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Method for synthesizing methyl phenyl oxalate and phenostal under catalysis of oxide of bimetal

A technology of methyl phenyl oxalate and double metal oxide, applied in the field of double metal oxide catalytic synthesis of methyl phenyl oxalate and diphenyl oxalate, to improve and reduce the conversion rate and product selectivity Production cost, save the effect of separation process and equipment

Inactive Publication Date: 2005-01-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But in above-mentioned all patents, relate to when using dimethyl oxalate as raw material to prepare the raw material of synthetic diphenyl carbonate by transesterification, i.e. methyl phenyl oxalate or diphenyl oxalate, although the transesterification catalyst used is constantly Update, change and improve, it can be alkali metal, cadmium, zirconium, lead, iron, copper, zinc compound or organic tin compound, aluminum, titanium, vanadium organic acid compound, etc., but all are homogeneous soluble in the reaction system Catalyst, that is, all transesterification reactions to be carried out are homogeneous reactions, so all the above-mentioned patented technologies use complex separation systems or equipment to separate catalysts and reaction products

Method used

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  • Method for synthesizing methyl phenyl oxalate and phenostal under catalysis of oxide of bimetal
  • Method for synthesizing methyl phenyl oxalate and phenostal under catalysis of oxide of bimetal
  • Method for synthesizing methyl phenyl oxalate and phenostal under catalysis of oxide of bimetal

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Experimental program
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Effect test

Embodiment 1

[0015] 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 0.5 mole, and the supported double metal oxide catalyst MoO 3 -SnO 2 / SiO 2 The consumption amount of is 1.8 grams, adds under normal pressure, and wherein the load of metal molybdenum and tin is respectively 1% (weight, the same below). Stir and heat up, the reaction temperature is controlled at 180.0±2°C, and the reaction time is 2 hours. Reaction (1)-(3) The reaction equilibrium constants of each step are extremely small. In order to break the restriction of thermodynamic equilibrium and improve the conversion rate of ...

Embodiment 2-9

[0022] Changing the Supported Bimetallic Catalyst MoO 3 -SnO 2 / SiO 2 The loads of molybdenum and tin in the medium are respectively 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, under the completely identical situation of other conditions and embodiment 1, carry out transesterification Reaction, form embodiment 2-9 respectively, examine reaction result.

[0023] Table 1: MoO 3 -SnO 2 / SiO 2 Series catalyst transesterification results (weight percentage)

[0024] DMO selectivity, % yield, %

Embodiment

[0025] Examples Tin loading, % Molybdenum loading, %

[0026] Conversion rate%

[0027] Anisole MPO DPO MPO DPO

[0028] 1 1 1 46.0 0.5 86.8 12.7 39.9 5.9

[0029] 2 2 2 47.3 0.7 88.7 10.6 41.9 5.0

[0030] 3 4 4 50.2 0.9 88.4 10.7 44.4 5.4

[0031] 4 6 6 47.7 0.8 88.6 10.6 42.2 5.1

[0032] 5 8 8 55.5 0.7 86.7 12.6 48.1 7.0

[0033] 6 10 10 56.7 0.6 86.7 12.7 49.1 7.2

[0034] 7 12 12 57.3 0.6 86.7 12.7 49.7 7.3

[0035] 8 14 14 74.6 0.5 81.5 18.0 60.8 13.4

[0036] 9 16 16 58.8 0.6 85.2 14.2 50.1 8.3

[0037] It can be seen from the reaction results of the above examples that when the supported double metal oxide is used as the catalyst in the process of the present invention, there is a better reaction result. loaded on SiO 2 The bimetallic catalysts with appropriate Mo and Sn contents on the catalysts showed high activity and selectivity.

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Abstract

This invention relates the process for producing methyl phenyl oxalate and diphenyl oxalate, both of them being of raw materials of diphenyl carbonate (DPC). Dimethyl oxalate and phenol are used as raw materials with mole ratio of 1:20-20:1, reaction time of 1-5 hrs, temp. of 170-190 deg.C, pressure of 0-1.0 MPa, catalyst of bimetallic oxide as an amount of 1 / 64-1 / 16 of total feed being presence. Advantages are: mild reaction condition, short reaction time, high yield, catalyst being of easy to be separated from system, continuous prodn. to be achieved easily.

Description

technical field [0001] The invention relates to a method for synthesizing methylphenyl oxalate and diphenyl oxalate by double metal oxide catalysis, belonging to the production of methylphenyl oxalate and diphenyl oxalate as raw materials for the preparation of diphenyl carbonate (DPC) process method. Background technique [0002] The preparation of methylphenyl oxalate and diphenyl oxalate from dimethyl oxalate and phenol is the key technology for all the preparation of diphenyl carbonate from dimethyl oxalate and phenol. The reaction steps experienced by this key technology are as follows: [0003] [0004] or [0005] [0006] The diphenyl carbonate 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, EP083...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/36
Inventor 马新宾巩金龙杨霞王胜平
Owner TIANJIN UNIV
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