ZIF@TU-POP composite catalyst, and preparation method and application thereof

A composite catalyst and reaction technology, applied in the direction of organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of expensive metal catalysts, secondary pollution, and easy poisoning of catalysts and other issues, to achieve the effect of improving reusability, easy recycling, and improving 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 characteristics of expensive metal catalysts, easy poisoning of catalysts, and easy to cause secondary pollution in the existing catalytic process, the purpose of the present invention is to provide a ZIF@TU-POP composite catalyst and its preparation method and application. Prepare the POP precursor product, then prepare the ZIF shell material, and then use the interaction between POP and ZIF to load POP on the surface of ZIF to form an efficient ZIF@TU-POP composite catalyst

Method used

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  • ZIF@TU-POP composite catalyst, and preparation method and application thereof
  • ZIF@TU-POP composite catalyst, and preparation method and application thereof
  • ZIF@TU-POP composite catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 Preparation of ZIF shell material

[0028] Preparation of ZIF-8: Zn(NO 3 ) 2 ·6H 2 O 1.68g was dissolved in 80ml of methanol to obtain solution A, 3.7g of 2-methylimidazole was dissolved in 80ml of methanol to obtain solution B, solution A and solution B were mixed and stirred for 24h, filtered and washed with methanol, and vacuum-dried at 60°C for 12h Get ZIF-8.

[0029] Preparation of ZIF-67: Co(NO 3 ) 2 ·6H 2 O 1.69g was dissolved in 80ml of methanol to obtain solution A, 3.7g of 2-methylimidazole was dissolved in 80ml of methanol to obtain solution B, solution A and solution B were mixed and stirred for 24 hours, filtered and vacuum-dried to obtain ZIF-67.

Embodiment 2

[0030] Example 2 ZIF-8@TU-POP composite catalyst

[0031] 1. Synthetic route of ZIF-8@TU-POP composite catalyst

[0032]

[0033] 2. Preparation of ZIF-8@TU-POP composite catalyst

[0034] Add 3 g of urea, 2 ml of 39% sodium bisulfite solution and 2 ml of acetic acid into 50 ml of deionized water containing 4 g of p-phenylenediamine, and stir the mixture at 90° C. for 24 h, then filter and wash with a large amount of hot water, and then vacuum Drying gives the product 1,3-bis(4-aminophenyl)urea. Add 1g of 1,3-bis(4-aminophenyl)urea, 1.5g of cyanuric chloride, and 500mg of ZIF-8 into 10ml of dry dimethyl sulfoxide, keep the reaction temperature at 15°C, and add N , N-diisopropylethylamine 2ml, stirred for 24 hours, after the reaction was completed, the crude product was added to ice to form a solid, which was then filtered and washed with dichloromethane, tetrahydrofuran, and ethyl acetate to obtain ZIF-8@TU - POP composite catalyst. And did FT-IR on the catalyst ( figu...

Embodiment 3

[0039] Example 3 ZIF-67@TU-POP composite catalyst

[0040] 1. Synthetic route of ZIF-67@TU-POP composite catalyst

[0041]

[0042]2. Preparation of ZIF-67@TU-POP composite catalyst

[0043] Add 3 g of urea, 2 ml of 39% sodium bisulfite solution and 2 ml of acetic acid into 50 ml of deionized water containing 4 g of p-phenylenediamine, and stir the mixture at 90° C. for 24 h, then filter and wash with a large amount of hot water, and then vacuum Drying gives the product 1,3-bis(4-aminophenyl)urea. Add 1g of 1,3-bis(4-aminophenyl)urea, 1.4g of cyanuric chloride, and 400mg of ZIF-67 into 10ml of dry dimethyl sulfoxide, keep the reaction temperature at 15°C, and add N , N-diisopropylethylamine 2ml, stirred for 24 hours, after the reaction was completed, the crude product was added to ice to form a solid, and then it was filtered and washed with dichloromethane, tetrahydrofuran, and ethyl acetate to obtain ZIF-67@TU - POP composite catalyst.

[0044] 3. Application of ZIF-6...

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Abstract

The invention belongs to the technical field of chemical catalytic materials, and particularly provides a ZIF@TU-POP composite catalyst, and a preparation method and an application thereof. The preparation method comprises the following steps: adding urea, a sodium sulfite solution and acetic acid into deionized water containing phenylenediamine, stirring for 24-36 h at 90-120 DEG C, filtering, washing, and carrying out vacuum drying to obtain 1,3-bis(4-aminophenyl)urea; adding 1,3-bis(4-aminophenyl)urea, cyanuric chloride and a ZIF material into dry dimethyl sulfoxide, reacting at 15-25 DEG C, adding N,N-diisopropylethylamine, stirring, adding a crude product into ice to form a solid after the reaction is finished, filtering, and sequentially washing with dichloromethane, tetrahydrofuranand ethyl acetate to obtain the target product. The ZIF@TU-POP composite catalyst catalyzes epoxypropane and carbon dioxide to generate cyclic carbonate, the highest yield can reach 99%, and the conversion rate can still reach 90% or above after the catalyst is repeatedly used for four times.

Description

technical field [0001] The invention relates to a ZIF@TU-POP composite catalyst and its preparation method and application, belonging to the technical field of chemical catalytic materials. Background technique [0002] For a long time, CO from fossil fuel combustion 2 Emissions are increasing and are widely recognized as a major cause of global climate change and related environmental problems. Post Combustion Carbon Capture and Separation of CO from Flue Gas 2 is to reduce industrial CO 2 Emissions and access to atmospheric CO 2 Feasible method of concentration control. 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. Therefore the CO 2 Conversion to cyclic carbonates will have better economic benefits. At present, the preparation methods of cyclic carbonates are mainly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/06B01J35/10C07D317/36
CPCB01J31/1691B01J31/06B01J31/1815B01J35/1052C07D317/36B01J2531/26B01J2531/845
Inventor 韩正波房挺
Owner LIAONING UNIVERSITY
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