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Synthetic method for n-butyl isocyanate

A technology of n-butyl isocyanate and synthesis method, which is applied in the direction of carbamate preparation and organic chemistry, etc., can solve problems such as hidden safety hazards, difficulties in transportation and storage processes, and achieve production safety, reasonable process, and high reaction yield high effect

Inactive Publication Date: 2019-09-10
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because phosgene is a highly toxic gas, there are great potential safety hazards in laboratories, experiments or industrial production.
Although diphosgene is a liquid, it is easily decomposed into phosgene when it encounters activated carbon, iron or organic amines, and the transportation and storage process is relatively difficult, and there are also major safety hazards in the use process.

Method used

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  • Synthetic method for n-butyl isocyanate
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  • Synthetic method for n-butyl isocyanate

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preparation example Construction

[0021] A kind of synthetic method of n-butyl isocyanate of the present embodiment is characterized in that, comprises the steps:

[0022] Select n-butylcarbamoyl chloride, in an organic solvent, under the catalysis of a catalyst, react at a temperature of 80-160°C for 8-15h, and obtain n-butyl isocyanate through thermal decomposition. The reaction equation is:

[0023]

[0024] Wherein, the catalyst is triethylamine, pyridine, N-methylpyrrole or N-methylpyridine.

[0025] Wherein, the organic solvent is any one of toluene, xylene, n-hexane, methylene chloride, chloroform, ethylene dichloride, chlorobenzene and dichlorobenzene.

[0026] Wherein, the molar ratio of the n-butylcarbamoyl chloride to the catalyst is 1:0.05-0.1.

[0027] Wherein, the molar ratio of the n-butylcarbamoyl chloride to the catalyst is 1:0.05.

[0028] Wherein, the molar ratio of the amount of the organic solvent to the added amount of n-butylcarbamoyl chloride is 3-20:1.

Embodiment 1

[0031] In a 1000ml four-neck flask equipped with mechanical stirring, a constant pressure dropping funnel, a reflux condenser and a thermometer, add 200g of n-butylcarbamoyl chloride, 10g of triethylamine and 700g of toluene, start stirring, and heat up under reflux. , stirred and reacted for 10 h, after the reaction was finished, 138.8 g of n-butyl isocyanate was distilled out, the yield was 95%, and the content was above 99% (GC).

Embodiment 2

[0033] In a 1000ml four-neck flask equipped with mechanical stirring, a constant pressure dropping funnel, a reflux condenser and a thermometer, add 1mol of n-butylcarbamoyl chloride, 0.1mol of N-methylpyrrole and 3mol of chlorobenzene, and start stirring , heating up, stirring and reacting at a temperature of about 90° C. for 15 hours, after the reaction was completed, 91 g of n-butyl isocyanate was distilled out, the yield was 92%, and the content was above 99% (GC).

[0034] The invention has an advanced process route, avoids highly toxic phosgene and diphosgene, has simple and safe operation, high reaction yield, low production cost, less three wastes, and has great implementation value and social and economic benefits.

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Abstract

The invention discloses a synthetic method for n-butyl isocyanate. The method comprises the following steps: selecting n-butylcarbamyl chloride, performing a reaction in an organic solvent for 8-15 hunder catalysis of a catalyst at a temperature of 80-160 DEG C, and performing thermal decomposition to obtain the n-butyl isocyanate, wherein the reaction equation is shown in the description. According to the synthetic method for the n-butyl isocyanate provided by the invention, the n-butylcarbamyl chloride is directly subjected to the reaction in the inert solvent to obtain the n-butyl isocyanate, and the chemical synthesis method eliminates safety hazards from a process source, and is a preparation method having a reasonable process, safe production, a high reaction yield, low production costs and substantially no three waste (waste water, waste gas and industrial residue) for the n-butyl isocyanate; and the method has an advanced technological route, avoids highly toxic phosgene and diphosgene, and has simple and safe operation, a high reaction yield, low production costs, less three waste (waste water, waste gas and industrial residue), larger implementation values and social andeconomic benefits.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing n-butyl isocyanate. Background technique [0002] N-butyl isocyanate is an important intermediate in organic synthesis. The chemical synthesis method of n-butyl isocyanate in the prior art is to synthesize isopropylamine and highly toxic phosgene or diphosgene as raw materials. Because phosgene is a highly toxic gas, there is a greater potential safety hazard in laboratories, experiments or industrial production. Although diphosgene is a liquid, it is easily decomposed into phosgene when it encounters activated carbon, iron or organic amines, and the transportation and storage process is relatively difficult, and there is a greater safety hazard in the use process. Therefore, how to provide a safe and reliable method for synthesizing n-butyl isocyanate is an urgent problem to be solved at present. Contents of the invention [0003] The tec...

Claims

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Application Information

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IPC IPC(8): C07C263/04C07C265/04
CPCC07C263/04C07C265/04
Inventor 纪传武李国鹏吴瑞磊佟林
Owner XINYI AGRI CHEM PLANT JIANGSU PROV
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