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Preparation method of polyether amine

A polyether amine and alcohol amine technology, applied in the chemical industry, can solve the problem of difficult amine compounds connecting only one polyether main chain, and achieve the effect of avoiding requirements and reducing side reactions

Active Publication Date: 2012-07-25
WUXI ACRYL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the first two methods have higher requirements on equipment and technology. Compared with them, the third method is easier to realize. However, because the selected amine compounds often contain several amine groups at the same time, or contain hydroxyl groups, carboxyl groups, etc. The group of active hydrogen atoms, so it is difficult to ensure that an amine compound is only connected to one polyether main chain when it is connected to the polyether chain, so choose a suitable amine compound and selectively connect it to the polyether chain , is the key to such methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: a kind of preparation method of polyether amine adopts the following process steps:

[0029] (1) Dissolve 100g of ethanolamine (1.64mol) and 131g of NaOH (3.28mol) in 500ml of water, cool to 0°C, and dissolve 375g of di-tert-butyl dicarbonate (BOC 2 O) be dissolved in 500g acetone to obtain the acetone solution of di-tert-butyl dicarbonate, slowly drop the acetone solution of di-tert-butyl dicarbonate into ethanolamine, control the dropping temperature to be 0°C, complete the dropwise addition in 2 hours, keep the temperature 0°C, continue to react for 4 hours, and the pH value after the reaction is about 11;

[0030] (2) The product obtained in step (1) is subjected to vacuum distillation to remove acetone in the product, the vacuum pressure is 500 Pa, and the distillation temperature is 60° C.;

[0031](3) adding 500ml ethyl acetate to the product obtained in step (2) for extraction, to obtain an aqueous layer and an organic layer; after the aqueous lay...

Embodiment 2

[0036] Embodiment 2: a kind of preparation method of polyether amine adopts following processing steps:

[0037] (1) 100g ethanolamine (1.64mol) and 375g di-tert-butyl dicarbonate (1.72mol) were dissolved in 1000ml water, cooled to -5°C, 131g NaOH (3.28mol) was dissolved in 500ml water to obtain NaOH aqueous solution, and NaOH aqueous solution is slowly added dropwise to ethanolamine under stirring, and the dropwise addition is completed in 2 hours, and the dropping temperature is -5°C; after the dropwise addition is completed, keep at -5°C, and continue to react for 6 hours. After the reaction is completed, the pH value of the reaction system is 10;

[0038] (2) adding 500ml ethyl acetate to the compound obtained in step (1) for extraction to obtain an aqueous layer and an organic layer; after the aqueous layer was extracted once more with 250ml ethyl acetate, the organic phase obtained was combined with the organic layer; Wash the organic layer twice with 300ml saturated br...

Embodiment 3

[0043] Embodiment 3: a kind of preparation method of polyether amine adopts following process steps:

[0044] (1) Dissolve 100g ethanolamine (1.64mol) in 1000ml water, cool to 5°C, dissolve 131g NaOH (3.28mol) in 500ml water to obtain an aqueous NaOH solution, mix the aqueous NaOH solution and 375g di-tert-butyl dicarbonate (1.72mol ) was slowly added dropwise to ethanolamine under stirring, the dropwise addition was completed in 3 hours, and the dropwise addition temperature was 5°C; after the dropwise addition was completed, the temperature was maintained at 5°C, and the reaction was continued for 6 hours. After the reaction was completed, the pH value of the reaction system was 11 ;

[0045] (2) add 500ml toluene to the compound that step (1) obtains and extract, obtain water layer and organic layer; After water layer is extracted once again with 250ml toluene, the organic phase that obtains is combined with organic layer; Wash twice with 300ml of saturated saline, add anh...

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PUM

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Abstract

The invention relates to a preparation method of polyether amine. In the structure of polyether amine, the main chain is polypropylene oxide, polyethylene oxide, polytetrahydrofuran or a copolymer of polypropylene oxide, polyethylene oxide and polytetrahydrofuran; and one end of the main chain is hydroxyl, and the other end of the main chain is an alcohol amine compound terminated end having a H2N-R-O-H structure. Polyether amine is prepared by the following steps: (1) protecting the amino of the alcohol amine compound by using BOC (tertbutyloxycarbonyl) and maintaining hydroxyl to obtain BOC-NH-R-OH; (2) in the catalysis of strong base or double-metal cyanide, by using BOC-NH-R-OH, initiating polyethylene oxide, polypropylene oxide, tetrahydrofuran or the mixture of polyethylene oxide, polypropylene oxide and tetrahydrofuran to react for ring opening polymerization; and (3) under the acidic condition, carrying out BOC deprotection reaction to obtain polyether amine. According to the invention, polyether main chains having different hydrophilic properties can be obtained by regulating the ratio of polypropylene oxide to polyethylene oxide to polytetrahydrofuran in the polyether chain; and one end of the polyether chain contains the amino, thus the amino can provide strong hydrophilic property after acidification. Polyether amine prepared by using the method can be applied to the fields of a surfactant, a flocculant, textile dyeing and finishing auxiliary, electrophoretic paint and the like.

Description

technical field [0001] The invention relates to a preparation method of polyetheramine, in particular to a preparation method of polyetheramine containing an amine group at one end and a hydroxyl group at the other end, and belongs to the technical field of chemical industry. Background technique [0002] Polyether amine is a kind of compound whose main chain contains polyoxyalkylene structure and active functional group is amine group. By choosing different polyoxyalkylene structures, a series of properties such as toughness, viscosity and hydrophilicity of polyetheramine can be adjusted, and the amine group provides the possibility of polyetheramine reacting with various compounds. Due to its special structure, polyetheramine exhibits unique properties in many application fields, and its application range is becoming wider and wider. [0003] Currently disclosed synthetic methods, the method of introducing amine groups at the end of polyether mainly includes three types: ...

Claims

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Application Information

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IPC IPC(8): C08G65/28
Inventor 张文泉朱学军尤卫民
Owner WUXI ACRYL TECH
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