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A kind of covalent organic polymer for methane adsorption storage and preparation method thereof

A covalent organic, polymer technology, applied in separation methods, mechanical equipment, chemical instruments and methods, etc., can solve the problems of poor thermal stability and water stability, limited large-scale industrial application, poor chemical stability, etc. The effect of skeletal density, good hydrothermal and chemical stability, high specific surface area

Active Publication Date: 2019-11-15
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, from the perspective of chemical structure, MOF materials are composed of coordination bonds between metals and organic monomers, and their chemical stability is poor compared to covalent bonds.
Although BASF has also scaled up and synthesized some MOF materials, most of the prepared MOF materials show defects of poor thermal stability and water stability, which limits large-scale industrial applications.
In addition, there are many heavy metals in MOF materials, the preparation cost is high, and it is not conducive to environmental protection. Recycling waste MOF materials is also facing great challenges.

Method used

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  • A kind of covalent organic polymer for methane adsorption storage and preparation method thereof
  • A kind of covalent organic polymer for methane adsorption storage and preparation method thereof
  • A kind of covalent organic polymer for methane adsorption storage and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] First, dissolve 0.432g of bis-(1,5-cyclooctadiene)nickel ([Ni(cod)2]) in 30mL of DMF solution, stir until completely dissolved, then add 0.246g of 2,2'-bipyridine and 0.192ml of 1,5-cyclooctadiene (cod) were added to the mixture and stirred for about 30 minutes, then 0.1065g of TBM and 0.07g of XTBB were added into the solution, and the reaction was stirred at 85°C for 10 hours. After cooling, add an appropriate amount of concentrated hydrochloric acid until the medium solution turns transparent green, filter with CHCl 3 (5×15mL), THF (5×15mL) and H 2 O (5 x 15 mL) washes. The filtered sample was then vacuum dried at 120° C. for 24 hours. This sample was named COP-10. The experimental characterization results are as follows:

[0026] COP-10 was degassed at 180°C for 8 hours, and then ASAP 2020 was used for specific surface area and pore size analysis. figure 2 is the nitrogen adsorption curve of COP-10, at P / P 0 When image 3 The results are consistent. The pore ...

Embodiment 2

[0031] First, dissolve 0.324g of bis-(1,5-cyclooctadiene)nickel ([Ni(cod)2]) in 30mL of DMF solution, stir until completely dissolved, then add 0.184g of 2,2'-bipyridine 0.144ml of 1,5-cyclooctadiene (cod) was added to the mixture and stirred for about 30 minutes, then TBM and XTBB were added to the solution, and the reaction was stirred at 100°C for 1.5 hours using microwave method. After cooling, add concentrated hydrochloric acid until the medium solution turns transparent green, filter with CHCl 3 (5×15mL), THF (5×15mL) and H 2 O (5 x 15 mL) washes. The filtered sample was then vacuum dried at 120° C. for 24 hours.

[0032] According to the analysis and test method in Example 1, it is determined that the covalent organic polymer of the present invention has a methane adsorption capacity of 300 V / V at ambient temperature (25° C.) and 6.0 MPa.

Embodiment 3

[0034] First, bis-(1,5-cyclooctadiene)nickel ([Ni(cod)2], 1.125g, 4.09mmol) was dissolved in 65mL DMF solution, stirred until completely dissolved, and then 2,2'-cod Pyridine (0.640 g, 4.09 mmol) and 1,5-cyclooctadiene (cod, 0.50 mL, 3.96 mmol) were added to the mixture and stirred for approximately 30 minutes, then TBM and XTBB were added to the solution. Using the supergravity method, the rotating speed of the packed bed rotor was 2000r / min, and the reaction was stirred at 80°C for 1 hour. After cooling, add concentrated hydrochloric acid until the medium solution turns transparent green, filter with CHCl 3 (5×15mL), THF (5×15mL) and H 2 O (5 x 15 mL) washes. The filtered sample was then vacuum dried at 120° C. for 24 hours.

[0035] According to the analysis and test method in Example 1, it is determined that the covalent organic polymer of the present invention has a methane adsorption capacity of 300 V / V at ambient temperature (25° C.) and 6.0 MPa.

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Abstract

The invention discloses a preparation method of a covalent organic polymer for adsorbing and storing methane, and relates to the technical field of covalent organic polymer materials. The covalent organic polymer is prepared by taking tetrabromo-tetraphenylmethane and 1,3,5-tribromobenzene as monomers through a Yamamoto-type coupling reaction. The covalent organic polymer can be synthesized through different methods such as a solvothermal method, a microwave method and a high gravity method; the polymer prepared through the method has the great specific surface area and the rich hierarchical porous structure, the methane adsorption capacity of the polymer is far more than the America DOE standard, and the polymer can be widely applied to the industries of gas-fueled vehicles, natural gas separation, natural gas storage and transportation and the like.

Description

Technical field: [0001] The invention relates to the technical field of covalent organic polymer materials, in particular to a method for natural gas adsorption using tetrabromotetraphenylmethane and 1,3,5-tribromobenzene as reaction monomers and using Yamamoto-type coupling reaction Covalent organic polymer materials for storage. Background technique: [0002] Although people have invested a lot of financial and material resources in the development of energy-saving and high-efficiency technologies in recent decades, the depletion of traditional fossil energy sources such as oil and coal is still a challenge that human development has to face. At the same time, the excessive use of fossil fuels has caused a large amount of CO 2 , nitrogen sulfide, and dust particles are discharged into the air, causing climate problems such as global warming, acid rain pollution, and smog. Therefore, it is imperative to develop clean, efficient and recyclable energy sources. [0003] Nat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/30B01D53/02C08G61/02F17C11/00
CPCB01D53/02B01D2253/202B01J20/26B01J2220/445B01J2220/4812C08G61/02C08G2261/312C08G2261/412F17C11/007
Inventor 向中华郭佳宁谢呈鹏
Owner BEIJING UNIV OF CHEM TECH
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