Preparation method of methyl phenyl oxalate and phenostal

A technology of methyl phenyl oxalate and diphenyl oxalate, applied in the field of raw materials for the preparation of diphenyl carbonate, to achieve the effects of reducing production costs, improving selectivity, and saving separation processes and equipment

Inactive Publication Date: 2004-09-01
TIANJIN UNIV
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  • 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 catalysts soluble in the system , 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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  • Preparation method of methyl phenyl oxalate and phenostal
  • Preparation method of methyl phenyl oxalate and phenostal
  • Preparation method of methyl phenyl oxalate and phenostal

Examples

Experimental program
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Effect test

Embodiment 1

[0015] The present invention is the implementation investigation of the process method for preparing methyl phenyl oxalate and diphenyl oxalate by using dimethyl oxalate and phenol as raw materials under heterogeneous catalytic reaction conditions. It is heated by electromagnetic stirring and equipped with a thermometer to display the temperature of the reaction system. The dosage of technical grade DMO is 0.1 mole, the amount of chemically pure phenol is 0.5 mole, the dosage of tin-modified TS-1 molecular sieve (Ti content is 2.5%, the same below) catalyst is 1.8 g, and the tin loading is 1%. It was added under normal pressure, stirred and heated up, the reaction temperature was controlled at 180.0±2°C, and the reaction time was 2 hours. The reaction equilibrium constants of each step of reaction (1)-(3) are extremely small. In order to break the restriction of thermodynamic equilibrium and improve the conversion rate of raw materials, a constant temperature of 70 °C (slightl...

Embodiment 2

[0021] The catalyst was changed to Sn and the loading amount was 2% (wt) TS-1 molecular sieve. Under the same conditions as in Example 1, the transesterification reaction was carried out, and the reaction result was investigated.

Embodiment 3

[0023] The catalyst was changed to Sn with a loading of 4% (weight) TS-1 molecular sieve. Under the same conditions as in Example 1, the transesterification reaction was carried out, and the reaction results were investigated.

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Abstract

The present invention uses dimethyl oxalate and phenol as raw material, under the condition of that the raw material feeding mole ratio of dimethyl oxalate: phenol is 1:20-20:1, reaction time is 1-4 hr, reaction temp. is 170-190 deg.C, autoreaction pressure is 0-1.0 MPa and in the presence of catalyst the ester exchange reaction process is made, a it is characterized by that it catalyst is tin modified TS-1 molecular sieve, and the dose of said catalyst is 1 / 64-1 / 16 of total feeding amount.

Description

technical field [0001] The present invention relates to a kind of process method for preparing the raw material of diphenyl carbonate (DPC), specifically, relate to the preparation method of methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO), especially Using tin-modified TS-1 molecular sieve as catalyst, methyl phenyl oxalate and diphenyl oxalate are prepared by transesterification of dimethyl oxalate (DMO) and phenol under heterogeneous conditions. Background technique [0002] Using dimethyl oxalate and phenol as raw materials to prepare methyl phenyl oxalate and diphenyl oxalate is the key technology for all 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 preparation process of diphenyl carbonate with this key technology as the core appeared in the 1990s, but it has developed rapidly, especially Japan's Ube company has been comm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/28C07C67/30C07C69/36C07C69/612
Inventor 马新宾王胜平郭宏利那平许根慧
Owner TIANJIN UNIV
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