Macro-scale preparation and morphology control method of hybrid zeolite imidazole framework materials

A technology of zeolite imidazole and framework materials, which is applied in the field of macro-scale preparation and shape control of hybrid zeolite imidazole framework materials, can solve the problems of inability to scale up synthesis and long time, and achieve the convenience of large-scale production, shortening of reaction time, and synthesis The process requires simple effects

Active Publication Date: 2021-08-10
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method takes a long time and needs to be carried out under very high pressure and in a closed environment, so it is impossible to scale up the synthesis

Method used

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  • Macro-scale preparation and morphology control method of hybrid zeolite imidazole framework materials
  • Macro-scale preparation and morphology control method of hybrid zeolite imidazole framework materials
  • Macro-scale preparation and morphology control method of hybrid zeolite imidazole framework materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Heating and stirring: ①Zn(CH 3 COO) 2 2H 2 O (0.176g, 0.8mmol), 2-mim (0.098g, 1.2mmol), H 2 MoO 4 (0.03g, 0.2mmol), put the raw material in a round bottom flask, add DMF, reflux and stir at a temperature of 160°C for 2 hours, filter the obtained product, wash the separated solid with water, and put it in an oven at 80°C Dry to obtain HZIF-1Mo crystals.

[0055] ②Zn(CH 3 COO) 2 2H 2 O (0.176g, 0.8mmol), 2-mim (0.098g, 1.2mmol), H 2 MoO 4 (0.03g, 0.2mmol), put the raw material in a round bottom flask, add methanol, reflux and stir at a temperature of 60°C for 2 hours, filter the obtained product, wash the separated solid with water, and put it in an oven at 80°C Dry to obtain HZIF-1Mo crystals.

Embodiment 2

[0057] Ultrasonic response: Zn(CH 3 COO) 2 2H 2 O (0.180g, 0.8mmol), 2-mim (0.096g, 1.2mmol), H 2 MoO 4 (0.028g, 0.2mmol), put the raw materials in a beaker, add DMF, and sonicate in an ultrasonic instrument for 4 hours, filter the obtained product, wash the separated solid with water, and dry it in an oven at 80°C to obtain HZIF-1Mo crystalline matter.

Embodiment 3

[0059] Microwave reaction: Zn(CH 3 COO) 2 2H 2 O (0.174g, 0.8mmol), 2-mim (0.098g, 1.2mmol), H 2 MoO 4 (0.034g, 0.2mmol), put the raw materials in a bottle, add DMF, microwave in a microwave oven for 45 minutes, filter the obtained product, wash the separated solid with water, and dry it in an oven at 80°C to obtain HZIF-1Mo crystalline matter.

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Abstract

The invention belongs to the technical field of crystal material preparation, and in particular relates to a method for macro-preparation and shape control of a hybrid zeolite imidazole framework material. The method comprises the following steps: 1) mixing a transition metal compound, an imidazole compound, and a molybdenum or tungsten compound, and reacting under heating and stirring, or ultrasonic, microwave, or ball milling conditions; 2) performing a reaction on the reacted mixture Separation gave crystalline material. The method of the invention overcomes the problems that the conventional preparation method of the hybrid zeolite imidazole frame material needs to be reacted under a closed high-pressure condition, and cannot be scaled up for preparation. At the same time, the synthesis process requires simple, greatly shortened reaction time, and is convenient for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of crystal material preparation, and in particular relates to a method for macro-preparation and shape control of a hybrid zeolite imidazole framework material. Background technique [0002] Metal-organic frameworks (metal-organic frameworks, MOFs) are a new class of porous materials generated by the self-assembly process of metal ions and organic ligands. They have large specific surface area, regular pore structure, and adjustable pore and surface chemical properties. and other features. MOFs have shown broad application prospects in adsorption, separation, and catalysis. [0003] The target material of the present invention, HZIF-1, is a MOF material reported in Angewandte Chemie, 2011, 50, 450-453. The method used in this document is the solvothermal method, and the specific synthesis method is to mix zinc acetate, 2-methylimidazole, molybdic acid and DMF in a 23ml reactor, place it in an oven at 160°C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 王滢王飞张健
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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