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Metal organic framework glass film and preparation method thereof

A technology of metal-organic framework and glass membrane, which is applied in the field of membrane technology separation

Active Publication Date: 2021-08-20
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, before applying for this patent, there is no suitable method to prepare such materials into films

Method used

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  • Metal organic framework glass film and preparation method thereof
  • Metal organic framework glass film and preparation method thereof
  • Metal organic framework glass film and preparation method thereof

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preparation example Construction

[0027] In the preparation method of the MOF glass film of the present invention, the melting and quenching method is used to convert the crystalline MOF material into MOF glass, and the melting temperature has different adaptive values ​​according to different MOF material selections, and the general melting temperature selection standard Yes: higher than the melting point of the material to be tested and lower than the decomposition temperature of the material. Of course, this is only the most basic guiding principle, and there are still many factors to be considered in the process of applying this principle to the melting process of specific materials. In actual tests, there are still many MOF materials that cannot be successfully melted within this temperature range. In the present invention, the preferred melting temperature of MOFs is 370-600°C, and the most preferred melting temperature of ZIF-62 and ZIF-76 materials is 440-450°C. During the melting process, the tempera...

Embodiment 1

[0032] Preparation of ZIF-62 glass self-supporting film by traditional method of pressing and sintering

[0033] (1) Preparation of ZIF-62 powder: uniformly mix zinc nitrate hexahydrate, imidazole, benzimidazole, and DMF in a molar ratio of 1:12.5:3:200. Take 50mL of the solution in a reaction kettle, react at 130°C for 48h, wash with fresh DMF three times, and dry under vacuum at 100°C to obtain ZIF-62 powder.

[0034] (2) Tablet compression: place 0.1 g of the prepared ZIF-62 powder in the tank of the tablet press, and stay for 15 minutes under the condition of 15Mpa to obtain self-supporting ZIF-62 discs.

[0035] (3) Melting and quenching: firstly, the ZIF-62 powder is detected by differential scanning calorimetry, and the heat change of the material in the heating process is analyzed ( figure 1 ), the analysis shows that the melting point of ZIF-62 material is 434°C, and the glass transition temperature is 335°C. At 440°C-500°C, ZIF-62 can undergo a melting process without...

Embodiment 2

[0037] Prepare supported ZIF-62 glass membrane by solvothermal method:

[0038] (1) Seed crystal growth: uniformly mix zinc nitrate hexahydrate, imidazole, benzimidazole, and DMF in a molar ratio of 1:12.5:3:200. Take 10mL of the solution in a 25mL beaker, and put α-Al with a surface pore size of 70nm 2 o 3 The carrier piece was placed at the bottom of the beaker and allowed to stand for 48 hours.

[0039] (2) Melting and quenching: Dry the carrier sheet with the grown seed layer at 100°C for 2 hours, then transfer it to a tube furnace, and raise the temperature from room temperature to 10°C / min under argon protection. 440°C, stop heating, and quickly cool to room temperature.

[0040] The ZIF-62 glass film was characterized as follows:

[0041] Detection of ZIF-62 powder by X-ray diffraction ( image 3 ) and ZIF-62 seed layer ( Figure 4 ), according to the detected peak position, further judge the crystal structure of the material. Compared with the corresponding crys...

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Abstract

A metal-organic framework glass film and a preparation method thereof, the preparation method comprises the steps of heating a crystalline metal-organic framework material to a melting temperature at a rate of 1-15°C / min, and then naturally cooling, wherein the crystalline state The metal-organic framework material contains metal nodes and ligands A; the metal nodes are zinc ions and / or cobalt ions; the ligands A are imidazole or phosphoric acid. Using the method of the invention to synthesize the metal-organic framework glass film, the film-forming conditions are wide, the material can be melted without being decomposed within the control range, and a continuous glass layer can be formed, and the repeatability is good. The prepared membrane product has good temperature resistance and has a good application prospect in the field of gas separation.

Description

technical field [0001] The invention belongs to the field of membrane technology separation, and in particular relates to a preparation method of a metal organic framework glass membrane and its application in gas mixture separation. Background technique [0002] Glass generally refers to amorphous inorganic non-metallic materials, usually using inorganic minerals as the main raw material, mixed with a certain proportion of metal oxides or salts to prepare colored glass. With the development of polymers, some transparent plastics are also included in the category of glass, called plexiglass. [0003] Most glass materials are produced by melting and quenching. During rapid cooling, the viscosity increases, which prevents crystallization and promotes the formation of glass. From a chemical point of view, traditional melt-quenched glasses can be divided into three categories: inorganic non-metallic, organic and metallic glasses, and their chemical bonds are ion-covalent mixed ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/06B01D71/04B01D67/00B01D53/22
CPCB01D71/06B01D71/04B01D67/0079B01D53/228B01D2323/12B01D2323/081B01D67/00411B01D2256/10B01D2257/504B01D24/06B01D29/01B01D2323/219B01D69/106B01D69/108
Inventor 李砚硕金花王雨寒
Owner NINGBO UNIV