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Process for preparing butyl isocyanate

A technology of butyl isocyanate and n-butylamine, which is applied in the field of organic compound synthesis, can solve the problems of no industrial value, large amount of bromine, low product content, etc., so as to reduce the occurrence of side reactions, improve the conversion rate, and improve the conversion of products. rate effect

Active Publication Date: 2007-09-26
JIANGSU ANPON ELECTROCHEM
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  • 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, pass dry hydrogen chloride gas under stirring until saturated, then pass excess phosgene at 110-160°C, and then pass phosgene into the solution until the solution becomes clear After 20-30 minutes, pass through, collect the fraction before 160°C by distillation, then collect the fraction at 106-120°C by distillation, add anhydrous sodium carbonate to stand still, and filter to obtain butyl isocyanate. This method has low product content and low yield. Generally not more than 80%
In addition, it has been reported in the literature that the target product can also be obtained by reacting bromobutane and potassium cyanate in an organic solvent (dimethylformamide), but the amount of bromine used in the process is large and does not have industrial value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: In a 500L reactor, 200 kg of xylene was added, 30 kg of phosgene was introduced through the phosgene introduction tube, and 14.6 kg of n-butylamine was slowly added dropwise at 10°C. After 2 hours of dripping, The reaction was stirred for 1.5 hours, and the temperature was raised to a reflux state at a heating rate of 20°C / h, and 10 kg of phosgene was slowly added until the material was in a clear and transparent state. The phosgene was stopped. After reaction for 1 hour, the phosgene was purged with nitrogen for 1 hour. Weigh and analyze the ester content in the phosgenation reaction solution, and the calculated reaction yield is 96.6%. The product was rectified to obtain a pure product with a purity of 99.3%, and the total yield of butyl isocyanate was 95.5% based on n-butylamine.

Embodiment 2

[0028] Example 2: In a 500L reactor, 200 kg of xylene was added, 20 kg of phosgene was introduced through the phosgene introduction tube, and 14.6 kg of n-butylamine was slowly added dropwise at 0°C. After 2 hours of dripping, The reaction was stirred for 3 hours, and the temperature was raised to a reflux state at a heating rate of 20°C / h, and 20 kg of phosgene was added slowly until the material was in a clear and transparent state. The phosgene was stopped. After reacting for 1 hour, the phosgene was purged with nitrogen for 1 hour. Weigh and analyze the ester content in the phosgenation reaction solution, and the calculated reaction yield is 97.0%. The product was rectified to obtain a pure product with a purity of 99.0%, and the total yield of butyl isocyanate was 95.8% based on n-butylamine.

Embodiment 3

[0029] Example 3: In a 500L reactor, 200 kg of xylene was added, 20 kg of phosgene was introduced through the phosgene introduction tube, and 14.6 kg of n-butylamine was slowly added dropwise at 30°C. After 2 hours of dripping, The reaction was stirred for 1.5 hours, and the temperature was raised to a reflux state at a heating rate of 20°C / h, and 10 kg of phosgene was added slowly until the material was in a clear and transparent state. The phosgene was stopped. After reacting for 1 hour, the phosgene was purged with nitrogen for 1 hour. Weigh and analyze the ester content in the phosgenation reaction solution, and the calculated reaction yield is 94.6%. The product was rectified to obtain a pure product with a purity of 99.1%, and the total yield of butyl isocyanate was 93.5% based on n-butylamine.

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Abstract

The invention discloses a Method for preparation of butylisocyanate, using n-butylamine as raw materal, dimethylbenzene as dissolvant, reacting with excess carbonyl chloride, getting the product which the purity is higher than 99% after two steps photo aerification reaction of low-temperature, high-temperature and distillation. Adopting two steps photo aerification reaction of low-temperature, high-temperature can reduce occurrence of secondary reaction effectly. In n-butylamine terms, the total yield of this invention is more than 95%.

Description

1. Technical Field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for preparing butyl isocyanate. 2. Background technology [0002] Isocyanate is an important organic synthesis intermediate. It can undergo nucleophilic addition reactions, participate in the cycloaddition of unsaturated systems, carry out Diels-Alder reactions, or add bifunctional compounds to form heterocyclic derivatives. This type of compound has a wide range of applications in the synthesis of pesticides and drugs. [0003] Butyl isocyanate is a colorless transparent liquid with strong irritation. It is an important organic intermediate and can be used as an intermediate for medicine and pesticide. The traditional process is to add n-butylamine and o-dichlorobenzene into the reactor, and pass dry hydrogen chloride gas with stirring until it is saturated, and then pass in excess phosgene at 110~160℃, and then pass in phosgene after the solution becomes cle...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C263/10C07C265/04
Inventor 姜育田刘跃安礼如
Owner JIANGSU ANPON ELECTROCHEM
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