CN112979985A - Composite metal organic framework material and preparation method thereof - Google Patents
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Abstract
The invention discloses a composite metal organic framework material, which is Fe3O4@ MIL-100 (Fe), molecular formula: fe3C18H10O16. The preparation method comprises the step one of adding FeCl3·6H2Dissolving O and anhydrous sodium acetate in ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, and placing the reaction kettle in a constant-temperature drying oven for solvothermal reaction to obtain a solid product; drying in a vacuum drying oven at 60 deg.C for 12 hr to obtain ferroferric oxide nanoparticles; step two, mixing the trimesic acid,ferroferric oxide nanoparticles and H2O reacts under microwave to generate orange brown solid which is collected by a magnet; washing with hot water and hot ethanol, and vacuum drying at 60 deg.C overnight to obtain composite metal organic framework material Fe3O4@ MIL-100 (Fe). The advantages are that: simple preparation process, low preparation cost, good stability and strong adsorption force.
Description
Technical Field
The invention relates to the technical field of metal organic framework material preparation, in particular to a composite metal organic framework material and a preparation method thereof.
Background
The metal organic framework Material (MOF) is a novel porous crystal material formed by combining metal ions and organic ligands through coordination bonds, has the characteristics of large specific surface area, high porosity, adjustable pore diameter, functionalization and the like, and is widely applied to the fields of selective adsorption separation, storage, sensing, catalysis and the like of gases.
In recent years, with the rapid development of industry, the problem of water pollution has become one of the serious problems that must be controlled. The water contaminants mainly include: organic dyes, antibiotics, cyanides, and the like; among the numerous water contaminants, the organic contaminants are the most harmful. The application range of the dye is wider and wider, and the dye not only meets the material requirements of people, but also brings no small burden to the environment. Organic dyes have carcinogenic and teratogenic hazards, and once a large amount of organic dyes are discharged into water, the organic dyes not only pollute the environment, but also cause certain social effects.
Various methods are currently used to remove water contaminants, including adsorption, membrane separation, precipitation, oxidation, biological treatment, and electrochemical techniques. However, these techniques have certain limitations and disadvantages, such as high cost and poor contaminant removal. In addition, some technologies only have adsorption effect on specific pollutants, and cannot deal with the increasingly serious problem of environmental water pollution. Among these techniques, the adsorption method is considered to be more suitable for the removal of organic dyes due to its effectiveness and economy. Therefore, it is an important problem to be solved to find a fast and efficient method and adsorbent for removing water pollutants.
Disclosure of Invention
The invention aims to make up the defects and discloses a composite metal organic framework material which is simple in preparation process, low in preparation cost, good in stability and strong in adsorption force and a preparation method thereof to the society.
The technical scheme of the invention is realized as follows:
a composite metal-organic skeleton material is prepared from Fe3O4@ MIL-100 (Fe), the molecular formula of which is: fe3C18 H10O16。
A preparation method of a composite metal organic framework material is characterized by comprising the following steps: the method comprises the following steps:
step one, FeCl is firstly added3·6H2Dissolving O and anhydrous sodium acetate in ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle in a constant-temperature drying box, and carrying out solvothermal reaction to obtain a solid product; washing the solid product with ethanol and high-purity water respectively to remove impurities, and then drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain ferroferric oxide nanoparticles;
step two, trimesic acid, ferroferric oxide nano particles and H2O reacts under microwave to generate orange brown solid which is collected by a magnet; washing the collected product with hot water and hot ethanol for multiple times, and finally vacuum drying at 60 ℃ overnight to obtain the composite metal organic framework material Fe3O4 @ MIL-100（Fe）。
The measures for further optimizing the technical scheme are as follows:
in the first step, FeCl3·6H2The molar ratio of O to anhydrous sodium acetate is 1: 1-1: 2.5.
in the step one, the average diameter of the obtained ferroferric oxide nano particles is 470-530 nm.
In the first step, the constant temperature of the solvothermal reaction is 200 ℃, and the reaction time is 5 to 8 hours. Preferably, it is
The reaction time was 7 h.
In the second step, the molar ratio of the trimesic acid to the ferroferric oxide nanoparticles is 2: 1.
In the second step, the reaction is carried out under the microwave condition of 150-180 ℃ for 15-30 min by a microwave method. The reaction is preferably carried out under microwave conditions at 150 ℃ for 30 min.
Compared with the prior art, the invention has the advantages that:
the invention relates to a composite metal organic framework material and a preparation method thereof, wherein an MIL-100 (Fe) metal organic framework which has a stable structure and coordination unsaturated metal ions is selected. At the same time, magnetic Fe3O4The addition of the nano particles further improves the recoverable convenience of the composite metal organic framework material, removes the complicated recovery process of centrifugal collection, and increases the absorption and degradation capacity of the material to organic dyes due to the coordination unsaturated metal ions in the MOF structure. The composite metal organic framework material of the invention integrates the adsorption and degradation capacities of MOF porous material to organic dye and Fe3O4The magnetic property of the nano particles enables the nano particles to have stronger chemical stability, quick separation and reusability. The raw materials used in the preparation method are low in cost, wide in source, simple and easy to operate in the preparation process, low in requirement on equipment and short in reaction time.
Drawings
FIG. 1 is a scanning electron microscope image of the composite metal organic framework material of the present invention.
Detailed Description
A composite metal-organic skeleton material is prepared from Fe3O4@ MIL-100 (Fe), the molecular formula of which is: fe3C18 H10O16。
A preparation method of a composite metal organic framework material comprises the following steps:
step one, FeCl is firstly added3·6H2O and anhydrousDissolving sodium acetate in ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle in a constant-temperature drying box, and carrying out solvothermal reaction to obtain a solid product; washing the solid product with ethanol and high-purity water respectively to remove impurities, and then drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain ferroferric oxide nanoparticles; wherein FeCl3·6H2The molar ratio of O to anhydrous sodium acetate is 1: 1-1: 2.5, the average diameter of the obtained ferroferric oxide nano particles is 470-530 nm, the constant temperature of the solvothermal reaction is 200 ℃, the reaction time is 5-8 h, and the preferable reaction time is 7 h.
Step two, trimesic acid (H)3BTC), ferroferric oxide nanoparticles and H2O reacts under microwave to generate orange brown solid which is collected by a magnet; washing the collected product with hot water and hot ethanol for multiple times, and finally vacuum drying at 60 ℃ overnight to obtain the composite metal organic framework material Fe3O4@ MIL-100 (Fe); wherein the molar ratio of the trimesic acid to the ferroferric oxide nanoparticles is 2:1, and the reaction is carried out under the microwave condition of 150-180 ℃ for 15-30 min by a microwave method, preferably at 150 ℃ for 30 min.
Composite metal organic framework material Fe prepared by the preparation method3O4FIG. 1 shows a scanning electron micrograph of @ MIL-100 (Fe).
This is further illustrated by the specific examples below.
Example 1
A preparation method of a composite metal organic framework material comprises the following steps:
step one, Fe3O4Preparation of nanoparticles: first 3.46g of FeCl3·6H2Completely dissolving O and 2.66g of anhydrous sodium acetate in 80mL of ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle into an electric heating blowing constant-temperature drying oven, and carrying out solvothermal reaction for 7 hours at the temperature of 200 ℃ to obtain a solid product; washing the solid product with ethanol and high purity water respectively for 3 times to remove impurities, and vacuum drying the sampleDrying at 60 ℃ for 12 hours to obtain the ferroferric oxide nano particles. The average diameter of the obtained ferroferric oxide nano particles is 500 nm.
Step two, Fe3O4Preparation of @ MIL-100 (Fe) composite: fe3O4@ MIL-100 (Fe) is synthesized by a simple and rapid microwave method, and H is specifically synthesized3BTC (1.05 g), ferroferric oxide nanoparticles (0.58 g) and H2O (12.5 mL) was reacted at 150 ℃ for 30min under microwave to give an orange-brown solid which was collected with a magnet. In order to remove unreacted ions and H3BTC washing the collected product with hot water and hot ethanol for multiple times, and finally vacuum drying at 60 deg.C overnight to obtain composite metal organic framework material Fe3O4 @ MIL-100（Fe）。
Example 2
A preparation method of a composite metal organic framework material comprises the following steps:
step one, Fe3O4Preparation of nanoparticles: first 3.46g of FeCl3·6H2Completely dissolving O and 2.66g of anhydrous sodium acetate in 80mL of ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle into an electric heating blowing constant-temperature drying oven, and carrying out solvothermal reaction for 5 hours at the temperature of 200 ℃ to obtain a solid product; and (3) washing the solid product respectively with ethanol and high-purity water, washing for 3 times respectively to remove impurities, and finally drying the sample in a vacuum drying oven at 60 ℃ for 12 hours to obtain the ferroferric oxide nanoparticles. The average diameter of the obtained ferroferric oxide nano particles is 470 nm.
Step two, Fe3O4Preparation of @ MIL-100 (Fe) composite: fe3O4@ MIL-100 (Fe) is synthesized by a simple and rapid microwave method, and H is specifically synthesized3BTC (1.05 g), ferroferric oxide nanoparticles (0.58 g) and H2O (12.5 mL) was reacted at 150 ℃ for 30min under microwave to give an orange-brown solid which was collected with a magnet in order to remove unreacted ions and H3BTC washing the collected product with hot water and hot ethanol for several times, and vacuum drying at 60 deg.C overnight to obtain composite metal organic boneFrame material Fe3O4 @ MIL-100（Fe）。
Example 3
A preparation method of a composite metal organic framework material comprises the following steps:
step one, Fe3O4Preparation of nanoparticles: first 3.46g of FeCl3·6H2Completely dissolving O and 2.66g of anhydrous sodium acetate in 80mL of ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle into an electric heating blowing constant-temperature drying oven, carrying out solvothermal reaction for 6 hours at the temperature of 200 ℃ to obtain solid products, respectively washing the solid products with ethanol and high-purity water for 3 times to remove impurities, and finally placing a sample into a vacuum drying oven to be dried for 12 hours at the temperature of 60 ℃ to obtain the ferroferric oxide nanoparticles. The average diameter of the obtained ferroferric oxide nano particles is 490 nm.
Step two, Fe3O4Preparation of @ MIL-100 (Fe) composite: fe3O4@ MIL-100 (Fe) is synthesized by a simple and rapid microwave method, and H is specifically synthesized3BTC (1.05 g), ferroferric oxide nanoparticles (0.58 g) and H2O (12.5 mL) was reacted at 150 ℃ for 30min under microwave to give an orange-brown solid which was collected with a magnet. In order to remove unreacted ions and H3BTC washing the collected product with hot water and hot ethanol for multiple times, and finally vacuum drying at 60 deg.C overnight to obtain composite metal organic framework material Fe3O4 @ MIL-100（Fe）。
Example 4
A preparation method of a composite metal organic framework material comprises the following steps:
step one, Fe3O4Preparation of nanoparticles: first 3.46g of FeCl3·6H2Completely dissolving O and 2.66g of anhydrous sodium acetate in 80mL of ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle into an electric heating blowing constant-temperature drying oven, and carrying out solvothermal reaction for 7 hours at the temperature of 200 ℃ to obtain a solid product; washing the solid product with ethanol and high purity water respectively for 3 times to remove impurities, and washing with ethanol and high purity water respectivelyAnd (3) drying the sample in a vacuum drying oven at 60 ℃ for 12 hours to obtain the ferroferric oxide nanoparticles. The average diameter of the obtained ferroferric oxide nano particles is 530 nm.
Step two, Fe3O4Preparation of @ MIL-100 (Fe) composite: fe3O4@ MIL-100 (Fe) is synthesized by a simple and rapid microwave method, and H is specifically synthesized3BTC (1.05 g), ferroferric oxide nanoparticles (0.58 g) and H2O (12.5 mL) was reacted at 150 ℃ for 15min under microwave to give an orange-brown solid which was collected with a magnet. In order to remove unreacted ions and H3BTC the collected product was washed several times with hot water and hot ethanol. Finally vacuum drying overnight at 60 ℃ to obtain the composite metal organic framework material Fe3O4 @ MIL-100（Fe）。
Example 5
The preparation process is basically the same as that of the example 1, except that: in the second step, the reaction is carried out for 15min at 180 ℃ under microwave.
Example 6
The preparation process is basically the same as that of the example 1, except that: in the second step, the reaction is carried out for 30min at 180 ℃ under microwave.
The composite metal organic framework material Fe prepared by the invention3O4The @ MIL-100 (Fe) combines the excellent properties of the MOF, such as overlarge specific surface area, high porosity and superparamagnetism of magnetic nanoparticles, so that the composite metal organic framework material has good adsorption property and magnetic responsiveness, the problem that practical application is limited due to the fact that most of conventional adsorbents are not easy to separate from an aqueous solution can be effectively solved, and the application of the adsorbent in the field of water treatment is expanded. The composite metal organic framework material Fe of the invention3O4The @ MIL-100 (Fe) can be used for treating organic dyes in sewage, has large absorption capacity on rhodamine B, methylene blue and the like, has degradation capability and is compounded with magnetic Fe3O4The nano particle material has the characteristics of simple and convenient recovery and high reuse rate.
The magnetic nanoparticles and the metal organic framework material are compounded, the respective advantages of the magnetic nanoparticles and the metal organic framework material are fully exerted, the synergistic effect on performance is generated, and the magnetic metal organic framework material has the characteristics of good adsorption performance, simplicity and rapidness in synthesis, capability of being quickly recovered, high repeated utilization rate, wide raw material source and the like, so that the magnetic metal organic framework material has wider application in the field of water treatment.
While the preferred embodiments of the present invention have been illustrated, various changes and modifications may be made by one skilled in the art without departing from the scope of the present invention.
Claims (9)
1. A composite metal organic framework material is characterized in that: the organic framework material is Fe3O4@ MIL-100 (Fe), the molecular formula of which is: fe3C18 H10O16。
2. The method for preparing a composite metal organic framework material according to claim 1, which is characterized in that: the method comprises the following steps:
step one, FeCl is firstly added3·6H2Dissolving O and anhydrous sodium acetate in ethylene glycol, transferring the ethylene glycol into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle in a constant-temperature drying box, and carrying out solvothermal reaction to obtain a solid product; washing the solid product with ethanol and high-purity water respectively to remove impurities, and then drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain ferroferric oxide nanoparticles;
step two, trimesic acid, ferroferric oxide nano particles and H2O reacts under microwave to generate orange brown solid which is collected by a magnet; washing the collected product with hot water and hot ethanol for multiple times, and finally vacuum drying at 60 ℃ overnight to obtain the composite metal organic framework material Fe3O4 @ MIL-100（Fe）。
3. A composite metal organic framework material according to claim 2, wherein: in the first step, FeCl3·6H2The molar ratio of O to anhydrous sodium acetate is 1: 1-1: 2.5.
4. a composite metal organic framework material according to claim 2, wherein: in the step one, the average diameter of the obtained ferroferric oxide nano particles is 470-530 nm.
5. A composite metal organic framework material according to claim 2, wherein: in the first step, the constant temperature of the solvothermal reaction is 200 ℃, and the reaction time is 5 to 8 hours.
6. A composite metal organic framework material according to claim 5, wherein: the reaction time is 7 h.
7. A composite metal organic framework material according to claim 2, wherein: in the second step, the molar ratio of the trimesic acid to the ferroferric oxide nanoparticles is 2: 1.
8. A composite metal organic framework material according to claim 2, wherein: in the second step, the reaction is carried out under the microwave condition of 150-180 ℃ for 15-30 min by a microwave method.
9. A composite metal organic framework material according to claim 8, wherein: in the second step, the reaction is carried out under the microwave condition of 150 ℃ for 30 min.
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| CN115254071A (en) * | 2022-08-04 | 2022-11-01 | 华侨大学 | Magnetic metal organic framework composite material and preparation method and application thereof |
| CN115779685A (en) * | 2023-02-10 | 2023-03-14 | 北京理工大学 | Preparation method of photo-Fenton film based on metal organic framework material |
| CN116444809A (en) * | 2023-03-23 | 2023-07-18 | 河南大学 | Hollow nano flower-like double MOF-based heterojunction material and preparation method and application thereof |
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Cited By (5)
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| CN115779685A (en) * | 2023-02-10 | 2023-03-14 | 北京理工大学 | Preparation method of photo-Fenton film based on metal organic framework material |
| CN116444809A (en) * | 2023-03-23 | 2023-07-18 | 河南大学 | Hollow nano flower-like double MOF-based heterojunction material and preparation method and application thereof |
| CN116444809B (en) * | 2023-03-23 | 2023-12-08 | 河南大学 | Hollow nano flower-like double MOF-based heterojunction material and preparation method and application thereof |
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