CN110756163A - Nano CoFe2O4Carbon fiber felt composite material and preparation method and application thereof - Google Patents
Nano CoFe2O4Carbon fiber felt composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000835 fiber Substances 0.000 title claims description 6
- 239000004917 carbon fiber Substances 0.000 claims abstract description 117
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 114
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 113
- 229910002518 CoFe2O4 Inorganic materials 0.000 claims abstract description 41
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 29
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 29
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 27
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 27
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
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- 239000008367 deionised water Substances 0.000 claims abstract description 10
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- 239000002351 wastewater Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
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- 238000012824 chemical production Methods 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- FIKAKWIAUPDISJ-UHFFFAOYSA-L paraquat dichloride Chemical compound [Cl-].[Cl-].C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 FIKAKWIAUPDISJ-UHFFFAOYSA-L 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
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- 229920006395 saturated elastomer Polymers 0.000 description 1
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- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
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- 241000894007 species Species 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
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- B01J35/33—
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- B01J35/39—
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- 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
- C02F2101/00—Nature of the contaminant
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- C02F2101/306—Pesticides
Abstract
The invention relates to nano CoFe2O4The material is prepared from carbon fiber felt and magnetic nano material CoFe2O4The components of the composition are as follows,nano CoFe2O4Uniformly attached on the carbon fiber felt. The preparation method comprises dissolving ferric chloride and cobalt chloride in ethylene glycol, adding anhydrous sodium acetate, and stirring; adding the carbon fiber felt into the solution, and carrying out hydrothermal reaction after vacuum placement; soaking with deionized water to neutrality, and oven drying. The method is simple and environment-friendly, and the synthesized composite material has a larger specific surface area due to the use of the carbon fiber felt as a carrier, so that the adsorption capacity of the material on the pollutants is increased, and the adsorption catalytic degradation capacity of the composite material on the pollutants in the wastewater is further improved. And CoFe2O4The carbon fiber felt has certain magnetism, is easy to recover under the action of a magnetic field, and has wide application prospect in the field of adsorbing-catalyzing water pollutants.
Description
Technical Field
The invention relates to the fields of high polymer materials, inorganic non-metallic materials and water pollutant degradation, in particular to nano CoFe2O4A preparation method and application of a carbon fiber felt composite material.
Background
In recent years, environmental pollution is enhanced, which poses serious threats to ecological balance, human health and sustainable development of social economy, and environmental purification is widely regarded worldwide. Among the pollution, water pollution is the key point of environmental purification due to wide pollution range, high harm degree and difficult treatment. In fact, a large amount of wastewater is generated in various fields in production and life, such as chemical production, medical pharmacy, textile production, pesticide irrigation, domestic sewage discharge and the like. The discharged wastewater can cause great harm to the natural environment without being treated, and the untreated wastewater which is discharged randomly flows into rivers, lakes and seas, thereby causing great harm to the life and health of human beings. At present, the treatment methods used for the pollution include adsorption, biological treatment, chemical treatment, catalytic oxidation, phase transfer, photocatalytic degradation and the like. Among them, adsorption, catalytic oxidation and biological treatment are one of the more common methods. The pollutants can be rapidly removed by adsorption, but saturated adsorption is easily achieved to be inactivated, and secondary pollution can be caused by desorption regeneration of the adsorbent. The technology combining catalytic oxidation and biological treatment has a good effect on treating water body pollution, but wastes time and labor and has large investment. The photocatalysis technology is an environment-friendly green technology. Under the excitation of light, the semiconductor material generates active species with strong oxidizability, and the species can generate oxidation-reduction reaction with most organic pollutant molecules to completely mineralize the organic pollutant molecules into carbon dioxide, water, mineral acid or salt and the like. Compared with the traditional pollutant treatment method, the photocatalysis technology has the advantages that (1) the removal degree is high, and no secondary pollution is caused; (2) no other chemical species need to be introduced into the reaction; (3) the organic matter can be degraded by using cheap solar energy.
The invention discloses a cobalt ferrite loaded graphene aerogel catalyst which is used for efficiently degrading and removing various pollutants such as phenols, dyes, antibiotics and the like. The invention discloses CoFe for activating persulfate to deeply treat coking wastewater2O4The nitrogen-doped sludge-based activated carbon catalyst treats wastewater and solves the problem of sludge disposal of a coking plant under the action of a magnetic field. Ferrite materials are considered to be a relatively effective semiconductor among many catalysts, both magnetic and photocatalytic. The material can generate electrons and holes under ultraviolet or visible light, and generate redox reaction with organic matters to decompose some organic matters into inorganic matters such as water, carbon dioxide and the like without introducing other impurities; meanwhile, the catalyst has magnetism, and can be separated from the solvent by using the action of an external magnetic field, so that the catalyst can be recycled. CoFe2O4The nanoparticles are nearThe alloy is concerned by researchers in the year, and has the advantages of small radius, high chemical stability, high hardness and the like. As a magnetic material, CoFe2O4Can be directly used as a photocatalyst which can be separated magnetically. However, the existing CoFe2O4The structure and properties of the material itself have limited its commercial production on a large scale. The main problems are shown in that: firstly, the forbidden band is too wide, and only ultraviolet light can be absorbed and utilized, and the utilization rate of solar energy is too low; secondly, the rate of photon-generated electron-hole recombination is high, the effective utilization rate of photon-generated excitons is low, and the reaction rate is slow, so that the water pollutants are difficult to degrade rapidly. The properties of the material are not only related to the composition and the crystal structure of the material, but also closely related to the granularity, the morphology and the structure of the material. When CoFe2O4When the particle size of the particles is reduced to a nanometer level, the properties of the material are greatly improved. When the particle size of the semiconductor particles is reduced to a nanometer size range, the photocatalytic activity of the material can be greatly improved.
In order to overcome the defect of single material in performance, researchers adopt an organic or inorganic mode to prepare the nano CoFe2O4The composite material is used for improving the catalytic performance and the adsorption performance of the material. The adsorption technology is combined with the photocatalysis technology, the respective advantages of adsorption and catalysis are exerted, and the water body pollutants are rapidly degraded under the synergistic effect. At present, CoFe is used at home and abroad2O4The porous active adsorption material is adopted for most of the loads, and the materials with adsorption activity can effectively adsorb target products to CoFe2O4The photocatalytic activity is improved around the catalyst. Based on the method, the nano spinel type CoFe is prepared2O4The carbon fiber felt composite material has high adsorption-catalysis performance, is environment-friendly and can be recycled for many times.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the nanometer CoFe with larger specific surface area and good adsorption performance2O4Carbon fiber felt composite material and preparation thereofThe method is applied to removing water body pollutants.
The invention also provides nano CoFe2O4The application of the carbon fiber felt composite material in the aspect of catalyzing and degrading organic pollutants in waste water.
The purpose of the invention can be realized by the following technical scheme:
nano CoFe2O4A carbon fiber felt composite material which is made of nano CoFe2O4And carbon fiber felt, nano CoFe2O4Uniformly attached to the fiber surface of the carbon fiber felt.
The nano CoFe2O4The particle size of (A) is 90 to 100 nm.
The invention also provides the nanometer CoFe2O4The preparation method of the carbon fiber felt composite material comprises the following steps:
(1) uniformly dispersing ferric chloride and cobalt chloride in an organic solvent, and then adding anhydrous sodium acetate and uniformly stirring to obtain a mixed solution;
(2) adding a carbon fiber felt into the mixed solution, standing at room temperature for 20-40 min under a vacuum environment with a vacuum degree of 0.09MPa, and then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle for hydrothermal reaction;
(3) taking out the carbon fiber felt after the hydrothermal reaction, putting the carbon fiber felt into deionized water, soaking the carbon fiber felt to be neutral, and drying the carbon fiber felt to obtain the nano CoFe2O4A carbon fiber felt composite material.
The concentration of ferric chloride in the mixed solution in the step (1) is 1 mmol/L-1 mol/L, and the concentration of cobalt chloride is 0.5 mmol/L-0.5 mol/L. Preferably, the concentration of ferric chloride is 50-200 mmol/L and the concentration of cobalt chloride is 20-100 mmol/L.
The organic solvent in the step (1) is ethylene glycol.
The molar concentration of anhydrous sodium acetate in the mixed solution in the step (1) is 0.35-1.0 mol/L, preferably 0.5-1.0 mol/L, and the molar ratio of anhydrous sodium acetate to ferric chloride to cobalt chloride is (5.1-10.2): 1: (0.4-0.7), preferably (7-9): 1: (0.4-0.7).
The solid-to-liquid ratio of the carbon fiber felt to the mixed solution in the step (2) is 0.0008-0.01 g/mL, and preferably 0.001-0.005 g/mL.
In the step (2), the hydrothermal reaction temperature is 100-260 ℃, and the hydrothermal reaction time is 6-72 h.
And (4) drying at the temperature of 50-70 ℃.
The invention also provides the nanometer CoFe2O4The application of the carbon fiber felt composite material in the aspect of catalyzing and degrading organic pollutants in waste water. The organic pollutants comprise atrazine, paraquat and the like.
Compared with the prior art, the invention has the advantages that:
(1) nano CoFe prepared by the invention2O4The carbon fiber felt composite material uses ferric chloride and cobalt chloride as raw materials, and the two medicines are easy to prepare, low in price and simple in process.
(2) Nano CoFe prepared by the invention2O4The carbon fiber felt composite material has a large specific surface area, is beneficial to adsorbing water pollutants, is beneficial to improving the photocatalytic performance, and promotes the catalytic degradation of the composite material to the water pollutants.
(3) Nano CoFe prepared by the invention2O4Carbon fiber felt composite material, so that magnetic nano material CoFe2O4The carbon fiber felt is uniformly wrapped on the fibers of the carbon fiber felt, so that the carbon fibers have certain magnetism, are favorable for recycling after use, and are environment-friendly.
Drawings
FIG. 1 is a diagram of nano CoFe prepared in example 12O4SEM image of/carbon fiber felt composite material, wherein FIG. 1a is nanometer CoFe2O4Low power SEM image of/carbon fiber felt composite material, and figure 1b shows nano CoFe2O4High power SEM images of/carbon fiber felt composites;
FIG. 2 is the nano CoFe prepared in example 12O4XRD images of the carbon fiber felt composite material;
FIG. 3 is the nano CoFe prepared in example 12O4Carbon fiberThe removal rate curve of the felt composite material after the adsorption catalysis water body pollution degradation experiment is carried out;
FIG. 4 shows the preparation of nano CoFe in example 12O4The removal rate curve of the carbon fiber felt composite material after the adsorption catalysis water body pollution degradation experiment is carried out under different pH values.
Detailed Description
The invention is described in detail with reference to the figures and the specific embodiments.
The carbon fiber felt used in the examples was purchased from environmental protection limited, kolite, Jiangsu, under the model number STF-1500. Both ferric chloride and cobalt chloride are hydrates.
Example 1
(1) Accurately weighing 1.3525g (0.005mol) of ferric chloride and 0.595g (0.0025mol) of cobalt chloride, placing the materials in 60mL of glycol solution, stirring until the ferric chloride and the cobalt chloride are completely dissolved in the glycol solution, then weighing 3.6g (0.044mol) of anhydrous sodium acetate in the solution, and carrying out ultrasonic stirring until the anhydrous sodium acetate is uniformly mixed to obtain a mixed solution;
(2) adding a piece of carbon fiber felt into the mixed solution, wherein the solid-to-liquid ratio of the carbon fiber felt to the mixed solution is 0.005g/mL, placing the mixture for 30min at room temperature in a vacuum environment with the vacuum degree of 0.09MPa, then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle, and carrying out hydrothermal treatment for 24h at the temperature of 180 ℃;
(3) taking out the carbon fiber felt after the hydrothermal reaction, soaking the carbon fiber felt in deionized water to be neutral, and drying the carbon fiber felt at 60 ℃ to obtain the nano CoFe2O4A carbon fiber felt composite material.
For the nano CoFe prepared in example 12O4The morphology and the material components of the carbon fiber felt composite material are characterized, and scanning electron microscope images (SEM) and wide-angle ray diffraction patterns (XRD) shown in figures 1 and 2 are obtained.
As can be seen from FIG. 1, the resulting composite material was CoFe2O4Uniformly distributed over the fibers of the carbon fiber felt; the loaded nano CoFe can be seen under a high-magnification scanning electron microscope2O4The particle structure is a granular structure, and the diameter of the particle is 90-100 nm. As can be seen from FIG. 2, NaRice CoFe2O4CoFe in/carbon fiber felt composite material2O4Is spinel type ferrite.
Comparative example 1
(1) Accurately weighing 0.6762g (0.0025mol) of ferric chloride and 0.2975g (0.00125mol) of cobalt chloride, putting the materials into 60mL of glycol solution, stirring until the ferric chloride and the cobalt chloride are completely dissolved in the glycol solution, then weighing 2.6g (0.032mol) of anhydrous sodium acetate into the solution, and carrying out ultrasonic stirring until the anhydrous sodium acetate is uniformly mixed to obtain a mixed solution;
(2) adding a piece of carbon fiber felt into the mixed solution, wherein the solid-to-liquid ratio of the carbon fiber felt to the mixed solution is 0.005g/mL, placing the mixture for 30min at room temperature in a vacuum environment with the vacuum degree of 0.09MPa, then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle, and carrying out hydrothermal treatment for 24h at 180 ℃;
(3) taking out the carbon fiber felt after the hydrothermal reaction, soaking the carbon fiber felt in deionized water to be neutral, and drying the carbon fiber felt at 60 ℃ to obtain the nano CoFe2O4A carbon fiber felt composite material.
Nano CoFe prepared in comparative example 12O4The content of the/carbon fiber felt composite material is lower than that of the example 1. This is because the concentrations of ferric chloride and ferric chloride in the mixed solution are lower than those in example 1, and the molar ratio of anhydrous sodium acetate to ferric chloride and cobalt chloride is higher than that in example 1, so that the content of the composite material after the reaction is completed is lower than that in example 1.
Comparative example 2
(1) Accurately weighing 5.41g (0.02mol) of ferric chloride and 2.38g (0.01mol) of cobalt chloride, putting the ferric chloride and the cobalt chloride into 60mL of glycol solution, stirring until the ferric chloride and the cobalt chloride are completely dissolved in the glycol solution, weighing 3.6g (0.044mol) of anhydrous sodium acetate into the solution, and ultrasonically stirring until the anhydrous sodium acetate is uniformly mixed to obtain a mixed solution;
(2) adding a piece of carbon fiber felt into the mixed solution, wherein the solid-to-liquid ratio of the carbon fiber felt to the mixed solution is 0.005g/mL, placing the mixture for 30min at room temperature in a vacuum environment with the vacuum degree of 0.09MPa, then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle, and carrying out hydrothermal treatment for 24h at 180 ℃;
(3) hydrothermal reaction is carried outTaking out the carbon fiber felt, soaking the carbon fiber felt in deionized water to be neutral, and drying the carbon fiber felt at 60 ℃ to obtain the nano CoFe2O4A carbon fiber felt composite material.
Nano CoFe obtained in comparative example 22O4The carbon fiber felt composite material contains Fe2O3. This is due to the increased concentration of ferric chloride and cobalt chloride, while the low concentration of sodium acetate is insufficient to provide the required alkalinity for the reaction.
Comparative example 3
(1) Accurately weighing 1.3525g (0.005mol) of ferric chloride and 0.595g (0.0025mol) of cobalt chloride, placing the materials in 60mL of glycol solution, stirring until the ferric chloride and the cobalt chloride are completely dissolved in the glycol solution, then weighing 1.6g (0.0195mol) of anhydrous sodium acetate in the mixed solution, and carrying out ultrasonic stirring until the anhydrous sodium acetate is uniformly mixed to obtain a mixed solution;
(2) adding a piece of carbon fiber felt into the mixed solution, wherein the solid-to-liquid ratio of the carbon fiber felt to the mixed solution is 0.005g/mL, placing the mixture for 30min at room temperature in a vacuum environment with the vacuum degree of 0.09MPa, then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle, and carrying out hydrothermal treatment for 24h at 180 ℃;
(3) taking out the carbon fiber felt after the hydrothermal reaction, soaking the carbon fiber felt in deionized water to be neutral, and drying the carbon fiber felt at 60 ℃ to obtain the nano CoFe2O4A carbon fiber felt composite material.
Nano CoFe obtained in comparative example 32O4The carbon fiber felt composite material contains part of Fe2O3. This is due to the small amount of anhydrous sodium acetate, which is insufficient to provide the alkaline environment required for the reaction.
Comparative example 4
(1) 1.3525g (0.005mol) of ferric chloride and 0.595g (0.0025mol) of cobalt chloride were accurately weighed into 60mL of an ethylene glycol solution, and stirred until the ferric chloride and the cobalt chloride were completely dissolved in the ethylene glycol solution. Then 5.6g (0.068mol) of anhydrous sodium acetate is weighed into the mixed solution, and the mixed solution is obtained after ultrasonic stirring is carried out until the anhydrous sodium acetate is uniformly mixed;
(2) adding a piece of carbon fiber felt into the mixed solution, wherein the solid-to-liquid ratio of the carbon fiber felt to the mixed solution is 0.001g/mL, placing the mixture for 30min at room temperature in a vacuum environment with the vacuum degree of 0.09MPa, then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle, and carrying out hydrothermal treatment for 24h at the temperature of 180 ℃;
(3) taking out the carbon fiber felt after the hydrothermal reaction, soaking the carbon fiber felt in deionized water to be neutral, and drying the carbon fiber felt at 60 ℃ to obtain the nano CoFe2O4A carbon fiber felt composite material.
Nano CoFe obtained in comparative example 42O4The carbon fiber felt composite material contains a small amount of anhydrous sodium acetate. This is because the concentration of anhydrous sodium acetate is too high, resulting in the residue of anhydrous sodium acetate, even if the subsequent washing is carried out, the nano CoFe2O4The/carbon fiber felt composite still has a small amount of residue.
Comparative example 5
(1) Accurately weighing 1.3525g (0.005mol) of ferric chloride and 0.595g (0.0025mol) of cobalt chloride, placing the materials in 60mL of glycol solution, stirring until the ferric chloride and the cobalt chloride are completely dissolved in the glycol solution, then weighing 3.6g (0.044mol) of anhydrous sodium acetate in the solution, and carrying out ultrasonic stirring until the anhydrous sodium acetate is uniformly mixed to obtain a mixed solution;
(2) adding a piece of carbon fiber felt into the mixed solution, wherein the solid-to-liquid ratio of the carbon fiber felt to the mixed solution is 0.005g/mL, placing the mixture for 30min at room temperature in a vacuum environment with the vacuum degree of 0.09MPa, then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle, and carrying out hydrothermal treatment for 24h at the temperature of 90 ℃;
(3) taking out the carbon fiber felt after the hydrothermal reaction, soaking the carbon fiber felt in deionized water to be neutral, and drying the carbon fiber felt at 60 ℃ to obtain the nano CoFe2O4A carbon fiber felt composite material.
Nano CoFe obtained in comparative example 52O4The reaction of the/carbon fiber felt composite material is incomplete. This is because the hydrothermal reaction temperature is too low to complete the reaction.
Comparative example 6
(1) Accurately weighing 1.3525g (0.005mol) of ferric chloride and 0.595g (0.0025mol) of cobalt chloride, placing the materials in 60mL of glycol solution, stirring until the ferric chloride and the cobalt chloride are completely dissolved in the glycol solution, then weighing 3.6g (0.044mol) of anhydrous sodium acetate in the mixed solution, and carrying out ultrasonic stirring until the anhydrous sodium acetate is uniformly mixed to obtain a mixed solution;
(2) adding a piece of carbon fiber felt into the mixed solution, wherein the solid-to-liquid ratio of the carbon fiber felt to the mixed solution is 0.001g/mL, placing the mixture for 30min at room temperature in a vacuum environment with the vacuum degree of 0.09MPa, then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle, and carrying out hydrothermal treatment for 4h at the temperature of 180 ℃;
(3) taking out the carbon fiber felt after the hydrothermal reaction, soaking the carbon fiber felt in deionized water to be neutral, and drying the carbon fiber felt at 60 ℃ to obtain the nano CoFe2O4A carbon fiber felt composite material.
Nano CoFe obtained in comparative example 62O4Incomplete reaction of/carbon fiber felt composite material, and loaded CoFe2O4The amount is small. This is because the hydrothermal reaction time is too short to complete the reaction, resulting in insufficient loading. After the completion of the reaction, the solution had a pH of about 7, and the solution after 4 hours of the reaction was alkaline above 7, and the alkaline condition was an external condition provided for the formation of the target product.
Performance testing
Nano CoFe prepared in example 12O4The carbon fiber felt composite material is used for carrying out a photocatalytic experiment for degrading pesticide residues in water:
(1) nano CoFe obtained in example 1 was weighed2O4The carbon fiber felt composite material is put into atrazine pesticide solution (the initial reaction concentration of the atrazine pesticide solution is 1-15 mg/L). Simultaneously adding trace H into the atrazine solution2O2And adjusting the pH value of the solution to about 3-6.
(2) Adding a xenon lamp (with the wavelength of 320-780) to the solution prepared in the step (1), irradiating the solution for photocatalysis, setting a control group without light for dark reaction, taking a sample every 1h, carrying out an absorbance test by using an ultraviolet spectrophotometer, and analyzing the concentration of atrazine in the solution.
Adsorption-catalysis of the residual pesticide in the waterThe data measured by chemical experiments are plotted and analyzed, the degradation curve of the pesticide atrazine is shown in figure 3, and the nano CoFe2O4Carbon fiber felt composite material relative to pure CoFe2O4The degradation rate of the composite material is greatly improved. Nano CoFe2O4The removal rate curve of the carbon fiber felt composite material after the adsorption catalysis water body pollution degradation experiment is carried out under different pH values is added in a graph shown in FIG. 4.
The catalyst can be recovered by a magnetic field and reused, and the catalytic activity is basically unchanged.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention. The terms appearing in the present invention are used for illustration and understanding of the technical aspects of the present invention, and do not constitute limitations of the present invention.
Claims (10)
1. Nano CoFe2O4The carbon fiber felt composite material is characterized in that: from nano-CoFe2O4And carbon fiber felt, nano CoFe2O4Uniformly attached to the fiber surface of the carbon fiber felt.
2. Nano CoFe according to claim 12O4The carbon fiber felt composite material is characterized in that: the nano CoFe2O4The particle size of (A) is 90 to 100 nm.
3. Nano CoFe according to claim 12O4The preparation method of the carbon fiber felt composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) uniformly dispersing ferric chloride and cobalt chloride in an organic solvent, and then adding anhydrous sodium acetate and uniformly stirring to obtain a mixed solution;
(2) adding a carbon fiber felt into the mixed solution, placing the mixed solution at room temperature in a vacuum environment, and then sealing the mixed solution and the carbon fiber felt into a hydrothermal kettle for hydrothermal reaction;
(3) taking out the carbon fiber felt after the hydrothermal reaction, putting the carbon fiber felt into deionized water, soaking the carbon fiber felt to be neutral, and drying the carbon fiber felt to obtain the nano CoFe2O4A carbon fiber felt composite material.
4. Nano CoFe according to claim 32O4The preparation method of the carbon fiber felt composite material is characterized by comprising the following steps: the concentration of ferric chloride in the mixed solution in the step (1) is 1 mmol/L-1 mol/L, the concentration of cobalt chloride is 0.5 mmol/L-0.5 mol/L, and the molar concentration of anhydrous sodium acetate is 0.35-1.0 mol/L.
5. Nano CoFe according to claim 32O4The preparation method of the carbon fiber felt composite material is characterized by comprising the following steps: the molar ratio of the anhydrous sodium acetate to the ferric chloride to the cobalt chloride in the step (1) is (5.1-10.2): 1: (0.4-0.7).
6. Nano CoFe according to claim 32O4The preparation method of the carbon fiber felt composite material is characterized by comprising the following steps: and (3) the solid-to-liquid ratio of the carbon fiber felt to the mixed solution in the step (2) is 0.0008-0.01 g/mL.
7. Nano CoFe according to claim 32O4The preparation method of the carbon fiber felt composite material is characterized by comprising the following steps: the organic solvent in the step (1) is ethylene glycol.
8. Nano CoFe according to claim 32O4The preparation method of the carbon fiber felt composite material is characterized by comprising the following steps: in the step (2), the hydrothermal reaction temperature is 100-260 ℃, and the hydrothermal reaction time is 6-72 h.
9. Nano CoFe according to claim 32O4The preparation method of the carbon fiber felt composite material is characterized by comprising the following steps: the drying temperature in the step (3) is 50-70 DEG℃。
10. Nano CoFe according to claim 1 or 22O4The application of the carbon fiber felt composite material in the aspect of catalyzing and degrading organic pollutants in waste water.
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