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Preparation method and application of nitrogen-containing super-crosslinked polymer derived Co@CN catalyst

A polymer and hypercrosslinking technology, applied in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve unfavorable industrial applications, high cost of catalyst preparation and use, and weak electron transfer promotion effect. and other problems, to achieve the effect of facilitating large-scale production and application, improving electron transfer performance, and reducing preparation and use costs

Pending Publication Date: 2021-04-06
JINGCHU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the catalysts for the selective hydrogenation of quinolines to prepare 1, 2, 3, 4-tetrahydroquinolines that have been developed and reported mainly use noble metals, such as Au, Ru, Pd, etc. (Adv Synth Catal, 2015 , 357,753; Nano Research 2016, 9, 2632; CN107824209A), the cost of catalyst preparation and use is high, which is not conducive to industrial application
The Chinese invention patent with the publication number CN109759134A discloses a Cu@C catalyst derived from MOFs. Although the use of noble metals is avoided, the pure carbon matrix does not have a strong effect on promoting the electron transfer in the catalytic process, so the catalytic reaction requires a higher temperature. get a better conversion rate

Method used

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  • Preparation method and application of nitrogen-containing super-crosslinked polymer derived Co@CN catalyst
  • Preparation method and application of nitrogen-containing super-crosslinked polymer derived Co@CN catalyst
  • Preparation method and application of nitrogen-containing super-crosslinked polymer derived Co@CN catalyst

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Experimental program
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Effect test

Embodiment 1

[0026] A method for preparing a Co@CN catalyst derived from a nitrogen-containing hypercrosslinked polymer, comprising the steps of:

[0027] S1. Dissolve 10 mmol benzotriazole, 30 mmol benzene, 6.5 g dimethoxymethane, and 9.5 g anhydrous ferric chloride in 100 mL 1,2-dichloroethane, heat to 80 °C, and It fully reacted for 24 h. The product was Soxhlet-extracted with methanol for 24 hours to remove impurities, and then spin-dried with a rotary evaporator to obtain a nitrogen-containing hypercrosslinked polymer.

[0028] S2. Disperse 1 g of the above polymer and 1.48 g of cobalt nitrate hexahydrate into 50 mL of deionized water, add 0.5 g of urea and transfer to a polytetrafluoroethylene-lined stainless steel reactor, and fix the sealed autoclave in a uniform The rotating shaft of the phase reactor was turned over at a speed of 60 rpm, the temperature was set at 170 °C, and the treatment time was 9 h. After cooling, the solid was collected by filtration, washed with deionized...

Embodiment 2

[0035] S1. Dissolve 10 mmol benzotriazole, 30 mmol benzene, 6.5 g dimethoxymethane, and 9.5 g anhydrous ferric chloride in 100 mL 1,2-dichloroethane, heat to 80 °C, and It fully reacted for 24 h. The product was Soxhlet-extracted with methanol for 24 hours to remove impurities, and then spin-dried with a rotary evaporator to obtain a nitrogen-containing hypercrosslinked polymer.

[0036] S2. Disperse 1 g of the above polymer and 0.80 g of cobalt acetate into 50 mL of deionized water, add 0.5 g of urea and transfer to a polytetrafluoroethylene-lined stainless steel reactor, and fix the sealed autoclave in a homogeneous reaction Turn over at a speed of 60 rpm on the rotating shaft of the machine, set the temperature at 170 °C, and process for 9 h. After cooling, the solid was collected by filtration, washed with deionized water until neutral, and dried overnight at 80 °C to obtain the precursor for purification.

[0037] S3. Spread 500 mg of the precursor on the bottom of the ...

Embodiment 3

[0040] A method for preparing a Co@CN catalyst derived from a nitrogen-containing hypercrosslinked polymer, comprising the steps of:

[0041] S1. Dissolve 10 mmol of benzimidazole, 30 mmol of benzene, 6.5 g of dimethoxymethane, and 9.5 g of anhydrous ferric chloride in 100 mL of 1,2-dichloroethane, and heat to 80 °C to fully React for 24 h. The product was Soxhlet-extracted with methanol for 24 h to remove impurities, and then spin-dried with a rotary evaporator to obtain a nitrogen-containing hypercrosslinked polymer.

[0042] S2. Disperse 1 g of the above polymer and 1.35 g of cobalt nitrate hexahydrate into 50 mL of deionized water, add 0.5 g of urea and transfer to a polytetrafluoroethylene-lined stainless steel reactor, and fix the sealed autoclave in a uniform The rotating shaft of the phase reactor was turned over at a speed of 60 rpm, the temperature was set at 170 °C, and the treatment time was 9 h. After cooling, the solid was collected by filtration, washed with d...

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Abstract

The invention discloses a preparation method and application of a nitrogen-containing super-crosslinked polymer derived Co@CN catalyst. The preparation method comprises the following steps: dissolving a benzo nitrogen-containing heterocyclic compound, benzene, dimethoxymethane and anhydrous ferric trichloride in an organic solvent, heating to fully react, and purifying and drying the product to obtain the nitrogen-containing super-crosslinked polymer; then, dispersing the polymer and cobalt salt into deionized water, adding urea, transferring into a reaction kettle, carrying out heat treatment under an overturning condition, cooling, separating, washing, drying and purifying to obtain a precursor; and finally, pyrolyzing the precursor in a nitrogen atmosphere to prepare the nitrogen-containing super-crosslinked polymer derived Co@CN catalyst with high catalytic activity, and applying the Co@CN catalyst to a reaction for catalyzing selective hydrogenation of quinoline compounds to prepare tetrahydroquinoline compounds. According to the method, the yield of the tetrahydroquinoline compound prepared from the quinoline compound is increased, and the reaction temperature is reduced.

Description

technical field [0001] The invention belongs to the technical field of quinoline selective hydrogenation catalyst synthesis, and relates to a preparation method and application of a Co@CN catalyst derived from a nitrogen-containing hypercrosslinked polymer. Background technique [0002] 1, 2, 3, 4-Tetrahydroquinoline compounds are the active components of many natural alkaloids, and are an important class of nitrogen-containing heterocyclic compounds. They have many important biological functions such as antioxidant, antibacterial, and antitumor activity, can be used to inhibit glutamic acid toxicity and lipid peroxidation, prevent and treat diseases such as tumors, thrombosis, and arrhythmia; it can also be used as raw materials for the synthesis of chiral drugs such as natural alkaloids, and the research on its synthesis method has been receiving much attention focus on. There are many synthetic methods of tetrahydroquinoline, such as aza-Michael addition reaction, amino ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10B01J37/08C07D215/20
CPCB01J27/24B01J37/082C07D215/20B01J35/60Y02P20/584
Inventor 张华新张丽丽王洪林杨红梅李立威
Owner JINGCHU UNIV OF TECH
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