CN110606960A - Preparation method of rectangular strip-shaped Al-MOF material - Google Patents
Preparation method of rectangular strip-shaped Al-MOF material Download PDFInfo
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- CN110606960A CN110606960A CN201910995535.XA CN201910995535A CN110606960A CN 110606960 A CN110606960 A CN 110606960A CN 201910995535 A CN201910995535 A CN 201910995535A CN 110606960 A CN110606960 A CN 110606960A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
Abstract
The invention discloses a preparation method of a rectangular strip Al-MOF material, which comprises the following steps: mixing AlCl3·6H2Mixing the O and the DMF solution, adding pyromellitic acid to prepare a mixed solution, transferring the mixed solution into a hydrothermal reaction kettle lined with a polytetrafluoroethylene container, and reacting in an electric heating constant-temperature air-blowing drying oven at the temperature of 110-; naturally cooling to room temperature, centrifuging the product, and washing; and finally, drying in an electric heating constant-temperature blast drying oven to obtain the rectangular strip Al-MOF material. The rectangular strip Al-MOF material obtained by the method has uniform appearance, simple and easy operation and no pollution in the synthesis process.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a preparation method of a rectangular strip-shaped Al-MOF material.
Background
The MOFs material is a coordination polymer with a three-dimensional pore structure, has the advantages of large specific surface area, adjustable pore particles, easy structure functionalization and the like, and has wide application in catalysis, energy storage, separation and catalysis; the MOFs materials have diversity with organic ligands and metal ions, the structure types are diversified immediately, and the research and development of the MOFs materials are further progressed continuously due to the combination of directionality and modification of functional groups.
The metal aluminum raw material is easy to obtain, and the cost of the metal ions used for developing the MOFs material is lower than that of other MOFs materials. At the present stage, the development of aluminum-based MOFs materials with certain morphologies, particularly materials with controllable morphology, is still a hot point of research.
Disclosure of Invention
The invention provides a preparation method of a rectangular strip Al-MOF material aiming at the problems.
In order to achieve the above purpose, the method of the invention is as follows: mixing AlCl3·6H2Mixing O with DMF solution, adding pyromellitic acid to prepare mixed solution, and mixing in AlCl ratio3·6H2The molar ratio of O to pyromellitic acid is 1.15 ~ 1.25.25: 1, the mixed solution is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene container lining, and is reacted in an electrothermal constant-temperature blast drying oven at the temperature of 110-.
Compared with the prior art, the invention has the beneficial effects that: the method disclosed by the invention is green and environment-friendly, is simple and easy to operate, overcomes the defects of the conventional method, is high in product yield, and obtains the preparation method of the rectangular strip-shaped Al-MOF material.
Detailed Description
The following detailed description of the invention is provided to illustrate the practice and resulting advantages of the invention. It is to be understood that the particulars described herein are by way of illustration and explanation only and are not intended to limit the present invention.
The endpoints of the ranges and any values recited herein are not limited to the precise range or value, and are to be understood as inclusive of and proximate to those ranges and values recited. As between the endpoints of the ranges and between the individual points of value, one or more new value ranges and individual points of value may be combined with each other and these values and ranges should be considered as specifically disclosed herein.
Example 1
0.4104g of CuNO was weighed out3Placed in a 50ml beaker, which is then dissolved in 35ml of DMF; adding 0.3558g of pyromellitic acid, stirring until the pyromellitic acid is dissolved, and transferring the mixture into a polytetrafluoroethylene container with a lining; transferring the polytetrafluoroethylene-lined container into a hydrothermal synthesis reaction kettle, placing the kettle in an electric heating constant-temperature air-blast drying oven, and reacting for 24 hours at 140 ℃; after the reaction is finished, naturally cooling to room temperature, centrifuging the product (10000 r/min), washing the product for 3 times by using ethanol and ultrapure water, then transferring the product into an electric heating constant-temperature blast drying oven again, and drying the product for 4 hours at the temperature of 80 ℃ to obtain a white rectangular strip-shaped Al-MOF material product.
Example 2
0.4104g of CuNO was weighed out3Placed in a 50ml beaker, which is then dissolved in 35ml of DMF; adding 0.3558g of pyromellitic acid, stirring until the pyromellitic acid is dissolved, and transferring the mixture into a polytetrafluoroethylene container with a lining; transferring the polytetrafluoroethylene-lined container into a hydrothermal synthesis reaction kettle, placing the kettle in an electric heating constant-temperature air-blowing drying oven, and reacting for 24 hours at the temperature of 120 ℃; after the reaction is finished, naturally cooling to room temperature, centrifuging the product (4000 r/min), washing the product for 3 times by using ethanol and ultrapure water, then transferring the product into an electric heating constant-temperature blast drying oven again, and drying the product for 5 hours at the temperature of 60 ℃ to obtain a white rectangular strip-shaped Al-MOF material product.
The above description is only a preferred embodiment of the present invention, it should be noted that the present invention is not limited thereto, and that within the scope of the present invention concept, many simple modifications can be made to the technical solution of the present invention, including various technical features being combined in any other appropriate manner, and these simple modifications and combinations should also be regarded as the disclosure of the present invention, and all fall within the protection scope of the present invention.
Claims (4)
1. A preparation method of a rectangular strip Al-MOF material is characterized by comprising the following steps:
(1) mixing AlCl3·6H2Mixing O with DMF solution, adding pyromellitic acid to prepare mixed solution, and mixing in AlCl ratio3·6H2The molar ratio of O to pyromellitic acid is 1.15 ~ 1.25.1.25: 1;
(2) transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene-lined container, and reacting for 18-24h in an electric heating constant-temperature air-blast drying box at the temperature of 110-;
(3) naturally cooling to room temperature, centrifuging the product, and then washing with ethanol and ultrapure water;
(4) and finally, drying in an electric heating constant-temperature blast drying oven to obtain the rectangular strip Al-MOF material.
2. The method for preparing the rectangular strip Al-MOF material according to claim 1, wherein the AlCl is adopted in the step (1)3·6H2The molar ratio of O to pyromellitic acid was 1.15 ~ 1.25.1.25: 1.
3. The method for preparing the Al-MOF material with the rectangular strip shape as claimed in claim 1, wherein the reaction temperature of the solution in the step (2) is 110-150 ℃, and the reaction time is 18-24 h.
4. The preparation method of the rectangular strip Al-MOF material according to claim 1, wherein the cooling mode after the reaction in the step (3) or (4) is natural cooling, the centrifugal rotation speed is 4000 ~ 10000r/min during cleaning, ethanol and ultrapure water are cleaned for 3 times, and the drying temperature is 60 ~ 80 ℃.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112054178A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Porous silicon @ silicon oxide @ Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
CN112054187A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Plate brick type Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
CN112054186A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Preparation method and application of Al-MOF negative electrode material synthesized by solvothermal method |
-
2019
- 2019-10-18 CN CN201910995535.XA patent/CN110606960A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112054178A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Porous silicon @ silicon oxide @ Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
CN112054187A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Plate brick type Al-MOF negative electrode material for lithium ion battery and preparation method and application thereof |
CN112054186A (en) * | 2020-09-14 | 2020-12-08 | 大连理工大学 | Preparation method and application of Al-MOF negative electrode material synthesized by solvothermal method |
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