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Preparing process of tetrabutyl urea

A preparation process, the technology of tetrabutyl urea, applied in the field of preparation process of tetrabutyl urea, can solve the problems of energy consumption, time increase, influence of solvent purity, slow reaction time, etc., to reduce energy consumption, increase product purity, less toxic effect

Inactive Publication Date: 2016-08-10
YUEYANG ZHONGSHUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems of high equipment requirements, slow reaction time, and the need to stand still after the reaction in the preparation of tetrabutylurea by the phosgene method, the reaction process needs to be cooled and the potential threat to personnel and the surrounding environment brought by highly toxic raw materials should be avoided; In order to solve the problems of energy consumption and time increase caused by solvent recovery when preparing tetrabutylurea by triphosgene method, and the influence of solvent on purity; the invention provides a preparation process of tetrabutylurea

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Take 100g of bis(trichloromethyl)carbonate, grind it and mix it with 213g of pure water, the grinding particle size is unlimited.

[0025] (2) Completely add the mixture of bis(trichloromethyl)carbonate and water into 340g of industrial 31% liquid caustic soda, and mix well.

[0026] (3) Fully stir the mixed solution so that bis(trichloromethyl)carbonate particles are uniformly dispersed in the liquid phase.

[0027] (4) Add the uniformly distributed solid-liquid mixture dropwise into 265 g of di-n-butylamine, and control the dropping temperature below 70°C.

[0028] (5) After the dropwise addition, the temperature was raised to 108°C, at which time reflux occurred, and the temperature did not rise any more. Under these conditions, the stirring reaction was maintained for 30 minutes to obtain crude tetrabutylurea.

[0029] (6) The crude product of tetrabutyl urea can be distilled to obtain the final product of tetrabutyl urea after being cooled under the normal pr...

Embodiment 2

[0031] (1) Take 100g of bis(trichloromethyl) carbonate, grind it and mix it with 100g of pure water, the grinding particle size is unlimited.

[0032] (2) Completely add the mixture of bis(trichloromethyl)carbonate and water into 350g of industrial 31% liquid caustic soda, and mix well.

[0033] (3) Fully stir the mixed solution so that bis(trichloromethyl)carbonate particles are uniformly dispersed in the liquid phase.

[0034] (4) Add the uniformly distributed solid-liquid mixture dropwise into 270 g of di-n-butylamine, and control the dropping temperature below 70°C.

[0035] (5) After the dropwise addition, raise the temperature to 90°C, at this time, there will be no reflux, and the temperature will be kept constant. Under these conditions, the reaction was kept under stirring for 2 hours to obtain crude tetrabutylurea.

[0036] (6) The crude product of tetrabutyl urea can be distilled to obtain the final product of tetrabutyl urea after being cooled at a vacuum degree ...

Embodiment 3

[0038] (1) Take 100g of bis(trichloromethyl)carbonate, grind it and mix it with 50g of pure water, the grinding particle size is unlimited.

[0039] (2) Completely add the mixture of bis(trichloromethyl)carbonate and water into 400g of industrial 31% liquid caustic soda, and mix well.

[0040] (3) Fully stir the mixed solution so that bis(trichloromethyl)carbonate particles are uniformly dispersed in the liquid phase.

[0041] (4) Add the uniformly distributed solid-liquid mixture dropwise into 280 g of di-n-butylamine, and control the dropping temperature below 70°C.

[0042] (5) After the dropwise addition, raise the temperature to 60°C, at this time, there will be no reflux, and the temperature will be kept constant. Under these conditions, the stirring reaction was maintained for 12 hours to obtain crude tetrabutylurea.

[0043] (6) The crude product of tetrabutyl urea can be distilled to obtain the final product of tetrabutyl urea after being cooled at a vacuum degree o...

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PUM

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Abstract

The invention discloses a preparation process of tetrabutylurea. The raw materials of the preparation process are di-n-butylamine, bis(trichloromethyl)carbonate, liquid caustic soda and pure water; the steps of the preparation process are to Bis(trichloromethyl)carbonate is crushed and mixed with pure water, and then added to a certain amount of liquid caustic soda, and the liquid-solid mixture is added dropwise into di-n-butylamine under the state of full stirring, stirred and heated and refluxed to obtain four Crude butyl urea, the crude product is obtained by rectification to obtain the final product. The invention does not use organic solvents, which reduces the cost of solvent recovery and the difficulty of purification; does not use phosgene as a raw material, and the synthesis process is safe and risk-free; and uses liquid caustic soda to avoid the generation of hydrogen chloride gas.

Description

technical field [0001] The invention relates to a preparation process of tetrabutyl urea, in particular to a process for preparing tetrabutyl urea by using di-n-butylamine, bis(trichloromethyl)carbonate, liquid caustic soda and pure water. technical background [0002] Tetrabutylurea (TBU for short), is a transparent or slightly yellowish liquid with a viscosity slightly larger than water, and its molecular formula is C 17 h 36 N 20 ; It is a widely used organic synthesis intermediate, 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. It is mainly used as a hydroanthraquinone solvent in the new process of producing hydrogen peroxide by anthraquinone method. Compared with the traditional solvent trioctyl phosphate, it has high solubility of hydroanthraquinone; H 2 o 2 The distribution coefficient in the two phases is large; the density difference between tetrabuty...

Claims

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Application Information

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IPC IPC(8): C07C273/02C07C275/06
CPCC07C273/02
Inventor 陈攀
Owner YUEYANG ZHONGSHUN CHEM
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