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Carbon dioxide-based polyurea and its preparation method and application

A technology of carbon dioxide and polyurea, which is applied in the direction of single-component polyurea artificial filaments, etc., can solve the problems that cannot be further applied, low molecular weight of carbon dioxide-based polyurea, etc., and achieve good mechanical properties, thermal stability, and excellent performance

Active Publication Date: 2017-06-23
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the technical problem that the carbon dioxide-based polyurea prepared by the carbon dioxide-based polyurea preparation method in the prior art has a low molecular weight and cannot be further applied, and provides a carbon dioxide-based polyurea and its preparation method and application

Method used

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  • Carbon dioxide-based polyurea and its preparation method and application
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  • Carbon dioxide-based polyurea and its preparation method and application

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preparation example Construction

[0035]The preparation method of the carbon dioxide-based polyurea of ​​the present invention adopts continuous purging of carbon dioxide to react with the prepolymer, and the carbon dioxide can not only react with the prepolymer, but also take away the by-product water of the reaction, and the efficient removal of water inhibits the polyurea The hydrolysis reaction occurs, thereby increasing the molecular weight of polyurea. The reaction temperature is 120-400°C, the reaction pressure is 0.1-20MPa, and the reaction time is 0.5-50h. The specific method can be either melt polymerization or solid phase polymerization.

[0036] The method of melt polymerization: add the prepolymer directly into the reaction device, continuously purge carbon dioxide into the reaction device for 1-30min, remove the air in the reaction device, keep the carbon dioxide under 0.1-20MPa purge, and first heat the reaction device at 1-20°C / min to raise the temperature above the melting point of the prepo...

Embodiment 1

[0088] Add 40g of dodecamethylenediamine carbamate into a 100ml mechanically stirred reactor, seal it, and purge it with carbon dioxide gas for 5 minutes, keep the pressure at 1MPa, raise the temperature to 180°C, and increase the pressure after the temperature is stable to 11 MPa, react in a closed state for 9 hours, stop the reaction and release the pressure, and obtain the prepolymer as a white solid.

[0089] After the prepolymer slices are passed through a 20-mesh sieve, 25g of prepolymer slices are taken and added to the solid-phase reactor. First, the prepolymer slices are purged with carbon dioxide gas for 10 minutes, and the carbon dioxide is kept at normal pressure for continuous purging. Heating, firstly raise the temperature from room temperature to 180°C at 10°C / min, and after stabilizing for 5 minutes, continue to raise the temperature to 280°C at 1°C / min, keep the constant temperature, and continue to react for 0.5h under constant purge with carbon dioxide at nor...

Embodiment 2

[0096] Add 600g of nonanediamine into a 2L mechanically stirred reactor. After airtight, after purging with carbon dioxide gas for 3min, keep the pressure at 2MPa, and raise the temperature to 200°C. After the temperature is stable, raise the pressure to 12MPa, and react in an airtight state. After 12 hours, the reaction was stopped and the pressure was released to obtain the prepolymer as a white solid.

[0097] Transfer the prepolymer to a horizontal tank reactor, purge with carbon dioxide gas for 10 minutes, keep the carbon dioxide at normal pressure and continue to purge, start heating, first increase the temperature from room temperature to 200°C at 20°C / min, and stabilize for 5 minutes , continue to heat up to 270°C at 3°C / min, keep constant temperature, and keep carbon dioxide at normal pressure and continue to react for 10 hours. After the reaction is completed, cool and release the pressure and store it to obtain carbon dioxide-based polyurea with a number average mole...

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Abstract

The invention discloses carbon dioxide based polyurea and a preparation method and application thereof, belongs to the technical field of macromolecular materials, and solves the technical problem in the prior art that the molecular weight of the carbon dioxide based polyurea prepared by the preparation method of the carbon dioxide based polyurea is low, so that the carbon dioxide based polyurea cannot be further applied. The method comprises the following steps: adding a prepolymer or a sliced prepolymer in a reaction device, then continuously blowing carbon dioxide into the reaction device, and completely reacting amino in the prepolymer so as to generate the carbon dioxide based polyurea, wherein the reaction temperature is 120-400 DEG C, the reaction pressure is 0.1-20 MPa, and the reaction time is 0.5-50h. The carbon dioxide which is continuously blown in the method not only can take away a by-product, water, which is not eliminated in the polymerization of the carbon dioxide under a high pressure but also can be inserted into a reaction system, the average molecular weight of the prepared polyurea is between 5000-50000, and the properties are excellent.

Description

technical field [0001] The invention relates to a carbon dioxide-based polyurea and its preparation method and application, belonging to the technical field of polymer materials. Background technique [0002] Polyurea is a polymer material with good mechanical properties, chemical resistance, and heat resistance. It can be processed by film laying, injection molding, extrusion, etc. It can be used as fibers, lubricants, films, engineering plastics, Elastomers and coatings etc. are used. The existing polyurea preparation method is mainly formed by reacting diamine or polyamine with isocyanate, but isocyanate is highly toxic, so the operation method seriously affects human health. [0003] In order to solve the above technical problems, Chinese patent (publication number 102432871A) discloses a preparation method of polyurea, which uses amine compounds and excess CO 2 The condensation reaction is carried out in a closed reaction vessel to synthesize polyurea in one step. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G71/02D01F6/72
Inventor 应忠赵凤玉
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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