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Preparation method and application of heterogeneous metal catalyst

A metal catalyst and heterogeneous technology, applied in the field of preparation of heterogeneous metal catalysts, can solve the problem of low reaction activity, achieve the effects of efficient and stable catalytic reaction, simple and effective recovery method, and reduced catalytic activity

Pending Publication Date: 2020-11-17
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this kind of catalyst should have very low activity in the catalytic reaction and hardly react in the water system.
Although some achievements have been made after people's exploration, so far, the catalysts with high catalytic activity, easy separation and reusability in catalytic reactions are still very limited.

Method used

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  • Preparation method and application of heterogeneous metal catalyst
  • Preparation method and application of heterogeneous metal catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Preparation of heterogeneous metal catalysts

[0014] Weigh 10mg RuCl successively 3 and 10mg polymethacrylic acid were dissolved in 2mL dimethyl sulfoxide solvent, then added to 20mL10wt% ethanolamine solution, and then added the solution of polymer ionic liquid PIL (10mg polymer ionic liquid was dissolved in 2mL dimethyl sulfoxide Middle), after mixing and ultrasonication, the produced solid was repeatedly washed and purified with ethanol, and dried to obtain a complex of immobilized metal compounds. After dispersing the above complex in 10 mL THF, add 1 g NaBH 4 , reacted at room temperature for 24h, then centrifuged, and the solid was repeatedly washed with ethanol and dried to obtain a heterogeneous catalyst loaded with Ru.

Embodiment 2

[0016] The heterogeneous catalyst of immobilized Ru prepared in embodiment 1 catalyzes the hydrogen transfer reaction of 1-tetralone

[0017] The heterogeneous catalyst (1mol% of 1-tetralone) that takes by weighing the immobilized Ru obtained in Example 1 joins in the centrifuge tube of 5mL, injects 0.5mL solvent water to it, ultrasonic makes catalyst evenly dispersed in in the solvent; then use a pipette gun to draw formic acid (1.65mmol, 62μL), triethylamine (1.35mmol, 187μL), and 1-tetralone (0.5mmol, 66μL) into centrifuge tubes, and place them in React in a water bath at 40°C for 12 hours. After the reaction was completed, the catalyst was recovered by centrifugation, extracted with ethyl acetate, and the organic phase obtained was washed with saturated sodium chloride solution, dried with anhydrous magnesium sulfate for 24 hours, filtered, rotary evaporated, and vacuum-dried at 30°C for 24 hours to obtain the target product , the yield was 89%.

Embodiment 3

[0019] The heterogeneous catalyst of immobilized Ru prepared in Example 1 catalyzes the hydrogen transfer reaction of 1-acetylnaphthone

[0020] Weigh the heterogeneous catalyst (1mol% of 1-acetonaphthone) of immobilized Ru obtained in Example 1 and join in a 5mL centrifuge tube, inject 0.5mL solvent water to it, and ultrasonically disperse the catalyst in the solvent. Then use a pipette gun to draw formic acid (1.65mmol, 62μL), triethylamine (1.35mmol, 187μL), and 1-acetonaphthone (0.5mmol, 76μL) into the centrifuge tube, and place it at 40°C React in a water bath for 12h. After the reaction was completed, the catalyst was recovered by centrifugation, extracted with ethyl acetate, and the organic phase obtained was washed with saturated sodium chloride solution, dried with anhydrous magnesium sulfate for 24 hours, filtered, rotary evaporated, and vacuum-dried at 30°C for 24 hours to obtain the target product , and the yield was 87%.

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Abstract

The invention discloses a preparation method of a heterogeneous metal catalyst, which comprises the following steps: preparing a metal-compound-immobilized composite from a carboxylic acid group-containing polymer, a metal compound and a polymer ionic liquid PIL in an ethanolamine solution by an in-situ ion complexing manner; dispersing the metal-compound-immobilized composite in a dry organic solvent; then adding NaBH4 for reduction to prepare the metal-immobilized heterogeneous catalyst. The metal-immobilized heterogeneous catalyst can stably exist, can be used for catalyzing a hydrogen transfer reaction of ketone compounds in a water system, and has efficient and stable catalytic activity. In addition, the recovery method of the metal-immobilized heterogeneous catalyst is simple and effective, and the metal-immobilized heterogeneous catalyst can be repeatedly recycled without significantly reducing the catalytic activity.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of a heterogeneous metal catalyst, and in particular relates to a preparation method and application of a heterogeneous metal catalyst. Background technique [0002] It is of great significance to develop stable and efficient metal catalysts. However, metal catalysts are not efficient in catalytic reactions, are easily lost and cannot be recycled. In recent years, in order to solve these problems, the concept of heterogeneous metal catalysts has been proposed and has been extensively researched and developed. However, this type of catalyst should have very low activity in the catalytic reaction and hardly react in the water system. Although some achievements have been made after people's exploration, so far, the catalysts with high catalytic activity, easy separation and reusability in catalytic reactions are still very limited. [0003] In order to overcome these difficulti...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J37/16C07C29/143C07C35/36C07C33/46
CPCB01J31/06B01J37/16C07C29/143B01J2523/821B01J2523/822C07C2602/10C07C35/36C07C33/46Y02P20/584
Inventor 李新娟王萌萌孙艳平贾献彬
Owner HENAN NORMAL UNIV
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