A kind of biodegradable polybutylene succinate fumarate and preparation method thereof
A technology of butylene fumarate and polysuccinic acid is applied in the field of polymer materials, which can solve the problems of high crystallinity of PBS, complex reaction conditions, high intrinsic viscosity, etc., and achieves improved machining performance and simple post-processing. , the effect of high intrinsic viscosity
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Embodiment 1
[0036] In a 500ml three-necked flask, the molar ratio of maleic anhydride to 1,4-butanediol is 1:1.05-1:1.5, and the catalyst zirconium acetylacetonate is 500ppm, equipped with mechanical stirring, water separator, and condenser, and nitrogen gas Protection, esterification reaction at 160°C for 2-6h, transfer to a high-pressure reactor, heat up to 130°C, catalyst is palladium carbon, dosage 2%, pressure 4.0MPa, hydrogenation reaction 3-6h, remove the catalyst to obtain the product, add Fumaryl chloride undergoes double bond inversion, and the resulting product is polycondensed in a three-necked flask with a vacuum of 0.5 mmHg and a temperature of 250°C for 2-6 hours, and the intrinsic viscosity of the product is 0.80 dL / g.
Embodiment 2
[0038] In a 500ml three-neck flask, the molar ratio of maleic anhydride to 1,4-butanediol is 1:1.1, and the catalyst zirconium acetylacetonate is 500ppm, equipped with a mechanical stirrer, a water separator, and a condenser, and nitrogen protection, at 130°C Esterification reaction at -160°C for 2-6h, transfer to a high-pressure reactor, heat up to 130°C, the catalyst is Raney nickel, the dosage is 5%, the pressure is 4.0MPa, the hydrogenation reaction is 3-6h, the product is removed and the catalyst is added. Fumaryl chloride undergoes double bond inversion, and the resulting product is polycondensed in a three-necked flask with a vacuum of 0.5mmHg and a temperature of 250°C for 2-6h.
Embodiment 3
[0040] In a 500ml three-necked flask, the molar ratio of maleic anhydride to 1,4-butanediol is 1:1.1, and the catalyst zirconium acetylacetonate is 500ppm, equipped with a mechanical stirrer, a water separator, and a condenser, and nitrogen protection is introduced, and the temperature is 160°C Under the esterification reaction for 6 hours, transfer to a high-pressure reactor, heat up to 110-150 ° C, the catalyst is palladium carbon, the dosage is 2%, the pressure is 4.0 MPa, the hydrogenation reaction is 3-6 hours, and the catalyst is removed to obtain the product, and fumaryl chloride is added. The double bond is reversed, and the product obtained is in a three-necked flask with a vacuum of 0.5mmHg and a temperature of 250°C for 2-6 hours of polycondensation.
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