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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AI-Extracted 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 ...

Method used

The preparation method of a kind of allylamine mixture that the present invention proposes, adopts chloropropene and ammoniacal liquor to be main raw material, carries out ammonolysis reaction and makes, and reaction condition is gentle, replaces the ammonia in the existing method with am...

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.

Application Domain

Amino preparation by functional substitution

Technology Topic

ChemistryAmmonium hydroxide +7

Examples

Experimental program(5)

Example Embodiment

[0020] Example one

[0021] The method for preparing an allylamine mixture provided by the present invention includes the following steps:

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

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

[0024] S3. Perform a 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 rectification temperature in step S3 is 53°C, collect the fraction-allylamine at this time;

[0026] S5. When the rectification temperature in step S3 is 108°C, collect the diallylamine fraction at this time;

[0027] S6. When the rectification temperature in step S3 is 152°C, collect the fraction triallylamine at this time;

[0028] S7. Add the collected mixture of monoallylamine, diallylamine and triallylamine to the solid-liquid separation equipment, and then add 0.4 times the amount of caustic soda to the mixture for liquid separation operation, namely Get the purer three mixtures.

Example Embodiment

[0029] Example two

[0030] The method for preparing an allylamine mixture provided by the present invention includes the following steps:

[0031] S1. Pour Lewis acid into the reaction kettle, then add 28% ammonia water in an amount 13 times the amount of Lewis acid, raise the reaction temperature to 36°C, and then add propylene chloride to the reaction kettle to carry out the ammonolysis reaction;

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

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

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

[0035] S5. When the distillation temperature in step S3 is 106°C, collect the diallylamine fraction at this time;

[0036] S6. When the rectification temperature in step S3 is 154°C, collect the fraction triallylamine at this time;

[0037] S7. Add the collected mixture of monoallylamine, diallylamine and triallylamine to the solid-liquid separation equipment, and then add 0.2 times the amount of the mixture to the mixture for liquid separation operation, namely Get the purer three mixtures.

Example Embodiment

[0038] Example three

[0039] The method for preparing an allylamine mixture provided by the present invention includes the following steps:

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

[0041] S2. After the ammonolysis reaction in step S1 is completed, the temperature of 35° C. is kept unchanged, and after the constant temperature is 40 minutes, 41% liquid caustic soda is added to the reaction product;

[0042] S3. Perform a 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 rectification temperature in step S3 is 105°C, collect the diallylamine fraction at this time;

[0045] S6. When the rectification temperature in step S3 is 153°C, collect the fraction triallylamine at this time;

[0046] S7. Add the collected mixture of monoallylamine, diallylamine and triallylamine to the solid-liquid separation equipment, and then add 0.6 times the amount of the mixture to the mixture for liquid separation operation, namely Get the purer three mixtures.

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Classification and recommendation of technical efficacy words

mild reaction conditions
reduce manufacturing cost

Preparation method of allyl amine mixture

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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