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Immobilized metal organic catalyst for disproportionation reaction, and preparation method thereof

A metal-organic, disproportionation reaction technology, applied in the preparation of organic carbonates, organic compounds/hydrides/coordination complex catalysts, physical/chemical process catalysts, etc. Achieve the effect of improving acidity and activity, improving separation, and large specific surface area

Active Publication Date: 2020-08-28
湖北三宁碳磷基新材料产业技术研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a solid-supported organometallic catalyst and a preparation method thereof, which can solve the problems of difficult separation, easy loss, and difficult utilization of other catalysts, and has the characteristics of regeneration and reuse

Method used

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  • Immobilized metal organic catalyst for disproportionation reaction, and preparation method thereof
  • Immobilized metal organic catalyst for disproportionation reaction, and preparation method thereof
  • Immobilized metal organic catalyst for disproportionation reaction, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add HKUST-1 to Bu 2 In SnO solution (Bu 2 The mass ratio of SnO to HKUST-1 is 3:7), adding anhydrous toluene, heating to reflux at 110°C for 6h, filtering, washing, and vacuum drying overnight to obtain the solid-supported organometallic catalyst 1.

[0023] Methylphenyl carbonate is subjected to decompression disproportionation reaction under the above-mentioned catalyst 1. The reaction process conditions are: under nitrogen condition, 0.5mol methyl phenyl carbonate is added in a 150ml three-necked flask, and the catalyst is added. The amount of catalyst It is 2 wt% of the mass of methyl phenyl carbonate, and reacted for 5 hours at a pressure of 228mmHg and a reaction temperature of 170°C. Diphenyl carbonate was obtained, and the results are shown in Table 1.

Embodiment 2

[0025] Add graphene to Bu 2 In SnO solution (Bu 2 The mass ratio of SnO to graphene is 3:7), adding anhydrous toluene, heating to reflux at 110°C for 6h, filtering, washing, and vacuum drying overnight to obtain the solid-supported organometallic catalyst 2.

[0026] The disproportionation reaction method and conditions are the same as in Example 1, and the results are shown in Table 1.

Embodiment 3

[0028] Add silicone to Bu 2 In SnO solution (Bu 2 The mass ratio of SnO to organic silica gel is 3:7), adding anhydrous toluene, heating to reflux at 110°C for 6h, filtering, washing, and vacuum drying overnight to obtain the solid-supported organometallic catalyst 3.

[0029] The disproportionation reaction method and conditions are the same as in Example 1, and the results are shown in Table 1.

[0030] Table 1

[0031]

[0032] It can be seen from Table 1 that the same organometallic catalyst is immobilized on different supports, and the catalytic activity of the catalyst is different, mainly because the content of OH on different supports is different. The more content on the carrier, the higher the catalytic activity of the catalyst. From the data in the table, using HKUST-1 as the catalyst carrier has a good catalytic effect.

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PUM

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Abstract

The invention discloses an immobilized metal organic catalyst for a disproportionation reaction, and a preparation method thereof. The method comprises the following steps: adding a carrier into an organic metal solution, adding an organic solvent, carrying out heating reflux for 5-12 h, filtering, washing, and carrying out vacuum drying overnight to obtain the immobilized metal organic catalyst.The catalyst can be used in an experiment for preparing diphenyl carbonate through the disproportionation reaction of methyl phenyl carbonate, and is obtained by immobilizing an organic catalyst on asolid carrier. The method further solves the problem that a homogeneous catalyst is difficult to separate and utilize, the catalyst has very high catalytic activity on the disproportionation reactionof methyl phenyl carbonate, and the product selectivity can be greater than 99%.

Description

technical field [0001] The invention belongs to the technical field of surface organometallic chemistry, and relates to a preparation method and application of a solid-supported catalyst. Background technique [0002] Among the methods for preparing diphenyl carbonate, the transesterification method is the main method, and the most studied method is the transesterification method of dimethyl carbonate and phenol. In this method, the research on the disproportionation reaction has also received more attention. [0003] The disproportionation reaction of methyl phenyl carbonate to prepare diphenyl carbonate uses catalysts such as organotin, organotitanium and metal oxides. Fu Qiang et al. have studied the process of the disproportionation reaction of methyl phenyl carbonate, using dibutyl tin oxide as a catalyst, under reduced pressure, the reaction is 4h, and the yield of diphenyl carbonate is 89%. The catalyst and The product is not easily separated. Ge Qing et al. have al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/12B01J31/22B01J31/04B01J35/10C07C68/06C07C69/96
CPCB01J31/122B01J31/12B01J31/1691B01J31/2239B01J31/04C07C68/06B01J2231/49B01J2531/16B01J2531/0213B01J35/60B01J35/61C07C69/96Y02P20/52Y02P20/584
Inventor 魏天荣陈坤孙苏红於国伟薛耘芸
Owner 湖北三宁碳磷基新材料产业技术研究院有限公司
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