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
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[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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