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Preparation method of shaped metal organic framework material

A technology of metal-organic framework and organic framework, which is applied in the field of preparation of shaped porous materials, can solve the problems of low utilization rate of material efficiency, influence on performance, and barriers to popularization and application, and achieve low cost, avoid clogging, and narrow particle size distribution Effect

Active Publication Date: 2021-11-05
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the blocking and coverage of the MOFs pore structure and active metal sites by the binder is inevitable, which will seriously affect its performance.
The embedding molding method represented by spray drying and electrospinning cannot avoid the clogging of the pore structure by the organic polymer chain (D. Lozano-Castelló, D. Cazorla-Amorós, A. Linares-Solano, et al. for methane storage: influence of binder[J].Carbon,2002,40(15):2817-2825.)
And its complex molding process and low utilization rate of material efficiency set up obstacles for its practical application

Method used

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  • Preparation method of shaped metal organic framework material
  • Preparation method of shaped metal organic framework material
  • Preparation method of shaped metal organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In the first step, accurately weigh 3.6g of PES and 0.4g of PVP, place them in a conical flask, add 14.3mL of N,N-dimethylformamide, and mechanically stir at 60°C until dissolved.

[0030] In the second step, add 2.4g of terephthalic acid and continue to stir until it dissolves evenly.

[0031] In the third step, take 5mL of the above solution with a syringe and place it on the syringe pump, adjust the speed of the syringe pump to 0.7mL / min, and squeeze out the droplets into 500mL of deionized water directly below the needle of the syringe for phase separation and gelation.

[0032] In the fourth step, after 12 hours, take out the millimeter-sized polymer beads and dry them at room temperature.

[0033] The fifth step, accurately weigh 2.0gCr(NO 3 ) 3 9H 2 O, dissolved in 35mL deionized water, added 0.15mL hydrofluoric acid (40%), and transferred to a 50mL polytetrafluoroethylene reactor.

[0034] In the sixth step, take 2.5 g of millimeter-sized polymer beads, add ...

Embodiment 2

[0037] Step 1: Accurately weigh 3.6g PES and 0.4g PVP, place them in a conical flask, add 15.6mL N,N-dimethylformamide, stir mechanically at 60°C until dissolved.

[0038] In the second step, add 1.2g of terephthalic acid and continue to stir until it dissolves evenly.

[0039] In the third step, take 5mL of the above solution with a syringe and place it on the syringe pump, adjust the speed of the syringe pump to 0.8mL / min, and squeeze out the droplets to 500mL of deionized water directly below the syringe needle for phase separation and gelation.

[0040] In the fourth step, after 12 hours, take out the millimeter-sized polymer beads and dry them at room temperature.

[0041] The fifth step, accurately weigh 1.25gCr(NO 3 ) 3 9H 2 O, dissolved in 22 mL of deionized water, added 0.1 mL of hydrofluoric acid (40%), and transferred to a 50 mL polytetrafluoroethylene reactor.

[0042] In the sixth step, take 2.0 g of millimeter-sized polymer beads, add them to the above reacti...

Embodiment 3

[0045] In the first step, accurately weigh 3.6g of PES and 0.4g of PVP, place them in a conical flask, add 14.3mL of N,N-dimethylformamide, and mechanically stir at 60°C until dissolved.

[0046] In the second step, add 2.4g of terephthalic acid and continue to stir until it dissolves evenly.

[0047] In the third step, take 5mL of the above solution with a syringe and place it on the syringe pump, adjust the speed of the syringe pump to 0.7mL / min, and squeeze out the droplets into 500mL of deionized water directly below the needle of the syringe for phase separation and gelation.

[0048] In the fourth step, after 12 hours, take out the millimeter-sized polymer beads and dry them at room temperature.

[0049] The fifth step, accurately weigh 0.50gCr(NO 3 ) 3 9H 2 O, dissolved in 15 mL of deionized water, added 0.1 mL of hydrofluoric acid (40%), and transferred to a 50 mL polytetrafluoroethylene reactor.

[0050] In the sixth step, take 1.04 g of millimeter-sized polymer bea...

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Abstract

The invention discloses a preparation method of a shaped metal organic framework material. The method couples the non-solvent-induced phase separation method with the preparation process of metal-organic framework materials, and millimeter-scale polymer beads with a single particle size distribution can be obtained through the extrusion process of a syringe pump, and a pore-forming agent is added to the system, so that When the fractal phase is gelled, a large number of interconnected pores such as sponge-like pores-finger-like pores can be formed, forming a developed pore structure. The molded metal organic framework material obtained by the in-situ growth of the solvothermal method in the present invention has a rich pore structure, effectively avoids the clogging of the pores by the binder, has the advantages of simple preparation, and is easy to expand industrial production. The prepared molded metal organic framework The material has broad application prospects in the fields of catalysis, separation, and environmental pollution remediation.

Description

technical field [0001] The invention belongs to the technical field of preparation of shaped porous materials, and relates to a preparation method of shaped metal organic framework materials. Background technique [0002] Metal Organic Frameworks (MOFs) is a crystalline porous material formed by the coordination and complexation of organic ligands and metal ions, because of its large specific surface area, adjustable pore size, and controllable structural properties. It has broad application prospects in adsorption separation, energy storage, catalysis and other fields. At present, whether it is at the laboratory level or a new material factory, limited by the preparation methods of MOFs, most of the obtained MOFs materials are nano-scale powdery substances. In practical application, they all face the technical problems of low bulk density, difficulty in storage, transportation and recycling. Especially in gas phase applications, problems such as large gas flow resistance,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C08J9/26C08L87/00
CPCC08G83/008C08J9/26C08J2201/0424C08J2381/06C08J2387/00C08J2439/06
Inventor 李健生齐俊文张雨婷孙义龙王连军孙秀云沈锦优韩卫清刘晓东
Owner NANJING UNIV OF SCI & TECH