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Preparation method of allyl amine mixture

The technology of allylamine and mixture is applied in the field of preparation of allylamine mixture, which can solve the problems of complicated equipment, cumbersome preparation process, long reaction time and the like, and achieves the effects of saving production cost, simple operation and improving purity

Inactive Publication Date: 2017-01-25
ZHEJIANG TAI CHUEN NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of existing allylamine is mostly made in the device of reflux with allyl chloride and ammonia, needs to make thioisocyanate propylene and 20% hydrochloric acid react 15h in the reflux device, the reaction product After concentrating and crystallizing, add water to dilute, then dropwise add liquid caustic soda to distill out allylamine, collect the crude product and then fractionate it to obtain the fine product, the preparation process is cumbersome, the equipment is complex and the reaction time is long, the cost is high and the purity is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method of allylamine mixture that the present invention proposes, comprises the following steps:

[0022] S1. Pour the Lewis acid into the reactor, then add 30% ammonia in an amount 15 times the amount of the Lewis acid, raise the reaction temperature to 38°C, and then add allyl chloride to the reactor to carry out the ammonolysis reaction;

[0023] S2. After the ammonolysis reaction in step S1 is completed, keep the temperature at 38°C constant, and after constant temperature for 25 minutes, add liquid caustic soda with a concentration of 40% to the reaction product;

[0024] S3. Perform rectification operation on the reaction product in step S2, remove excess ammonia when the rectification temperature is 38°C, and distill water when the rectification temperature is 102°C;

[0025] S4. When the rectifying temperature in step S3 is 53° C., collect the fraction—allylamine;

[0026] S5. When the rectifying temperature in step S3 is 108° C., collect ...

Embodiment 2

[0030] A kind of preparation method of allylamine mixture that the present invention proposes, comprises the following steps:

[0031] S1. Pour the Lewis acid into the reactor, then add ammonia water with a concentration of 28% that is 13 times the amount of the Lewis acid, raise the reaction temperature to 36°C, and then add allyl chloride to the reactor to carry out the ammonolysis reaction;

[0032] S2. After the ammonolysis reaction in step S1 is completed, keep the temperature of 36°C constant, and after constant temperature for 30min, add liquid caustic soda with a concentration of 42% to the reaction product;

[0033] S3. Perform rectification operation on the reaction product in step S2, remove excess ammonia when the rectification temperature is 36°C, and distill water when the rectification temperature is 100°C;

[0034] S4. When the rectifying temperature in step S3 is 54° C., collect the fraction—allylamine at this time;

[0035] S5. When the rectification tempera...

Embodiment 3

[0039] A kind of preparation method of allylamine mixture that the present invention proposes, comprises the following steps:

[0040] S1. Pour the Lewis acid into the reactor, then add 34% ammonia in an amount that is 17 times the amount of the Lewis acid, raise the reaction temperature to 35° C., then add allyl chloride to the reactor to carry out the ammonolysis reaction;

[0041] S2. After the ammonolysis reaction in step S1 is completed, keep the temperature of 35°C constant, and after constant temperature for 40min, add liquid caustic soda with a concentration of 41% to the reaction product;

[0042] S3. Perform rectification operation on the reaction product in step S2, remove excess ammonia when the rectification temperature is 35°C, and distill water when the rectification temperature is 99°C;

[0043] S4. When the rectification temperature in step S3 is 52° C., collect the fraction—allylamine at this time;

[0044] S5. When the rectifying temperature in step S3 is 1...

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PUM

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Abstract

The invention discloses a preparation method of an allyl amine mixture. The preparation method includes following steps: S1, pouring a catalyst into a reation kettle, adding a certain amount of ammonium hydroxide, rising temperature, and adding chloropropene for ammonolysis reaction; S2, holding the temperature of the step 1, and adding liquid caustic soda; S3, rectifying a reaction product to evaporate water and excessive ammonia; S4, at corresponding temperature, collecting fraction-monoallyl amine; S, at corresponding temperature, collecting fraction-diallyl amine; S6, at corresponding temperature, collecting fraction-trially amine; S7, adding caustic soda flakes into a collected fraction mixture, and performing liquid separation to obtain. The preparation method is mild in reaction condition, ammonium hydroxide is used to replace ammonia in existing methods, and complex ventilation equipment is not needed, so that production cost is saved; by adding the caustic soda flakes, water absorbing effect can be realized, purity of the allyl amine mixture prepared by the method can be effectively improved, and the preparation method is simple to operate, high in yield and worthy of popularization.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of an allylamine mixture. Background technique [0002] Allylamine is a colorless liquid with a strong ammonia and burning smell and is toxic. Used in the manufacture of pharmaceutical intermediates, as well as intermediates for agricultural chemicals, dyes and coatings, organic synthesis and resin modifiers. It can also be used to prepare amphoteric polymers, etc., and is a very important class of compounds. The preparation method of existing allylamine is mostly made in the device of reflux with allyl chloride and ammonia, needs to make thioisocyanate propylene and 20% hydrochloric acid react 15h in the reflux device, the reaction product After concentrating and crystallizing, add water to dilute, add dropwise liquid caustic soda to distill allylamine, collect the crude product and then fractionate it to obtain the refined product. The preparat...

Claims

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Application Information

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IPC IPC(8): C07C209/08C07C211/21
CPCC07C209/08C07C211/21
Inventor 黎常宏俞益平郭亚运
Owner ZHEJIANG TAI CHUEN NEW MATERIAL TECH CO LTD
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