单、可操作性好。
Description
技术领域
本发明具体涉及一种富勒醇/水铁矿光催化材料。
背景技术
随着现代工业的飞速发展，工业生产过程中使用的大量有机试剂以及反应后的副产物排放导致了日常生活中各种各样的污染。其中，印染工业中排放的染料给环境造成了巨大污染。因为印染行业的有机染料具有生物毒性大、抗氧化性强、组分复杂、生物降解难等特点，不仅给工业废水的处理带来了很大的麻烦，而且也给我们日常生活带来了严重污染，严重地危害到了人类的身体健康。因而如何有效地降解有机废水已经成为全球研究学者共同面临的重大问题。
目前工业上染料废水的处理工艺通常是采用物理化学法和生物法相结合。选择合适的处理方法需要考虑工艺（处理效率、装置简单等）和经济上（投资和运营成本等）的可行性。常用的染料废水处理方法存在以下缺点：（1）费用高，例如吸附脱色法中活性炭再生费用昂贵；（2）生物处理成本较低，但微生物对营养物质、pH等条件有一定要求，难以适应染料废水水质波动大，染料种类多，毒性高等特点；（3）污染物从水相中转移到其他相造成污染，例如物理吸附法。因此，越来越多的研究致力于发明一种高效、环境友好型的染料处理方法，其中，高级氧化技术（AOP）能有效的处理水和固体中的有机污染物，是一种很有应用前景的处理方法。主要的AOP技术有O3/H2O2、O3/UV、UV/H2O2、Fenton和光助Fenton等反应类型。其中光助Fenton法因具有反应速度快、能有效地降解有毒且难生化降解的有机污染物以及操作简单等优点而越来越受到人们的关注。
水铁矿是自然环境中一种常见的土壤矿物，其具有颗粒尺寸小（通常在2～100 nm左右），比表面积大，并且表面拥有大量的羟基官能团等特点，是一种天然的吸附剂，同时还是一种天然的Fenton催化剂。然而当水铁矿作为光Fenton催化剂时，其在可见光下的催化效果远远不及紫外光辐射下的催化效果。由于太阳光中只有3%-5%的紫外光能到达地球表面，因此对水铁矿进行改性来促进其在可见光辐射下的催化很有必要。
碳纳米材料如富勒烯及其衍生物富勒醇由于其特殊的纳米效应而表现出优异的力学、光学、电学、催化等性能，在电子、医学、制药、环保、能源等众多领域得到了广泛的应用。但是利用富勒烯/富勒醇在异相Fenton催化材料中还未见报道。
发明内容
本发明的目的在于提供一种富勒醇/水铁矿光催化材料，该材料的制备方法操作简单，成本低廉，对设备的要求低。本方法合成的富勒醇/水铁矿光催化材料可作为光催化材料，适用于各种废水的深度处理，环保无二次污染。
本发明所采取的技术方案是：
一种富勒醇/水铁矿光催化材料，其制备方法包括以下步骤：
1)将三价铁化合物溶液和氢氧化钠溶液同时缓慢加入富勒醇溶液中，并维持pH为6.5～7.5，搅拌0.5～2 h后，分离出沉淀物，洗涤干净；
2)将沉淀物干燥后研磨成粉末状，即得富勒醇/水铁矿光催化材料。
优选的，步骤1）中三价铁化合物选自氯化铁、硝酸铁或硝酸铁水合物。
优选的，步骤1）中三价铁化合物、氢氧化钠和富勒醇溶液使用超纯水或者纯水溶解配制。
优选的，步骤1）三价铁化合物水溶液的浓度为0.4～1 mol/L。
优选的，步骤1）中氢氧化钠溶液的浓度为1～6 mol/L。
优选的，步骤1）中所述富勒醇溶液制备时需先超声10～15分钟，然后调整浓度为0.5～1 g/L。
优选的，步骤1）中三价铁化合物溶液和氢氧化钠溶液滴加到富勒醇溶液中的速度为1～10 mL/min。
优选的，步骤1）中在室温条件下搅拌，转速为600～1000 r/min。
优选的，步骤2）干燥为冷冻干燥，温度为-40±5℃，干燥时间不低于24 h。
富勒醇/水铁矿光催化材料在光催化降解有机污染物中的应用，所述富勒醇/水铁矿光催化材料如上述任一项所述。
优选的，应用领域包括染料废水，造纸废水等。
本发明的有益效果是：
本研究首次发现以水铁矿为代表的地质吸附剂能有效的吸附富勒醇，利用富勒醇和水铁矿复合制备得到新型光催化材料。
本发明的富勒醇/水铁矿光催化材料受光激发时，能大大加速Fe3+向Fe2+的转变，从而加速双氧水的分解，产生更多的羟基自由基，进一步促进有机物的催化降解。富勒醇/水铁矿光催化材料的催化降解有机物的效果要远远高于纯水铁矿。
本发明方法制备得到的富勒醇/水铁矿光催化材料中水铁矿与富勒醇结合更牢固，有利于回收利用，重复使用次数高，可降低废水处理成本，是一个环保、经济的工艺技术；且本发明制备方法简单、可操作性好。
本发明的材料具有粒径均匀、无团聚、分散性好等优点，在可见光辐射下去除水中高浓度有机污染物，有机废水处理效果好，环保且无二次污染。
鉴于目前富勒醇的使用越来越多，未来使用后的富勒醇纳米材料被当做垃圾排放进入环境中聚集后可能产生生态毒性，进而造成环境污染。利用本发明的技术可以用水铁矿与污水中的富勒醇反应制备得到富勒醇/水铁矿光催化材料，从而在反应过程中去除富勒醇。此外，由于水铁矿比表面积大，在本发明的反应过程中能去除高浓度的富勒醇，大大优于传统的吸附方法。所以本发明技术可用于未来富勒醇污染的治理。
附图说明
图1是实施例1产物的XRD光谱图。
具体实施方式
下面结合具体的实施例对本发明作进一步的说明，但并不局限于此。
实施例1
1、一种富勒醇/水铁矿光催化材料，其制备方法包括以下步骤：
1）称取10.81 g（40 mmol）六水合氯化铁溶于40 mL超纯水中；称取4.8 g氢氧化钠（120 mmol）置于40 mL的超纯水中；称取0.2 g富勒醇置于超纯水中并超声10分钟，然后定容至500 mL；
2）将上述氯化铁溶液和氢氧化钠溶液同时缓慢滴入富勒醇溶液中，滴加速度为2mL/min，磁力搅拌2 h，搅拌速度为800 r/min，分离出沉淀物，用超纯水洗涤数次，去除氯离子和钠离子；
3）将上述洗干净的沉淀物在-40℃条件下冷冻干燥24 h后，置于研钵中研磨成粉末状，研磨后过200目及以上的筛，即得富勒醇/水铁矿光催化材料。
2、X-射线衍射分析实验（XRD）
XRD 表征结果如图1所示，实施例1制备材料中，富勒醇/水铁矿光催化材料和水铁矿原土的衍射峰一致，均是在35°和62°处有2个大宽峰，表明富勒醇的引入不会改变水铁矿的结构。
3、污水处理实验
实验方法：以偶氮染料酸性红18为处理对象，在500 mL废水（废水中偶氮染料酸性红18浓度为100 mg/L）中加入4 mM H2O2和0.8 g实例1所得的材料，经过3小时可见光照射后，该材料降解酸性红18的TOC去除率为92%。
实施例2
一种富勒醇/水铁矿光催化材料，其制备方法包括以下步骤：
1）称取10.81 g（40 mmol）六水合氯化铁溶于80 mL超纯水中；称取4.8 g氢氧化钠（120 mmol）置于80 mL的超纯水中；称取0.1 g富勒醇置于超纯水中并超声10分钟，然后定容至500 mL；
2）将上述氯化铁溶液和氢氧化钠溶液同时缓慢滴入富勒醇溶液中，滴加速度为1mL/min，磁力搅拌2 h，搅拌速度为800 r/min，分离出沉淀物，用超纯水洗涤数次，去除氯离子和钠离子；
3）将上述洗干净的沉淀物在-40℃条件下冷冻干燥28 h后，置于玛瑙研钵中研磨成粉末状，研磨后过200目及以上的筛，即得富勒醇/水铁矿光催化材料。
实施例3
一种富勒醇/水铁矿光催化材料，其制备方法包括以下步骤：
1）称取10.81 g（40 mmol）六水合氯化铁溶于100 mL超纯水中；称取4.8 g氢氧化钠（120 mmol）置于100 mL的超纯水中；称取0.05 g富勒醇置于超纯水中并超声10分钟，然后定容至500 mL；
2）将上述氯化铁溶液和氢氧化钠溶液同时缓慢滴入富勒醇溶液中，滴加速度为4mL/min，磁力搅拌2 h，搅拌速度为600 r/min，分离出沉淀物，用超纯水洗涤数次，去除氯离子和钠离子；
3）将上述洗干净的沉淀物在-40℃条件下冷冻干燥32 h后，置于研钵中研磨成粉末状，研磨后过200目及以上的筛，即得富勒醇/水铁矿光催化材料。
实施例4
一种富勒醇/水铁矿光催化材料，其制备方法包括以下步骤：
1）称取10.81 g（40 mmol）六水合氯化铁溶于60 mL超纯水中；称取4.8 g氢氧化钠（120 mmol）置于60 mL的超纯水中；称取0.4 g富勒醇置于超纯水中并超声10分钟，然后定容至500 mL；
2）将上述氯化铁溶液和氢氧化钠溶液同时缓慢滴入富勒醇溶液中，滴加速度为5mL/min，磁力搅拌2 h，搅拌速度为600 r/min，分离出沉淀物，用超纯水洗涤数次，去除氯离子和钠离子；
3）将上述洗干净的沉淀物在-40℃条件下冷冻干燥24 h后，置于研钵中研磨成粉末状，研磨后过200目及以上的筛，即得富勒醇/水铁矿光催化材料。
重复利用实验
对实施例1用于污水处理实验后的富勒醇/水铁矿光催化材料进行回收利用，离心去除上清液，并将固体用于重复实验。
对回收后的富勒醇/水铁矿光催化材料再次进行光催化污水处理实验。
实验方法：以偶氮染料酸性红18为处理对象，在500 mL废水（废水中偶氮染料酸性红18浓度为100 mg/L）中加入4 mM H2O2和上述回收得到的富勒醇/水铁矿光催化材料，经过3小时可见光照射后，该材料降解酸性红18的TOC去除率为88%，说明该材料的稳定性强，重复使用效果好。
综上所述，本发明方法制备得到的富勒醇/水铁矿光催化材料中水铁矿与富勒醇结合更牢固，有利于回收利用，重复使用次数高，可降低废水处理成本，是一个环保、经济的工艺技术；且本发明制备方法简单、可操作性好。
对比例1
一种水铁矿光催化材料，其制备方法包括以下步骤：
1）称取10.81 g（40 mmol）六水合氯化铁溶于60 mL超纯水中；称取4.8 g氢氧化钠（120 mmol）置于60 mL的超纯水中；
2）将氢氧化钠溶液和氯化铁溶液同时滴加进入500 mL的水中，滴加速度为5 mL/min，磁力搅拌2 h，搅拌速度为600 r/min，分离出沉淀物，用超纯水洗涤数次，去除氯离子和钠离子；
3）将上述洗干净的沉淀物在-40℃条件下冷冻干燥24 h后，置于研钵中研磨成粉末状，研磨后过200目及以上的筛，即得水铁矿光催化材料。
下面对对比例1制备的材料作效果检测。
污水处理实验方法：以偶氮染料酸性红18为处理对象，在500 mL废水（废水中偶氮染料酸性红18浓度为100 mg/L）中加入4 mM H2O2和0.8 g对比例1所得的材料，经过3小时可见光照射后，该材料对降解酸性红18的TOC去除率为52%。结果表明：对比例1制备得到的水铁矿光催化材料对于有机物的催化降解能力低于本发明制备得到的富勒醇/水铁矿光催化材料。
对比例2
利用富勒醇进行污水处理实验。
污水处理实验方法：以偶氮染料酸性红18为处理对象，在500 mL废水（废水中偶氮染料酸性红18浓度为100 mg/L）中加入4 mM H2O2和0.8 g富勒醇，经过3小时可见光照射后，该材料对降解酸性红18的TOC去除几乎无效果。结果表明：单纯利用富勒醇作为光催化材料，其对于有机物的催化降解能力完全低于本发明制备得到的富勒醇/水铁矿光催化材料。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (10)
1.一种富勒醇/水铁矿光催化材料，其特征在于，其制备方法包括以下步骤：
1）将三价铁化合物溶液和氢氧化钠溶液同时缓慢加入富勒醇溶液中，并维持pH为6.5～7.5，搅拌0.5～2 h后，分离出沉淀物，洗涤干净；
2）将沉淀物干燥后研磨成粉末状，即得富勒醇/水铁矿光催化材料。
2.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤1）中三价铁化合物选自氯化铁、硝酸铁或硝酸铁水合物。
3.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤1）中三价铁化合物、氢氧化钠和富勒醇溶液使用超纯水或者纯水溶解配制。
4.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤1）三价铁化合物水溶液的浓度为0.4～1 mol/L。
5.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤1）中氢氧化钠溶液的浓度为1～6 mol/L。
6.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤1）中富勒醇溶液制备时需先超声10～15分钟，然后调整浓度为0.5～1 g/L。
7.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤1）中三价铁化合物溶液和氢氧化钠溶液滴加到富勒醇溶液中的速度为1～10 mL/min。
8.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤1）中在室温条件下搅拌，转速为600～1000 r/min。
9.根据权利要求1所述的富勒醇/水铁矿光催化材料，其特征在于：步骤2）干燥为冷冻干燥，温度为-40±5℃，干燥时间不低于24 h。
10.富勒醇/水铁矿光催化材料在光催化降解有机污染物中的应用，其特征在于：所述富勒醇/水铁矿光催化材料如权利要求1-9任一项所述。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610097427.7A CN105749916B (zh) | 2016-02-22 | 2016-02-22 | 一种富勒醇/水铁矿光催化材料 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610097427.7A CN105749916B (zh) | 2016-02-22 | 2016-02-22 | 一种富勒醇/水铁矿光催化材料 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105749916A CN105749916A (zh) | 2016-07-13 |
| CN105749916B true CN105749916B (zh) | 2018-07-24 |
Family
ID=56331076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610097427.7A Expired - Fee Related CN105749916B (zh) | 2016-02-22 | 2016-02-22 | 一种富勒醇/水铁矿光催化材料 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105749916B (zh) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110252316B (zh) * | 2019-07-04 | 2020-05-22 | 华南理工大学 | 中空二氧化铈微球负载水铁矿多相类芬顿催化剂及其制备方法与应用 |
| CN113351162B (zh) * | 2021-06-07 | 2023-03-17 | 东北农业大学 | 一种炭基掺磷水铁矿的制备方法及其应用 |
| CN113926487A (zh) * | 2021-09-14 | 2022-01-14 | 杭州师范大学 | 一种富勒醇/钯纳米复合光催化剂及其制备方法、应用 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190423A (zh) * | 2014-09-25 | 2014-12-10 | 四川理工学院 | 一种圆球状α-Fe2O3的制备方法 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5782229B2 (ja) * | 2010-03-31 | 2015-09-24 | 株式会社神鋼環境ソリューション | 排水処理方法 |
-
2016
- 2016-02-22 CN CN201610097427.7A patent/CN105749916B/zh not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190423A (zh) * | 2014-09-25 | 2014-12-10 | 四川理工学院 | 一种圆球状α-Fe2O3的制备方法 |
Non-Patent Citations (2)
| Title |
|---|
| Visible light enhanced removal of a sulfur mustard gas surrogate from a vapor phase on novel hydrous ferric oxide/graphite oxide composites;Javier A. Arcibar-Orozco等;《J. Mater. Chem. A》;20141028;第3卷;第220-231页 * |
| 富勒醇-二氧化钛纳米复合材料制备及光催化性能的研究;杨凯;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20150115;第20-29页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105749916A (zh) | 2016-07-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Khan et al. | Heterogeneous photodegradation of industrial dyes: An insight to different mechanisms and rate affecting parameters | |
| Ziembowicz et al. | Limitations and future directions of application of the Fenton-like process in micropollutants degradation in water and wastewater treatment: A critical review | |
| Wang et al. | Recent advances in biochar-based catalysts: properties, applications and mechanisms for pollution remediation | |
| Hu et al. | Catalytic degradation of p-nitrophenol by magnetically recoverable Fe3O4 as a persulfate activator under microwave irradiation | |
| Nawaz et al. | Fabrication and characterization of new ternary ferrites-chitosan nanocomposite for solar-light driven photocatalytic degradation of a model textile dye | |
| Shi et al. | Degradation of organic dyes by a new heterogeneous Fenton reagent-Fe2GeS4 nanoparticle | |
| Rayaroth et al. | Advanced oxidation processes for the removal of mono and polycyclic aromatic hydrocarbons–A review | |
| Chen et al. | Fe2O3/TiO2 functionalized biochar as a heterogeneous catalyst for dyes degradation in water under Fenton processes | |
| Alizadeh et al. | Removal of Cd (ӀӀ) and phenol using novel cross-linked magnetic EDTA/chitosan/TiO2 nanocomposite | |
| Karimipourfard et al. | Novel heterogeneous degradation of mature landfill leachate using persulfate and magnetic CuFe2O4/RGO nanocatalyst | |
| Hung et al. | N-doped metal-free biochar activation of peroxymonosulfate for enhancing the degradation of antibiotics sulfadiazine from aquaculture water and its associated bacterial community composition | |
| Rizwan et al. | Hydrogen-based sono-hybrid catalytic degradation and mitigation of industrially-originated dye-based pollutants | |
| Huang et al. | Kinetic study of an immobilized iron oxide for catalytic degradation of azo dye reactive black B with catalytic decomposition of hydrogen peroxide | |
| Shi et al. | Magnetite nanoparticles modified β-cyclodextrin PolymerCoupled with KMnO4 oxidation for adsorption and degradation of acetaminophen | |
| Diao et al. | A new insight on enhanced Pb (II) removal by sludge biochar catalyst coupling with ultrasound irradiation and its synergism with phenol removal | |
| Wang et al. | Enhanced photocatalytic New Coccine degradation and Pb (II) reduction over graphene oxide-TiO2 composite in the presence of aspartic acid-β-cyclodextrin | |
| Wei et al. | Photo-Fenton degradation of methyl orange using H3PW12O40 supported Fe-bentonite catalyst | |
| CN110756163A (zh) | 一种纳米CoFe2O4/碳纤维毡复合材料及其制备方法和应用 | |
| CN105749916B (zh) | 一种富勒醇/水铁矿光催化材料 | |
| Ji et al. | Treatment of reverse osmosis (RO) concentrate from an old landfill site by Fe0/PS/O3 process | |
| Yaping et al. | Photo-Fenton degradation of 17β-estradiol in presence of α-FeOOHR and H2O2 | |
| Zeng et al. | Immobilization of phototroph-derived extracellular polymer for simultaneous removal of antibiotics and heavy metals: a sustainable approach for advanced treatment of secondary effluent | |
| Wu et al. | Heterogeneous Fenton-like degradation of an azo dye reactive brilliant orange by the combination of activated carbon–FeOOH catalyst and H2O2 | |
| Van et al. | Enhanced heterogeneous Fenton degradation of p-nitrophenol by Fe3O4 nanoparticles decorated cellulose aerogel from banana stem | |
| Iqbal et al. | Efficient removal of norfloxacin using nano zerovalent cerium composite biochar-catalyzed peroxydisulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180724 Termination date: 20210222 |