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Macroscopic quantity preparation method and morphology control method of hybrid zeolite imidazole framework materials

A technology for zeolite imidazole and frame materials, which is applied in the field of macro-scale preparation and shape control of hybrid zeolite imidazole frame materials, can solve the problems of inability to scale up synthesis and long time, and achieve the convenience of large-scale production, shortened reaction time, and post-processing Handling simple and easy effects

Active Publication Date: 2019-10-25
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Macroscopic quantity preparation method and morphology control method of hybrid zeolite imidazole framework materials
  • Macroscopic quantity preparation method and morphology control method of hybrid zeolite imidazole framework materials
  • Macroscopic quantity preparation method and morphology control method of hybrid zeolite imidazole framework materials

Examples

Experimental program
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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 particularly relates to a macroscopic quantity preparation method and morphology control method of hybrid zeolite imidazole framework materials. The macroscopic quantity preparation method comprises the following steps that (1) transition metal compounds, imidazole compounds and molybdenum or tungsten compounds are mixed and react under the conditions of heating and stirring, or ultrasound, or microwave, or ball milling; and (2) a reacted mixture is separated to obtain a crystalline object. The problem that in aconventional preparation method of the hybrid zeolite imidazole frameworks, reaction needs to be conducted under the airtight high-pressure conditions, and amplification preparation cannot be achievedis solved, meanwhile, a synthesis technology is simple in requirement, the reaction time is greatly shortened, and large-scale production is facilitated.

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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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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