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A mof@pop-n composite catalyst and its preparation method and application

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 the problem of easy poisoning of catalysts and high price of noble metal catalysts , secondary pollution and other issues, to achieve the effect of improved catalytic activity, improved reusability, and easy recycling

Active Publication Date: 2022-07-19
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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  • A mof@pop-n composite catalyst and its preparation method and application
  • A mof@pop-n composite catalyst and its preparation method and application
  • A mof@pop-n composite catalyst and its preparation method and application

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: 0.144g 2,5-dihydroxyterephthalic acid and 0.713g Co(NO 3 ) 2 ·H 2 O Sonication Dissolve in 60 mL of a mixture of 1 / 1 / 1 (v / v / v) N,N-dimethylformamide-ethanol-water. Then the clear solution was transferred to a stainless steel autoclave lined with Teflon, and the autoclave was placed in an oven at 100 °C for 24 hours, and the MOF-74-Co was obtained by filtration and centrifugation, and it was tested by FT-IR ( figure 1 ), which is at 3850cm -1 There are characteristic peaks of hydroxyl group, which confirms 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 with stirring. After the reagents were dissolved, 5 ml of deionized water was added. The solution was transferred to an autoclave lined with Teflon, capped tightly, and placed in an oven at 120°C for 24h. After ...

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. The above solution is at 120 ° C, N 2 Heating under atmosphere for 24 h, cooled to room temperature, and the product was isolated by filtration, and washed with 50 ml of toluene and 50 ml of diethyl ether until the filtrate was colorless. Then 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 ultrasonicated for 30min , heated at 150°C for 24h under nitrogen atmosphere, 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-benzyl bromide 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, Put the above solution at 120 °C N 2Heating under atmosphere for 24 h, cooled to room temperature, and the product was isolated by filtration, and washed with 50 ml of toluene and 50 ml of diethyl ether until the filtrate was colorless. Then, 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 ultrasonicated 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 aceta...

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Abstract

The invention relates to a MOF@POP-n composite catalyst, a preparation method and application thereof, and belongs to the technical field of chemical catalytic materials. The preparation method includes the following steps: dissolving benzyl dibromide in toluene to obtain solution A, dissolving 1-vinylimidazole in toluene to obtain solution B, uniformly mixing solution A and solution B, at 100-120° C., under N2 atmosphere Under heating for 12-24h, after cooling, filtering, washing to obtain the precursor; adding the precursor, divinylbenzene and MOF to the N,N-dimethylformamide solution containing azobisisobutyronitrile, ultrasonicating for 15 ‑45min, heated under nitrogen atmosphere at 120‑160℃ for 24‑48h, cooled to room temperature and separated to obtain the target product. The MOF@POP-n composite catalyst catalyzes propylene oxide and carbon dioxide to generate cyclic carbonate with a yield of up to 98%, and the conversion rate can still reach more than 90% after 6 times of reuse.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/06B01J35/10C07D317/36
CPCB01J31/1691B01J31/06B01J31/2239B01J35/1023B01J35/1052C07D317/36B01J2531/26B01J2531/845
Inventor 韩正波房挺
Owner LIAONING UNIVERSITY
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