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MOF@POP-n composite catalyst, preparation method and application thereof

A composite catalyst, mof-74-zn technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve secondary pollution and expensive precious metal catalysts , Catalysts are easy to poison and other problems, to achieve the effects of easy recycling, improved reusability, and improved catalytic activity

Active Publication Date: 2020-06-02
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems existing in the existing catalytic process, such as expensive noble metal catalysts, easy poisoning of catalysts, and easy to cause secondary pollution, the purpose of the present invention is to provide a MOF@POP-n composite catalyst and its preparation method and application. Prepare the POP precursor product, then prepare the MOF shell material, and then use the interaction between POP and MOF to load POP on the surface of MOF to form an efficient MOF@POP-n composite catalyst

Method used

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  • MOF@POP-n composite catalyst, preparation method and application thereof
  • MOF@POP-n composite catalyst, preparation method and application thereof
  • MOF@POP-n composite catalyst, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Example 1 Preparation of MOF shell material

[0029] Preparation of MOF-74-Co: Mix 0.144g 2,5-dihydroxyterephthalic acid and 0.713g Co(NO 3 ) 2 ·H 2 O was sonicated and dissolved in 60 mL of a 1 / 1 / 1 (v / v / v) N,N-dimethylformamide-ethanol-water mixture. Then the transparent solution was transferred to a Teflon-lined stainless steel autoclave, and the autoclave was placed in an oven at 100 °C for 24 hours, filtered and centrifuged to obtain MOF-74-Co, and it was subjected to FT-IR test ( figure 1 ), which at 3850cm -1 There are characteristic peaks of hydroxyl groups, confirming the successful preparation.

[0030] Preparation of MOF-74-Zn: 2,5-dihydroxyterephthalic acid (0.5 g, 2.6 mmol) and zinc nitrate (2.0 g, 7.6 mmol) were dissolved in 100 ml DMF under stirring. After the reagents were dissolved, 5 ml of deionized water was added. The solution was transferred to a Teflon-lined autoclave, tightly capped, and placed in an oven at 120 °C for 24 h. After decanting ...

Embodiment 2

[0031] Example 2 MOF@POP-n composite catalyst

[0032] 1. Preparation of MOF@POP-n composite catalyst

[0033] Put 6.59g of p-dibromobenzyl into 20ml of toluene to obtain solution A, dissolve 4.94g of 1-vinylimidazole in 20ml of toluene to obtain solution B, mix solution A and solution B, and stir at room temperature for 30min to make the stirring uniform, and The above solution was heated at 120°C under N 2 Heated under atmosphere for 24h, cooled to room temperature, separated the product by filtration, and washed with 50ml of toluene and 50ml of ether until the filtrate was colorless. After that, the precursor was obtained; 1.06g of the precursor, 487mg of divinylbenzene and 400mg of MOF-74-Co were added to 100ml of N,N-dimethylformamide solution containing 30mg of azobisisobutyronitrile and sonicated for 30min , heated at 150°C under a nitrogen atmosphere for 24h, cooled to room temperature, filtered and washed several times with N,N-dimethylformamide, ethanol, ethyl acet...

Embodiment 3

[0038] Example 3 MOF@POP-n composite catalyst

[0039] 1. Preparation of MOF@POP-n composite catalyst

[0040] Put 6.59g of o-dibromobenzyl in 20ml of toluene to obtain solution A, dissolve 4.94g of 1-vinylimidazole in 20ml of toluene to obtain solution B, mix solution A and solution B, and stir at room temperature for 30min to make the stirring uniform. The above solution was heated at 120°C under N 2Heated under atmosphere for 24h, cooled to room temperature, separated the product by filtration, and washed with 50ml of toluene and 50ml of ether until the filtrate was colorless. Afterwards, the precursor was obtained; 1.06g of the precursor, 487mg of divinylbenzene and 400mg of MOF-74-Zn were added to 100ml of N,N-dimethylformamide solution containing 30mg of azobisisobutyronitrile and sonicated for 30min, Heated at 150°C under nitrogen atmosphere for 24h, cooled to room temperature, filtered and washed several times with N,N-dimethylformamide, ethanol, ethyl acetate, aceto...

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Abstract

The invention relates to an MOF@POP-n composite catalyst, a preparation method and application thereof, and belongs to the technical field of chemical catalytic materials. The preparation method comprises the following steps of: dissolving cyclite in toluene to obtain a solution A, dissolving 1-vinylimidazole in toluene to obtain a solution B, mixing the solution A and the solution B uniformly, performing heating for 12-24h at 100-120DEG C in an N2 atmosphere, and conducting cooling, filtering, and washing to obtain a precursor; and adding the precursor, divinyl benzene and MOF into an N, N-dimethylformamide solution containing azodiisobutyronitrile, carrying out ultrasonic treatment for 15-45min, performing heating for 24-48h in a nitrogen atmosphere at 120-160DEG C, conducting cooling toroom temperature, and performing separation to obtain the target product. The MOF@POP-n composite catalyst catalyzes epoxypropane and carbon dioxide to generate cyclic carbonate, the highest yield can reach 98%, and the conversion rate can still reach 90% or above after the MOF@POP-n composite catalyst is repeatedly used six times.

Description

technical field [0001] The invention relates to a simple and efficient MOF@POP-n composite catalyst and its preparation method and application, belonging to the technical field of chemical catalytic materials. Background technique [0002] As an important organic solvent, cyclic carbonates are widely used in the production of carbonate polymers, aprotic polar solvents, pharmaceutical and fine chemical intermediates, and petroleum additives. They are important chemical raw materials. At present, the preparation methods of cyclic carbonates are mainly as follows: phosgene method, direct oxidative carbonylation of olefins, CO 2 Cycloaddition epoxides. The highly toxic phosgene used in the phosgene method has been basically eliminated; the direct oxidative carbonylation of olefins can be used to prepare cyclic carbonates from olefins in one step, but it requires the addition of noble metal oxidation catalysts, which increases the cost. [0003] The structure and topology of me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/06B01J35/10C07D317/36
CPCB01J31/1691B01J31/06B01J31/2239C07D317/36B01J2531/26B01J2531/845B01J35/617B01J35/64
Inventor 韩正波房挺
Owner LIAONING UNIVERSITY
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