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Production process of 1, 4-phenylene diisocyanate

A p-phenylene diisocyanate and production process technology, which is applied in the field of sampling component machinery manufacturing, can solve the problem of low sampling efficiency when the depth of the reaction liquid cannot be selected for sampling, and achieve the effect of improving the stirring effect, ensuring uniformity, and simple control

Active Publication Date: 2017-08-04
UPCHEM CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above problems, the present invention proposes a production process of p-phenylene diisocyanate, which solves the problem that the sampling position of the reactor in the existing production process of p-phenylene diisocyanate is fixed, the depth of sampling of the reaction liquid cannot be selected and the sampling efficiency is low. defect

Method used

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  • Production process of 1, 4-phenylene diisocyanate
  • Production process of 1, 4-phenylene diisocyanate
  • Production process of 1, 4-phenylene diisocyanate

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment one: the present invention discloses a kind of production technique of p-phenylene diisocyanate, comprising the following steps:

[0038] 1) Warm up the chlorobenzene solution of p-phenylenediamine and triethylamine to 100°C, and add the chlorobenzene solution of bis-(trichloromethyl)carbonate into the reaction kettle together, the whole adding process In the process, the temperature of the reaction system is controlled below 50°C;

[0039] 2) Warm up to reflux, continue to add the chlorobenzene solution of the chlorobenzene solution of bis-(trichloromethyl)carbonate, finish adding in 1.5 hours; reflux for 2.5 hours;

[0040] 3) After removing the solvent under reduced pressure, rectify and collect the distillate product at 130-136°C / 8mmHg;

[0041] Wherein, the molar ratio of the p-phenylenediamine to bis-(trichloromethyl)carbonate is 1:(0.67-5). The content of p-phenylene diisocyanate analyzed by GC was 99.5%, the isocyanate value was determined to be 52....

Embodiment 2

[0042] Embodiment two: the present invention discloses a kind of production technique of p-phenylene diisocyanate, comprises the following steps:

[0043] 1) Warm up the chlorobenzene solution of p-phenylenediamine and triethylamine to 100°C, and add the chlorobenzene solution of bis-(trichloromethyl)carbonate or trichloromethyl chloroformate to the In the reaction kettle, the temperature of the reaction system is controlled below 50°C during the entire addition process;

[0044] 2) Warm up to reflux, continue to add the chlorobenzene solution of bis-(trichloromethyl)carbonate or the chlorobenzene solution of trichloromethyl chloroformate, finish adding in 3 hours; reflux for 5 hours;

[0045]3) After removing the solvent under reduced pressure, rectify and collect the distillate product at 130-136°C / 8mmHg;

[0046] The molar ratio of the p-phenylenediamine and trichloromethyl chloroformate is 1:(1-5).

[0047] GC analysis showed that the content of phenylene diisocyanate wa...

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Abstract

The invention discloses a production process of 1, 4-phenylene diisocyanate. The production process includes: heating a solution of p-phenylenediamine and triethylamine to 100 DEG C, adding the heated solution and the chlorobenzene solution of di-(trichloromethyl) carbonate or the chlorobenzene solution of trichloromethyl chlorocarbonate into a reaction kettle, heating until reflux occurs, continuing adding the chlorobenzene solution of di-(trichloromethyl) carbonate or the chlorobenzene solution of trichloromethyl chlorocarbonate, rectifying, and collecting a 130-136 DEG C / 8mmHg rectifying product, wherein the reaction kettle comprises a drive motor, a stirring shaft and stirring blades, an automatic sampling device is mounted on the stirring shaft and comprises a sleeve and a sampling component, the sleeve is provided with a liquid storage cavity inside, and the sleeve comprises an annular fixed component located on the upper portion and an annular rotatable component located on the lower portion. The production process has the advantages that the sleeve, the sampling component and the stirring shaft can rotate synchronously by the annular fixed component and the annular rotatable component, real-time sampling during reaction is achieved, and sampling efficiency is increased.

Description

technical field [0001] The invention relates to the field of mechanical manufacturing of sampling components, in particular to a production process of p-phenylene diisocyanate. Background technique [0002] At present, p-phenylene diisocyanate is synthesized by phosgene method. Phosgene is a highly toxic gas with low boiling point and high volatility, which poses great danger in the process of use, transportation and storage. The use of phosgene in production requires complex reaction equipment, refrigeration systems, various strict safety measures and operating procedures. Generally, the chlorobenzene solution of p-phenylenediamine and triethylamine is used to react with the chlorobenzene solution of bis-(trichloromethyl)carbonate or trichloromethyl chloroformate. [0003] At present, adopt the chlorobenzene solution of p-phenylenediamine and triethylamine and the chlorobenzene solution of bis-(trichloromethyl)carbonate or the reactor in the production process of trichlor...

Claims

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Application Information

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IPC IPC(8): C07C263/10C07C265/14B01J19/18
CPCB01J19/18C07C263/10C07C265/14
Inventor 夏晨东陈国全练海滨陈映波蔡延庆
Owner UPCHEM CHINA
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