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

Process for producing dicyclohexyl methyl hydride diisocyanate and its midbody

A technology of dicyclohexylmethane and diaminodicyclohexylmethane, which is applied in the field of preparation of diisocyanate and its intermediates, can solve the problems of shortened catalyst life, increased production cost, and reduced catalyst activity, and achieve extended use Effects of longevity, reduction in toxicity, and reduction in production costs

Active Publication Date: 2009-05-13
WANHUA CHEMICAL (NINGBO) CO LTD
View PDF2 Cites 24 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using this raw material, the impurities contained in the raw material such as isomers, oligomers and other impurities can lead to a rapid decrease in the activity of the catalyst during the hydrogenation reaction, shorten the life of the catalyst, and increase the production cost in the industrial process.

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
  • Process for producing dicyclohexyl methyl hydride diisocyanate and its midbody
  • Process for producing dicyclohexyl methyl hydride diisocyanate and its midbody
  • Process for producing dicyclohexyl methyl hydride diisocyanate and its midbody

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] use figure 1In the process shown, the bicyclic MDA and polycyclic MDA from the condensation process of the diphenylmethane diisocyanate (MDI) plant are fully preheated to 220°C by the preheater and the falling film evaporator, and then enter the distillation tower with a diameter of 50mm , the column is filled with corrugated structured packing, the number of trays is 5, the bottom temperature is 250°C, the top temperature is 230°C and the top pressure is 3.5 mbar; the feed composition is 4,4'-diaminodiphenyl The methane content is 68wt%, the 2,4'-diaminodiphenylmethane content is 5wt%, and the polycyclic MDA is about 27wt%. The vapor phase material at the top of the distillation tower enters the middle of the rectification tower. The temperature at the bottom of the rectification tower is 244°C, the temperature at the top of the tower is 190°C, the temperature of the side line gas phase in the tower is 240°C, and the number of trays in the rectification tower is 25. ...

Embodiment 2

[0059] use figure 2 In the process shown, 4,4'-diaminodiphenylmethane content of 99.7wt% diaminodiphenylmethane and tetrahydrofuran are added to the autoclave at a mass ratio of 1:1, and 3wt% Rh / Al 2 o 3 The catalyst is added into the kettle, and the amount of the catalyst added accounts for 1.2wt% of the feeding amount of diaminodiphenylmethane. After replacing the reactor with nitrogen and hydrogen, fill the reactor with hydrogen to 5MPa, raise the temperature of the material in the reactor to 185°C, maintain the temperature, and maintain the hydrogen pressure in the reactor at 5MPa for 240 minutes. Cool down to 40°C and replace with pressure release, filter the reaction liquid in the kettle, flush the catalyst with trapped solids into the reaction kettle through backwashing operation and continue to be used for the hydrogenation reaction of the next batch, the main component of the filtrate It is a solution of diaminodicyclohexylmethane in tetrahydrofuran. The filtrat...

Embodiment 3

[0061] use figure 2 In the process shown, the diaminodiphenylmethane isomer mixture with a 4,4'-diaminodiphenylmethane content of 50.12wt% and cyclohexylamine are added to the high-pressure stirred tank at a mass ratio of 3:10. 5wt% Ru / C catalyst was added into the kettle, and the amount of catalyst added accounted for 5wt% of the feeding amount of diaminodiphenylmethane. After replacing the reactor with nitrogen and hydrogen, fill the reactor with hydrogen to 9MPa, raise the temperature of the material in the reactor to 180°C, maintain the temperature, and maintain the hydrogen pressure in the reactor at 9MPa for 360 minutes. After cooling and filtering, the filtrate sample was taken for gas chromatography analysis, and the content of diaminodiphenylmethane was 2.36wt%, and the content of diaminodicyclohexylmethane was 91.75wt%.

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 for preparing dicyclohexyl methane diisocyanate. The method comprises the following steps: a) a diamino diphenylmethane isomer mixture reacts in an organic solvent at a reaction temperature between 90 and 200 DEG C, under the hydrogen pressure between 3.0 and 12.0 MPa and under the action of a catalyst, so as to obtain a diamino dicyclohexyl methane isomer mixture; and b) the diamino dicyclohexyl methane isomer mixture obtained in the step a) and phosgene are heated to 330 to 400 DEG C so as to be gasify respectively and then are sent into a reactor with a mixing device to be mixed and react, have hydrogen chloride and phosgene removed, and are distilled, so as to obtain the dicyclohexyl methane diisocyanate. The method has the advantages of prolonging the life span of the catalyst and reducing cost. The invention also provides a complete technological process for preparing the dicyclohexyl methane diisocyanate.

Description

technical field [0001] The present invention relates to a preparation method of diisocyanate and its intermediate, in particular to a dicyclohexylmethane diisocyanate isomer with a 4,4'-dicyclohexylmethane diisocyanate mass percentage of 48%-100% Process for the preparation of mixtures and intermediates thereof. Background technique [0002] Diaminodicyclohexylmethane (H 12 MDA), also known as hydrogenated diaminodiphenylmethane, can be used in epoxy resin curing agent, and as the preparation of dicyclohexylmethane diisocyanate (H 12 MDI) raw material. Usually H 12 MDA can be obtained by catalytic hydrogenation of diaminodiphenylmethane at high pressure, followed by H 12 MDA can then be phosgenated to obtain H 12 MDI. [0003] And the starting material of preparing diaminodicyclohexylmethane generally adopts the higher homologue (abbreviation: polyamine, polycyclic MDA) that contains diaminodiphenylmethane (abbreviation: bicyclic MDA) and diaminodiphenyldiamine mixtur...

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
IPC IPC(8): C07C265/14C07C263/10
Inventor 齐旺顺尚永华赵磊胡爽倪自林隋宝华罗务习王永胜华卫琦马德强
Owner WANHUA CHEMICAL (NINGBO) CO LTD
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