CN114146707A - Preparation method of iron oxide film/glass fiber photo-assisted Fenton composite material - Google Patents
Preparation method of iron oxide film/glass fiber photo-assisted Fenton composite material Download PDFInfo
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- CN114146707A CN114146707A CN202010925831.5A CN202010925831A CN114146707A CN 114146707 A CN114146707 A CN 114146707A CN 202010925831 A CN202010925831 A CN 202010925831A CN 114146707 A CN114146707 A CN 114146707A
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- glass fiber
- iron oxide
- ferric
- composite material
- oxide film
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000003365 glass fiber Substances 0.000 title claims abstract description 76
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 230000001699 photocatalysis Effects 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000007146 photocatalysis Methods 0.000 claims abstract 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 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
- 235000015165 citric acid Nutrition 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 229960002413 ferric citrate Drugs 0.000 claims description 3
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 3
- OHZCFWMJMWFNFP-ZVGUSBNCSA-L (2r,3r)-2,3-dihydroxybutanedioate;iron(2+) Chemical compound [Fe+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O OHZCFWMJMWFNFP-ZVGUSBNCSA-L 0.000 claims description 2
- SFOKDWPZOYRZFF-UHFFFAOYSA-H 2,3-dihydroxybutanedioate;iron(3+) Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O SFOKDWPZOYRZFF-UHFFFAOYSA-H 0.000 claims description 2
- JLLRXSCNTCSLFX-UHFFFAOYSA-H 2-hydroxybutanedioate;iron(3+) Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C(O)CC([O-])=O.[O-]C(=O)C(O)CC([O-])=O.[O-]C(=O)C(O)CC([O-])=O JLLRXSCNTCSLFX-UHFFFAOYSA-H 0.000 claims description 2
- YNVZDODIHZTHOZ-UHFFFAOYSA-K 2-hydroxypropanoate;iron(3+) Chemical compound [Fe+3].CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O YNVZDODIHZTHOZ-UHFFFAOYSA-K 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- DKKCQDROTDCQOR-UHFFFAOYSA-L Ferrous lactate Chemical compound [Fe+2].CC(O)C([O-])=O.CC(O)C([O-])=O DKKCQDROTDCQOR-UHFFFAOYSA-L 0.000 claims description 2
- 229910021575 Iron(II) bromide Inorganic materials 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- GPWHDDKQSYOYBF-UHFFFAOYSA-N ac1l2u0q Chemical compound Br[Br-]Br GPWHDDKQSYOYBF-UHFFFAOYSA-N 0.000 claims description 2
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 claims description 2
- 229940046149 ferrous bromide Drugs 0.000 claims description 2
- 235000013925 ferrous lactate Nutrition 0.000 claims description 2
- 239000004225 ferrous lactate Substances 0.000 claims description 2
- 229940037907 ferrous lactate Drugs 0.000 claims description 2
- 229960001781 ferrous sulfate Drugs 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 229940057006 ferrous tartrate Drugs 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- WHRBSMVATPCWLU-UHFFFAOYSA-K iron(3+);triformate Chemical compound [Fe+3].[O-]C=O.[O-]C=O.[O-]C=O WHRBSMVATPCWLU-UHFFFAOYSA-K 0.000 claims description 2
- LHOWRPZTCLUDOI-UHFFFAOYSA-K iron(3+);triperchlorate Chemical compound [Fe+3].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O LHOWRPZTCLUDOI-UHFFFAOYSA-K 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- GYCHYNMREWYSKH-UHFFFAOYSA-L iron(ii) bromide Chemical compound [Fe+2].[Br-].[Br-] GYCHYNMREWYSKH-UHFFFAOYSA-L 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims 3
- 150000007513 acids Chemical class 0.000 claims 1
- 159000000014 iron salts Chemical class 0.000 claims 1
- 238000003980 solgel method Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000003618 dip coating Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000010802 sludge Substances 0.000 description 3
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 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
- 238000003756 stirring Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
Classifications
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- B01J35/39—
-
- 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
-
- B01J35/61—
-
- 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
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
-
- 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
Abstract
The invention discloses a preparation method of an iron oxide film/glass fiber photo-assisted Fenton composite material, and relates to application of the iron oxide film/glass fiber composite material in photocatalysis. The preparation method comprises the steps of cleaning glass fiber, then soaking the glass fiber into iron oxide sol prepared by a sol-gel method, and then coating a film by a dip-coating method. And then calcined in a muffle furnace to obtain the sample. The method is simple and convenient, is easy to operate and is convenient for large-area production.
Description
Technical Field
The invention relates to the preparation of photocatalytic composite materials. In particular to a preparation method of an iron oxide film/glass fiber composite material. Belongs to the technical field of photocatalytic composite materials.
Background
With the development of economy, the proportion of urban industrialization is continuously increased, and a large amount of wastewater is generated in the production process of numerous chemical enterprises. More and more water resources are contaminated by contaminants, such as antibiotics, herbicides, dyes and dairy waste, etc., that are generated during the production process and are not effectively disposed of. The traditional wastewater treatment methods in China are many, such as ozone treatment, biodegradation, coagulation sedimentation and advanced oxidation technology. In advanced oxidation technology, Fenton (Fenton-like) isThe wide scientists consider it to be one of the most effective methods. Fenton reaction using Fe2+And H2O2Reaction to form OH and O2 -The organic matters can be mineralized rapidly by utilizing the strong oxidizing property of the organic matters. The conventional fenton reaction still has drawbacks. Wherein the utilization ratio of the light source, H2O2The control of the amount of use, the narrow range of pH use and the residual iron sludge after fenton reaction remain problems to be overcome.
According to the invention, iron oxide is uniformly loaded on the surface of the glass fiber, and the light source is effectively and reasonably utilized by utilizing the property that the glass fiber gathers and transmits light. The problem of iron sludge in the catalytic process is solved. And the prepared iron oxide film is composed of nano-structure iron oxide particles, so that the contact area with sewage is effectively increased, and more active sites are added in the catalysis process. In addition, the iron oxide film/glass fiber composite material has the advantages of simple synthesis process, low raw material price, small environmental pollution, easy large-scale production and easy recovery, so that the iron oxide film/glass fiber composite material can treat sewage on a large scale and relieve the river pollution problem.
Disclosure of Invention
Aiming at the problems and improvement requirements of the prior ferric oxide in the traditional Fenton reaction for sewage treatment, the invention aims to provide a preparation method of a ferric oxide film/glass fiber photo-assisted Fenton composite material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an iron oxide film/glass fiber photo-assisted Fenton composite material comprises the following steps: (1) cleaning glass fiber with isopropanol for 1-5 times, soaking in dilute hydrochloric acid solution for 10-180 min, cleaning with anhydrous alcohol for 1-5 times, cleaning with deionized water for 1-5 times, cleaning, soaking, and drying. (2) Adding a certain amount of ferric salt (including ferrous nitrate, ferrous chloride, ferrous sulfate, ferrous bromide, ferrous lactate, ferrous acetate, ferrous tartrate, ferric nitrate, ferric chloride, ferric sulfate, ferric tribromide, ferric perchlorate, ferric dihydrogen phosphate, ferric formate, ferric citrate, ferric lactate, ferric acetate, ferric tartrate and ferric malate) and glycol into a beaker in sequence, wherein the volume of the glycol is 5-100mL, continuously heating under magnetic stirring, and adding a certain molar ratio of polycarboxylic acid (including one of citric acid, tartaric acid, oxalic acid, malic acid, citric acid and ascorbic acid) when the temperature reaches 20-80 ℃. The ratio of the ferric salt to the polycarboxylic acid is 1: 0.25-1: 10, the temperature is continuously raised to 80-120 ℃, and the mixture is kept stirring for 0.5-10h to continue the reaction. Pouring the sol into a clean beaker after the reaction is finished, and (3) soaking the cleaned glass fiber into the prepared sol for 0.1-24 h. Then pulling the fiber from the solution at the speed of 1mm/min-20cm/min, drying the pulled fiber at room temperature, and calcining the fiber at the temperature of 100-1000 ℃ for 1-10h to obtain the iron oxide film/glass fiber.
The obtained iron oxide/glass fiber composite material is tested for catalytic performance in a photoreactor, and prepared methyl orange dye is added into a beaker, and then catalyst and H are added2O2Then, the photocatalytic degradation is carried out under the irradiation of a xenon lamp, and a certain solution is taken out at certain time intervals to measure the absorbance of the solution, so that the degradation rate of the dye is calculated.
Compared with other preparation methods, the preparation method of the iron oxide film/glass fiber photo-assisted Fenton composite material provided by the invention has the advantages that the source of the required material is wide and easy to obtain, the equipment is simple, the operation is convenient, the economy and the safety are realized, and the prepared material has high catalytic activity. The reason is that the glass fiber gathers and transmits light, so that a light source can be more fully utilized in the light Fenton process, the light loss is reduced, the pH application range of the Fenton reaction is widened, and the generation of iron sludge in the reaction process is reduced. The iron oxide prepared by the sol-gel method has a grid structure, the specific surface area of the material is increased, more active sites can be exposed in the catalysis process, and the catalysis efficiency is improved.
Drawings
FIG. 1 XRD pattern of iron oxide/glass fiber
FIG. 2 SEM image of iron oxide/glass fiber
FIG. 3 is a graph showing the degradation efficiency of iron oxide/glass fiber on methyl orange solution
Detailed description of the preferred embodiments
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
The experimental procedures in the following examples are conventional unless otherwise specified. The test materials used in the following examples were purchased from a conventional reagent store unless otherwise specified. In the quantitative tests in the following examples, three replicates were set, and the data are the mean or mean standard deviation of the three replicates.
The preparation method of the iron oxide film/glass fiber photo-assisted Fenton composite material comprises the following steps:
example 1
Cleaning the glass fiber in isopropanol for 3 times, then soaking the cleaned glass fiber in dilute hydrochloric acid for 30min, then cleaning the glass fiber with deionized water for 3 times, cleaning the glass fiber with absolute ethyl alcohol for 2 times, and drying the glass fiber for later use.
Adding 0.01mol of ferric nitrate into 20mL of glycol, adding 0.005mol of citric acid when the temperature rises to 50 ℃, continuing to rise the temperature to 90 ℃, and continuing to react for 1h to obtain sol.
The cleaned glass fibers were dipped into the prepared sol for 3 hours, then pulled up at a speed of 10cm/min, and then dried at room temperature. Then calcined at 300 ℃ for 5h to obtain a sample.
Example 2
Cleaning the glass fiber in isopropanol for 5 times, soaking the cleaned glass fiber in dilute hydrochloric acid for 80min, cleaning with deionized water for 3 times, cleaning with absolute ethyl alcohol for 2 times, and drying for later use.
Adding 0.01mol of ferric chloride into 20mL of ethylene glycol, adding 0.005mol of oxalic acid when the temperature is raised to 40 ℃, continuously raising the temperature to 100 ℃, and continuously reacting for 5 hours to obtain sol.
The cleaned glass fibers were dipped into the prepared sol for 3 hours, then pulled up at a speed of 10cm/min, and then dried at room temperature. Then calcined at 400 ℃ for 2h to obtain a sample.
Example 3
Cleaning the glass fiber in isopropanol for 3 times, soaking the cleaned glass fiber in dilute hydrochloric acid for 50min, cleaning with deionized water for 4 times, cleaning with absolute ethyl alcohol for 5 times, and drying for later use.
Adding 0.01mol of ferric citrate into 50mL of ethylene glycol, adding 0.005mol of tartaric acid when the temperature is raised to 70 ℃, continuously raising the temperature to 110 ℃, and continuously reacting for 1h to obtain sol.
The cleaned glass fibers were dipped into the prepared sol for 5 hours, then pulled up at a speed of 1cm/min, and then dried at room temperature. Then calcined at 500 ℃ for 2h to obtain a sample.
Example 4
Cleaning the glass fiber in isopropanol for 3 times, soaking the cleaned glass fiber in dilute hydrochloric acid for 50min, cleaning with deionized water for 4 times, cleaning with absolute ethyl alcohol for 2 times, and drying for later use.
0.01mol of ferric sulfate is added into 70mL of glycol, 0.01mol of tartaric acid is added when the temperature rises to 80 ℃, the temperature is continuously raised to 120 ℃, and the reaction is continuously carried out for 1h, so as to obtain the sol.
The cleaned glass fibers were dipped into the prepared sol for 3 hours, then pulled up at a speed of 10cm/min, and then dried at room temperature. Then calcined at 500 ℃ for 2h to obtain a sample.
Example 5
Cleaning the glass fiber in isopropanol for 3 times, then soaking the cleaned glass fiber in dilute hydrochloric acid for 30min, then cleaning the glass fiber with deionized water for 3 times, cleaning the glass fiber with absolute ethyl alcohol for 2 times, and drying the glass fiber for later use.
Adding 0.01mol of ferric chloride into 20mL of glycol, adding 0.005mol of citric acid when the temperature rises to 50 ℃, continuing to rise the temperature to 90 ℃, and continuing to react for 1h to obtain sol.
The cleaned glass fibers were dipped into the prepared sol for 3 hours, then pulled up at a speed of 1cm/min, and then dried at room temperature. Then calcined at 300 ℃ for 5h to obtain a sample.
Example 6
Cleaning the glass fiber in isopropanol for 3 times, soaking the cleaned glass fiber in dilute hydrochloric acid for 20min, cleaning with deionized water for 1 time, cleaning with absolute ethyl alcohol for 4 times, and drying for later use.
Adding 0.01mol of ferric nitrate into 60mL of glycol, adding 0.03mol of citric acid when the temperature rises to 30 ℃, continuing to heat to 100 ℃, and continuing to react for 5 hours to obtain sol.
The cleaned glass fibers were dipped into the prepared sol for 4 hours, then pulled up at a speed of 1cm/min, and then dried at room temperature. Then calcined at 400 ℃ for 2h to obtain a sample.
Example 7
Cleaning the glass fiber in isopropanol for 3 times, then soaking the cleaned glass fiber in dilute hydrochloric acid for 60min, then cleaning with deionized water for 3 times, cleaning with absolute ethyl alcohol for 2 times, and drying for later use.
Adding 0.01mol of ferrous chloride into 20mL of ethylene glycol, adding 0.03mol of malic acid when the temperature rises to 70 ℃, continuing to heat to 110 ℃, and continuing to react for 2h to obtain sol.
The cleaned glass fibers were dipped into the prepared sol for 3 hours, then pulled up at a speed of 5cm/min, and then dried at room temperature. Then calcined at 400 ℃ for 2h to obtain a sample.
The research result of the iron oxide film/glass fiber photo-assisted Fenton composite material is as follows:
(1) photocatalytic performance analysis
As can be seen in the degradation graph of iron oxide/glass fibers versus methyl orange, there was substantially no degradation for 120min under Ultraviolet (UV) irradiation alone, little degradation for 120min under UV irradiation and the presence of iron oxide/glass fibers, and H in the dark2O2And Fe2O3Under the conditions of (1) the degradation rate at 120min is 18.3%, H in the dark2O2And Fe2O3The degradation rate of the glass fibers at 120min was 14.3%, and under UV irradiation, H2O2In the presence of 120miThe degradation rate of n was 70.97%, but under UV irradiation, there was H2O2And Fe2O3The degradation rate of 120min under the condition of glass fiber is 100%, and the iron oxide/glass fiber composite material prepared by different catalytic process comparison shows that the iron oxide/glass fiber composite material has excellent catalytic performance.
(2) Structural analysis of materials
The prepared iron oxide is the most stable alpha-Fe obtained from the XRD pattern of the prepared iron oxide/glass fiber composite material2O3，α-Fe2O3Is Fe under ambient conditions2O3Shows weak ferromagnetism at room temperature, alpha-Fe2O3The unit cell of (A) is hexagonal and contains only octahedrally coordinated Fe3+The atoms can cause the regular displacement of Fe ions or other metal ions to become active sites, and greatly promote the catalytic capability and catalytic property. The iron oxide can be well loaded on the surface of the glass fiber through an SEM image of the composite material, and the prepared iron oxide has a mesh structure, so that the iron oxide has a large specific surface area and has good catalytic performance in a catalytic process.
The above embodiments are merely provided to help understanding the method and core concept of the present invention, and all modifications and variations that do not depart from the spirit of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. The preparation method of the iron oxide film/glass fiber photo-assisted Fenton composite material is characterized by comprising the following steps of:
(1) cleaning and soaking the glass fiber by using isopropanol, dilute hydrochloric acid, deionized water and absolute ethyl alcohol solution;
(2) adding iron salts with different concentrations into ethylene glycol, heating to a certain temperature, adding polycarboxylic acids with different concentrations, continuously heating to a certain temperature, and reacting for a period of time to obtain iron oxide sol;
(3) soaking the treated glass fiber in iron oxide sol for a certain time, and then lifting the glass fiber from the iron oxide sol at different lifting rates, so that the iron oxide sol is uniformly coated on the surface of the glass fiber;
(4) and calcining the glass fiber coated with the oxidized iron gel in the air atmosphere to obtain the ferric oxide film/glass fiber photo-assisted Fenton composite material.
2. The method for preparing an iron oxide film/glass fiber photo-assisted Fenton composite material according to claim 1, wherein the method for cleaning and soaking the glass fiber in the step (1) comprises cleaning in isopropanol 1-5 times, soaking in diluted hydrochloric acid for 10min-180min, cleaning with absolute ethyl alcohol 1-5 times, and cleaning with deionized water 1-5 times.
3. The method for preparing an iron oxide film/glass fiber photo-assisted fenton composite material according to claim 1, wherein the iron salt added in step (2) is one of ferrous nitrate, ferrous chloride, ferrous sulfate, ferrous bromide, ferrous lactate, ferrous acetate, ferrous tartrate, ferric nitrate, ferric chloride, ferric sulfate, ferric tribromide, ferric perchlorate, ferric dihydrogen phosphate, ferric formate, ferric citrate, ferric lactate, ferric acetate, ferric tartrate and ferric malate, and the volume of ethylene glycol used is 5-100 mL. The added polycarboxylic acid is one of citric acid, tartaric acid, oxalic acid, malic acid, citric acid and ascorbic acid, and the molar ratio of the iron salt to the polycarboxylic acid is 1: 0.25-1: 10.
4. The method for preparing an iron oxide film/glass fiber photo-assisted Fenton composite material according to claim 1, wherein in the step (2), the iron salt is added into the ethylene glycol to be heated at a temperature of 20-80 ℃, then the polycarboxylic acid is added, the temperature is continuously raised to 80-120 ℃, and the reaction is carried out for 0.5-10 h.
5. The method for preparing an iron oxide film/glass fiber photo-assisted Fenton composite material according to claim 1, wherein the cleaned glass fiber is soaked in the prepared sol for 0.1-24h in the step (3), and then pulled at a speed of 1mm/min-20 cm/min.
6. The method for preparing an iron oxide film/glass fiber photo-assisted Fenton composite material according to claim 1, wherein the step (4) comprises calcining the glass fiber coated with the oxidized iron gel in an air atmosphere, wherein the calcining temperature is 100 ℃ and 1000 ℃, and the holding time is 1-10 h.
7. An iron oxide/glass fiber composite material obtained by the production method according to any one of claims 1 to 6.
8. Use of the iron oxide/glass fiber composite according to claim 7 in photocatalysis, in particular in fenton's reactions.
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