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Large-scale adsorbing material ZIF-8 preparation method and forming method

A ZIF-8, adsorption material technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of good repeatability and insufficient yield of synthetic methods, and achieve high crystallinity, improved yield, and good repeatability. Effect

Active Publication Date: 2013-08-07
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the materials synthesized by the solvothermal method are nano-scale powder substances, and their application must face two bottlenecks: (1) they can be synthesized in large quantities, and the synthesis method is reproducible; (2) the molding of powdery raw powder
[0003] The synthesis methods of ZIFs recorded in the literature are all carried out in a reactor with a small volume, and the yield is less than 0.1g each time.
At present, the research on the forming method of ZIFs material is still blank. Considering that the structure of the material is similar to that of zeolite, so, taking the catalyst forming as a reference, and combining the characteristics of the material itself, to find an appropriate binder and peptizer. Molding for further research

Method used

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  • Large-scale adsorbing material ZIF-8 preparation method and forming method
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  • Large-scale adsorbing material ZIF-8 preparation method and forming method

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Weigh 0.9556g of Zn(NO 3 ) 2 ·6H 2 O and 0.791g of 2-methylimidazole, the ratio of the amount of the two substances is approximately 1:3, and the DMF of 72ml is weighed with a measuring cylinder of 100ml. The reaction was carried out in a hydrothermal reactor with a Teflon liner. First add weighed DMF to the inner liner of polytetrafluoroethylene, then add the weighed 2-methylimidazole and Zn(NO 3 ) 2 ·6H 2 O, stir evenly with a glass rod until the crystal raw material is completely dissolved; then put the polytetrafluoroethylene lining into the hydrothermal kettle, tighten the stainless steel outer kettle, and carry out the crystallization reaction by self-generated pressure; finally, put the reaction kettle into the oven During the process, the room temperature was raised to 140°C at a rate of 5°C / min, and the temperature was kept constant for 24 hours. Suction filter the synthesized product, then in CH 3 Soak in OH solution for 48 hours, and then dry in an ove...

Embodiment 2

[0041] Weigh 0.5 g of the powdered material of Example 1, use trichloroacetic acid as the peptizer, and select the turnip powder as the binder, the amount of which is 10% of the original powder mass, and the amount of trichloroacetic acid is about 0.3ml. Then grind evenly, the product is carried out tabletting on the tablet machine, finally make the sheet material that radius is 0.9mm. Each molding material was characterized by BET to investigate the influence of molding conditions on the specific surface area of ​​the sample, as shown in the attached figure 2 shown. The molded samples were characterized by XRD, and the results are shown in the attached image 3 shown.

[0042] Figure 4 It shows that the specific surface area of ​​the molded product is reduced by 135.37m2 by adding 10% of the mass of the original powder. 2 / g, the specific surface area loss is 11.4%. It shows that the choice of molding conditions did not cause a large loss to the adsorption properties o...

Embodiment 3

[0044] Weigh 0.5 g of the powdered material of Example 1, use trichloroacetic acid as the peptizer, select methyl cellulose as the binder, the amount is 10% of the original powder mass, and the amount of trichloroacetic acid is about 0.3 ml. Then grind evenly, the product is carried out tabletting on the tablet machine, finally make the sheet material that radius is 0.9mm. Each molding material was characterized by BET to investigate the influence of molding conditions on the specific surface area of ​​the sample, as shown in the attached Image 6 shown. The molded samples were characterized by XRD, and the results are attached Figure 7 shown.

[0045] Image 6 It shows that the specific surface area of ​​the molded product decreases by 123.38m3 by adding methyl cellulose with 10% of the original powder mass. 2 / g, the specific surface area loss is 10.4%. It shows that the choice of molding conditions did not cause a large loss to the adsorption properties of the materia...

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Abstract

The invention discloses a large-scale adsorbing material ZIF-8 synthesizing and forming methods, and belongs to the technical field of adsorbing materials. The method comprises the steps of: pouring 70-75ml of dimethyl formamide (DMF) into a polytetrafluoroethylene liner with the volume of 100ml, and adding Zn(NO3)2.6H2O and 2-methylimidazole according to a molar ratio of 1:(2-4) to be fully dissolved; crystallizing under self-generated pressure; heating from a room temperature to a preset crystallization temperature through programs, and then preserving a constant temperature for a plurality of hours; cooling, filtering in vacuum and washing; weighing and putting ZIF-8 powder into a mortar, and adding an adhesion agent to be completely ground together; then adding a peptizing agent, and completely grinding the peptizing agent in the mortar until wet fine powder is formed; and tabletting the obtained wet fine powder through a tabletting machine so as to obtain a platy ZIF-8 mateiral. The ZIF-8 synthesized by the method has high crystallinity and good adsorption property.

Description

technical field [0001] The invention relates to a preparation method and a molding method of an adsorption material ZIF-8, belonging to the technical field of adsorption materials. Background technique [0002] As a conventional porous adsorption material, zeolites account for a large part of the global economy due to their benefits in petroleum cracking, water purification, and gas adsorption. However, zeolite has a rigid structure, relatively short bridge oxygen bonds, and lacks flexibility, so there are certain defects. In recent years, a new class of MOFs—imidazolate-metal-organic frameworks (ZIFs) has attracted attention. The material structure is very similar to that of zeolite, and has large specific surface area, high pore volume, good hydrothermal stability, and resistance to organic solvents. The above characteristics make this material have excellent application prospects in the field of gas adsorption. However, the materials synthesized by the solvothermal met...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30
Inventor 朱吉钦魏浩然黄巍刘新斌郭翔
Owner BEIJING UNIV OF CHEM TECH
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