CN112604717A - Preparation method of quantum dot iron-based metal organic framework composite material - Google Patents
Preparation method of quantum dot iron-based metal organic framework composite material Download PDFInfo
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- 239000013082 iron-based metal-organic framework Substances 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000002096 quantum dot Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 39
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000012670 alkaline solution Substances 0.000 claims abstract description 4
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 15
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 15
- 239000012498 ultrapure water Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910001868 water Inorganic materials 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- UXGNZZKBCMGWAZ-UHFFFAOYSA-N dimethylformamide dmf Chemical compound CN(C)C=O.CN(C)C=O UXGNZZKBCMGWAZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 150000002505 iron Chemical class 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000005342 ion exchange Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 13
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000006385 ozonation reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000007210 heterogeneous catalysis Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 108010001336 Horseradish Peroxidase Proteins 0.000 description 1
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- 239000002041 carbon nanotube Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
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- 238000002386 leaching Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of a quantum dot modified iron-based metal organic framework composite material3·H2O) and 2-amino-p-dibenzoic acid (NH)2BDC) dosage can further adjust the size of Fe-MOFs and the particle size and porosity of the MOF structure, and Fe-MOFs structures with different morphologies can be obtained. And then, fully dissolving Fe-MOFs in an alkaline solution containing a certain red phosphorus concentration, thoroughly cleaning, and calcining the precipitate at high temperature to prepare the quantum dot/Fe-MOFs composite material. The quantum dots are synthesized in situ in the Fe-MOFs by adopting an ion exchange mode, so that the rapid degradation or polymerization of the quantum dots under a polar condition is avoided, and the stability of the quantum dots in an aqueous solution is improved.
Description
Technical Field
The invention relates to preparation and application of a novel composite material. In particular to a preparation method of a quantum dot modified iron-based metal organic framework composite material. The invention belongs to the field of composite catalyst preparation.
Background
Heterogeneous catalytic ozonation can effectively remove organic matters in drinking water or wastewater, so that the catalytic mechanism of ozonation is researched to enhance the catalytic efficiency of ozonation, and the development of related fields is benefited. Conventional ozone oxidation catalysts are: a metal ion supported catalyst (Chinese patent: a preparation method of an epoxy catalyst, an epoxy catalyst prepared by the catalyst and application thereof, publication number: CN 106964337A); a metal oxide catalyst (Chinese patent: preparation method of composite metal oxide catalyst, composite metal oxide catalyst and application, publication number: CN 109569667A); a metal-free catalyst (Chinese patent: a catalytic ozonation treatment method for refinery sewage, publication number: CN 106256787A). Metal-based catalysts often suffer from environmental pollution caused by metal leaching during heterogeneous catalysis. The active sites in the solid catalyst cannot be in sufficient contact with the substrate, and thus the substrate degradation efficiency cannot be fully exerted. In addition, non-metal catalysts, such as activated carbon, carbon nanotubes, etc., have low activity, are easily deactivated, are difficult to separate, and prevent their wide application, although they can avoid environmental pollution. Therefore, the exploration of the efficient ozone oxidation catalyst has great application value.
The iron-based metal organic framework material (Fe-MOFs) has good horseradish peroxidase catalytic performance, has the advantages of high specific surface area, large porosity, good thermal stability and the like, has potential application prospects in the aspects of gas storage, selective adsorption, heterogeneous catalysis, magnetism, molecular sensing and the like, and particularly has potential application prospects in the fields of photocatalytic degradation of organic matters and the like. Quantum Dots (QDs) are nano materials with the size of about 2-10 nm, and can be used as electron donors and acceptors to enhance the conductivity of the composite material. Therefore, the research on the quantum dot/Fe-MOFs composite material can improve the conductivity of the material, enhance the electron conduction rate and enhance the catalytic capability and anti-poisoning capability of Fe-MOFs.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a quantum dot modified iron-based metal organic framework composite material.
The purpose of the invention is realized by the following scheme: a process for preparing the composite Fe-MOFs material of quantum dot includes synthesizing Fe-MOFs material by ferric chloride (Fe Cl)3·H2O) and 2-amino-p-dibenzoic acid (NH)2BDC) dosage can further adjust the size of Fe-MOFs and the particle size and porosity of the MOF structure, and Fe-MOFs structures with different morphologies can be obtained. And then, fully dissolving Fe-MOFs in an alkaline solution containing a certain red phosphorus concentration, thoroughly cleaning, and calcining the precipitate at high temperature to prepare the quantum dot/Fe-MOFs composite material, wherein the preparation method comprises the following steps:
(1) preparing Fe-MOFs: 1.6-4.5 g Fe Cl3·H2O and 1.4-2.8 g NH2BDC was well dissolved in 100 mL Dimethylformamide (DMF) to form a clear solution; transferring the solution to a reaction kettle, and reacting for 3-12 h at 150 ℃; cooling to room temperature, centrifuging, collecting precipitate, washing with DMF, ethanol and ultrapure water for 3 times, drying at 60 deg.C for 24 hr, and collecting precipitate.
(2) Preparing a quantum dot/Fe-MOFs composite material: dissolving 1-5g of red phosphorus in alkali liquor, then adding 0.5-1 g of Fe-MOFs material, thoroughly and uniformly stirring, then centrifuging to collect precipitate, fully washing for 3 times by adopting ethanol and ultrapure water, drying for 24 hours at 50 ℃, and collecting precipitate. And transferring the precipitate to a tubular furnace, calcining at high temperature for 2-4 h under the condition of nitrogen, thoroughly cleaning the obtained precipitate by using ethanol and ultrapure water, drying at 60 ℃ for 24 h, and collecting the precipitate to obtain the FeP @ Fe-MOFs composite material.
In the preparation method provided by the invention, in the step (1), the size of the Fe-MOFs is 50-200 nm.
In the step (2) of the preparation method provided by the invention, the mass ratio of the Fe-MOFs to the red phosphorus is 1: 1-1: 10.
In the preparation method provided by the invention, the pH value of the alkali liquor in the step (2) is 4-6.
In the preparation method, the high-temperature calcination temperature in the step (2) is 400-600 ℃.
The method for preparing the fiber is simple in process, easy to operate, cheap and easily available in raw materials, and suitable for industrial production.
The quantum dots are synthesized in situ in the Fe-MOFs by adopting an ion exchange mode, so that the rapid degradation or polymerization of the quantum dots under a polar condition is avoided, and the stability of the quantum dots in an aqueous solution is improved. The quantum dot/Fe-MOFs composite material can improve the conductivity of Fe-MOFs materials, enhance the electron conduction rate and enhance the catalytic capability and anti-poisoning capability of Fe-MOFs. The prepared membrane can be applied to the fields of organic oxidation, biosensing and the like in sewage or atmospheric treatment.
Drawings
FIG. 1 shows FeP @ Fe-MOFs materials prepared in example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further described below by specific examples. The following examples are further illustrative of the present invention and do not limit the scope of the present invention.
Example 1
A quantum dot iron-based metal organic framework composite material is prepared by firstly synthesizing Fe-MOFs material and then adding ferric chloride Fe Cl3·H2O and 2-amino-p-dibenzoic acid NH2Adjusting the BDC dosage, further adjusting the size of Fe-MOFs and the particle size and porosity of the MOF structure, and simultaneously obtaining Fe-MOFs structures with different appearances; and then, fully dissolving Fe-MOFs in an alkaline solution containing a certain red phosphorus concentration, thoroughly cleaning, and calcining the precipitate at high temperature to prepare the quantum dot/Fe-MOFs composite material, wherein the preparation method comprises the following steps:
(1) preparing Fe-MOFs: 1.6 g Fe Cl3·H2O and 2 g NH2BDC was well dissolved in 100 mL dimethylformamide DMF to form a clear solution; transferring the solution to a reaction kettle, and reacting for 12 h at 150 ℃; cooling to room temperature, centrifuging, collecting precipitate, cleaning with DMF, ethanol and ultrapure water for 3 times, drying at 60 deg.C for 24 hr, and collecting precipitate;
(2) preparing a quantum dot/Fe-MOFs composite material: dissolving 1.5g of red phosphorus in alkaline liquor with pH of 5, then adding 0.5g of Fe-MOFs material, thoroughly and uniformly stirring, then centrifuging to collect precipitate, fully washing for 3 times by adopting ethanol and ultrapure water, drying for 24 hours at 50 ℃, and collecting precipitate; and transferring the precipitate to a tubular furnace, calcining for 2h at the high temperature of 500 ℃ under the nitrogen condition, thoroughly cleaning the obtained precipitate by using ethanol and ultrapure water, drying for 24 h at the temperature of 60 ℃, and collecting the precipitate to obtain the FeP @ Fe-MOFs composite material, wherein the structure is shown in figure 1.
Example 2
A quantum dot iron-based metal organic framework composite material is prepared by the following steps, which are similar to the steps in the embodiment 1:
(1) preparing Fe-MOFs: 4 Fe Cl3·H2O with 2.5g NH2BDC was well dissolved in 100 mL Dimethylformamide (DMF) to form a clear solution; transferring the solution to a reaction kettle, and reacting for 3 hours at 150 ℃; cooling to room temperature, centrifuging, collecting precipitate, cleaning with DMF, ethanol and ultrapure water for 3 times, drying at 60 deg.C for 24 hr, and collecting precipitate;
(2) preparing a quantum dot/Fe-MOFs composite material: dissolving 3 g of red phosphorus in alkaline liquor with pH of 5.5, then adding 0.5g of Fe-MOFs material, thoroughly and uniformly stirring, then centrifuging to collect precipitate, fully washing for 3 times by adopting ethanol and ultrapure water, drying for 24 hours at 50 ℃, and collecting precipitate; and transferring the precipitate to a tubular furnace, calcining for 3 h at 450 ℃ under the nitrogen condition, thoroughly cleaning the obtained precipitate by using ethanol and ultrapure water, drying for 24 h at 60 ℃, and collecting the precipitate to obtain the FeP @ Fe-MOFs composite material.
Example 3
A quantum dot iron-based metal organic framework composite material is prepared by the following steps, which are similar to the steps in the embodiment 1:
(1) preparing Fe-MOFs: 4.5 Fe Cl3·H2O with 2.8 g NH2BDC was well dissolved in 100 mL Dimethylformamide (DMF) to form a clear solution; transferring the solution to a reaction kettle, and reacting for 3 hours at 150 ℃; cooling to room temperature, centrifuging, collecting precipitate, cleaning with DMF, ethanol and ultrapure water for 3 times, drying at 60 deg.C for 24 hr, and collecting precipitate;
(2) preparing a quantum dot/Fe-MOFs composite material: dissolving 2 g of red phosphorus in alkaline liquor with the pH value of 4.8, then adding 0.75 g of Fe-MOFs material, thoroughly and uniformly stirring, then centrifuging to collect precipitate, fully washing for 3 times by adopting ethanol and ultrapure water, drying for 24 hours at the temperature of 50 ℃, and collecting the precipitate; and transferring the precipitate to a tubular furnace, calcining for 2h at 400 ℃ under the nitrogen condition, thoroughly cleaning the obtained precipitate by using ethanol and ultrapure water, drying for 24 h at 60 ℃, and collecting the precipitate to obtain the FeP @ Fe-MOFs composite material.
Claims (5)
1. A preparation method of a quantum dot iron-based metal organic framework composite material is characterized in that Fe-MOFs materials are synthesized firstly, and ferric chloride Fe Cl is used for preparing the Fe-MOFs materials3·H2O and 2-amino-p-dibenzoic acid NH2Adjusting the BDC dosage, further adjusting the size of Fe-MOFs and the particle size and porosity of the MOF structure, and simultaneously obtaining Fe-MOFs structures with different appearances; and then, fully dissolving Fe-MOFs in an alkaline solution containing a certain red phosphorus concentration, thoroughly cleaning, and calcining the precipitate at high temperature to prepare the quantum dot/Fe-MOFs composite material, wherein the method comprises the following steps:
(1) preparing Fe-MOFs: 1.6-4.5 g Fe Cl3·H2O and 1.4-2.8 g NH2BDC was well dissolved in 100 mL dimethylformamide DMF to form a clear solution; the solution was transferred to a reaction vessel, 1Reacting for 3-12 h at 50 ℃; cooling to room temperature, centrifuging, collecting precipitate, cleaning with DMF, ethanol and ultrapure water for 3 times, drying at 60 deg.C for 24 hr, and collecting precipitate;
(2) preparing a quantum dot/Fe-MOFs composite material: dissolving 1-5g of red phosphorus in alkali liquor, then adding 0.5-1 g of Fe-MOFs material, thoroughly and uniformly stirring, then centrifuging to collect precipitate, fully washing for 3 times by adopting ethanol and ultrapure water, drying for 24 hours at 50 ℃, and collecting precipitate; and transferring the precipitate to a tubular furnace, calcining at high temperature for 2-4 h under the condition of nitrogen, thoroughly cleaning the obtained precipitate by using ethanol and ultrapure water, drying at 60 ℃ for 24 h, and collecting the precipitate to obtain the FeP @ Fe-MOFs composite material.
2. The preparation method of the quantum dot iron-based metal organic framework composite material according to claim 1, wherein the size of Fe-MOFs in the step (1) is 50-200 nm.
3. The preparation method of the quantum dot iron-based metal organic framework composite material according to claim 1, wherein the mass ratio of Fe-MOFs to red phosphorus in the step (2) is 1: 1-1: 10.
4. The preparation method of the quantum dot iron-based metal organic framework composite material according to claim 1, wherein the pH of the alkali liquor in the step (2) is 4-6.
5. The preparation method of the quantum dot iron-based metal organic framework composite material according to claim 1, wherein the high-temperature calcination temperature in the step (2) is 400-600 ℃.
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| CN202011591555.XA CN112604717A (en) | 2020-12-29 | 2020-12-29 | Preparation method of quantum dot iron-based metal organic framework composite material |
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| CN115137820A (en) * | 2022-06-13 | 2022-10-04 | 西南交通大学 | Preparation method of nano enzyme compound for treating tumors |
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| CN115137820A (en) * | 2022-06-13 | 2022-10-04 | 西南交通大学 | Preparation method of nano enzyme compound for treating tumors |
| CN115137820B (en) * | 2022-06-13 | 2023-06-27 | 西南交通大学 | Preparation method of nano enzyme complex for treating tumors |
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