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Preparation method and application of silica microsphere immobilized nanometer metal compound catalyst

A technology of silica and nano-metals, applied in the direction of organic compound/hydride/coordination complex catalysts, carbon-based compound preparation, organic compound preparation, etc., can solve the problem of unstable deactivation of metalloporphyrin catalysts, The problems such as the inability to recycle morphine can be solved, and the effect of improving activity and selectivity, high stability and good catalytic performance can be achieved

Inactive Publication Date: 2017-02-08
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in a homogeneous catalytic system, metalloporphyrins cannot be recovered and are easy to self-polymerize or degrade. Although loading metalloporphyrins on a carrier with a large specific area can prevent problems such as dimerization of metalloporphyrins However, there are still problems such as instability and rapid deactivation of supported metal porphyrin catalysts.

Method used

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  • Preparation method and application of silica microsphere immobilized nanometer metal compound catalyst
  • Preparation method and application of silica microsphere immobilized nanometer metal compound catalyst
  • Preparation method and application of silica microsphere immobilized nanometer metal compound catalyst

Examples

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Effect test

Embodiment 1

[0020] This example prepares carbonized amino-modified silica microspheres loaded with manganese porphyrin (SiO 2 -NH 2 -MnTPCPP / AC) and carbonized amino-modified silica microspheres loaded iron porphyrin (SiO 2 -NH 2 -FeTPCPP / A), its preparation method is as follows:

[0021] (1) Synthesis of monocarboxyporphyrin, in a 500mL three-necked flask, add 250mL propionic acid, 5.565g benzaldehyde and 2.625g 4-carboxybenzaldehyde, heat to reflux, slowly drop 4.69g pyrrole into , control the flow rate, finish adding in 20 minutes, and continue to react for 30 minutes under reflux conditions. After the reaction solution is cooled, put it in the refrigerator overnight, filter it with suction, and separate it with a silica gel column to synthesize monocarboxyporphyrin;

[0022] (2) Synthesis of monocarboxymanganese porphyrin and monocarboxyiron porphyrin, in a 250mL three-necked flask, add 100mL dimethylformamide, 1.0g of monocarboxyporphyrin obtained in step (1), heat to reflux, divi...

Embodiment 2

[0034] This embodiment includes the following steps:

[0035] (1) Synthesis of monocarboxyporphyrin, disperse benzaldehyde and 4-carboxybenzaldehyde with a mass ratio of 1:3 in propionic acid, the mass ratio of propionic acid to benzaldehyde is 1:30, and heat to reflux , slowly drop in pyrrole equivalent to benzaldehyde, control the flow rate, finish adding in 20 minutes, and continue to react for 30 minutes under reflux conditions. Synthesis of monocarboxyporphyrin;

[0036] (2) Synthesis of monocarboxyl porphyrin, disperse the monocarboxy porphyrin obtained in step (1) in dimethylformamide, the mass ratio of monocarboxy porphyrin to dimethyl formamide is 1:150, heat to reflux , within 1h, add MnCl with a mass ratio of 1:2 to monocarboxyporphyrin in batches 2 4H 2 O and FeCl 2 4H 2 O. After the addition, point the plate to monitor the reaction process. When the raw material point disappears, stop the reaction. After the reaction solution is cooled, add distilled water wi...

Embodiment 3

[0042] This embodiment includes the following steps:

[0043] (1) Synthesis of monocarboxyporphyrin, disperse benzaldehyde and 4-carboxybenzaldehyde in propionic acid with a mass ratio of 1:4, the mass ratio of propionic acid to benzaldehyde is 1:60, and heat to reflux , slowly drop pyrrole equivalent to benzaldehyde, control the flow rate, finish adding in 30 minutes, and continue to react for 60 minutes under reflux conditions. Synthesis of monocarboxyporphyrin;

[0044] (2) Synthesis of monocarboxyl porphyrin, disperse the monocarboxyl porphyrin obtained in step (1) in dimethylformamide, the mass ratio of monocarboxyl porphyrin to dimethylformamide is 1:200, heat to reflux , within 1h, add MnCl with a mass ratio of 1:5 to monocarboxyporphyrin in batches 2 4H 2 O and FeCl 2 4H 2 O, after the addition, point the plate to monitor the reaction process. When the raw material point disappears, stop the reaction. After the reaction solution is cooled, add distilled water with...

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Abstract

The invention relates to a silica-microsphere-immobilized nanometer metal compound catalyst as well as a preparation method and an application thereof. The preparation method comprises the following steps: (1) the synthesis of monocarboxyl porphyrin; (2) the synthesis of monocarboxyl metal porphyrin; (3) the synthesis of amino-modified silica microspheres; (4) the synthesis of amino-modified silica microsphere-loaded metal porphyrin; (5) the synthesis of carbonized amino-modified silica microsphere-loaded metal porphyrin. The invention further provides the application of the nanometer metal compound catalyst in an ethylbenzene oxidation reaction. The silica-microsphere-immobilized nanometer metal compound catalyst has good catalytic performance and high stability and can be recycled and used repeatedly. The microporous surface of the organosilicone microspheres has an alternate hydrophilic and hydrophobic property, a microenvironment beneficial to the reaction can be provided, and the activity and selectivity of the catalyst are improved.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a silica microsphere-immobilized nanometer metal compound catalyst and a preparation method and application thereof. Background technique [0002] Due to the good catalytic effect of metalloporphyrins on the activation of C-H bonds, the research on immobilized metalloporphyrin catalysts has been in the ascendant in the past few decades. However, in a homogeneous catalytic system, metalloporphyrins cannot be recovered and are easy to self-polymerize or degrade. Although loading metalloporphyrins on a carrier with a large specific area can prevent problems such as dimerization of metalloporphyrins However, the supported metal porphyrin catalysts still have problems such as instability and rapid deactivation. [0003] In order to solve the deactivation problem of metalloporphyrin catalysts, highly dispersed multivalent metal compound catalysts were obtained by calcining immobil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C27/12C07C49/78C07C45/36C07C33/22C07C29/50
Inventor 刘志刚吉琳韬刘佳汪秋安
Owner HUNAN UNIV