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

Process for preparing n-butyl isocyanate

A technology of n-butyl isocyanate and butyl isocyanate, which is applied in the field of synthesis of organic compounds, can solve the problems of no industrial value, low product content, low yield, etc., and achieve improved conversion rate, improved conversion rate, and reduced side reactions Effect

Active Publication Date: 2010-12-15
JIANGSU ANPON ELECTROCHEM
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional process is to add n-butylamine and o-dichlorobenzene into the reactor, and pass in excess phosgene at 110-160°C, and then pass in phosgene for 20-30 minutes after the solution becomes clear. The previous fraction is collected by distillation at 106-120°C to obtain n-butyl isocyanate. This method has low product content and low yield
In addition, it has been reported in the literature that the target product can also be obtained by the action of bromobutane and potassium cyanate in an organic solvent, but it does not have industrial value

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 preparing n-butyl isocyanate
  • Process for preparing n-butyl isocyanate
  • Process for preparing n-butyl isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Slowly dissolve 10,000 kilograms of n-butylamine in 30,000 kilograms of m-dichlorobenzene to form a solution, and continuously send it to the phosgenation reaction tower from the top of the tower at a flow rate of 500 kilograms / hour through a metering pump; Hours of phosgene is continuously fed into the phosgenation reaction tower from the bottom of the tower; by adjusting the flow rate of coolant or steam in the shell side of the phosgenation reaction tower, the reaction temperature is controlled in 5 stages from the top of the tower to the bottom of the tower to be 0 ° C ~ 5 ° C , 10°C to 20°C, 80°C to 90°C, 110°C to 120°C, 140°C to 150°C; the material flowing out from the bottom of the phosgenation reaction tower is rectified to obtain n-butyl isocyanate with a purity of 99.2%. Based on n-butylamine, the total yield was 96.3%.

Embodiment 2

[0024] Slowly dissolve 10,000 kilograms of n-butylamine in 40,000 kilograms of m-dichlorobenzene to form a solution, and continuously send it to the phosgenation reaction tower from the top of the tower at a flow rate of 500 kilograms / hour through a metering pump; Hours of phosgene is continuously fed into the phosgenation reaction tower from the bottom of the tower; by adjusting the coolant or steam flow rate in the shell side of the phosgenation reaction tower, the reaction temperature is controlled in 5 stages from the top to the bottom of the tower to -5°C~0 ℃, 20℃~30℃, 80℃~90℃, 100℃~110℃, 120℃~130℃; the material flowing out from the bottom of the phosgenation reaction tower is rectified to obtain n-butyl isocyanate with a purity of 99.1%. Based on n-butylamine, the total yield is 96.1%.

Embodiment 3

[0026] Slowly dissolve 10,000 kg of n-butylamine in 50,000 kg of m-dichlorobenzene to form a solution, and continuously send it to the phosgenation reaction tower from the top of the tower at a flow rate of 500 kg / hour through a metering pump; Hours of phosgene is continuously fed into the phosgenation reaction tower from the bottom of the tower; by adjusting the coolant or steam flow rate in the shell side of the phosgenation reaction tower, the reaction temperature is controlled in 5 stages from the top to the bottom of the tower to -5°C~0 ℃, 10℃~20℃, 60℃~80℃, 90℃~110℃, 130℃~140℃; the material flowing out from the bottom of the phosgenation reaction tower is rectified to obtain n-butyl isocyanate with a purity of 94.7%. Based on n-butylamine, the total yield is 83.9%.

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 preparation method for butyl isocyanate, which includes the following steps: n-butyl amine and m-dichlorobenzene are mixed into solution based on a weight ratio of 1:1.5 to 10, and the solution is fed into a phosgenation reaction tower from the top of tower continuously; the excess phosgenation is fed into the phosgenation reaction tower from the bottom of tower continuously; the phosgenation reaction tower is kept within -5 to 160 DEG C from the top of tower to the bottom of tower; the temperature is controlled by 5 to 10 segments, and the temperature is increased one by one from the top of tower to the bottom of tower; butyl isocyanate is obtained after the distillation of the material which flows from the bottom of the phosgenation reaction tower. The preparation method has the advantages that products with more than 99.0 percent purity can be prepared under the processing condition; industrial production is easily realized; the occurrence of side reactioncan be reduced effectively; the total yield of the invention counting according to n-butyl amine is more than or equal to 96.0 percent.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for preparing n-butyl isocyanate. Background technique [0002] N-butyl isocyanate is an important intermediate in organic synthesis with active chemical properties and can be used to synthesize medicines, pesticides and other products. The traditional process is to add n-butylamine and o-dichlorobenzene into the reactor, pass in excess phosgene at 110-160°C, and then pass in phosgene for 20-30 minutes after the solution becomes clear, and then distill and collect at 160°C The previous fraction is collected by distillation at 106-120°C to obtain n-butyl isocyanate. This method has low product content and low yield. In addition, it has been reported in the literature that the target product can also be obtained by the action of bromobutane and potassium cyanate in an organic solvent, but it has no industrial value. Contents of the invention [0003] The t...

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): C07C265/04C07C263/04
Inventor 郑坚姜育田程恒洲
Owner JIANGSU ANPON ELECTROCHEM
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