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Preparation method of N-(3-aminopropyl)-1,3-propane diamine

A technology of aminopropyl and propylenediamine, which is applied to the preparation of amino compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high energy consumption, poor selectivity, and low yield, and achieve simple process and three wastes The effect of less and lower cost

Inactive Publication Date: 2010-09-01
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Document OrganicSyntheses, 27,3-5,1947; J Am Chem Soc, 67,92-94,1945; Fine chemical industry, 3,57-58, 1999 reported to prepare N-(2-cyanogen by reacting with acrylonitrile and concentrated ammonia water (ethyl ethyl)-3-aminopropionitrile, yield 57~70%, but this method selectivity is poor, and yield is low, needs to evaporate the water in the reaction liquid simultaneously, and energy consumption is big, is not suitable for suitability for suitability for industrialized production

Method used

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  • Preparation method of N-(3-aminopropyl)-1,3-propane diamine
  • Preparation method of N-(3-aminopropyl)-1,3-propane diamine
  • Preparation method of N-(3-aminopropyl)-1,3-propane diamine

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Embodiment 1

[0015] Close the first needle valve 11, the raw material vent valve 15, the second ball valve 16 and the third ball valve 17, open the constant pressure valve 3, the pressure valve 13 and all the first ball valves 2, and the reactor 9 is filled with 3A spherical molecular sieves, Use nitrogen to set the pressure of the constant pressure valve 3 and the pressure valve 13 to 5 MPa, then close 3 and 13, open the second ball valve 16, use the first temperature controller 14 to control the temperature of the reactor 9 to 50 ° C, and open the condensation at the same time water12. After the temperature and pressure are stabilized, use metering pump 6 to mix liquid ammonia and acrylonitrile with a molar ratio of 1.5:1 and a total volume space velocity of 0.5h -1 At the same time, it is sent into the reactor 9, and the first needle valve 11 is adjusted to control the pressure of the reaction system to be about 5MPa. After the device was running for 5 hours, a small amount of reaction...

Embodiment 2

[0017] Close the first needle valve 11, the raw material vent valve 15, the second ball valve 16 and the third ball valve 17, open the constant pressure valve 3, the pressure valve 13 and all the first ball valves 2, and the reactor 9 is filled with 3A spherical molecular sieves, Use nitrogen to set the pressure of the constant pressure valve 3 and the pressure valve 13 to 4MPa, then close 3 and 13, open the second ball valve 16, use the first temperature controller 14 to control the temperature of the reactor 9 to be 80°C, and open the condensation at the same time water12. After the temperature and pressure are stabilized, use metering pump 6 to mix liquid ammonia and acrylonitrile with a molar ratio of 1:1 and a total volume space velocity of 0.5h -1 At the same time, it is sent into the reactor 9, and the first needle valve 11 is adjusted to control the pressure of the reaction system to be about 4MPa. After the device was running for 5 hours, a small amount of reaction l...

Embodiment 3

[0019] Close the first needle valve 11, the raw material vent valve 15, the second ball valve 16 and the third ball valve 17, open the constant pressure valve 3, the pressure valve 13 and all the first ball valves 2, and the reactor 9 is filled with 5A spherical molecular sieves, Use nitrogen to set the pressure of the constant pressure valve 3 and the pressure valve 13 to 5 MPa, then close 3 and 13, open the second ball valve 16, use the first temperature controller 14 to control the temperature of the reactor 9 to be 15 °C, and open the condensation at the same time water12. After the temperature and pressure are stabilized, use metering pump 6 to mix liquid ammonia and acrylonitrile with a molar ratio of 5:1 and a total volume space velocity of 0.8h -1 At the same time, it is sent into the reactor 9, and the first needle valve 11 is adjusted to control the pressure of the reaction system to be about 5MPa. After the device was running for 3 hours, a small amount of reaction...

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Abstract

The invention discloses a preparation method of N-(3-aminopropyl)-1,3-propane diamine (also called bis-(3-aminopropyl)amine or dipropilidene triamine), belonging to the technical field of organic chemical industry. The invention is characterized by comprising the following steps: first using a fixed bed as a reaction vessel and using a molecular sieve to catalyze the reaction between ammonia and acrylonitrile to prepare N-(2-cyanoethyl)-3-aminopropionitrile, and enabling the reactant liquor of the N-(2-cyanoethyl)-3-aminopropionitrile to be subject to direct catalytic hydrogenation without isolation and purification to prepare the N-(3-aminopropyl)-1,3-propane diamine, wherein the overall yield of the N-(3-aminopropyl)-1,3-propane diamine can reach more than 80% in the two-step reaction. The invention has the advantages of simple process, less three wastes, low cost, high product selectivity and easy industrialization.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry and relates to a preparation method of N-(3-aminopropyl)-1,3-propanediamine. Background technique [0002] N-(3-aminopropyl)-1,3-propanediamine (also known as bis(3-aminopropyl)amine or dipropylenetriamine) having the following structure is a very versatile Fine organic chemicals, which can be used in the synthesis of epoxy resins, polyamide resins, emulsifiers, corrosion inhibitors, metal chelates and pharmaceutical intermediates, etc. [0003] [0004] Patent CN101111468A has developed a method of passing 1,3-propylenediamine and hydrogen into the reaction tower under the Pd catalyst supported by zirconia, and preparing N-(3-aminopropyl)-1 through reactive distillation and continuous reaction. The method of 3-propylenediamine, through the design of the reaction tower, the occurrence of side reactions can be suppressed and the conversion rate of 1,3-propylenediamine can be i...

Claims

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Application Information

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IPC IPC(8): C07C211/14C07C209/48
Inventor 孟庆伟刘洋都健刘广志高志刚丁一嵘郭洪臣
Owner DALIAN UNIV OF TECH
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