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Method for preparing 3-alkoxypropylamine

A technology for alkoxypropylamine and alkoxypropionitrile, applied in the field of preparing 3-alkoxypropylamine, can solve the problems of low yield, unsatisfactory and the like, achieve high conversion rate, easy operation and mild reaction conditions Effect

Inactive Publication Date: 2010-01-27
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires complicated operations to remove alkali metal hydroxides, and its yield is low
The process is therefore not yet satisfactory as a process for the preparation of alkoxypropylamines via alkoxypropionitriles on an industrial scale

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 150g (0.75mol) of isotridecanol and 1.35g of aqueous sodium hydroxide solution, heat to 60°C, then add 50ml (0.75mol) of acrylonitrile dropwise, after the addition is completed, stir at 60°C, and age for 3.5h Afterwards, the heating was stopped, the temperature was lowered, and the material was discharged to obtain 3-alkoxypropionitrile with a conversion rate of 92.95%.

[0022] Then put 150g of 3-alkoxypropionitrile, 3g of skeleton nickel and 4.5g of water in the autoclave, feed hydrogen into the still to replace the air in the still, stir, feed hydrogen into the still to replace the air in the still, stir, Heat the reaction system to 140°C, pressurize it with 2.0 MPa of hydrogen and 1.0 MPa of ammonia, and carry out the reaction under the pressure. After 3 hours of reaction, stop heating, cool the reaction system and discharge, and remove the skeleton nickel by filtration. To obtain 3-alkoxypropylamine, the conversion rate is 95.57%.

Embodiment 2

[0024] Will C 8-10 Mix 150g (0.75mol) of alcohol and 1.8g of aqueous sodium hydroxide solution, heat to 40°C, then add dropwise 50ml (0.75mol) of acrylonitrile, after the addition is complete, stir at 40°C, and after aging for 5 hours, stop heating, Cool down, discharge, get 3-C 8-10 Alkoxypropionitrile, the conversion rate is 95.93%.

[0025] 3-C 8-10 Put 150g of alkoxypropionitrile, 4.5g of skeleton nickel and 3g of water in an autoclave, pass hydrogen into the kettle to replace the air in the kettle, stir, heat the reaction system to 160°C, and use hydrogen 2.5MPa and ammonia 1.4MPa Pressurize and keep the pressure to react. After 5 hours of reaction, stop heating, cool the reaction system and discharge, remove the catalyst by filtration to obtain 3-C 8-10 Alkoxypropylamine, the conversion rate is 96.57%.

Embodiment 3

[0027] Mix 150g (0.75mol) of isostearyl alcohol and 0.3g aqueous sodium hydroxide solution, heat to 70°C, then add 50ml (0.75mol) of acrylonitrile dropwise, after the addition is completed, stir at 70°C, and age for 5 hours , stop heating, lower the temperature, and discharge to obtain 3-isooctadecyloxypropionitrile with a conversion rate of 94.33%.

[0028] Then put 150g of 3-isooctadecyloxypropionitrile, 2g of skeleton nickel and 1g of water into the autoclave, pass hydrogen gas into the kettle to replace the air in the kettle, stir, heat the reaction system to 150°C, and use hydrogen gas 2.5 MPa and ammonia 1.0MPa are pressurized, and the reaction is carried out while maintaining the pressure. After the reaction is completed for 5 hours, the heating is stopped, the reaction system is cooled, and the material is discharged, and the catalyst is removed by filtration to obtain 3-isooctadecyloxypropylamine. The conversion rate was 96.57%.

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PUM

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Abstract

The invention discloses a preparing method of 3-alkoxy propylamine, which comprises the following steps: blending alcohol and 0. 2-1. 2wt% sodium hydroxide solution to stir; heating to 40-70 deg. c; dripping acrylic nitrile as equal mole as alcohol to react for 1. 5-5h; cooling temperature; obtaining 3-alkoxy propanenitrile; placing 3-alkoxy propanenitrile, aggregate nickel and H2O into autoclave according to proportion; aerating hydrogen into autoclave to replace air; stirring; heating to 100-160 deg. c; aerating ammonia gas and hydrogen to react 2-5h; cooling material; removing catalyst out of liquid material; obtaining the product. The invention possesses mild condition and simple technique, which improves producing rate.

Description

technical field [0001] The invention relates to a method for preparing 3-alkoxypropylamine. Background technique [0002] Primary aliphatic amines are an important class of chemical raw materials. They can be used to prepare surfactants, bactericides, fuel and lubricant additives, and can also be directly used in mineral flotation, anti-corrosion, road construction and water treatment. Usually, fatty amines can be prepared from animal and vegetable oils, and can also be obtained from petroleum components. [0003] 3-Alkoxypropylamine is a special fatty amine. What is special about it is that besides fats and oils, many forms of alcohols can also be used as raw materials for the synthesis of 3-alkoxypropylamines. 3-Alkoxypropylamine and its amine derivatives contain different carbon chain lengths and different surfactant properties. In addition to the typical properties of cationic surfactants, 3-alkoxypropylamines and their simple derivatives have the characteristics of h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/08C07C213/02
Inventor 康保安李海建武华萍
Owner CHINA RES INST OF DAILY CHEM IND