Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for auxiliary synthesis of 4,4'-diphenyl methane diamino acid methyl ester by microwave

A technology of methyl dicarbamate and diphenylmethane, which is applied in the field of ester synthesis, can solve the problems of long process reaction time, etc., and achieve the effects of simplifying the post-treatment process, high catalytic efficiency, and energy saving

Inactive Publication Date: 2013-02-13
HARBIN UNIV OF SCI & TECH
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to solve the problem that the process reaction time of 4'-methyl diphenylmethane dicarbamate is long and can only be produced by batch operation in order to solve the problem that dimethyl carbonate is used to prepare, and a method is provided. A kind of microwave-assisted synthesis method of 4,4'-diphenylmethane dicarbamate methyl ester

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
  • Method for auxiliary synthesis of 4,4'-diphenyl methane diamino acid methyl ester by microwave

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0009] Specific embodiment one: In this embodiment, microwave-assisted synthesis of 4,4'-diphenylmethane dicarbamic acid methyl ester method steps are as follows: 1, in microwave reactor, 4,4'-diaminodiphenylmethane and dicarbonate Methyl esters are mixed according to a weight ratio of 1:5 to 20, and then ZS-6 catalyst is added to obtain a mixture; 2. The mixture obtained in step 1 is placed in a microwave reactor with a power of 60W to 250W and a temperature of 150°C to 200°C react at room temperature for 0.5-10 minutes, then cool to room temperature, filter, separate, and recrystallize to obtain methyl 4,4'-diphenylmethane dicarbamate; the amount of ZS-6 catalyst added in step 1 is 4,4 0.1%~5% of the mass of '-diaminodiphenylmethane; the ZS-6 catalyst described in the step 1 is composed of 50%~80% zinc acetate, 10%~40% isooctyl zinc dimercaptoacetate and 5 % ~ 10% triethyl benzyl ammonium bromide composition.

[0010] In this embodiment, the conversion rate of 4,4'-diaminod...

specific Embodiment approach 2

[0011] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the particle size of the ZS-6 catalyst described in step one is 80 mesh to 100 mesh. Others are the same as in the first embodiment.

[0012] In this embodiment, the conversion rate of 4,4'-diaminodiphenylmethane can reach 89.3%-99.6%, and the yield of methyl 4,4'-diaminodicarbamate can reach 94.7%-98.1%.

specific Embodiment approach 3

[0013] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that in step one, the weight ratio of 4,4'-diaminodiphenylmethane and dimethyl carbonate is 1:10. Others are the same as in the first or second embodiment.

[0014] In this embodiment, the conversion rate of 4,4'-diaminodiphenylmethane can reach 89.3%-99.6%, and the yield of methyl 4,4'-diaminodicarbamate can reach 94.7%-98.1%.

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

PropertyMeasurementUnit
particle sizeaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for auxiliary synthesis of 4,4'-diphenyl methane diamino acid methyl ester by microwave, and relates to an ester synthesis method. The invention aims to solve the problems of long process reaction time and single intermittent operation production mode in the conventional method for preparing the 4,4'-diphenyl methane diamino acid methyl ester by using methyl carbonate. The method of the invention comprises the following steps of: mixing 4,4'-diaminodiphenyl methane and methyl carbonate in a microwave reactor, adding a ZS-6 catalyst, performing a reaction of the raw materials under a power of the microwave reactor of 60 to 250W and at the temperature of between 150 and 200 DEG C, cooling the product of the reaction to room temperature, and then performing filtration, separation and recrystallization to obtain the 4,4'-diphenyl methane diamino acid methyl ester. The method has the advantages of short reaction time and the suitability for continuous industrialized production; and the conversion rate of the 4,4'-diaminodiphenyl methane reaches 99.6 percent, and the 4,4'-diphenyl methane diamino acid methyl ester yield reaches 98.1 percent.

Description

technical field [0001] The present invention relates to a kind of synthetic method of ester. Background technique [0002] 4,4'-Methyl diphenylmethane dicarbamate (English name Methylene diphenyl dicarbamate,) is an important intermediate for the synthesis of diphenylmethane diisocyanate. The synthesis methods of 4,4'-diphenylmethane dicarbamate methyl ester reported in the literature mainly include carbonylation method, urea method, amino transesterification method and dimethyl carbonate amination method, etc. Oxidative carbonylation in the preparation of 4,4'-diaminodiphenylmethane by carbonylation requires the use of noble metals as catalysts, resulting in high production costs and serious safety issues in the use of CO. The urea method uses phenylurea as raw material to prepare phenylcarbamate through formaldehyde condensation and methanolysis. This process avoids the safety problems caused by the use of noble metal catalysts and the use of CO, and the reaction yield an...

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): C07C271/28C07C269/04
Inventor 刘波由君王毅张辉
Owner HARBIN UNIV OF SCI & TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com