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Magnetic porous supported metallic chiral catalyst and application thereof

A chiral catalyst, supported technology, used in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc.

Inactive Publication Date: 2015-01-28
WENZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation and exploration of this kind of catalyst and its application in carbonyl asymmetric catalytic hydrogenation have not been reported at home and abroad.

Method used

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  • Magnetic porous supported metallic chiral catalyst and application thereof
  • Magnetic porous supported metallic chiral catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] a), 1.0mmol FeCl 3 ·6H 2 O, 1.5mmol C 6 h 5 o 7 Na 3 2H 2 O, 2.0 mmol of urea and 1.0 g of PAM were added to 10 mL of distilled water with stirring, and after it was completely dissolved in water, the solution was transferred to a hydrothermal reaction kettle, sealed, heated to 150°C, and reacted for 8 hours. The obtained black precipitate was separated by centrifugation, washed three times with distilled water and absolute ethanol respectively, and dried in a vacuum drying oven for later use to obtain ferric oxide nanospheres.

[0053]b) Disperse the self-made iron ferric oxide nanospheres (0.6 g) in 20 mL of HCl (0.1 M) aqueous solution, and ultrasonically disperse in an ice bath for 10 min. Then ferric oxide nano-microspheres were magnetically separated, washed with distilled water for 3 times, and then mixed with a mixed solvent of 80 mL of ethanol, 16 mL of distilled water and 0.16 mL of ammonia water. The resulting mixed solution was ultrasonicated in an ic...

Embodiment 2

[0058] a), 1.5mmol FeCl 3 ·6H 2 O, 2.0 mmol C 6 h 5 o 7 Na 3 2H 2 O, 3.0 mmol of urea and 1.25 g of PAM were added to 15 mL of distilled water with stirring, and after it was completely dissolved in water, the solution was transferred to a hydrothermal reaction kettle, sealed, heated to 170°C, and reacted for 12 hours. The obtained black precipitate was separated by centrifugation, washed several times with distilled water and absolute ethanol respectively, and dried in a vacuum drying oven for later use to obtain ferric oxide nanospheres.

[0059] b) Disperse the self-made iron ferric oxide nanospheres (0.7 g) in 25 mL of HCl (0.1 M) aqueous solution, and ultrasonically disperse in an ice bath for 15 min. Then ferric oxide nano-microspheres were magnetically separated, washed 3 times with distilled water, and then mixed with 100 mL of ethanol, 25 mL of distilled water and 0.25 mL of ammonia water. The resulting mixed solution was ultrasonicated for 15 min in an ice bat...

Embodiment 3

[0065] a), 2.0mmol FeCl 3 ·6H 2 O, 2.5mmol C 6 h 5 o 7 Na 3 2H 2 O, 4.0mmol urea and 1.5g PAM were added to 20mL of distilled water under stirring conditions, and after it was completely dissolved in water, the solution was transferred to a hydrothermal reaction kettle, sealed, heated to 180°C, and reacted for 16h. The obtained black precipitate was separated by centrifugation, washed several times with distilled water and absolute ethanol respectively, and dried in a vacuum drying oven for later use to obtain ferric oxide nanospheres.

[0066] b) Disperse the self-made iron ferric oxide nanospheres (0.8 g) in 30 mL of HCl (0.1 M) aqueous solution, and ultrasonically disperse in an ice bath for 20 min. Then ferric oxide nano-microspheres were magnetically separated, washed three times with distilled water, and then mixed with 120 mL of ethanol, 36 mL of distilled water and 0.36 mL of ammonia water. The resulting mixed solution was ultrasonicated for 20 min in an ice bat...

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Abstract

The invention discloses a magnetic porous supported metallic chiral catalyst and an application thereof. The support of the catalyst is an amino-modified magnetic porous microsphere, and a preparation method of the amino-modified magnetic porous microsphere comprises the following steps: heating iron chloride in an aqueous solution comprising sodium citrate, urea and polyacrylamide for carrying out a hydrothermal reaction to prepare a ferriferrous oxide nanosphere, preparing a magnetic porous microsphere through a sol-gel process by using the ferriferrous oxide nanosphere as a magnetic core and tetrahexyl orthosilicate as a silicon source and adding a template cetyltrimethylammonium bromide, and carrying out a silane coupling reaction of the magnetic porous microsphere and 3-aminopropyltriethoxysilane to prepare the amino-modified magnetic porous microsphere. The catalyst provided by the invention is magnetic, allows reaction products to be easily separated through applying a magnetic field, and can be recycled several times, so the catalyst loss is reduced. The catalyst has a high catalytic efficiency, allows the e.e. values of the products to be high, and still has a very good catalytic capability in the repeated use.

Description

(1) Technical field [0001] The invention relates to a magnetic porous loaded metal chiral catalyst and its application to asymmetric catalytic hydrogenation of carbonyl ketones. (2) Background technology [0002] The asymmetric catalytic hydrogenation of carbonyl ketones is often divided into heterogeneous and homogeneous catalytic hydrogenation. Because in the homogeneous asymmetric catalytic hydrogenation, the catalyst used in the homogeneous catalytic hydrogenation reaction is difficult to separate from the product, resulting in the loss of expensive catalyst and the contamination of toxic metals in the product, which makes many of them have excellent catalytic performance The homogeneous catalysts cannot be used in actual production. The heterogeneous asymmetric catalytic hydrogenation not only overcomes the problem of difficult separation, but also has many advantages compared with the homogeneous catalytic hydrogenation, for example, the active components of the catal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28C07C33/46C07C29/145
Inventor 邰玉蕾赵亚娟晁国库李晓燕官儒奇
Owner WENZHOU UNIV
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