Method for preparing methyl phenyl oxalate and phenostal

A technology of methyl phenyl oxalate and diphenyl oxalate, which is applied in the field of preparation of methyl phenyl oxalate and diphenyl oxalate to reduce production costs, improve selectivity, and save separation processes and equipment Effect

Inactive Publication Date: 2003-04-23
TIANJIN UNIV
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  • Abstract
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  • 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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0013] The catalyst was changed to HZSM-5 (Si / Al=25, molar ratio), under the same conditions as in Example 1, the transesterification reaction was carried out, and the reaction results were investigated. [Example 3]

Embodiment 3

[0014] The catalyst was changed to Hβ (Si / Al=35, molar ratio), under the same conditions as in Example 1, the transesterification reaction was carried out, and the reaction results were investigated. [Example 4-7]

Embodiment 4-7

[0015] Catalyst uses TS-1 (Ti content is 2.5% by weight) instead, and the reaction time carries out 1 hour, 2 hours, 3 hours, 4 hours respectively, under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, Investigate reaction result, form embodiment 4, embodiment 5, embodiment 6 and embodiment 7 respectively. The reaction results are shown in Table 1.

[0016] Table 1: Example 1-7 transesterification results (weight percentage)

[0017] Reaction DMO Selectivity, % Yield, % Example Catalyst

[0018] Time, hours conversion % Anisole MPO DPO MPO DPO1 Mordenite 2 1.4 15.2 84.8 0 1.2 02 H-ZSM-5 2 12.5 43.9 38.1 15.4 4.8 1.93 Hβ 2 54.0 31.0 53.6 12.2 29.0 6.65 2.64 TS 4.9 1 2 1 22.3 1.45 TS-1 2 26.5 0.8 89.2 10.0 23.6 2.76 TS-1 3 29.2 0.7 89.9 9.4 26.2 2.77 TS-1 4 30.0 0.7 87.8 11.5 26.3 3.4

[0019] As can be seen from the above reaction results, the reaction result of using TS...

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Abstract

The method for preparing methyl phenyl oxalate and phenyl oxalate uses dimethyl oxalate and phenol as raw material, under the condition of that raw material feeding mole ratio of dimethyl oxalate: phenol is 1:2-2:1, reaction time is 1-4 hr, reaction temp. is 170-190 deg.C, autoreaction pressure is 0-1.0 MP and presence of catalyst the ester exchange reaction process can be made, and it is characterized by that said catalyst is mordenite, HZSM-5, H beta or TS-1 molecular sieve, and the dose of catalyst is 1/64-1/16 of total feeding amount.

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 the method for preparing methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO), particularly Using molecular sieve as a catalyst, methyl phenyl oxalate and diphenyl oxalate are prepared through the transesterification reaction between dimethyl oxalate (DMO) and phenol under heterogeneous conditions. 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: or [0003] 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 res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/28C07C69/353C07C69/36
Inventor 马新宾郭宏利王胜平李振花王保伟许根慧
Owner TIANJIN UNIV
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