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Synthesis process of phenyl dimethylene diisocyanate

A technology of xylylene diisocyanate and synthetic method, which is applied in the preparation of isocyanic acid derivatives, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of complex post-processing, environmental pollution, etc., and achieve environmental friendliness , easy process operation, convenient storage and transportation

Inactive Publication Date: 2007-03-21
杭州崇舜化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the disadvantages of complex post-treatment and environmental pollution in the existing synthesis process of xylylene diisocyanate, the purpose of the present invention is to provide a kind of reaction condition mild, easy to control, simple to operate, low in production cost and can realize clean production The synthetic method of xylylene diisocyanate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 1300 milliliters of chlorobenzene and 136.2 grams (1.0mol) xylylenediamine in a 3000 milliliter reaction flask equipped with a reflux condenser, air guide tube, thermometer, dropping funnel for liquid, efficient stirrer, and start stirring.

[0033] After stirring evenly, pass dry carbon dioxide gas through the air duct at a ventilation rate of 0.5L / min, maintain the temperature at 20°C to 30°C, stop the ventilation after 3 hours of reaction, and continue to stir and age for 30 minutes.

[0034] Add a solution consisting of 300 g (1.01 mol) of bis(trichloromethyl)carbonate and 300 ml of chlorobenzene at room temperature, stir for 30 minutes, heat up to 130°C to 135°C, and react for 1 hour. Under reflux, use Add dropwise a solution of 300 grams of bis(trichloromethyl)carbonate (1.01mol) and 300 milliliters of chlorobenzene in 10 hours, continue the reflux reaction for 1 hour after the addition, evaporate the solvent, and distill under reduced pressure to obtain phthal...

Embodiment 2

[0036] Add 1300 milliliters of chlorobenzene and 136.2 grams (1.0mol) xylylenediamine in a 3000 milliliter reaction flask equipped with a reflux condenser, air guide tube, thermometer, dropping funnel for liquid, efficient stirrer, and start stirring.

[0037] After stirring evenly, pass dry carbon dioxide gas through the air duct at a ventilation rate of 0.5L / min, maintain the temperature at 20°C to 30°C, stop the ventilation after 3 hours of reaction, continue to stir and age for 30 minutes, and set aside.

[0038] 300 grams (1.01mol) of bis(trichloromethyl)carbonate (1.01mol) was dissolved in 500 milliliters of chlorobenzene, 6 grams of activated carbon and 6 grams of triethylamine were added thereto, and stirring and activation was maintained at 30° C. for 30 minutes.

[0039] Add the above solution into the xylylenediamine carbonate solution at a temperature of 20°C to 30°C, continue the reaction for 30 minutes, raise the temperature to 130°C to 135°C for 1 hour, and add 3...

Embodiment 3

[0041]Using the same reaction device in Example 1, add 1300 milliliters of isoamyl acetate and 109.0 grams (0.8mol) of xylylenediamine, after stirring evenly, pass into dry carbon dioxide gas through the airway tube, and the speed of ventilation is 0.4L / min, maintain the temperature at 0°C to 10°C, stop the ventilation after 2.5 hours of reaction, and continue to stir and age for 30 minutes.

[0042] Add dropwise a solution uniformly mixed with 300 g (1.01 mol) of bis(trichloromethyl)carbonate and 400 ml of isoamyl acetate into the above solution at room temperature, stir and react for 30 minutes after the dropwise addition; heat up to 140°C React at ~145°C for 1 hour. Under reflux, add a solution consisting of 401 grams of bis(trichloromethyl)carbonate (1.35mol) and 500 milliliters of isoamyl acetate dropwise for 12 hours, and continue to reflux after the addition is complete. 1 After 1 hour, the solvent was distilled off and distilled under reduced pressure to obtain 125.6 ...

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PUM

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Abstract

The synthesis process of phenyl dimethylene diisocyanate belongs to the field of isocyanate synthesizing technology. In inert liquid medium, phenyl dimethylamine or its hydrochloride or carbonate reacts with bis(trichloromethyl) carbonate at the temperature of -20 deg.c to -60 deg.c, before heating and reflux reaction for 0.5-5 hr to synthesize phenyl dimethylene diisocyanate. The amount of bis(trichloromethyl) carbonate is 0.5-15 times that of phenyl dimethylamine or its hydrochloride or carbonate. The present invention has stable solid crystal materials, and is environment friendly and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of isocyanate synthesis, in particular to a method for synthesizing xylylene diisocyanate by reacting xylylenediamine or its hydrochloride or carbonate with bis(trichloromethyl)carbonate. Background technique [0002] Xylylene diisocyanate is an important diisocyanate, which is used as a raw material for the production of polyurethanes, polyureas, polyurethanes, polyisocyanurates and other materials in the coating and resin industries. [0003] In the prior art, the phosgenation method of preparing isocyanates by reacting organic primary amines with phosgene in an inert solvent is well known. The phosgene method can be divided into the direct method and the salt-forming method. The direct method is to prepare the corresponding isocyanate by directly reacting the primary amine and phosgene; salt, and then react the amine salt with phosgene. [0004] Chinese patent CN1038503C "preparation method of xylylene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C265/14C07C263/00
Inventor 聂天明俞介兵
Owner 杭州崇舜化学有限公司
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