Preparation process for tetrabutyl urea

A technology of tetrabutylurea and preparation process is applied in the preparation of urea derivatives, the preparation of organic compounds, organic chemistry, etc., and can solve the problems of only 80%-85% yield of finished products, many by-products, and difficult industrialization. , to achieve the effect of cheap raw materials, good product quality and easy availability of raw materials

Inactive Publication Date: 2012-10-03
CHONGQING CHANGFENG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Phosgene method includes monophosgene method, diphosgene method, triphosgene method, etc.; diphosgene method and triphosgene method need to use solvent in the process of preparing tetrabutylurea, although monophosgene method is not applicable during reaction Solvent, but in the follow-up treatment, benzene or toluene needs to be used for extraction. According to related reports, the yield of finished product is only 80%-85%. Non-phosgene methods include carbon monoxide method, carbon dioxide method, acetanilide method, etc.; carbon monoxide method needs to use oxygen Or auxiliary reagents such as potassium iodide, reaction under pressurized condition, yield is low, and by-product is many, use dibutylamide lithium and di-n-butylamine and carbon monoxide reaction then be difficult to industrialization; Acetanilide method reacts with di-n-butylamine, Although less toxic, the product is an equal amount of tetrabutylurea and by-products
At present, there are basically no enterprises producing tetrabutylurea in China, and most of the market demand depends on foreign imports.

Method used

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  • Preparation process for tetrabutyl urea
  • Preparation process for tetrabutyl urea

Examples

Experimental program
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Effect test

Embodiment 1

[0018] (1), add di-n-butylamine, phosgene and 20% sodium hydroxide solution in a molar ratio of 2: 1: 2 in a reaction vessel;

[0019] (2), the acylation reaction temperature is 60°C, and the acylation reaction time is 5 hours, and the crude product of tetrabutylurea is obtained;

[0020] (3) After the crude tetrabutylurea was left to stand for 30 minutes, the mother liquid water in the lower layer was separated, and the crude tetrabutylurea was distilled at a vacuum degree of -0.092MPa and a kettle temperature of 200°C to obtain the final product of tetrabutylurea .

Embodiment 2

[0022] (1), add di-n-butylamine, phosgene and 20% sodium hydroxide solution in a molar ratio of 2: 1.05: 2.1 in the reaction vessel;

[0023] (2), the acylation reaction temperature is 70°C, and the acylation reaction time is 6 hours, and the crude product of tetrabutylurea is obtained;

[0024] (3) After the crude tetrabutylurea was left to stand for 30 minutes, the mother liquid water in the lower layer was separated, and the separated crude tetrabutylurea was distilled at a vacuum degree of -0.094MPa and a kettle temperature of 210°C to obtain the final product of tetrabutylurea .

Embodiment 3

[0026] (1), add di-n-butylamine, phosgene and 20% sodium hydroxide solution in a molar ratio of 2: 1.05: 2.1 in the reaction vessel;

[0027] (2), the acylation reaction temperature is 80°C, and the acylation reaction time is 8 hours, and the crude product of tetrabutylurea is obtained;

[0028] (3) After the crude tetrabutylurea was left to stand for 30 minutes, the mother liquid water in the lower layer was separated, and the separated crude tetrabutylurea was distilled at a vacuum degree of -0.096MPa and a kettle temperature of 220°C to obtain the final product of tetrabutylurea .

[0029] The detection results of three embodiments are as follows:

[0030]

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Abstract

The invention provides a preparation process for synthesizing tetrabutyl urea by using di-n-butylamine and carbonyl chloride as major materials in an alkaline organic solvent by means of phosgenation synthesis, wherein the process comprises the following steps: (1) adding di-n-butylamine, carbonyl chloride and organic solvent to a reactor in certain proportion; (2) adjusting the temperature of acylation reaction and controlling the reaction time to obtain crude tetrabutyl urea; (3) standing, separating, distilling and purifying the crude tetrabutyl urea to obtain a final product of tetrabutyl urea. The preparation method provided by the invention is simple in procedure, the raw materials are cheap and easily available, the product is good in quality, the reaction yield is over 90%, and the purity is more than 99%.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a preparation process of an organic compound tetrabutylurea. Background technique [0002] Tetrabutylurea (C 17 h 36 N 20 ), is an organic synthesis intermediate with a wide range of uses, and can also be used as a solvent, extractant and catalyst in organic chemistry, especially as a solvent in the hydrogen peroxide production process in large quantities. The methods for synthesizing tetrabutylurea are roughly divided into phosgene method and non-phosgene method. Phosgene method includes monophosgene method, diphosgene method, triphosgene method, etc.; diphosgene method and triphosgene method need to use solvent in the process of preparing tetrabutylurea, although monophosgene method is not applicable during reaction Solvent, but in the follow-up treatment, benzene or toluene needs to be used for extraction. According to related reports, the yield of finished product is only...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C275/06C07C273/18
Inventor 李定山
Owner CHONGQING CHANGFENG CHEM IND
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