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Catalytic synthesis of phenyloxalate and methyl phenyl oxalate

A technology of methyl phenyl oxalate and diphenyl oxalate is applied in the field of raw materials for preparing diphenyl carbonate, and achieves the effects of reducing production cost, improving conversion rate and product selectivity, and eliminating separation process and equipment.

Inactive Publication Date: 2005-02-23
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 organotin compound, aluminum, titanium, vanadium organic acid compound, etc., but all are homogeneous soluble in the reaction system Catalyst, that is, all the transesterification reactions to be carried out are homogeneous reactions, so all the above-mentioned patented technologies use complex separation systems or equipment to separate the catalyst and the reaction

Method used

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  • Catalytic synthesis of phenyloxalate and methyl phenyl oxalate
  • Catalytic synthesis of phenyloxalate and methyl phenyl oxalate
  • Catalytic synthesis of phenyloxalate and methyl phenyl oxalate

Examples

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Embodiment 1

[0011] 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 composite TiO 2 -SiO 2 The consumption amount of the catalyst is 1.8 g, which is added under normal pressure, wherein the content of titanium oxide is 1% (by 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 raw materials, a constant temperature ...

Embodiment 2-5

[0017] Change composite metal oxide catalyst TiO 2 -SiO 2 The content of titanium oxide in the medium is 2.5%, 5%, 10%, 20% respectively, and under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, form embodiment 2-5 respectively, examine reaction result.

[0018] Table 1: TiO 2 -SiO 2 Series catalyst transesterification results (weight percentage)

[0019] Titanium Oxide Containing DMO Selectivity, % Yield, %

Embodiment

[0021] Amount, wt% Conversion % Anisole MPO DPO MPO DPO

[0022] 1 1 43.5 0.2 83.4 16.1 36.3 7.0

[0023] 2 2.5 39.7 0.4 78.2 21.4 31.1 8.5

[0024] 3 5 29.5 0.7 86.3 12.9 25.5 3.8

[0025] 4 10 27.3 0.8 85.0 14.1 23.2 3.9

[0026] 5 20 49.6 0.2 77.0 22.6 38.2 11.2

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Abstract

A catalytic synthesis process for preparing methylphenyl oxalate and diphenyl oxalate features that under existance of the titanium silicon oxide as catalyst, the dimethyl oxalate proportionally reacts on phenol at 150-190 deg.c for 1-10 hr.

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 and take composite metal oxide as catalyst, pass dimethyl oxalate (DMO) and phenol under heterogeneous condition Transesterification reaction, catalytic synthesis of phenyl oxalate, namely methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO). 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] 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, s...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C67/28C07C69/36C07C69/612
Inventor 马新宾杨霞王胜平巩金龙
Owner TIANJIN UNIV
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