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Method for preparing catalyst used for gas phase catalytic synthesis of diphenyl oxalate from dimethyl oxalate

A technology of diphenyl oxalate and dimethyl oxalate, which is used in physical/chemical process catalysts, chemical instruments and methods, preparation of ester groups and hydroxyl groups, etc. problem, to achieve the effect of high reactivity, low cost and easy control

Inactive Publication Date: 2011-01-26
江苏丹化煤制化学品工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This series of updates improves the efficiency of the transesterification reaction, and the separation of the catalyst and the reaction solution becomes easier, but the reaction conditions are limited to the tank-type liquid phase reaction, which affects the continuity of the reaction and is not conducive to industrialization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of catalyst preparation method of dimethyl oxalate gas-phase catalytic synthesis of diphenyl oxalate, the specific steps of the preparation method are as follows: (1) 500 g of tetrabutyl titanate-ethanol solution is placed in a three-necked flask, and the concentration of tetrabutyl titanate is 50% (weight percent), slowly stirring; (2) Slowly add 1243g of 25% (weight percent) silica gel solution while stirring slowly; (3) After the addition is completed, continue to stir for 30min and then filter; (4) Filter Dry the cake at 60°C for 2 hours, then grind it slightly to make it into a uniform powder, then add 0.5% graphite for tableting, and press it into cylindrical particles with a diameter of 4mm and a height of 5mm; Burn at 400°C for 3h, and then cool to room temperature to obtain the final catalyst A. The specific surface area of ​​A catalyst is 143m 2 / g, the pore volume is 0.2cm 3 / g, the average pore radius is 7nm.

Embodiment 2

[0023] A kind of catalyst preparation method of gas-phase catalytic synthesis of diphenyl oxalate from dimethyl oxalate, the specific steps of the preparation method are as follows: (1) 500 g of tetrabutyl titanate-toluene solution is placed in a three-necked flask, and the concentration of tetrabutyl titanate is 40% (weight percent), stirring slowly; (2) Slowly add 20% (weight percent) silica gel solution 1843g while stirring slowly; (3) After the addition is completed, continue to stir for 45min and then filter; (4) Filter Dry the cake at 70°C for 2.5 hours, then grind it slightly to make it into a uniform powder, then add 1% graphite for tableting, and press it into cylindrical particles with a diameter of 4mm and a height of 5mm; The catalyst was burned at 450°C for 3h, and then cooled to room temperature to obtain the final catalyst B. B catalyst specific surface area is 182m 2 / g, the pore volume is 0.3cm 3 / g, the average pore radius is 9nm.

Embodiment 3

[0025] A kind of catalyst preparation method of dimethyl oxalate gas-phase catalytic synthesis of diphenyl oxalate, the specific steps of the preparation method are as follows: (1) 500 g of tetrabutyl titanate-acetone solution is placed in a three-necked flask, and the concentration of tetrabutyl titanate is 60% (weight percent), stir slowly; (2) Slowly add 786g of 25% (weight percent) silica gel solution while stirring slowly; (3) After the addition is completed, continue to stir for 60min and then filter; (4) Filter Dry the cake at 80°C for 3 hours, then grind it slightly to make it into a uniform powder, and then add 1% graphite for tableting, and press it into cylindrical particles with a diameter of 4mm and a height of 5mm; Burn at 500°C for 3h, and then cool to room temperature to obtain the final catalyst C. The specific surface area of ​​C catalyst is 217m 2 / g, the pore volume is 0.5cm 3 / g, the average pore radius is 12nm.

[0026]

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Abstract

The invention relates to a method for preparing a catalyst for the gas phase catalytic synthesis of diphenyl oxalate from dimethyl oxalate, which comprises the following steps of: slowly adding a silica gel solution to an organic titanate-dispersant solution to completely hydrolyze, filtering, drying, grinding, tabletting, firing and so on to prepare the catalyst. The invention also relates to the application of the catalyst. The catalyst has high reactivity in a gas phase ester exchange reaction between diphenyl oxalate and phenol, the selectivity of diphenyl oxalate is high, the reaction is smooth and easy to control, and the catalyst has simple preparation method, low cost and long service life.

Description

technical field [0001] The present invention relates to a kind of catalyst preparation method of gas-phase catalytic synthesis of diphenyl oxalate from dimethyl oxalate, the catalyst is prepared by hydrolysis precipitation method, and is used to catalyze the transesterification reaction of dimethyl oxalate and phenol under gas-phase conditions, and then The reaction solution was separated and purified to obtain diphenyl oxalate. Background technique [0002] Diphenyl oxalate can be used as a raw material for the manufacture of various pharmaceutical and pesticide intermediates, and can also be used as a raw material and additive for polymer manufacturing. In particular, diphenyl oxalate can be decarboxylated into diphenyl carbonate (DPC), and diphenyl carbonate Ester (DPC) is one of the important monomers for the synthesis of polycarbonate (PC). Diphenyl oxalate can be prepared by the transesterification reaction of dimethyl oxalate and phenol, and the brief steps are descr...

Claims

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Application Information

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IPC IPC(8): B01J21/06C07C69/36C07C67/03
Inventor 吴晓金魏超许叶飞胡晓鸣
Owner 江苏丹化煤制化学品工程技术有限公司
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