A kind of preparation method of alkanolamine

A technology of alkanolamines and amines, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxy compounds, etc., to achieve the effects of improving product purity, reducing the generation of colored impurities, and promoting complete progress.

Active Publication Date: 2022-05-06
FUJIAN FURUN BUILDING MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In addition, most of the preparation methods of alkanolamines reported in the prior art are based on monoamine compounds. For the synthesis of alkanolamines with diamines, especially straight-chain alkylenediamines as the core, the prior art rarely involves

Method used

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  • A kind of preparation method of alkanolamine
  • A kind of preparation method of alkanolamine
  • A kind of preparation method of alkanolamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Preparation of 1,6-bis(bis(2-hydroxyethyl)amino)hexane-2,5-ol

[0043]

[0044] Add liquid ammonia 374g, 1,5-hexadiene diepoxide 1141g, catalyst CuI76g, cocatalyst ZrO in the reactor 2 25g and a small amount of hexamethylenetetramine (about 28g), then replace the air in it with nitrogen, seal the reactor and heat it to 60°C, react for 4h; then feed ethylene oxide gas into it, and react The temperature was increased to 85°C, the pressure in the reactor was maintained at 0.25-0.3Mpa, and the reaction was continued for 5h. After the reaction is completed, filter and recover the catalyst while it is hot, and rectify the filtrate to remove low-boiling substances first, then gradually heat to 140-150°C under a vacuum of 10 mmHg to recover the mixture of ethanolamine and diethanolamine, and the remaining bottom liquid is the target product 1 ,6-bis(bis(2-hydroxyethyl)amino)hexan-2,5-ol 3127g, based on 1,5-hexadiene diepoxide, the yield is 96.4%, and the purity ...

Embodiment 2

[0048] Example 2: Preparation of 1,8-bis(bis(2-hydroxyethyl)amino)octan-2,7-ol

[0049]

[0050] Add liquid ammonia 374g, 1,7-octadiene diepoxide 1422g, catalyst CuI76g, cocatalyst ZrO in the reactor 2 25g and a small amount of hexamethylenetetramine (about 28g), then replace the air therein with nitrogen, seal the reactor and heat it to 65°C, and react for 4.5h; then feed ethylene oxide gas into it, and The reaction temperature was increased to 90°C, the pressure in the reactor was maintained at 0.28-0.32Mpa, and the reaction was continued for 6h. After the reaction is completed, filter and recover the catalyst while it is hot, and rectify the filtrate to remove low-boiling substances first, then gradually heat to 140-150°C under a vacuum of 10 mmHg to recover the mixture of ethanolamine and diethanolamine, and the remaining bottom liquid is the target product 1 ,8-bis(bis(2-hydroxyethyl)amino)octan-2,7-ol 3344g, based on 1,7-octadiene diepoxide, the yield is 94.9%, and ...

Embodiment 3

[0054] Example 3: Preparation of 1,6-bis(bis(2-hydroxyethyl)amino)hexane-2,5-ol

[0055] Add liquid ammonia 374g, 1,5-hexadiene diepoxide 1141g, catalyst CuI76g, cocatalyst ZrO in the reactor 2 15g and a small amount of hexamethylenetetramine (about 14g), then replace the air therein with nitrogen, seal the reactor and heat it to 60°C, react for 5h; then feed ethylene oxide gas into it, and react The temperature was increased to 85°C, the pressure in the reactor was maintained at 0.25-0.3Mpa, and the reaction was continued for 5h. After the reaction is completed, filter and recover the catalyst while it is hot, and rectify the filtrate to remove low-boiling substances first, then gradually heat to 140-150°C under a vacuum of 10 mmHg to recover the mixture of ethanolamine and diethanolamine, and the remaining bottom liquid is the target product 1 ,6-bis(bis(2-hydroxyethyl)amino)hexan-2,5-ol 3088g, based on 1,5-hexadiene diepoxide, the yield is 95.2%, the purity is 98.5%; , t...

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Abstract

The present invention relates to a kind of preparation method of alkanolamine. The preparation method of the present invention does not need to use expensive noble metal catalysts, and does not introduce chloride ions into the product, and can obtain products with high purity and low chromaticity in high yield, and has high atom economy, and the three wastes are very low. Less, high environmental protection, suitable for industrial applications.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular, the invention relates to a preparation method of alkanolamines. Background technique [0002] Alkanolamine refers to a compound that replaces 1 to 3 hydrogen atoms on the nitrogen atom in the ammonia molecule with a hydroxyalkyl group having 2 to 4 carbons, such as a hydroxyethyl group or a hydroxypropyl group. Typical alkanolamines include diethanolamine, triethanolamine, diisopropanolamine, triisopropanolamine, diethanolmonoisopropanolamine, N,N-(2-hydroxypropyl)-N-(hydroxyethyl base) amine, etc. Alkanolamine is an important chemical product, mainly used as concrete admixture, cement additive, metal cutting fluid, coolant, antirust fluid, acid-base neutralizer, emulsifier, ink, surfactant, complexing agent, acid gas absorbent, etc. [0003] Alkanolamines, especially alkylethanolamines, are generally obtained by reacting primary or secondary amines with epoxides, such as ethyle...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/18C07C213/00B01J27/122C04B24/12C04B7/14C04B7/26
CPCC07C213/00C07C213/04B01J27/122C04B40/0039C04B7/14C04B7/26C07C215/18C04B22/147C04B22/08C04B24/122C04B22/143C04B22/10C04B22/00Y02P40/10
Inventor 温仁付
Owner FUJIAN FURUN BUILDING MATERIAL TECH
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