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Isocyanate preparing process

A technology of isocyanate and trichloromethyl chloroformate, which is applied in the field of preparation process of organic chemical raw material isocyanate, can solve problems such as difficult storage and transportation, not allowed storage and transportation, and high toxicity, so as to achieve convenient storage and transportation and benefit the environment Effects of protection and shortening reaction time

Inactive Publication Date: 2003-08-20
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) Phosgene is very dangerous in the process of preparation, storage and use, and storage and transportation are generally not allowed, so the preparation and use of phosgene must be used at the same time of preparation; and phosgene is a dangerous substance, phosgene Gas is a gas under normal temperature and pressure, not easy to store and transport, easy to explode, highly toxic
its production is strictly limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 300g of trichloromethyl chloroformate to a 2000ml four-necked reaction flask, add 1000ml of toluene, add 100g of β-phenylethylamine dropwise at 40°C, finish adding within half an hour, slowly heat to reflux, and The reaction was carried out at low temperature for 3 hours, the toluene was evaporated under reduced pressure, and the components at 98----105°C / 10mmHg were collected to obtain 99 g of the corresponding product with a yield of 81.5%.

Embodiment 2

[0019] Add 300g of trichloromethyl chloroformate to a 2000ml four-necked reaction flask, add 1000ml of toluene, add 100g of cyclohexylamine dropwise at 40°C, finish adding within half an hour, slowly heat to reflux, and react at 110°C for 3 hours , Toluene was distilled off under reduced pressure, and the components at 70----80°C / 20mmHg were collected to obtain 107.3 g of the corresponding product, with a yield of 85%.

Embodiment 3

[0021] Add 100 grams of cyclopentylamine and 1,000 ml of toluene to a 2000 ml four-necked reaction flask, add 300 grams of trichloromethyl chloroformate dropwise at 40°C, complete the addition within half an hour, slowly heat to reflux, and react at 110°C for 3 After 1 hour, the toluene was distilled off under reduced pressure, and the components at 95---105°C / 100mmHg were collected to obtain 113 g of the corresponding product, with a yield of 86.5%.

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PUM

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Abstract

The isocyanate preparing process is one reaction between proper primary amine and trichloromethyl chloroformate and features that at reaction temperature of -5 to 180 and normal pressure, primary amine is first dissolved in inert organic solvent and then reaction with liquid trichloromethyl chloroformate in the molar ratio to primary amine of 0.2-1. The present invention has the advantages caused by replacing trichloromethyl chloroformate for phosgene, including easy storage and transportation, decrease of toxic matter, easy operation, one half shortened reaction time and being ever suitable for industrial production.

Description

technical field [0001] The invention relates to an organic synthesis preparation process, in particular to a preparation process of organic chemical raw material isocyanate. Background technique [0002] In the process of preparing organic isocyanate, the commonly used method is: use excess phosgene to react with appropriate amine. Conventional methods for preparing isocyanates using phosgene have the following disadvantages: [0003] (1) Phosgene is very dangerous in the process of preparation, storage and use, and storage and transportation are generally not allowed, so the preparation and use of phosgene must be used at the same time of preparation; and phosgene is a dangerous substance, phosgene Gas is a gas under normal temperature and pressure, which is not easy to store and transport, easy to explode and highly toxic. Its production is strictly limited. [0004] (2) Excessive phosgene needs to be passed through for a long time in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/10C07C265/04
Inventor 段桂运宋丽华张滨高荣长
Owner SHANDONG XINHUA PHARMA CO LTD
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