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Refining method for n-butyl isocyanate intermediate

A technology of n-butyl isocyanate and refining method, which is applied in the preparation of isocyanic acid derivatives, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of low purity of n-butylamine and achieve the effect of improving efficiency

Inactive Publication Date: 2016-01-20
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purity of the existing production of n-butylamine is generally 50-55%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] First add ammonia water to the reaction kettle, then add catalyst molybdenum oxide to the ammonia water, stir for 20 minutes, then keep the temperature in the reaction kettle at 100°C for 45 minutes, then gradually raise the temperature to 120°C while stirring , the time is 45 minutes, the molybdenum oxide can be completely dissolved in ammonia water, and then the ammonia water can be converted into ammonia gas and water vapor by heating up, and the molybdenum oxide can further improve the catalytic activity of the catalyst;

[0028] Then feed 120°C n-butanol vapor into the aforementioned reactor, and simultaneously feed ammonia into the reactor; the reactor is warmed up to 195°C, and the reactor is kept stirring, and the reaction time is 3 Hours, under the catalysis of the catalyst, the reactants react to increase the rate of reaction, while reducing the generation of di- and tributylamine, thus increasing the ratio of n-butylamine and further reducing side reactions; ...

Embodiment 2

[0036] First add ammonia water to the reaction kettle, then add catalyst molybdenum oxide to the ammonia water, stir for 24 minutes, then keep the temperature in the reaction kettle at 95°C for 40 minutes, then gradually raise the temperature to 124°C while stirring , the time is 35 minutes, the molybdenum oxide can be completely dissolved in ammonia water, and then the ammonia water can be converted into ammonia gas and water vapor by heating up, and the molybdenum oxide can further improve the catalytic activity of the catalyst;

[0037] Then feed 121 DEG C of n-butanol steam into the aforementioned reactor, and simultaneously feed ammonia into the reactor; the reactor is heated to 190 DEG C, and the reactor is kept stirring, and the reaction time is 4 Hours, under the catalysis of the catalyst, the reactants react to increase the rate of reaction, while reducing the generation of di- and tributylamine, thus increasing the ratio of n-butylamine and further reducing side react...

Embodiment 3

[0045] First add ammonia water to the reaction kettle, then add catalyst molybdenum oxide to the ammonia water, stir for 26 minutes, then keep the temperature in the reaction kettle at 90°C for 35 minutes, then gradually raise the temperature to 126°C while stirring , the time is 30 minutes, the molybdenum oxide can be completely dissolved in ammonia water, and then the ammonia water can be converted into ammonia gas and water vapor by heating up, and the molybdenum oxide can further improve the catalytic activity of the catalyst;

[0046] Then feed 123°C n-butanol vapor into the aforementioned reactor, and feed ammonia into the reactor simultaneously; the reactor is warmed up to 185°C, and the reactor is kept stirring, and the reaction time is 5 Hours, under the catalysis of the catalyst, the reactants react to increase the rate of reaction, while reducing the generation of di- and tributylamine, thus increasing the ratio of n-butylamine and further reducing side reactions;

...

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PUM

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Abstract

The invention provides a refining method for an n-butyl isocyanate intermediate. The refining method comprises the steps that firstly, ammonium hydroxide is added into a reaction kettle, and then molybdenum oxide, being the catalyst, is added to the ammonium hydroxide; secondly, n-butyl alcohol steam is led into the reaction kettle, and meanwhile ammonia gas is led into the reaction kettle without stop; thirdly, nitrogen is added for primary gas expelling of reacted materials, and a primary collection tank is adopted to collect primarily expelled gas; fourthly, the gas in the primary collection tank is cooled; fifthly, nitrogen is led into the cooled primary collection tank for secondary gas expelling; sixthly, gas in a secondary collection tank is cooled, nitrogen is led into the secondary collection tank for third gas expelling, and liquid in the secondary collection tank is extracted; lastly, activated carbon is added to the extracted liquid for drying, and filtrate is reserved after filtration is conducted. By the adoption of the production process, the purity of n-butylamine, the n-butyl isocyanate intermediate, can be improved to 78.9-83.5%, and the yield is improved by 10-25%.

Description

technical field [0001] The invention relates to the field of plastic fine chemical production, in particular to a method for refining n-butyl isocyanate intermediates. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/07C07C209/84C07C263/10C07C265/04
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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