CN108311173A - A kind of preparation method of Ce-MOF metal organic frameworks load thin film - Google Patents
A kind of preparation method of Ce-MOF metal organic frameworks load thin film Download PDFInfo
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- CN108311173A CN108311173A CN201711445748.2A CN201711445748A CN108311173A CN 108311173 A CN108311173 A CN 108311173A CN 201711445748 A CN201711445748 A CN 201711445748A CN 108311173 A CN108311173 A CN 108311173A
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- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010409 thin film Substances 0.000 title claims abstract description 12
- 239000010408 film Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000012452 mother liquor Substances 0.000 claims abstract description 13
- 235000019441 ethanol Nutrition 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000013110 organic ligand Substances 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims abstract description 3
- 239000003960 organic solvent Substances 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 150000001735 carboxylic acids Chemical class 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 229940037003 alum Drugs 0.000 claims description 3
- 210000005252 bulbus oculi Anatomy 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 150000001991 dicarboxylic acids Chemical group 0.000 claims description 3
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- -1 dimethyl methyl Chemical group 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 150000003628 tricarboxylic acids Chemical class 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 abstract 2
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000000887 face Anatomy 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
-
- B01J35/39—
-
- 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
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/30—Complexes comprising metals of Group III (IIIA or IIIB) as the central metal
- B01J2531/38—Lanthanides other than lanthanum
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of Ce MOF metal organic framework load thin films, includes the following steps:The preparation of A.Ce MOF metal organic frameworks:1. by cerous nitrate and 2 carboxylic acid of pyrazine according to 2:1‑4:1 is dissolved in the mixed solution of water and ethyl alcohol, is transferred in closed reaction vessel after 2 4h of stirring at normal temperature;2. controlling the temperature in closed reaction vessel between 70 80 DEG C, then 2 carboxylic acid of pyrazine and NaOH stirring and dissolvings in water and are added in above-mentioned reaction system by sealing 1 2h of reaction, the reaction was continued 48 72h;3. being down to room temperature, precipitate is washed with water and ethyl alcohol successively, is dried to obtain Ce MOF metal organic frameworks;B. inorganic supporting body is reacted in the film mother liquor being mixed by metal salt, organic ligand and solvent, to generate one layer of metal organic framework crystal seed in supporting body surface, then continuous Ce MOF metal organic framework loaded films are prepared by the second secondary response.The Ce MOF metal organic framework loaded films that integrality is good and stability is high can be prepared by this method.
Description
Technical field
The invention belongs to thin film materials arts, are specifically related to a kind of preparation side of Ce-MOF metal organic frameworks load thin film
Method.
Background technology
Implementation with China's strategy of sustainable development and addition persistence organic pollutant pact, the water of colored dyes
Matter pollution problem has become one of China's letter problem to be solved.Wherein, photocatalysis is with its room temperature deep reaction and can be direct
Using special performances such as solar energy, and become a kind of ideal environmental pollution treatment technology and clear energy sources production technology.And it is honest and clean
Valence, stabilization, efficient catalysis material become research hotspot.Membrane separation technique has separative efficiency height, energy consumption relatively low, especially easy
The features such as combining combination with catalysis reaction and other membrane process, develops very rapidly, has become solution contemporary people in recent decades
The important means of key issues of energy that class faces, resource, environment, be support sustainable development important common technology it
One.
Invention content
The present invention provides a kind of preparation methods of Ce-MOF metal organic frameworks load thin film, can be prepared by this method
Go out the Ce-MOF metal organic framework loaded films that integrality is good and stability is high, and the loaded film in photocatalytic degradation containing organic
Good catalytic activity is shown in the waste water experiment of dyestuff, and Ke Xunhuanliyong.
As above design, the technical scheme is that:A kind of preparation method of Ce-MOF metal organic frameworks load thin film,
It is characterized in that:Include the following steps:
The preparation of A.Ce-MOF metal organic frameworks:
1. by cerous nitrate and -2 carboxylic acid of pyrazine according to 2:1-4:1 is dissolved in the mixed solution of water and ethyl alcohol, stirring at normal temperature 2-
It is transferred in closed reaction vessel after 4h;
2. the temperature in closed reaction vessel is controlled between 70-80 DEG C, sealing reaction 1-2h, then by -2 carboxylic of pyrazine
Acid and NaOH stirring and dissolvings in water and are added in above-mentioned reaction system, the reaction was continued 48-72h;
3. being down to room temperature, precipitate is washed with water and ethyl alcohol successively, is dried to obtain Ce-MOF metal organic frameworks;
B. inorganic supporting body is reacted in the film mother liquor being mixed by metal salt, organic ligand and solvent,
To generate one layer of metal organic framework crystal seed in supporting body surface, then continuous Ce-MOF metals are prepared by the second secondary response
Organic backbone loaded film.
The mass concentration of organic ligand is 0.2-3% in above-mentioned film mother liquor, and the mass concentration of metal salt is 1-5%, gold
It is Ce to belong to the metallic element in salt.
Solvent in above-mentioned film mother liquor be ethyl alcohol, dimethyl methyl phthalein amine, toluene, methanol, chlorobenzene, diethyl first phthalein amine,
Dimethyl alum, water, hydrogen peroxide, methylamine, sodium hydroxide solution, second eyeball, section base chlorine, triethylamine, one kind in ethylene glycol or
The mixture that two kinds of person.
Organic ligand in above-mentioned film mother liquor is dicarboxylic acids, one or both of tricarboxylic acids or tetrabasic carboxylic acid organic matter.
The present invention has the advantage that and good effect:
1, the present invention carries simple, easy to operate.
2, the Ce-MOF metal organic framework loaded film continuitys of the invention prepared are good, integrality is high.
3, present invention efficiently solves binding force between material and supporter is weak, the technological difficulties to form a film are not easy.
4, universality of the present invention is wide, is suitable for the preparation of various films, contains to the prepare with scale and photocatalytic degradation of film
The waste water of engine dyeing material has important directive significance.
Specific implementation mode
With reference to the embodiment technical solution that the present invention will be described in detail, but protection domain is not limited thereto.
A kind of preparation method of Ce-MOF metal organic frameworks load thin film, includes the following steps:
The preparation of A.Ce-MOF metal organic frameworks:
1. by cerous nitrate and -2 carboxylic acid of pyrazine according to 2:1-4:1 is dissolved in the mixed solution of water and ethyl alcohol, stirring at normal temperature 2h
After be transferred in closed reaction vessel;
2. the temperature in closed reaction vessel is controlled between 70-80 DEG C, sealing reaction 1h, then by -2 carboxylic acid of pyrazine
And NaOH stirring and dissolvings in water and are added in above-mentioned reaction system, the reaction was continued 48-72h;
3. being down to room temperature, precipitate is washed with water and ethyl alcohol successively, is dried to obtain Ce-MOF metal organic frameworks;
The preparation of B.Ce-MOF metal organic framework loaded films:
1. inorganic supporting body surface is polished smooth, impregnated with soda acid, then is dried for standby after being rinsed with water totally;
2. configuration film mother liquor, organic ligand, metal salt and solvent is mixed and stirred for uniformly, wherein the matter of organic ligand
A concentration of 0.2-3% is measured, the mass concentration of metal salt is 1-5%, and the metallic element in metal salt is Ce;
3. inorganic supporting body is put into reaction kettle, the film mother liquor configured is added, 48-60 is reacted at 100-120 DEG C
Hour, it is rinsed with water clean after cooling and dries, obtain Ce-MOF metal organic framework loaded films.
Solvent in above-mentioned film mother liquor be ethyl alcohol, dimethyl methyl phthalein amine, toluene, methanol, chlorobenzene, diethyl first phthalein amine,
Dimethyl alum, water, hydrogen peroxide, methylamine, sodium hydroxide solution, second eyeball, section base chlorine, triethylamine, one kind in ethylene glycol or
The mixture that two kinds of person.
Organic ligand in above-mentioned film mother liquor is dicarboxylic acids, one or both of tricarboxylic acids or tetrabasic carboxylic acid organic matter.
Claims (4)
1. a kind of preparation method of Ce-MOF metal organic frameworks load thin film, it is characterised in that:Include the following steps:
The preparation of A.Ce-MOF metal organic frameworks:
1. by cerous nitrate and -2 carboxylic acid of pyrazine according to 2:1-4:1 is dissolved in the mixed solution of water and ethyl alcohol, after stirring at normal temperature 2-4h
It is transferred in closed reaction vessel;
2. the temperature in closed reaction vessel is controlled between 70-80 DEG C, sealing reaction 1-2h, then by -2 carboxylic acid of pyrazine and
NaOH stirring and dissolvings in water and are added in above-mentioned reaction system, the reaction was continued 48-72h;
3. being down to room temperature, precipitate is washed with water and ethyl alcohol successively, is dried to obtain Ce-MOF metal organic frameworks;
B. inorganic supporting body is reacted in the film mother liquor being mixed by metal salt, organic ligand and solvent, to
One layer of metal organic framework crystal seed is generated in supporting body surface, then by the second secondary response to prepare continuous Ce-MOF metals organic
Skeleton adulteration film.
2. a kind of preparation method of Ce-MOF metal organic frameworks load thin film according to claim 1, it is characterised in that:
The mass concentration of organic ligand is 0.2-3% in above-mentioned film mother liquor, and the mass concentration of metal salt is 1-5%, in metal salt
Metallic element is Ce.
3. a kind of preparation method of Ce-MOF metal organic frameworks load thin film according to claim 1, it is characterised in that:
Solvent in above-mentioned film mother liquor is ethyl alcohol, dimethyl methyl phthalein amine, toluene, methanol, chlorobenzene, diethyl first phthalein amine, dimethyl Asia
It is one or two kinds of in alum, water, hydrogen peroxide, methylamine, sodium hydroxide solution, second eyeball, section base chlorine, triethylamine, ethylene glycol
Mixture.
4. a kind of preparation method of Ce-MOF metal organic frameworks load thin film according to claim 1, it is characterised in that:
Organic ligand in above-mentioned film mother liquor is dicarboxylic acids, one or both of tricarboxylic acids or tetrabasic carboxylic acid organic matter.
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Cited By (6)
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CN110632064A (en) * | 2019-09-20 | 2019-12-31 | 南京大学 | Multi-element paper-based sliding microfluidic chip based on cerium metal organic framework |
CN114011470A (en) * | 2021-11-29 | 2022-02-08 | 首都师范大学 | Catalyst for hydrolyzing adenosine triphosphate and preparation method and application thereof |
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2017
- 2017-12-27 CN CN201711445748.2A patent/CN108311173A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109847590A (en) * | 2019-01-17 | 2019-06-07 | 东华大学 | A kind of preparation method of the temperature sensitive metal organic frame nanometer chip base filter membrane of two dimension |
CN109847590B (en) * | 2019-01-17 | 2021-07-02 | 东华大学 | Preparation method of two-dimensional temperature-sensitive metal organic framework nanosheet-based filter membrane |
CN110124739A (en) * | 2019-06-03 | 2019-08-16 | 江南大学 | A kind of cross-linking type CD-MOF composite material and preparation method loading nano-photocatalyst |
CN110302839A (en) * | 2019-07-11 | 2019-10-08 | 南京工业大学 | A kind of smooth fenton catalyst and its preparation method and application |
CN110632064A (en) * | 2019-09-20 | 2019-12-31 | 南京大学 | Multi-element paper-based sliding microfluidic chip based on cerium metal organic framework |
CN114011470A (en) * | 2021-11-29 | 2022-02-08 | 首都师范大学 | Catalyst for hydrolyzing adenosine triphosphate and preparation method and application thereof |
CN114373971A (en) * | 2021-12-30 | 2022-04-19 | 上海应用技术大学 | Preparation method of proton exchange membrane blended by perfluorinated sulfonic acid resin and Ce-MOF |
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