CN112844322A - Preparation method of Fe-MOFs and fiber composite material and application of Fe-MOFs and fiber composite material in dye wastewater treatment - Google Patents
Preparation method of Fe-MOFs and fiber composite material and application of Fe-MOFs and fiber composite material in dye wastewater treatment Download PDFInfo
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- CN112844322A CN112844322A CN202110002582.7A CN202110002582A CN112844322A CN 112844322 A CN112844322 A CN 112844322A CN 202110002582 A CN202110002582 A CN 202110002582A CN 112844322 A CN112844322 A CN 112844322A
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- 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
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- 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
- B01J20/28014—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 form
- B01J20/28023—Fibres or filaments
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a preparation method of a Fe-MOFs and fiber composite material and application of the composite material in dye wastewater treatment. Respectively providing a solution containing ferric ions and an organic solvent and a solution containing an organic ligand and an organic solvent; mixing the fiber, a solution containing ferric ions and an organic solvent and a solution containing an organic ligand and an organic solvent, reacting for 2-3 days at the temperature of 140-160 ℃ under a closed condition, taking out, washing and drying to obtain the composite material; the organic ligand is terephthalic acid, 2-amino terephthalic acid, pyridine-2, 5-dicarboxylic acid, 4-diphenylethylene dicarboxylic acid or 2, 5-dihydroxy terephthalic acid. The product of the invention is used for adsorbing dye wastewater, has the advantages of large adsorption capacity, multiple types of adsorbable dyes and high adsorption rate, reduces the harm of the dye wastewater to the environment and human beings, realizes the compounding of Fe-MOFs and fibers in one step, and has simple operation and easy obtainment of the product.
Description
Technical Field
The invention relates to a nano composite material and application thereof, in particular to preparation of a Fe-MOFs and fiber composite material and application of the Fe-MOFs and fiber composite material in dye wastewater treatment.
Background
Metal-organic framework Materials (MOFs) are crystalline porous materials with periodic network structures formed by self-assembly of inorganic transition metal ions and organic ligands, are coordination polymers, and have wide application in the fields of fluorescence sensing detection, gas adsorption and desorption, biomedicine, catalysis, drug sustained release, small molecule detection and the like. The high selectivity and different attachment of metals to organic ligands allows them to exhibit a wide variety of structures and functions. In addition, due to the abundant pore structure of MOFs, the composite material has ultrahigh specific surface area, and is beneficial to the application of structural engineering. Fiber materials have been widely used in the fields of apparel, home textiles, medical use, packaging, etc. due to their various excellent properties of softness, breathability, plasticity, warmth, comfort, durability, etc. The present study has been made on the combination of fibers and MOFs for use in air filters and superhydrophobic cotton textiles with antimicrobial properties.
Water is an indispensable resource in life and is the material basis on which humans and all living beings live. However, with the rapid development of modern industry and the pace of social progress gradually increased in recent years, a realistic and cool problem, namely the problem of water pollution, is also increasingly highlighted. In the years, the amount of sewage deeply damaged in China is hundreds of billions of tons, and most of the sewage is dye wastewater. Because dye molecules in the dye wastewater are difficult to degrade and have great harm to the environment and human beings, the correct treatment of the dye wastewater discharged into the environment in the industries of textile, paper making and the like is particularly important along with the annual increase of the use amount of the dye. The method for treating the dye wastewater by adopting adsorption is simple and convenient and easy to operate. However, the traditional adsorbing material has the defects of small saturated adsorption quantity, poor selective adsorption effect and the like. Although the MOFs can treat dye wastewater, the MOFs have some defects. For example, the MOFs material has good stability in water and cannot coexist with the adsorption effect, the adsorption effect is influenced by the adsorption competition of dye molecules and water molecules, and the use cost is high compared with that of the traditional material.
Disclosure of Invention
The invention aims to provide a preparation method of a Fe-MOFs and fiber composite material, which can be used for adsorbing dye wastewater, has the advantages of large adsorption capacity, multiple adsorbable dye types and high adsorption rate when being used for treating the dye wastewater according to the characteristics of large specific surface area, high porosity and adjustable structure of the MOFs, and can reduce the harm of the dye wastewater to the environment and human beings.
In order to achieve the purpose, the technical scheme of the invention is as follows:
one, Fe-MOFs and fiber composite material:
the Fe-MOFs and fiber composite material is formed by compounding a metal organic framework material MIL-53, a carbon nano tube CNT and an ethylene-vinyl acetate copolymer EVA.
Secondly, a method for the preparation of the Fe-MOFs and fiber composite according to claim 1, comprising the steps of:
(1) respectively providing a solution containing ferric ions and an organic solvent and a solution containing an organic ligand and an organic solvent;
(2) mixing the fiber, a solution containing ferric ions and an organic solvent and a solution containing an organic ligand and an organic solvent, reacting for 2-3 days at the temperature of 140-160 ℃ under a closed condition, taking out the fiber, washing and drying to obtain the Fe-MOFs and fiber composite material;
wherein the organic ligand is terephthalic acid, 2-amino terephthalic acid, pyridine-2, 5-dicarboxylic acid, 4-diphenylethylene dicarboxylic acid or 2, 5-dihydroxy terephthalic acid.
The expression of the prepared Fe-MOFs and fiber composite material is metal organic framework material MIL-53/carbon nano tube CNT/ethylene-vinyl acetate copolymer EVA, and the composite material is a composite of three metal organic framework materials MIL-53/carbon nano tube CNT/ethylene-vinyl acetate copolymer EVA.
The fiber is formed by wrapping carbon nano tube CNT outside ethylene-vinyl acetate copolymer EVA, and the length is 15-20 cm.
The ferric ions adopt ferric chloride or ferric nitrate and the like.
In the step (1), the molar concentration of ferric ions is 0.300-0.864mmol/mL, and the molar concentration of organic ligands is 0.075-0.216 mmol/mL.
In the step (1), the organic solvent is selected from N, N-dimethylformamide, N-dimethylacetamide or N, N-diethylformamide.
In the step (2), the mixing is carried out by firstly carrying out ultrasonic treatment and then mixing.
The frequency of the ultrasonic wave is 20-30KHz, and the time is 10-15 min.
In the step (2), the washing is performed by using an organic solvent selected from the group consisting of N, N-dimethylformamide, N-dimethylacetamide and N, N-diethylformamide.
In the step (2), the molar ratio of the ferric ions to the organic ligand is (1-2): 1.
the Fe-MOFs and fiber composite material is used for treating dye wastewater.
The Fe-MOFs and fiber composite material can be used for adsorbing dye wastewater and reducing the harm of the dye wastewater to the environment and human beings.
The invention has the beneficial effects that:
(1) the Fe-MOFs and fiber composite material provided by the invention can be used for adsorbing dye wastewater, and has the advantages of large adsorption capacity, multiple adsorbable dye types and high adsorption rate when being used for treating the dye wastewater according to the characteristics of large specific surface area, high porosity and structure adjustability of the MOFs, so that the harm of the dye wastewater to the environment and human beings can be reduced.
(2) The Fe-MOFs and fiber composite material provided by the invention is prepared by adopting an in-situ growth mode, the Fe-MOFs and fiber composite is realized in one step, the operation is simple, and the product is easy to obtain.
Drawings
FIG. 1 is a scanning electron microscope image of the MIL-53/CNT/EVA composite material, the left side of FIG. 1 is an electron microscope image obtained by magnifying the fiber surface by 500 times, and the right side of FIG. 1 is an electron microscope image obtained by magnifying the fiber surface by 100000 times, and as can be seen from the image, the MIL-53 crystal on the fiber surface grows well and is distributed uniformly, and the method is proved to be capable of being implemented.
FIG. 2 is a graph showing the UV absorption spectrum of Fe-MOFs/fiber after adsorbing the dye MB.
Detailed Description
The invention is further illustrated by the following figures and examples.
The specific embodiment of the invention is as follows:
example 1:
(1) dissolving 254mg of terephthalic acid in 10mL of N, N-dimethylformamide solution to prepare a terephthalic acid mixed solution with the molar concentration of 0.513mmol/mL, and marking as a solution 1; 406mg of ferric chloride hexahydrate is dissolved in 5mL of N, N-dimethylformamide to prepare a ferric chloride mixed solution with the molar concentration of 0.300mmol/mL, and the solution is marked as solution 2.
(2) Placing the solution 1 in a lining of a reaction kettle, placing the solution 2 in a glass bottle, performing ultrasonic treatment for 15min at the ultrasonic frequency of 20KHz, mixing the solution 1 and the solution 2, adding fibers (15cm), then placing the mixture at 140 ℃ for 48h, cooling the mixture to normal temperature, taking out the fibers, washing the fibers with N, N-dimethylformamide, and drying the fibers to obtain the Fe-MOFs and fiber composite material, wherein the expression is as follows: MIL-53/CNT/EVA.
Example 2:
(1) dissolving 358.5mg of terephthalic acid in 10mL of N, N-dimethylacetamide solution to prepare a terephthalic acid mixed solution with the molar concentration of 0.216mmol/mL, and marking as a solution 1; 574mg of ferric chloride hexahydrate is dissolved in 5mL of N, N-dimethylacetamide to prepare a ferric chloride mixed solution with the molar concentration of 0.424 mmol/mL, and the solution is marked as solution 2.
(2) Placing the solution 1 in a lining of a reaction kettle, placing the solution 2 in a glass bottle, performing ultrasonic treatment at the ultrasonic frequency of 20KHz for 15min, mixing the solution 1 and the solution 2, adding fibers (16cm), then placing at 150 ℃ for 48h, cooling to normal temperature, taking out the fibers, washing the fibers with N, N-dimethylacetamide, and drying to obtain the Fe-MOFs and fiber composite material, wherein the expression is as follows: MIL-53/CNT/EVA.
Example 3:
(1) dissolving 125mg of 2-amino terephthalic acid in 10mL of N, N-diethylformamide solution to prepare a 2-amino terephthalic acid mixed solution with the molar concentration of 0.075mmol/mL, which is marked as solution 1; 406mg of ferric nitrate was dissolved in 5mL of N, N-diethylformamide to prepare a mixed ferric nitrate solution with a molar concentration of 0.300mmol/mL, which was designated as solution 2.
(2) Putting the solution 1 into a lining of a reaction kettle, putting the solution 2 into a glass bottle, carrying out ultrasonic treatment for 15min at the ultrasonic frequency of 20KHz, mixing the solution 1 with the solution 2, adding fibers (18cm), then putting the mixture at 160 ℃ for 48h, cooling the mixture to normal temperature, taking out the fibers, washing the fibers with N, N-diethylformamide, and drying the fibers to obtain the Fe-MOFs and fiber composite material, wherein the expression is as follows: MIL-53/CNT/EVA.
Example 4:
(1) dissolving 358.5mg of 2, 5-dihydroxyterephthalic acid in 10mL of N, N-dimethylformamide solution to prepare a 2, 5-dihydroxyterephthalic acid mixed solution with the molar concentration of 0.216mmol/mL, and marking as solution 1; 1169mg of ferric nitrate is dissolved in 5mL of N, N-dimethylformamide to prepare a ferric nitrate mixed solution with the molar concentration of 0.864mmol/mL, which is marked as solution 2.
(2) Placing the solution 1 in a lining of a reaction kettle, placing the solution 2 in a glass bottle, performing ultrasonic treatment for 15min at the ultrasonic frequency of 20KHz, mixing the solution 1 and the solution 2, adding fibers (20cm), then placing the mixture at 150 ℃ for 48h, cooling the mixture to normal temperature, taking out the fibers, washing the fibers with N, N-dimethylformamide, and drying the fibers to obtain the Fe-MOFs and fiber composite material, wherein the expression is as follows: MIL-53/CNT/EVA.
Test example
The Fe-MOFs and fiber composite material obtained in example 2 was placed in an MB solution having a concentration of 0.01mg/ml, placed in a constant-temperature water bath cabinet at 30 ℃ for two days, the color change of the solution was observed, and the solution was subjected to an ultraviolet test.
FIG. 2 shows the UV absorption spectrum of the dye MB adsorbed by Fe-MOFs/fiber, and it can be seen from the figure that Fe-MOFs/fiber has a significant adsorption effect on the dye MB, and can be used for treating dye wastewater.
Claims (10)
1. A Fe-MOFs and fiber composite characterized by: the Fe-MOFs and fiber composite material is formed by compounding a metal organic framework material MIL-53, a carbon nano tube CNT and an ethylene-vinyl acetate copolymer EVA.
2. A method for preparing Fe-MOFs and fibre composites according to claim 1, characterized in that: the method comprises the following steps:
(1) respectively providing a solution containing ferric ions and an organic solvent and a solution containing an organic ligand and an organic solvent;
(2) mixing the fiber, a solution containing ferric ions and an organic solvent and a solution containing an organic ligand and an organic solvent, reacting for 2-3 days at the temperature of 140-160 ℃ under a closed condition, taking out the fiber, washing and drying to obtain the Fe-MOFs and fiber composite material;
wherein the organic ligand is terephthalic acid, 2-amino terephthalic acid, pyridine-2, 5-dicarboxylic acid, 4-diphenylethylene dicarboxylic acid or 2, 5-dihydroxy terephthalic acid.
3. The method of preparation of Fe-MOFs and fiber composites according to claim 2, characterized in that: the fiber is formed by wrapping carbon nano tube CNT outside ethylene-vinyl acetate copolymer EVA, and the length is 15-20 cm.
4. The method of preparation of Fe-MOFs and fiber composites according to claim 2, characterized in that: in the step (1), the molar concentration of ferric ions is 0.300-0.864mmol/mL, and the molar concentration of organic ligands is 0.075-0.216 mmol/mL.
5. The method of preparation of Fe-MOFs and fiber composites according to claim 2, characterized in that: in the step (1), the organic solvent is selected from N, N-dimethylformamide, N-dimethylacetamide or N, N-diethylformamide.
6. The method of preparation of Fe-MOFs and fiber composites according to claim 2, characterized in that: in the step (2), the mixing is carried out by firstly carrying out ultrasonic treatment and then mixing.
7. The method of preparation of Fe-MOFs and fiber composites according to claim 5, characterized in that: the frequency of the ultrasonic wave is 20-30KHz, and the time is 10-15 min.
8. The method of preparation of Fe-MOFs and fiber composites according to claim 2, characterized in that: in the step (2), the washing is performed by using an organic solvent selected from the group consisting of N, N-dimethylformamide, N-dimethylacetamide and N, N-diethylformamide.
9. The method of preparation of Fe-MOFs and fiber composites according to claim 2, characterized in that: in the step (2), the molar ratio of the ferric ions to the organic ligand is (1-2): 1.
10. use of the Fe-MOFs and fiber composites prepared by the preparation method according to any of claims 2-9, characterized in that: the Fe-MOFs and fiber composite material is applied to dye wastewater treatment.
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| CN112755968A (en) * | 2020-12-31 | 2021-05-07 | 廊坊师范学院 | MOFs fiber membrane for adsorbing micro-nano plastics in trapped water and preparation method thereof |
| CN116606021A (en) * | 2023-06-09 | 2023-08-18 | 威海蓝创环保设备有限公司 | Metronidazole waste water treatment system |
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