Preparation method of hydrolysis-resistant hyperbranched polycaprolactone

A technology of polycaprolactone and hyperbranched polyether, applied in the field of biodegradable materials, can solve the problems of complex preparation process of hyperbranched polycaprolactone, metal residues, fast hydrolysis speed and the like

Active Publication Date: 2021-05-11
SHANDONG INOV NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a preparation method of hydrolysis-resistant hyperbranched polycaprolactone, which solves the problems of complicated preparation process of hyperbranched polycaprolactone, metal residues and excessive hydrolysis speed.

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  • Preparation method of hydrolysis-resistant hyperbranched polycaprolactone

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Embodiment 1

[0027] Ditrimethylolpropane 150.0g, phosphazene base (t-BuP 4 ) 3.0g, transferred to a high-pressure reactor, replaced with nitrogen three times, then heated up to 115°C for dehydration for 1 hour, added dropwise 1950g of 3-ethyl-3-hydroxymethylbutylene oxide, and controlled the pressure during the reaction to be less than 0.4MPa. The temperature is set at 115°C, the feeding time is 14 hours, the internal pressure is 4 hours after the feeding is completed, and the temperature is lowered after 1 hour of monomer removal, and the material is discharged to obtain a yellowish liquid. The hyperbranched polyether polyol 7g that reaction is made, phosphazene base (t-BuP 4 ) 0.35g and ε-caprolactone 63g were added to a 200mL eggplant-shaped reaction bottle, nitrogen was replaced three times and then sealed with a rubber stopper, 50mL of anhydrous toluene was added using a syringe, and the reaction bottle was placed in an oil bath at 120°C for 10 hours. After the reaction, the reaction...

Embodiment 2

[0030] Ditrimethylolpropane 75.0g, dipentaerythritol 82.4g, phosphazene base (t-BuP 2 ) 5.5g, transferred to a high-pressure reaction kettle, replaced with nitrogen three times, then heated up to 110°C for dehydration for 1h, added dropwise 1830g of 3-methyl-3-hydroxymethylbutene oxide, and controlled the pressure during the reaction to be less than 0.4MPa. The temperature is set at 120°C, the feeding time is 13 hours, the internal pressure is 4 hours after the feeding is completed, the temperature is lowered and the material is discharged after 1 hour of monomer removal, and a slightly yellow liquid is obtained. The hyperbranched polyether polyol 6.5g that reaction is made, phosphazene base (t-BuP 2 ) 0.33g and 62.5g of ε-caprolactone were added to a 200mL eggplant-shaped reaction bottle, nitrogen was replaced three times and then sealed with a rubber stopper, 55mL of anhydrous toluene was added with a syringe, and the reaction bottle was placed in an oil bath at 110°C for 11...

Embodiment 3

[0033] Mannitol 114.1g, phosphazene base (t-BuP 4 ) 5.0g, transferred to a high-pressure reactor, replaced with nitrogen three times, then raised the temperature to 110°C for dehydration for 1 hour, added 2336g of 3,3-dimethylolbutylene oxide dropwise, controlled the pressure during the reaction to be less than 0.4MPa, and set the reaction temperature to Set at 110°C, the feeding time is 16 hours, the internal pressure is 5 hours after the feeding is completed, the temperature is lowered and the material is discharged after 1 hour of monomer removal, and a light yellow liquid is obtained. The hyperbranched polyether polyol 8.0g that reaction is made, phosphazene base (t-BuP 2 ) 0.34g and ε-caprolactone 72.0g were added to a 200mL eggplant-shaped reaction bottle, nitrogen was replaced three times and then sealed with a rubber stopper, 70mL of anhydrous toluene was added using a syringe, and the reaction bottle was placed in an oil bath at 115°C for 14 hours. After the reaction...

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Abstract

The invention belongs to the technical field of biodegradable materials, and particularly relates to a preparation method of hydrolysis-resistant hyperbranched polycaprolactone. The preparation method comprises the steps of (1) mixing a hydroxyl-containing compound with a phosphazene catalyst, and then reacting with an epoxy compound to prepare hyperbranched polyether polyol; and (2) taking the hyperbranched polyether polyol as a macromolecular initiator, and continuously initiating a ring-opening polymerization reaction of caprolactone under the action of a phosphazene catalyst to prepare the hyperbranched polycaprolactone. The synthesis process is simple, the reaction activity is controllable, the prepared hyperbranched polycaprolactone has the advantages of no metal residue, excellent processability, controllable branching degree and hydrolysis resistance, and the application of the polycaprolactone material in the biomedical field is further widened.

Description

technical field [0001] The invention belongs to the technical field of biodegradable materials, and in particular relates to a preparation method of hydrolysis-resistant hyperbranched polycaprolactone. Background technique [0002] As an aliphatic material, polycaprolactone is finally decomposed into carbon dioxide and water after being degraded by enzymes in animals and plants, and will not be enriched in organisms, which is in line with the development trend of "green chemistry". Compared with linear polycaprolactone, hyperbranched polycaprolactone has a special topological structure, and the molecular chain entanglement and disentanglement process is more complicated. It not only has excellent solubility, but also has a significantly lower melt viscosity than linear materials, and is widely used Used in toughening, plasticizing and coating materials and other fields. Because hyperbranched polycaprolactone has biocompatibility and more reactive groups, its loading efficie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/664C08G65/28
CPCC08G63/664C08G65/2609C08G65/2687
Inventor 李健戈欢李剑锋孙兆任王浩
Owner SHANDONG INOV NEW MATERIALS CO LTD
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