Method for high-efficiency preparing zeolite imidazole metal organic frame ZIF-90

A technology of ZIF-90 and metal-organic framework, which is applied in separation methods, zinc organic compounds, chemical instruments and methods, etc., can solve the problem of low yield of ZIF-90, lower separation performance of ZIF-90 membrane, unfavorable synthesis of high permeability Gas separation membrane, etc.

Active Publication Date: 2013-04-17
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

First of all, since N, N-dimethylformamide is a difficult volatile solvent, it is difficult to activate and remove N, N-dimethylformamide entering the ZIF-90 channel, which affects the gas adsorption of ZIF-90 Performance, especially high temperature activation is likely to cause cracks in the prepared ZIF-90 membrane, reducing the separation performance of the ZIF-90 membrane
Secondly, the particle size of ZIF-90 prepared by the currently reported synthesis method is usually several hundred microns, which is not conducive to the synthesis of gas separation membranes with high permeability.
In addition, the currently reported synthetic method produces ZIF-90 in a low yield (about 63%)

Method used

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  • Method for high-efficiency preparing zeolite imidazole metal organic frame ZIF-90
  • Method for high-efficiency preparing zeolite imidazole metal organic frame ZIF-90
  • Method for high-efficiency preparing zeolite imidazole metal organic frame ZIF-90

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preparation example Construction

[0046] Preparation of ZIF-90

[0047] In the present invention, ZIF-90 is prepared by the following method: mixing and reacting an appropriate amount of formate, methanol, zinc source and 2-imidazole carboxaldehyde; then filtering and drying the product to obtain the porous material ZIF-90.

[0048] Wherein, the raw materials can be mixed and prepared into a solution, which is used as a ZIF-90 synthesis mother liquor, and then the ZIF-90 synthesis mother liquor is reacted. In another preferred embodiment, the synthetic mother liquor is prepared by the following method: dissolving 2-imidazole carboxaldehyde and formate in anhydrous methanol, stirring the solution until it becomes clear, and preparing solution A; then dissolving the zinc source in anhydrous Methanol is prepared into solution B; solution A is slowly added into solution B, and the solution is mixed evenly by stirring at the same time, and the ZIF-90 synthetic mother liquor is prepared.

[0049] Wherein, the forma...

Embodiment 1

[0065] Dissolve 0.5772g (7.8992mmol) of imidazole-2-carbaldehyde and 0.2628g (3.9496mmol) of sodium formate in 30mL of anhydrous methanol, stir magnetically until the solution becomes clear, and prepare solution A; 0.1346g (0.9876mmol) of anhydrous ZnCl 2 Dissolve in 10 mL of anhydrous methanol to prepare solution B; slowly add clear solution A to solution B, and at the same time stir the solution evenly to make ZIF-90 synthesis solution; finally put ZIF-90 synthesis solution into high pressure reaction The solvothermal reaction was carried out in the kettle at 150 °C, and the product ZIF-90 was generated after the reaction was carried out for 8 h. The product is filtered and dried to obtain the final product ZIF-90 powder with a yield of about 90% (calculated by the amount of zinc).

[0066] It has been determined that the particle size of the ZIF-90 is 5-8 microns (attached). figure 1 ), no other crystals exist (attached figure 2 ), and N was determined by a gas adsorptio...

Embodiment 2

[0069] Dissolve 0.5772g (5.9244mmol) of imidazole-2-carbaldehyde and 0.2628g (3.9496mmol) of sodium formate in 30mL of anhydrous methanol, stir magnetically until the solution becomes clear, and prepare solution A; 0.1346g (0.9876mmol) of anhydrous ZnCl 2 Dissolve in 10 mL of anhydrous methanol to prepare solution B; slowly add clear solution A to solution B, and at the same time magnetically stir to make the solution evenly mixed, then prepare ZIF-90 synthesis solution; finally, put ZIF-90 synthesis solution into high pressure reaction The solvothermal reaction is carried out in the kettle at 120°C, and the product ZIF-90 can be produced after the reaction is carried out for 10 hours. The product was filtered and dried to obtain the final product ZIF-90 powder with a yield of about 85% (calculated by the amount of zinc).

[0070] It is determined that the particle size of the ZIF-90 is about 10 microns, and the N 2 The adsorption capacity is 1000m 2 / g.

[0071] The prepar...

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Abstract

The invention discloses a method for preparing a zeolite imidazole metal organic frame ZIF-90, concretely the zeolite imidazole metal organic frame ZIF-90 is made from methanol, formats, a zinc source, 2-formylimidazole. The method can effectively resolve the problem of difficulty for activating ZIF-90; reduces activation temperature and activation time, greatly promotes and crystallization of ZIF-90, and raises yield of ZIF-90.

Description

technical field [0001] The invention relates to the technical field of metal organic framework porous materials used in gas adsorption, storage, separation and the like, in particular to a preparation technology of zeolite imidazole metal organic framework materials. Background technique [0002] Metal-organic framework compounds are a new type of inorganic porous crystalline material with regular pore structure that has been developed in recent years. Inorganic metal centers and organic functional groups are connected to each other through covalent bonds or ionic bonds. Metal-organic framework compounds have very high porosity and specific surface area, which are much higher than traditional porous materials such as molecular sieves, and have strong gas adsorption capacity. The pore size of metal-organic framework compounds is similar to the molecular size of many important industrial raw materials, and gas molecules can be well separated by molecular sieving or type-select...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06B01J20/22B01D71/06B01D53/22
Inventor 黄爱生刘倩
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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