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Method for continuously synthesizing diphenyl carbonate by micro reactor

A technology of diphenyl carbonate and microreactor, which is applied in the preparation of organic carbonate, organic chemistry, etc., can solve the problems of low selectivity and yield, and achieve the advantages of simple process flow, good heat transfer efficiency and saving production cost. Effect

Active Publication Date: 2015-03-11
SHAANXI YANCHANG PETROLEUM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when common microreactors are used in the synthesis process of diphenyl carbonate, the problems of selectivity and yield are not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Experiments were carried out according to this method, and microreactors were designed by themselves. One feed port of the microreactor is equipped with a dispersing membrane, and the dispersing membrane is a 500-mesh membrane. The cross-sectional area of ​​the reaction channel of the microreactor is 0.05×0.05 (mm 2 ), the runner length is 30cm.

[0029] Add 376g of phenol and 15.7g of homogeneous catalyst into the mixing tank, heat, stir, and mix evenly, then add 609g of methyl phenyl carbonate, continue to stir, mix evenly, the molar ratio of phenol and methyl phenyl carbonate The molar ratio of phenol and homogeneous catalyst is 1:1, and the molar ratio of phenol and homogeneous catalyst is 1:0.01; the feed liquid is transported to the microreactor with two advection pumps, the flow rate is 1ml / min respectively, and a stream of material at the feed inlet passes through the dispersion membrane The sheet is sprayed onto another stream of material to carry out the syn...

Embodiment 2

[0031] Experiments were carried out according to this method, and microreactors were designed by themselves. One feed port of the microreactor is equipped with a dispersing membrane, and the dispersing membrane is a 2000-mesh membrane. The cross-sectional area of ​​the reaction channel of the microreactor is 0.4×0.4 (mm 2 ), the runner length is 1m.

[0032] Add 376g of phenol and 31.4g of homogeneous catalyst into the mixing tank, heat, stir, and mix well, then add 1218g of methyl phenyl carbonate, continue to stir, mix well, the molar ratio of phenol and methyl phenyl carbonate The molar ratio of phenol to homogeneous catalyst is 1:0.02; two advection pumps are used to transport the feed liquid to the microreactor, the flow rate is 0.5mL / min respectively, and a stream of material at the feed inlet passes through the dispersed The diaphragm is sprayed onto another stream of material to carry out the synthesis reaction. The temperature of the reaction system is 200°C. Adjust...

Embodiment 3

[0034] Experiments were carried out according to this method, and microreactors were designed by themselves. One feed port of the microreactor is equipped with a dispersing membrane, and the dispersing membrane is a 1500-mesh membrane. The cross-sectional area of ​​the reaction channel of the microreactor is 0.25×0.25 (mm 2 ), the runner length is 2m.

[0035] Add 376g of phenol and 31.4g of homogeneous catalyst into the mixing tank, heat, stir, and mix well, then add 1218g of methyl phenyl carbonate, continue to stir, mix well, the molar ratio of phenol and methyl phenyl carbonate The molar ratio of phenol and homogeneous catalyst is 1:02; two advection pumps are used to transport the feed liquid to the microreactor, the flow rate is 1ml / min respectively, and a stream of material at the feed inlet passes through the dispersion membrane The sheet is sprayed onto another stream of material to carry out the synthesis reaction. The temperature of the reaction system is 220°C. A...

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PUM

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Abstract

The invention belongs to the technical field of preparation of fine chemical engineering products, and particularly relates to a method for preparing diphenyl carbonate. The method comprises the steps: uniformly mixing phenol and a homogeneous catalyst, and then adding the mixture to methyl phenyl carbonate for uniform mixing to obtain a reaction material; dividing the reaction material into two strands, and pumping out the two strands of the reaction material into a micro reactor, wherein the flowing speeds of the two strands of the reaction material are 0.05-20ml / min; jetting one strand of the material to the other strand of the material through a dispersing membrane at a material inlet of the micro reactor for synthesis reaction, wherein reaction liquid flowing out of the micro reactor is a coarse diphenyl carbonate product; the synthesis reaction temperature in the micro reactor is 150-250 DEG C, and the pressure is 0.1-5MPa. The method disclosed by the invention has the advantages of short material retention time, high selectivity, high yield, small equipment investment and the like; the production cost can be reduced, the material consumption is reduced, and the quantity of byproducts is reduced. The whole technical flow is reasonable and continuous; the energy consumption is low, and pollution is avoided; the method is a continuous high-efficiency and feasible diphenyl carbonate synthesis technology.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, in particular to a method for preparing diphenyl carbonate. Background technique [0002] Diphenyl carbonate is an important organic intermediate that can be used in the synthesis of pharmaceuticals, pesticides and other products, and it is an important intermediate for the preparation of polycarbonate by melt transesterification. The technique of synthesizing diphenyl carbonate has many kinds, and its process route mainly contains: 1, phosgene method, take phosgene and phenol as raw material, react in alkaline medium, as the disclosed method of CN8610765. But phosgene is highly toxic and corrosive, and the safener environmental problem is outstanding, and chlorine ions will remain in the produced DPC, which affects the quality of the polycarbon resin obtained by the reaction of this diphenyl carbonate and bisphenol A, and cannot It can be directly used as the raw m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06
CPCC07C68/06C07C69/96
Inventor 张金峰沈寒晰王燕张存社史李刚张丽娜卢美旭
Owner SHAANXI YANCHANG PETROLEUM GRP