Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of method and device for preparing diphenyl carbonate by one-step method of phenol and dimethyl carbonate

A technology of dimethyl carbonate and diphenyl carbonate, which is applied in the field of organic synthesis, can solve problems such as geometric or positional isomerization side reactions, complicated post-treatment, and a large amount of industrial waste water, and achieve low cost, good catalytic effect, and device The effect of simple structure

Active Publication Date: 2017-08-04
CHINA CONSTR IND & ENERGY ENG GRP CO LTD
View PDF10 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main reason is that NaOH is cheap and easy to get, but it also has obvious disadvantages: (1) The transesterification should be completed in two steps under reduced pressure and high temperature conditions. The first step neutralizes the free acid, removes moisture and disperses the catalyst Uniform; in the second step, the temperature is raised to a relatively high level for reaction
(2) When the conditions are not selected properly, geometric or positional isomerization side reactions may occur, resulting in a significant decrease in yield
(3) Neutralization and washing are required in the post-processing process, which brings a large amount of industrial wastewater, causing environmental pollution, and post-processing is also complicated

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of method and device for preparing diphenyl carbonate by one-step method of phenol and dimethyl carbonate
  • A kind of method and device for preparing diphenyl carbonate by one-step method of phenol and dimethyl carbonate
  • A kind of method and device for preparing diphenyl carbonate by one-step method of phenol and dimethyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: a kind of device that phenol and dimethyl carbonate one-step method prepares diphenyl carbonate comprises autoclave 1, extraction tower 2, catalyst recovery device 3, rectifying tower 4, condenser 5, reflux tank 6, The first drying tower 7, the second drying tower 8, the product tank 9, the high pressure reactor 1 is equipped with a PTFE inner cylinder, and the external connection temperature indicator 10 and pressure regulator 11, constantly adjust the pressure during the reaction process, improve the carbonic acid The productive rate of diphenyl ester, dimethyl carbonate raw material tank outlet is connected with described autoclave 1 inlet a, and phenol, ionic liquid catalyst raw material tank outlet is connected with described autoclave 1 inlet b, and described autoclave 1 The outlet is connected to the inlet of the extraction tower 2, the outlet of the inorganic phase of the extraction tower is connected to the inlet of the catalyst recovery device 3, ...

Embodiment 2

[0028] Embodiment 2: Dimethyl carbonate and phenol are dropped into the reactor at a feed ratio of 3: 1, and 0.8wt% of [(C 2 h 5 ) 3 N(CH 2 ) 4 SO 3 H][HSO 4 ] ionic liquid catalyst, heat up and reflux reaction under stirring conditions, the reaction temperature is 160 ° C, the reaction time is 2h, after the reaction is completed, the organic phase mixture is obtained by static separation, and the organic phase mixture is decompressed and refined under a vacuum degree of 5mmHg. Distilled and collected to obtain diphenyl carbonate product.

[0029] The device used in this embodiment is the same as in Example 1, the conversion rate of phenol is 92.5%, and the single pass yield of diphenyl carbonate is 31.2%.

Embodiment 3

[0030] Embodiment 3: dimethyl carbonate and phenol are dropped into reactor according to feed ratio 6: 1, and add 3wt% [(CH 3 ) 3 N(CH 2 ) 4 SO 3 H][HSO 4 ] ionic liquid catalyst, heat up and reflux reaction under stirring conditions, the reaction temperature is 180 ° C, the reaction time is 5h, after the reaction is completed, the organic phase mixture is obtained by standing still for liquid separation, and the organic phase mixture is decompressed and refined under a vacuum degree of 7mmHg. Distilled and collected to obtain diphenyl carbonate product.

[0031] The device used in this embodiment is the same as in Example 1, the conversion rate of phenol is 92.8%, and the single pass yield of diphenyl carbonate is 30.1%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method and device for preparing diphenyl carbonate in one step. Dimethyl carbonate and phenol are put into a reactor at a feeding ratio of 3:1 to 6:1, an ionic liquid catalyst is added, and the temperature is raised under stirring conditions. , reflux reaction, and after the reaction is completed, let it stand for liquid separation to obtain an organic phase mixture. The organic phase mixture is rectified under reduced pressure under a vacuum of 5 to 7 mmHg, and the diphenyl carbonate product is collected and obtained. The present invention uses an ionic liquid catalyst to promote phenol and dimethyl carbonate to prepare benzyl carbonate through one-step transesterification. When 1.6wt% of [MimN(CH2)4SO3H][HSO4] ionic liquid catalyst is added, the catalytic effect is better. Under the same conditions, the conversion rate of phenol can reach 93.5%, and the single-pass yield of diphenyl carbonate can reach 32.4%; the device of the invention has a simple structure, is easy to operate, can produce continuously, and improves the yield.

Description

technical field [0001] The invention relates to an organic synthesis method, in particular to a method and a device for preparing diphenyl carbonate in one step from phenol and dimethyl carbonate. Background technique [0002] At present, the traditional method of producing polycarbonate is the phosgene method. Although the process is mature and the product quality is good, this method is gradually being eliminated due to the use of highly toxic phosgene, which does not meet the inherent requirements of green chemistry. The new process of producing polycarbonate with diphenyl carbonate and bisphenol A as raw materials is expected to gradually replace the phosgene method. This process is very competitive in the production of polycarbonate due to its outstanding environmental protection advantages. Developed countries have very strict blockades on advanced manufacturing technologies and raw materials related to the polycarbonate industry chain. During the "Tenth Five-Year" a...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C68/06C07C69/96
CPCC07C68/06C07C69/96
Inventor 黄益平周俊超徐义明
Owner CHINA CONSTR IND & ENERGY ENG GRP CO LTD