Preparation process of tetrabutyl urea

A tetrabutyl urea, preparation technology, applied to the preparation of urea derivatives, preparation of organic compounds, chemical instruments and methods, etc., can solve the problem that the yield of finished products is only 80%-85%, there are many by-products, and it is difficult to industrialize and other issues, to achieve the effect of cheap raw materials, good product quality, and easy access to raw materials

Inactive Publication Date: 2018-04-03
青岛九洲千和机械有限公司
View PDF0 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 mono

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1), add di-n-butylamine, phosgene and 20% sodium hydroxide solution in a molar ratio of 2: 1: 2 in a reaction vessel;

[0017] (2), the acylation reaction temperature is 60°C, and the acylation reaction time is 5 hours, and the crude product of tetrabutylurea is obtained;

[0018] (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

[0020] (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;

[0021] (2), the acylation reaction temperature is 70°C, and the acylation reaction time is 6 hours, and the crude product of tetrabutylurea is obtained;

[0022] (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

[0024] (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;

[0025] (2), the acylation reaction temperature is 80°C, and the acylation reaction time is 8 hours, and the crude product of tetrabutylurea is obtained;

[0026] (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 .

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a preparation process for synthesizing tetrabutylurea by using the phosgene method, using di-n-butylamine and phosgene as the main ingredients in an alkaline organic solvent, and the process steps are as follows: (1) in a reaction vessel according to the composition than adding di-n-butylamine, carbonyl chloride and an organic solvent; (2) adjust the acylation reaction temperature, control the acylation reaction time, and obtain the crude product of tetrabutylurea; (3) the crude product of tetrabutylurea is subjected to standing, separation, Distillation and purification to obtain the final product of tetrabutylurea. The preparation method of the invention has simple and convenient operation steps, cheap and easy-to-obtain raw materials, good product quality, a reaction yield of more than 90 percent, and a purity of more than 99 percent.

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 2 0), 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C273/18C07C275/06
CPCC07C273/1809C07C275/06
Inventor 李辉
Owner 青岛九洲千和机械有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap