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

Production method and production device of phenyl isocyanate

A technology of phenyl isocyanate and production method, which is applied in the direction of purification/separation of isocyanate derivatives, preparation of carbamate, preparation of carbamate derivatives, etc., can solve problems such as increasing difficulty, improve reaction stability, improve Product quality and yield, the effect of reducing side reactions

Pending Publication Date: 2022-05-13
UPCHEM CHINA
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, catalysts such as triethylamine, pyridine, N-methylpyrrole or tetrabutylurea are used in the reaction process, which increases the difficulty of post-treatment.

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
  • Production method and production device of phenyl isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A production method of phenyl isocyanate, the production method mainly includes the following steps: 1) mix aniline and xylene uniformly in a mixing kettle 1 at a mass ratio of 1:3, and prepare an aniline solution for use; 2) Add solid phosgene and xylene with a mass ratio of 1:2.5 into the reaction kettle 3, and heat up to dissolve; 3) When the temperature in the reaction kettle 3 reaches 90-100°C, add the above step 1) dropwise into the reaction kettle 3 The prepared aniline solution makes aniline and solid phosgene generate an unstable intermediate aniline carbamoyl chloride in a solvent medium, and the intermediate aniline carbamoyl chloride is dehydrochlorinated to obtain phenyl isocyanate; the molar ratio of aniline and solid phosgene is 1 : 0.35; the length of the dropwise addition is 1h, and after the dropwise addition is completed, the reflux is kept for 1.5h; the reaction process is monitored by the DCS control system; the reaction mixture containing the produc...

Embodiment 2

[0031] A production method of phenyl isocyanate, the mass ratio of aniline to xylene is 1:4, the mass ratio of solid phosgene to xylene is 1:3, and the mass ratio of aniline to solid phosgene is 1:0.4. All the other are with embodiment 1. The production device is the same as in Example 1. The yield of the prepared phenyl isocyanate is 93%, and the product content is ≥99.2%.

Embodiment 3

[0033] A production method of phenyl isocyanate, the mass ratio of aniline to xylene is 1:5, the mass ratio of solid phosgene to xylene is 1:4, and the mass ratio of aniline to solid phosgene is 1:0.48. All the other are with embodiment 1. The production device is the same as in Example 1. The yield of the prepared phenyl isocyanate is 94%, and the product content is ≥99.5%.

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 production method of phenyl isocyanate. The production method comprises the following steps: preparing aniline and a solvent into an aniline solution for later use; adding triphosgene and a solvent into the reaction kettle; dropwise adding an aniline solution at the temperature of 60-130 DEG C for 0.5-1.5 hours, and carrying out reflux heat preservation for 0.5-1.5 hours; the reaction process is monitored by a DCS (Distributed Control System); a reaction mixed solution is obtained; a continuous distillation mode is adopted for purification, the product phenyl isocyanate is separated from byproducts, the yield reaches 94%, and the product content is larger than or equal to 99.5%. The production device comprises a mixing kettle, a reaction kettle, a distiller, a condenser and a product storage tank, and a low-boiling-point byproduct outlet, a product outlet and a high-boiling-point byproduct outlet are respectively formed in the top, the middle and the bottom of the distiller. The phenyl isocyanate is prepared by adopting a green process, low-toxicity chemical triphosgene and a solvent are adopted, and metering, conveying and operating parameters of materials are all controlled by adopting a DCS (Distributed Control System); one-step synthesis is adopted, the reaction is stable, and side reactions are few; and continuous distillation purification is adopted, so that the product quality and yield are high.

Description

technical field [0001] The invention relates to a production method and a production device of phenyl isocyanate, belonging to the field of chemical equipment. Background technique [0002] Phenyl isocyanate is an important intermediate of medicine, pesticide and polymer materials, and is widely used in the synthesis of substituted urea compounds. The traditional synthesis methods of phenyl isocyanate include phosgene method, Curtius rearrangement method, haloform β elimination method, one-step carbonyl method, phenylcarbamate thermal decomposition method, etc., among which phosgene method is most commonly used. For example, Zhang Fusheng (Synthetic technology of isocyanate TDI, MDI, etc., Liaoning Chemical Industry, 1996, 2: 14-16) dissolved molten diaminotoluene in chlorobenzene, reacted with phosgene at 35-45 ° C at low temperature, and then heated it at 130 High temperature reaction with phosgene at ℃, after the reaction, use nitrogen to drive out hydrogen chloride to o...

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 Applications(China)
IPC IPC(8): C07C263/04C07C263/20C07C265/12C07C269/00C07C271/04B01D3/00B01D3/14B01D3/32B01J4/00B01J19/00B01J19/18
CPCC07C263/04C07C263/20C07C269/00B01D3/009B01D3/14B01D3/32B01D3/322B01J4/001B01J4/007B01J4/008B01J19/0006B01J19/18B01J2204/007B01J2219/00006C07C271/04C07C265/12
Inventor 夏剑锋夏晨东傅华伟林玮陈映波陈海芳
Owner UPCHEM CHINA
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