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Method for catalyzer synthesizing methyl-phenyl-oxalate and phenostal

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

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 catalyzer synthesizing methyl-phenyl-oxalate and phenostal
  • Method for catalyzer synthesizing methyl-phenyl-oxalate and phenostal
  • Method for catalyzer synthesizing methyl-phenyl-oxalate and phenostal

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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 metal oxide catalyst MoO 3 / SiO 2 The consumption amount of is 1.8 grams, adds under normal pressure, wherein the load of metal molybdenum is 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 raw materials, a constant temperature of...

Embodiment 2-9

[0021] Changing the Supported Metal Oxide Catalyst MoO 3 / SiO 2 The load of molybdenum in the 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 2-9 respectively, examine reaction result.

[0022] Table 1: MoO 3 / SiO 2 Series of catalysts catalyzed transesterification reaction results (weight percentage)

[0023] DMO selectivity, % yield, %

Embodiment 10-13

[0037] The catalyst was changed to SnO with a tin content of 4% 2 / SiO 2 Catalyst, MoO with 8% molybdenum 3 / MgO catalyst, MoO with 8% molybdenum content 3 / Al 2 o 3 Catalyst, MoO with 8% molybdenum 3 / ZrO 2 Catalyst, under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, form embodiment 10-13 respectively, investigate reaction result.

[0038] Table 2: Transesterification results of different metals and different carrier catalysts (weight percentage)

[0039] DMO selectivity, % yield, %

[0040] Example Catalyst

[0041] Conversion rates%

[0042] Anisole MPO DPO MPO DPO

[0043] 10 SnO 3 / SiO 2 45.2 0.7 78.8 20.6 35.6 9.3

[0044] 11 M 3 / ZrO 2 53.7 0.7 85.9 8.4 46.1 4.5

[0045]12 M 3 / MgO 60.2 20.9 64.5 12.6 38.8 7.6

[0046] 13 MoO 3 / Al 2 o 3 62.7 35.4 53.9 5.9 33.7 3.7

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Abstract

In this invention process, dimethyl oxalate and phenol are used as raw materials with molar ratio of 1:20 to 20:1, reaction time 1-5 hours, temp. of 170-190 deg.C, pressure 0-1.0 MPa, under the presence of catalyst to proceed ester exchange. The characteristics are: catalyst being of supporting type molybdenum trioxide, and taking the ratio of total feed of 1 / 64 to 1 / 16. Advantages are: mild reaction condition, short reaction time, high yield, catalyst being easily separated from reaction system, easily to achieve continuous prodn.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing methylphenyl oxalate and diphenyl oxalate, belonging to a process for preparing methylphenyl oxalate and diphenyl oxalate as raw materials for diphenyl carbonate (DPC). 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, EP0832910A2, etc. But in above-mentioned all patent...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/36
Inventor 马新宾巩金龙王胜平杨霞
Owner TIANJIN UNIV
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