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Kaolin-loaded nano-iron catalyst and application thereof in catalyzing cross dehydrogenation coupling reaction

A technology of cross dehydrogenation coupling and kaolin, which is applied in the direction of catalytic reaction, heterogeneous catalyst chemical elements, physical/chemical process catalysts, etc., can solve the problems of difficult separation, recycling and reuse of catalysts, environmental pollution, high catalytic cost, etc., to achieve The effect of good catalytic effect

Active Publication Date: 2021-03-19
INNER MONGOLIA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, in the iron-catalyzed C(sp3)-H bond activation functionalization reaction, the catalytic system is mostly homogeneous catalysis, such as Fe(acac)3, FeCl2, porphyrin, etc., the catalyst is difficult to separate, recycle and reuse, which leads to high catalytic cost and easy to cause environmental pollution

Method used

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  • Kaolin-loaded nano-iron catalyst and application thereof in catalyzing cross dehydrogenation coupling reaction
  • Kaolin-loaded nano-iron catalyst and application thereof in catalyzing cross dehydrogenation coupling reaction
  • Kaolin-loaded nano-iron catalyst and application thereof in catalyzing cross dehydrogenation coupling reaction

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preparation example Construction

[0027] In the present invention, the preparation method of the silane-modified kaolin preferably comprises the following steps:

[0028] The raw kaolin clay, n-heptane and silane coupling agent are mixed, stirred, left standing, solid-liquid separation, solid washed and dried in sequence to obtain silane modified kaolin.

[0029] In the present invention, the silane coupling agent is preferably 3-aminopropyltriethoxysilane and / or phenyltrimethoxysilane; when the silane coupling agent is 3-aminopropyltriethoxy During silane, the gained silane-modified kaolin is aminosilane-modified kaolin; when the silane coupling agent is phenyltrimethoxysilane, the silane-modified kaolin is phenylsilane-modified kaolin; when the silane coupling agent When the coupling agent is 3-aminopropyltriethoxysilane and phenyltrimethoxysilane, the obtained silane-modified kaolin is aminophenylsilane-modified kaolin.

[0030] In the present invention, the ratio of the raw kaolin, n-heptane and silane co...

Embodiment 1

[0057] Weigh 1g of kaolin into a beaker, add 30mL of n-heptane, stir evenly, add 1.2mmol of 3-aminopropyltriethoxysilane and 1.2mmol of phenyltrimethoxysilane, and stir at room temperature for 6h. After stirring, let stand for 12 hours, then wash with n-heptane, and dry for 8 hours to obtain the amino- and phenyl-modified kaolin carrier, denoted as NH 2 & Ph @kaolin.

[0058] The resulting NH 2 &Ph@kaolin at a concentration of 0.01mol / L FeCl 3 Immerse in the solution for 10h to remove the NH after immersion 2 & Ph @kaolin, utilizing NaBH 4 Reducted at room temperature for 10 minutes to obtain a kaolin-supported nano-iron catalyst with an iron loading of 3 wt%, denoted as 3% Fe / NH 2 & Ph @kaolin.

[0059] The resulting 3% Fe / NH 2 &Ph@kaolin's SEM element distribution map is as follows figure 1 shown. From figure 1 It can be seen that the nano-iron is uniformly distributed in the NH 2 &Ph@kaolin in the carrier.

[0060] The resulting 3% Fe / NH 2 TEM image of &Ph@kaoli...

Embodiment 2

[0062] Weigh 1g of kaolin into a beaker, add 30mL of n-heptane, stir evenly, add 1.2mmol of 3-aminopropyltriethoxysilane, and stir at room temperature for 6h. After stirring, let stand for 12 hours, then wash with n-heptane, and dry for 8 hours to obtain a kaolin carrier modified with amino groups, which is denoted as NH 2 @kaolin.

[0063] The resulting NH 2 @kaolin FeCl at a concentration of 0.01mol / L 3 Immerse in the solution for 10h, take out the impregnated NH 2 @kaolin, using NaBH 4 Reducted at room temperature for 10 minutes to obtain a kaolin-supported nano-iron catalyst with an iron loading of 3 wt%, denoted as 3% Fe / NH 2 @kaolin.

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Abstract

The invention provides a kaolin-loaded nano-iron catalyst and the application thereof in catalyzing cross dehydrogenation coupling reaction, and belongs to the technical field of catalysts. Accordingto the kaolin-loaded nano-iron catalyst provided in the invention, the kaolin-loaded nano-iron catalyst comprises a kaolin carrier and nano-iron loaded in the kaolin carrier. When the kaolin-loaded nano-iron catalyst provided by the invention is used for catalyzing cross dehydrogenation coupling reaction of cyclic ether C(sp3) H bonds and aromatic formic acid, activation and direct esterificationof the cyclic ether C(sp3) H bonds can be catalyzed, and a good catalytic effect is achieved. Meanwhile, the kaolin-loaded nano-iron catalyst provided by the invention is a heterogeneous catalyst, hasthe advantages of low cost, no toxicity and environmental sustainability, can be recycled for multiple times, and is very beneficial to application in modern industrial production.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a kaolin-supported nano-iron catalyst and its application in catalytic cross-dehydrogenation coupling reactions. Background technique [0002] Transition metal-catalyzed direct functionalization of C-H bonds to construct C-X (X=C, O, N, S, etc.) bond reactions has the advantages of path economy, atom economy, and environmental sustainability, and has become an important and effective means of organic synthesis. hot research topics in recent years. In the past few years, transition metal-catalyzed C(sp)-H and C(sp 2 )-H bond activation to construct C-C bond reaction has been widely studied by scientists and great progress has been made. However, with C(sp 2 )-H bond activation compared to transition metal-catalyzed C(sp 3 )-H bond activated functionalization reaction is quite challenging, which is due to the fact that C(sp 3 )-H bond activation requires higher bond energy, ...

Claims

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Application Information

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IPC IPC(8): B01J23/745B01J31/02B82Y30/00C07D319/12
CPCB01J23/745B01J31/0274B01J31/0275B82Y30/00C07D319/12B01J2523/842B01J2523/41B01J2523/31B01J2231/4288
Inventor 特格希阿古拉包永胜贾美林乌仁夫
Owner INNER MONGOLIA NORMAL UNIVERSITY
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