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Methyl phenyl oxalate and diphenyl oxalate synthesizing process catalyzed with composite carrier supported metal oxide

A technology of methyl phenyl oxalate and diphenyl oxalate is applied in the field of catalyzing the synthesis of methyl phenyl oxalate and diphenyl oxalate by supporting metal oxides on composite carriers, and can solve the problems of distance and the like, and achieve The effect of selectivity improvement, high yield, and conversion rate improvement

Active Publication Date: 2007-06-27
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although heterogeneous catalysts have considerable advantages compared with homogeneous catalysts, the catalytic activity and DPO selectivity achieved at present are still far from the requirements of large-scale industrial production, so there is still an urgent need to further develop catalytic catalysts. Catalyst system with higher activity and DPO selectivity

Method used

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  • Methyl phenyl oxalate and diphenyl oxalate synthesizing process catalyzed with composite carrier supported metal oxide
  • Methyl phenyl oxalate and diphenyl oxalate synthesizing process catalyzed with composite carrier supported metal oxide
  • Methyl phenyl oxalate and diphenyl oxalate synthesizing process catalyzed with composite carrier supported metal oxide

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Experimental program
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Embodiment 1

[0016] In the present invention, under the condition of heterogeneous catalytic reaction, dimethyl oxalate and phenol are used as raw materials to prepare methyl phenyl oxalate and diphenyl oxalate process, which is carried out in a 250 ml three-necked flask. Electromagnetic stirring heating, equipped with a thermometer to display the temperature of the reaction system. The amount of industrial grade DMO is 0.1 mole, the amount of chemically pure phenol is 0.3 mole, catalyst MoO 3 / TiO 2 -SiO 2 The consumption is 1.8 grams, adds under normal pressure, wherein the content of molybdenum trioxide and titanium dioxide is respectively 16%, 8% (weight, the same below), silicon dioxide is particle diameter 4mm, specific surface area 146m 2 / g of coarse porous silica pellets. The preparation method of the composite carrier adopts the traditional impregnation method, and the specific method is as follows: use ethanol as a solvent, dissolve a certain amount of tetrabutyl titanate, an...

Embodiment 2-6

[0021] Changing the composite carrier supported catalyst MoO 3 / TiO 2 -SiO 2 The content of titanium dioxide in the medium is respectively 4%, 6%, 8%, 10%, 12%. Under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, form embodiment 2-6 respectively, examine reaction result.

[0022] Table 1: 16% MoO 3 / TiO 2 -SiO 2 Series catalyst transesterification results (weight percentage)

[0023]

Embodiment 7-10

[0025] Changing the composite carrier supported catalyst MoO 3 / TiO 2 -SiO 2 The loading capacity of molybdenum trioxide in the medium is respectively 1%, 4%, 8%, 12%. Under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, form embodiment 7-10 respectively, investigate reaction result.

[0026] Table 2: MoO 3 / 8%TiO 2 -SiO 2 Series catalyst transesterification results (weight percentage)

[0027]

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Abstract

The present invention is process of synthesizing methyl phenyl oxalate and diphenyl oxalate as the materials for preparing diphenyl carbonate under the catalysis of composite carrier supported metal oxide. Dimethyl oxalate and phenol in the molar ratio of 1 / 20-20 as materials produce ester exchange reaction at the temperature of 170-190 deg.c and pressure of 0-1.0 MPa in the presence of catalyst for 1-10 hr. The reaction features that the catalyst comprises composite carrier of TiO2 and other metal oxide and active component of metal oxide and has the use amount of 1 / 64-1 / 16 of total material weight. The present invention has the advantages of mild reaction condition, high material converting rate, target product selectivity over 98 %, etc.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing methylphenyl oxalate (MPO) and diphenyl oxalate (DPO) with a metal oxide supported on a composite carrier, which belongs to the technology of preparing MPO and DPO as raw materials for diphenyl carbonate (DPC) . Background technique [0002] The preparation of MPO and DPO from dimethyl oxalate (DMO) and phenol is the key technology for the preparation of DPC from DMO and phenol. The reaction steps experienced by this key technology are as follows: [0003] [0004] [0005] The DPC preparation process with this key technology as the core appeared in the 1990s, but it developed rapidly. In particular, Ube Corporation in Japan has been committed to research in this area and has applied for many patents, such as EP1013633A1, US5811573, CN1164529A, TW438765, US5834615, EP0832872A1, US5922827, EP0832910A2, etc. However, in all the above-mentioned patents, when DMO is used as raw mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/08B01J23/28B01J23/14B01J21/08B01J21/06
Inventor 马新宾刘悦王胜平
Owner TIANJIN UNIV
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