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Production method for n-butyl isocyanate

A technology of n-butyl isocyanate and production method, which is applied in the preparation of isocyanate derivatives, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as affecting product quality, reducing reaction yield and the like, and improving yield , the effect of improving purity and improving efficiency

Inactive Publication Date: 2016-02-03
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the presence of n-butyl isocyanate produced by the traditional n-butyl isocyanate synthesis method reduces the yield of subsequent reactions and affects the quality of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] First add xylene solution to the reaction kettle, and pass n-butylamine vapor at 80°C into the xylene solution in the reaction kettle. The n-butylamine is first dissolved in the xylene solution, which improves the efficiency of the overall reaction;

[0021] Then pass phosgene into the xylene solution, and slowly lower the temperature to 30°C, keep the reaction time for 30 minutes, stop feeding phosgene; then slowly cool down the temperature in the reactor to 0°C, keep the reaction time After 45 minutes, slowly lower the temperature in the reactor to -10°C, and keep the reaction time for 30 minutes, which can reduce the reaction time, reduce the production of urea by-products, and increase the production of intermediate products;

[0022] Continue to feed phosgene into the reactor for 20 minutes to stop, then slowly raise the temperature in the reactor to 100°C, and keep stirring in the reactor, the reaction time is 45 minutes, then continue to raise the temperature in ...

Embodiment 2

[0026] First add xylene solution to the reaction kettle, then pass 85°C n-butylamine vapor into the xylene solution in the reaction kettle, and keep stirring for 40 minutes, and continue to pass n-butylamine vapor, so that the gaseous The n-butylamine is first dissolved in the xylene solution, which improves the efficiency of the overall reaction;

[0027] Then pass phosgene into the xylene solution, and slowly lower the temperature to 31°C, keep the reaction time for 28 minutes, stop feeding phosgene; then slowly cool down the temperature in the reactor to 2°C, keep the reaction time After 50 minutes, slowly lower the temperature in the reactor to -8°C, and keep the reaction time for 35 minutes, which can reduce the reaction time, reduce the production of urea by-products, and increase the production of intermediate products;

[0028] Continue to feed phosgene into the reactor for 24 minutes to stop, then slowly raise the temperature in the reactor to 102°C, and keep stirring...

Embodiment 3

[0032] First add xylene solution to the reaction kettle, and pass n-butylamine vapor at 90°C into the xylene solution in the reaction kettle, after stirring continuously for 38 minutes, and continuously pass n-butylamine vapor, so that the gaseous The n-butylamine is first dissolved in the xylene solution, which improves the efficiency of the overall reaction;

[0033] Then pass phosgene into the xylene solution, and slowly lower the temperature to 33°C, keep the reaction time for 25 minutes, stop feeding phosgene; then slowly cool down the temperature in the reactor to 4°C, keep the reaction time 55 minutes, then slowly lower the temperature in the reactor to -6°C, and keep the reaction time for 40 minutes, which can reduce the reaction time, reduce the production of urea by-products, and increase the production of intermediate products;

[0034] Continue to feed phosgene into the reactor for 26 minutes to stop, then slowly raise the temperature in the reactor to 104°C, and k...

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PUM

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Abstract

The invention provides a production method for n-butyl isocyanate. The production method comprises the following steps that a xylene solution is added into a reaction kettle, and n-butylamine steam is introduced into the xylene solution in the reaction kettle; phosgene is introduced into the xylene solution; the phosgene is continuously introduced into the reaction kettle; the temperature of the reaction kettle is lowered, and nitrogen is introduced into the reaction kettle for gas driving. According to the production technology, the purity of an n-butylamine intermediate of the n-butyl isocyanate can be increased, so that the yield can be increased by 10%-20%, wherein the purity of the n-butylamine is increased to 75.9%-80.5%; in addition, the efficiency is improved, the phenomenon that the production efficiency and purity of the n-butyl isocyanate are influenced due to the fact that the n-butylamine has too many impurities is avoided, and by-products are few.

Description

technical field [0001] The invention relates to the field of plastic fine chemical production, in particular to a production method of n-butyl isocyanate. Background technique [0002] Pure n-butyl isocyanate (C 4 h 9 NCO) is a colorless transparent liquid that is highly irritating to the skin, mucous membranes of the respiratory tract, and eyes, and can cause burns. Its vapor and air can form explosive mixtures, and it is easy to burn and explode when exposed to open fire or high heat. [0003] N-butyl isocyanate is active in chemical properties and is an important chemical raw material. It is mainly used for the synthesis of fungicides such as IPBC and benomyl, and is also used as a catalyst for the synthesis of sulfonylurea herbicides. It can be used to synthesize medicines, pesticides and other products. The traditional process is to add n-butylamine and o-dichlorobenzene into the reactor, pass in excess phosgene at 110-160°C, and then pass in phosgene for 20-30 minute...

Claims

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Application Information

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IPC IPC(8): C07C263/10C07C265/04
Inventor 过学军胡安胜吴建平高焰兵戴玉婷张军刘长庆徐小兵黄显超朱张
Owner ANHUI GUANGXIN AGROCHEM
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