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Method for synthesizing phenyloxalate from dicthyl oxalate and phenol

A technology of diethyl oxalate and diphenyl oxalate, which is applied in the field of raw materials for preparing diphenyl carbonate, can solve problems such as difficult separation of products and catalysts, and achieve the effects of saving separation process and equipment and reducing production costs.

Active Publication Date: 2005-10-26
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the synthesis of diphenyl oxalate by transesterification of dimethyl oxalate and phenol with a supported oxide catalyzes the shortcoming that the product and the catalyst are not easy to separate when using a homogeneous catalyst, the intermediate product methyl phenyl oxalate (MPO) generation, the selectivity of the product diphenyl oxalate is only about 20%, which needs to be improved urgently

Method used

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  • Method for synthesizing phenyloxalate from dicthyl oxalate and phenol
  • Method for synthesizing phenyloxalate from dicthyl oxalate and phenol
  • Method for synthesizing phenyloxalate from dicthyl oxalate and phenol

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Embodiment 1

[0015] In the present invention, under the conditions of heterogeneous catalytic reaction, diethyl oxalate and phenol are used as raw materials to prepare diphenyl oxalate process. It is carried out in a three-necked flask of 250 milliliters, heated by heat-collecting electromagnetic stirring, equipped with a thermometer, to display the temperature of the reaction system. The amount of chemically pure DEO is 0.1 mole, the amount of chemically pure phenol is 0.5 mole, and the supported metal oxide catalyst SnO 2 / SiO 2 The consumption amount of is 1.8 grams, adds under normal pressure, wherein the load of metal tin is 1% (mass, the same below). Stir and heat up, the reaction temperature is controlled at 180.0±2°C, and the reaction time is 2 hours. The reaction equilibrium constant of reaction (1) is very little, for breaking the restriction of thermodynamic equilibrium, improve the transformation rate of raw material, the reflux condenser of the constant temperature circulati...

Embodiment 2-6

[0020] Changing the Supported Metal Oxide Catalyst SnO 2 / SiO 2 The loading capacity of middle tin is respectively 2%, 4%, 8%, 12%, 16%, and under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, form embodiment 2-6 respectively, examine Response results.

[0021] Example

Embodiment 7-14

[0023] The catalyst is changed to TiO 2 / SiO 2 Series of catalysts, supported metal oxide catalyst TiO 2 / SiO 2 The loaded amount of titanium in middle is respectively 1%, 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, under the situation that other conditions are completely identical with embodiment 1, carry out ester Exchange reaction, form embodiment 7-14 respectively, examine reaction result.

[0024] Example

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Abstract

The present invention discloses a method for catalytically synthesizing phenyloxalate by utilizing diethyl acetate and phenol as raw material. The mole ratio of diethyl acetaet and phenol is 1:20-20:1, its reaction time is 1-8 hr, reaction temperature is 160-240 deg.C and autogeneous reaction pressure is 0-1.0 MPa. Under the action of load metal oxide catalyst the above-mentioned raw material are undergone the process of ester-interchange reaction so as to obtain the invented phenyloxalate.

Description

technical field [0001] The present invention relates to a kind of processing method that is used to prepare the raw material of diphenyl carbonate (DPC), specifically, relate to be catalyzer with supporting metal oxide, pass diethyl oxalate (DEO) and phenolic ester under heterogeneous condition Exchange reaction, catalyze the method for synthesizing diphenyl oxalate (DPO). Background technique [0002] The preparation of diphenyl oxalate from diethyl oxalate and phenol is a key technology for the preparation of diphenyl carbonate from diethyl oxalate and phenol. The reaction steps experienced by this key technology are as follows: [0003] [0004] About the synthesis of diphenyl oxalate by transesterification of oxalate and phenol, the preparation process of diphenyl oxalate and then decarbonylation of diphenyl carbonate began to appear in the 1990s, but it developed rapidly. Japan's Ube company has been committed to this aspect Research, and applied for many patents, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36
Inventor 马新宾王胜平
Owner TIANJIN UNIV
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