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Preparation method for organic amine carbaminate

An organic amine amino, formate technology, applied in the preparation of carbamate derivatives, the preparation of organic compounds, organic chemistry and other directions, can solve the problems of high energy consumption, difficulty in solvent removal, etc., achieve less dosage and improve reaction rate. And the effect of salt formation rate and simple process

Inactive Publication Date: 2015-05-06
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The purpose of the present invention is to solve the technical problems of difficult solvent removal and high energy consumption in the preparation method of organic amine carbamate in the prior art, and to provide a preparation method of organic amine carbamate

Method used

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  • Preparation method for organic amine carbaminate
  • Preparation method for organic amine carbaminate
  • Preparation method for organic amine carbaminate

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preparation example Construction

[0025] The preparation method of organic amine carbamate, comprises the following steps:

[0026] Under normal temperature and pressure, add the organic amine and organic solvent with a mass ratio of 100:(2~500) into the closed reaction device, keep stirring at the speed of 300~2400rpm at -10℃~100℃, and add to the reaction The device is filled with CO 2 Gas, generally make the gas in the reaction device (mainly CO 2 Gas) pressure reaches 0.1MPa~15MPa, after 2min~10h of reaction, the organic amine fully reacts completely, releases the pressure, and obtains the post-reaction solution, if there is white solid in the post-reaction solution, filter the post-reaction solution, centrifuge or distill off the solvent, A white solid is obtained, and after drying, an organic amine carbamate with a purity of 90% to 98% is obtained; if there is no white solid in the solution after the reaction, the solvent is distilled off from the solution after the reaction, and the obtained mucus is an...

Embodiment 1

[0040] The preparation method of 1,6-hexanediamine carbamate:

[0041] Add 10ml of industrial ethanol and 20g of 1,6-hexanediamine into the 80ml reaction kettle, seal it, put it in an oil bath at 60°C, under continuous magnetic stirring (speed 1200rpm), preheat for 5min, then pump CO2 into the reaction kettle 2 Gas, the pressure reaches 3MPa. After 2 minutes of reaction, the pressure is released to open the kettle, the solvent is distilled off, and dried to obtain a white solid of 1,6-hexamethylenediamine carbamate with a yield of 90% and a melting point of 157°C-160°C.

[0042] The hexamethylenediamine carbamate prepared in embodiment 1 is carried out infrared spectrum detection, the result is as follows figure 1 shown, from figure 1 It can be seen that 3335cm -1 It is the N-H bond stretching vibration peak of primary amino group and secondary amino group in carbamate; 2930cm -1 and 2850cm -1 Antisymmetric and symmetric stretching vibration peaks of the C-H bond of methyl...

Embodiment 2

[0046] The preparation method of 1,6-hexanediamine carbamate:

[0047] In the 800ml reactor, add 40ml ethyl acetate and 200g 1,6-hexamethylenediamine, after airtight, in an oil bath at 65°C, under continuous magnetic stirring (speed 2400rpm), preheat for 5min, then pump into the reactor CO 2 Gas, pressure up to 9MPa, react for 3min, release the pressure and open the kettle, filter to remove the solvent, and dry to obtain a white solid of 1,6-hexamethylenediamine carbamate with a yield of 92% and a melting point of 157°C-160°C.

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Abstract

The invention discloses a preparation method for organic amine carbaminate, belongs to the technical field of preparation of organic amine carbaminate, and solves the problems that a solvent is difficult to separate out and the energy consumption is high of the preparation method for the organic amine carbaminate in the prior art. The preparation method comprises the steps of adding organic amine and an organic solvent into a reaction device according to the mass ratio of 100:(2-500), continuously stirring under the temperature of 10 DEG C below zero to 100 DEGC, filling the reaction device with CO2 gas to enable the gas pressure in the reaction device to reach 0.1-15 MPa, reacting for 2 minutes to 10 hours, and removing the organic solvent to obtain the organic amine carbaminate, wherein the organic solvent can be used for dissolving organic amine and the CO2 gas or is swelled by supercritical CO2. According to the method, the reaction rate and the salting rate are greatly increased; the organic amine carbaminate generated by reaction is easy to separate.

Description

technical field [0001] The invention relates to a preparation method of organic amine carbamate, belonging to the technical field of organic amine carbamate preparation. Background technique [0002] The carbamate of organic amine, at a certain temperature, can decompose organic amine and release carbon dioxide (CO 2 ), so it is often used as a polymer vulcanizing agent, widely used in fluorine rubber, polyacrylic rubber, ethylene propylene rubber, chlorosulfonated polyethylene, polyepichlorohydrin rubber, bromobutyl rubber and chlorinated butyl rubber Preparation, etc., and is often used to prepare elastomeric foam materials with excellent properties. The diamine carbamate in the organic amine carbamate is an important pharmaceutical intermediate. At the same time, it can also be used as a reaction substrate of carbon dioxide-based polyurea, and carbon dioxide-based polyurea with good mechanical properties, weather resistance and chemical resistance can be prepared throug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C271/02C07C269/00
CPCY02P20/54
Inventor 应忠赵凤玉程海洋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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