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Preparation method of tetrabutyl urea

A technology of tetrabutylurea and dibutylamine, applied in the field of preparation of tetrabutylurea, can solve the problems of troublesome transportation, storage, operation and use, high equipment protection requirements, large amount of three wastes, etc. High yield, easy and safe operation

Inactive Publication Date: 2003-02-05
SINO FOREIGN JOINT HUZHOU JICHANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this process method is that phosgene (COCl 2 ) is a highly toxic gas, transportation, storage and operation are very troublesome, the protection requirements for equipment are high, and the amount of three wastes is large and difficult to handle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1, feed ratio is dibutylamine: two trichloromethyl carbonate=5: 1 (molar ratio); , add 3 moles of dibutylamine and 200ml of chlorobenzene solution; start stirring, slowly add ditrichloromethyl carbonate solution dissolved in 100ml of chlorobenzene dropwise at room temperature under vigorous stirring, after the dropwise addition is completed, heat up to reflux, Keep it for 1.5 to 2 hours; pass nitrogen to drive away hydrogen chloride gas, and distill under reduced pressure to recover dibutylamine and chlorobenzene to obtain tetrabutylurea with a purity of 99.2% and a yield of 80%.

Embodiment 2

[0015] Embodiment 2, feed ratio is dibutylamine: bistrichloromethyl carbonate=6: 1 (molar ratio); In the reaction flask identical with embodiment 1, add 3 moles of dibutylamine and 100ml dichloroethane Solution, start stirring, and slowly add bistrichloromethyl carbonate solution dissolved in 200ml dichloroethane under normal temperature and vigorous stirring. After the addition is completed, heat up to reflux and keep for 5 hours; Gas; dibutylamine and dichloroethane were recovered by vacuum distillation to obtain tetrabutylurea, whose purity was determined to be 99.4%, and the reaction yield was 91%.

Embodiment 3

[0016] Embodiment 3, feed ratio (molar ratio) is dibutylamine: bistrichloromethyl carbonate=8: 1; In the reactor identical with embodiment 1, add 3 moles of dibutylamine and 100ml benzene solution, open Stirrer, at room temperature, under vigorous stirring, slowly add bistrichloromethyl carbonate solution dissolved in 200ml of benzene dropwise, after the dropwise addition, heat up to reflux and keep for 5 hours; blow nitrogen to drive away hydrogen chloride gas; vacuum distillation Dibutylamine and benzene were recovered to obtain a tetrabutylurea product, which was determined to have a purity of 99.5% and a reaction yield of 95%.

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Abstract

The preparation method of organic compound tetrabutyl carbamide uses dibutylamine and trichloromethyl carbonate as raw material, and makes synthesis is organic solvent to obtain the invented product. Said method is safe, has no production of three wastes, its raw materials are non-toxic, its reaction yield is high and quality is good.

Description

technical field [0001] The present invention relates to a kind of preparation method of organic compound tetrabutyl urea. Background technique [0002] Tetrabutylurea is a widely used intermediate in organic synthesis, and can also be used as a solvent, extraction agent and catalyst in organic chemistry, especially as a solvent in the production process of hydrogen peroxide. At present, the method for producing tetrabutylurea in the world is obtained by reacting dibutylamine and phosgene under alkaline conditions. The main disadvantage of this process method is that phosgene (COCl 2 ) is a highly toxic gas, which is very troublesome to transport, store, and operate. It requires high equipment protection, and the amount of three wastes is large and difficult to handle. Contents of the invention [0003] The purpose of the present invention is to provide a new tetrabutylurea preparation method, the preparation method raw materi...

Claims

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Application Information

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IPC IPC(8): C07C273/18C07C275/06
Inventor 施细毛潘冬明
Owner SINO FOREIGN JOINT HUZHOU JICHANG CHEM
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