Catalytic synthesis of methyl phenyl oxalate and phenostal by using load metal oxide

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 improving selectivity, saving separation process and equipment, and reducing production costs

Inactive Publication Date: 2004-09-22
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 methyl phenyl oxalate and phenostal by using load metal oxide
  • Catalytic synthesis of methyl phenyl oxalate and phenostal by using load metal oxide
  • Catalytic synthesis of methyl phenyl oxalate and phenostal by using load metal oxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 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 SnO 2 / SiO 2 The consumption amount of is 1.8 grams, adds under normal pressure, wherein the load of metal tin 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 70 ° C...

Embodiment 2-6

[0022] Changing the Supported Metal Oxide Catalyst SnO 2 / SiO 2 The loading capacity of middle tin is respectively 2%, 4%, 8%, 12%, 16%, and under the completely identical situation of other conditions and embodiment 1, carry out transesterification reaction, form embodiment 2-6 respectively, investigate Response results.

[0023] Table 1: SnO 2 / SiO 2 Series of catalysts catalyzed transesterification reaction results (weight percentage)

[0024] DMO selectivity, % yield, %

[0025] Example Tin loading, %

[0026] Conversion rates%

[0027] Anisole MPO DPO MPO DPO

[0028] 1 1 16.3 1.8 78.5 20.2 12.8 3.3

[0029] 2 2 31.6 1.0 78.6 20.5 24.8 6.5

[0030] 3 4 45.2 0.7 78.8 20.6 35.6 9.3

[0031] 4 8 46.7 0.8 76.7 22.5 35.8 10.5

[0032] 5 12 38.1 0.7 78.0 21.3 29.7 8.1

[0033] 6 16 35.2 0.6 86.9 12.2 30.6 4.3

Embodiment 7-15

[0035] The catalyst is changed to TiO 2 / SiO 2 Series of catalysts, supported metal oxide catalyst TiO 2 / SiO 2 The loaded amount of titanium in 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 7-15 respectively, examine reaction result.

[0036] Table 2: TiO 2 / SiO 2 Series of catalysts catalyzed transesterification reaction results (weight percentage)

[0037] DMO selectivity, % yield, %

[0038] Example Titanium loading, %

[0039] Conversion rates%

[0040] Anisole MPO DPO MPO DPO

[0041] 7 1 45.6 0.5 80.9 18.6 36.9 8.5

[0042] 8 2 48.2 0.7 80.3 19.1 38.7 9.2

[0043] 9 4 53.2 0.7 82.0 17.3 43.6 9.2

[0044]10 6 54.5 0.8 81.8 17.4 44.6 9.5

[0045] 11 8 57.1 1.0 81.4 17.5 46.5 10.0

[0046] 12 10 66.7 0.5 73.0 26.5...

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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, and it is characterized by that said catalyst is a load metal oxide, 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 processing method that is used to prepare the raw material of diphenyl carbonate (DPC), specifically, relate to be catalyzer with supporting metal oxide, pass dimethyl oxalate (DMO) and phenolic ester under heterogeneous condition Exchange 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] 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...

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 马新宾郭宏利王胜平李振花王保伟许根慧
Owner TIANJIN UNIV
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