Method for synthesizing n-butyl isocyanate by gas phase method

A technology of n-butyl isocyanate and gas phase method, applied in the preparation of isocyanate derivatives, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as complicated post-treatment processes, and achieve high reaction conversion and selectivity. , the effect of reducing costs and low labor intensity

Active Publication Date: 2022-02-15
NINGXIA RUITAI TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process still needs to consume a large amount of organic solvents, and the post-treatment process is cumbersome

Method used

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  • Method for synthesizing n-butyl isocyanate by gas phase method
  • Method for synthesizing n-butyl isocyanate by gas phase method
  • Method for synthesizing n-butyl isocyanate by gas phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Preheat n-butylamine to 110°C, preheat phosgene to 90°C, pass phosgene and n-butylamine into the fixed bed according to the molar ratio of 3:1 to react. The catalyst in the fixed bed is a ceramic filler containing 1% zinc chloride, the reaction temperature in the fixed bed is 140°C, the reaction pressure is 2.0MPa, and the residence time is 30s. After cooling, degassing and rectification, the discharged material has a FNC content of 99.5% and a yield of 72.3%.

Embodiment 2

[0040] Preheat n-butylamine to 80°C, preheat phosgene to 110°C, pass phosgene and n-butylamine into the fixed bed according to the molar ratio of 5:1 to react. The catalyst in the fixed bed is a ceramic filler containing 2% magnesium chloride, the reaction temperature in the fixed bed is 180°C, the reaction pressure is 3.0MPa, and the residence time is 60s. After cooling, degassing and rectification, the discharged material has a FNC content of 99.7% and a yield of 75.8%.

Embodiment 3

[0042] Preheat n-butylamine to 120°C, preheat phosgene to 100°C, pass phosgene and n-butylamine into the fixed bed for reaction according to the molar ratio of 1.5:1. The catalyst in the fixed bed is a ceramic filler containing 5% zinc chloride, the reaction temperature in the fixed bed is 200°C, the reaction pressure is 5.0MPa, and the residence time is 100s. After cooling, degassing and rectification, the discharged material has a FNC content of 99.6% and a yield of 58.2%.

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Abstract

The invention discloses a method for synthesizing n-butyl isocyanate by adopting a vapor phase method. The method comprises the following steps: firstly, preheating a raw material n-butylamine; preheating the raw material phosgene; introducing the preheated gaseous n-butylamine and preheated phosgene into a fixed bed reactor containing a catalyst to react, and condensing the materials, removing phosgene and rectifying the reacted material to prepare an FNC finished product. According to the method, the n-butyl isocyanate is continuously synthesized by adopting a gas-phase solvent-free method, the reaction time is greatly shortened, the process route is short, and the method is suitable for industrial production, wherein the FNC is catalytically synthesized by adopting a fixed bed, the reaction is carried out under a pressurized condition, and the reaction conversion rate and selectivity are relatively high; in addition, the FNC is synthesized by a solvent-free gas-phase one-step method, the post-treatment process is simple, the procedures of desolventizing, recovering the solvent and the like are not needed, the energy consumption is greatly reduced, and the cost is remarkably reduced.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing n-butyl isocyanate by a gas phase method. Background technique [0002] N-butyl isocyanate (hereinafter referred to as FNC) is mainly used in the synthesis of insecticides such as benomyl, and is also used as a catalyst for the synthesis of sulfonylurea herbicides. As an important intermediate, it can be used to synthesize medicines, pesticides and other products. The drug is a high-efficiency broad-spectrum, systemic fungicide with protective, eradicating and therapeutic effects, and can prevent and control various crop diseases. [0003] FNC is synthesized by the reaction of n-butylamine and phosgene. It is mainly divided into two methods: (1) n-butylamine and hydrogen chloride are formed into a salt and then reacted with hot phosgene to obtain FNC; (2) n-butylamine and phosgene are prepared through a two-step reaction at low temperature and high tem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/10C07C265/04
CPCC07C263/10C07C265/04
Inventor 严绘王明晨廖强孟海娟亢玉荣韩小文
Owner NINGXIA RUITAI TECH
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