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Refining method for n-butyl isocyanate

A technology of n-butyl isocyanate and refining method, which is applied to the preparation of isocyanic acid derivatives, purification/separation of isocyanic acid derivatives, chemical instruments and methods, etc., and can solve problems such as affecting product quality and reducing reaction yield. Achieve the effect of reducing temperature and time and improving purity

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

[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

[0026] Add xylene solution to the reaction kettle first, and cool the temperature in the reaction kettle to -10°C to allow cold reaction to reduce side reactions;

[0027] Pass phosgene into the xylene solution in the step 1 again, the time is 30 minutes, can make material can react completely;

[0028] Add n-butylamine solution dropwise to the reaction kettle again, and the temperature of the n-butylamine solution added dropwise is 20°C, while stirring while adding dropwise, the time is 1.0 hour, which can make the cold reaction react completely and reduce the generation of by-products;

[0029] Then continue to feed phosgene into the reaction kettle, the temperature in the reaction kettle is raised to 70°C, continue to stir, and at the same time continue to raise the temperature in the reaction kettle to 105°C for 1.0 hour, the second step of high temperature reaction can be carried out to generate n-butyl Isocyanate, and improve the reaction efficiency;

[0030] Into the r...

Embodiment 2

[0035] Add xylene solution to the reaction kettle first, and cool the temperature in the reaction kettle to -8°C to allow cold reaction to reduce side reactions;

[0036] Pass phosgene into the xylene solution in the step 1 again, the time is 35 minutes, can make material can react completely;

[0037] Add n-butylamine solution dropwise to the reaction kettle again, and the temperature of the n-butylamine solution added dropwise is 16°C, while stirring while adding dropwise, the time is 1.2 hours, which can make the cold reaction react completely and reduce the generation of by-products;

[0038] Then continue to feed phosgene into the reaction kettle, the temperature in the reaction kettle is raised to 74°C, continue to stir, and at the same time, continue to raise the temperature in the reaction kettle to 110°C for 1.5 hours, and the second step of high temperature reaction can be performed to generate n-butyl Isocyanate, and improve the reaction efficiency;

[0039] Into t...

Embodiment 3

[0044] Add xylene solution to the reaction kettle first, and cool the temperature in the reaction kettle to -4°C to allow cold reaction to reduce side reactions;

[0045] Pass phosgene into the xylene solution in the step 1 again, the time is 39 minutes, can make material can react completely;

[0046] Add n-butylamine solution dropwise to the reaction kettle again, and the temperature of the n-butylamine solution added dropwise is 14°C, while stirring while adding dropwise, the time is 1.5 hours, which can make the cold reaction completely react and reduce the generation of by-products;

[0047] Then continue to feed phosgene into the reaction kettle, the temperature in the reaction kettle is raised to 76°C, continue to stir, and at the same time continue to raise the temperature in the reaction kettle to 115°C for 1.8 hours, the second step of high temperature reaction can be carried out to generate n-butyl Isocyanate, and improve the reaction efficiency;

[0048] Into the ...

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PUM

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Abstract

The invention provides a refining method for n-butyl isocyanate. The refining method comprises the steps that xylene solution is added into a reaction kettle, and the temperature in the reaction kettle is reduced; phosgene is led into the xylene solution; n-butylamine solution is dripped into the reaction kettle; phosgene continues to be led into the reaction kettle; nitrogen is led into the reaction kettle, where reaction is conducted, for gas expelling and filtration; sodium hydroxide solution is added to filtered solution; after the solution is filtered, xylene solution is added thereto to extract n-butyl isocyanate. By the adoption of the production process, the purity of the n-butyl isocyanate can be improved, a great improvement is achieved compared with an existing rectification process, and production of by-products is reduced since temperature and time are easy to control.

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. 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 minutes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C265/04C07C263/10C07C263/20
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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