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Method for synthesizing high-content N-fatty alkyl-1,3-trimethylenediamine

A technology of aliphatic alkyl and propylene diamine, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc. High product purity, less reaction by-products, and good selectivity

Active Publication Date: 2019-09-20
山东汉鸿新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the author did not disclose the composition and preparation of the compound base
It is difficult to judge the results of synthetic reactions

Method used

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  • Method for synthesizing high-content N-fatty alkyl-1,3-trimethylenediamine
  • Method for synthesizing high-content N-fatty alkyl-1,3-trimethylenediamine
  • Method for synthesizing high-content N-fatty alkyl-1,3-trimethylenediamine

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Embodiment 1

[0035] A kind of synthetic method of high-content N-fatty alkyl-1,3-propylenediamine, described preparation method method is as follows:

[0036] (1) Condensation: Put 1120g of soybean oleylamine into a closed reaction kettle, replace it with nitrogen three times, start stirring to raise the temperature, gradually add acrylonitrile dropwise, and circulate cooling water to control the temperature of the reaction kettle to 70±2°C. After the dropwise addition, keep warm at 70±2°C for 1-2 hours. After vacuuming for 0.5 hours, the detection and analysis results are as follows:

[0037]

[0038] (2) Hydrogenation: Put cyanoethylalkylamine quantitatively into the autoclave, add catalyst, replace with nitrogen three times, replace with hydrogen three times, keep a certain pressure for 15 minutes, and check the airtightness of the hydrogenation autoclave. Heat up and control the temperature at 120-140°C. Control the hydrogen pressure in the kettle to 2.0-3.0MPa. Close the hydroge...

Embodiment 2

[0041] A kind of synthetic method of high-content N-fatty alkyl-1,3-propylenediamine, described preparation method method is as follows:

[0042] (1) Condensation: Put 1200g of hydrogenated tallow primary amine into a closed reaction kettle, replace it with nitrogen three times, start stirring to raise the temperature, gradually add acrylonitrile dropwise, and circulate cooling water to control the temperature of the reaction kettle to 70±2°C. After the dropwise addition, keep warm at 70±2°C for 1-2 hours. After vacuuming for 0.5 hours, the detection and analysis results are as follows:

[0043]

[0044] (2) Hydrogenation: Quantitatively put cyanoethylalkylamine into the autoclave, add catalyst, replace with nitrogen three times, replace with hydrogen three times, keep a certain pressure for 15 minutes, and check the airtightness of the hydrogenation autoclave. Heat up and control the temperature at 120-140°C. Control the hydrogen pressure in the kettle to 2.0-3.0MPa. Cl...

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Abstract

The invention relates to a method for synthesizing high-content N-fatty alkyl-1,3-trimethylenediamine, and belongs to the field of synthesis methods of compounds in organic chemicals. The preparation method comprises the following steps: (1) condensing: adding fatty primary amine, acrylonitrile and a catalyst softened water into a reaction kettle, sealing the reaction kettle, performing nitrogen substitution, and then carrying out a reaction; and (2) catalytically hydrogenating: adding cyanoethyl alkyl amine obtained by the condensation reaction in step (1) into a hydrogenation reactor, adding a hydrogenation catalyst, adding an alkaline metal oxide and an aqueous potassium hydroxide solution, and performing hydrogen displacement to obtain the high-content N-fatty alkyl-1,3-trimethylenediamine. The catalysts can be recovered for continuous application. The process is simple, an aqueous solution of calcium oxide and potassium hydroxide are used as an inhibitor, and the amounts of calcium oxide and potassium hydroxide are based on the addition amount of the catalyst palladium carbon or Raney nickel. The method has the advantages of good selectivity, high product purity, great reduction of the environmental pollution, continuous application of the recovered catalysts, and suitableness for industrial production.

Description

technical field [0001] The invention relates to a synthesis method of high-content N-fatty alkyl-1,3-propylenediamine, which belongs to the field of compound synthesis methods in organic chemical industry. Background technique [0002] N-fatty alkyl-1,3-propylenediamine is an important class of organic products. According to its carbon chain and the number of alkyl groups linked on the nitrogen atom, it can be divided into: cocoyl propylene diamine, oleyl propylene diamine, dodecyl propylene diamine, dodecyl / tetradecyl propylene diamine Pyrene diamine, tallow propylene diamine, hydrogenated tallow propylene diamine, stearyl propylene diamine, etc. It is mainly used as an asphalt emulsifier, which has the characteristics of strong emulsifying power, less dosage, and fast demulsification. It is also used in mineral flotation agents, binders, waterproofing agents, corrosion inhibition, etc., and is also an intermediate for the production of corresponding quaternary ammonium s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/25C07C209/48C07C211/10
CPCC07C253/30C07C209/48C07C255/25C07C211/10Y02P20/584
Inventor 高义宝冯新江
Owner 山东汉鸿新材料科技有限公司