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Preparation method of hydrolysis-resistant hyperbranched polycaprolactone

A technology of polycaprolactone and hyperbranched polyether, which is applied in the field of biodegradable materials, can solve the problems of metal residues, complex preparation process of hyperbranched polycaprolactone, fast hydrolysis speed, etc., and achieve excellent processing performance and reaction The effect of controllable activity and slowing down the hydrolysis rate

Active Publication Date: 2022-06-07
SHANDONG INOV NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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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] 150.0 g of ditrimethylolpropane, phosphazene base (t-BuP 4 ) 3.0g, transferred to the autoclave, heated to 115°C for 1h after nitrogen replacement, and 1950g of 3-ethyl-3-hydroxymethyl butylene oxide was added dropwise, and the pressure in the control reaction process was less than 0.4MPa, and the reaction The temperature was set at 115 °C, the feeding time was 14 h, the internal pressure was 4 h after the feeding was completed, and the temperature was lowered and discharged after 1 h of monomer removal to obtain a yellowish liquid. The hyperbranched polyether polyol 7g prepared by the reaction, phosphazene base (t-BuP 4 ) 0.35g and ε-caprolactone 63g were added to a 200mL eggplant-shaped reaction flask, replaced with nitrogen three times, and sealed with a rubber stopper. Using a syringe, 50mL of anhydrous toluene was added, and the reaction flask was placed in an oil bath at 120°C for 10h. After the reaction, the reaction flask was quenched in liquid nitrogen to term...

Embodiment 2

[0030] 75.0 g of bis-trimethylolpropane, 82.4 g of bis-pentaerythritol, phosphazene base (t-BuP 2 ) 5.5g, transferred to the autoclave, heated to 110°C for 1h after nitrogen replacement, and 1830g of 3-methyl-3-hydroxymethyl butylene oxide was added dropwise, and the pressure in the control reaction process was less than 0.4MPa, and the reaction The temperature was set at 120°C, the feeding time was 13h, the internal pressure was 4h after the feeding was completed, and the temperature was lowered and discharged after 1h of monomer removal to obtain a yellowish liquid. 6.5 g of hyperbranched polyether polyol obtained by the reaction, phosphazene base (t-BuP 2 ) 0.33g and ε-caprolactone 62.5g were added to a 200mL eggplant-shaped reaction flask, replaced with nitrogen three times and sealed with a rubber stopper, and 55mL of anhydrous toluene was added with a syringe, and the reaction flask was placed in an oil bath at 110°C for 11h. After the reaction, the reaction flask was q...

Embodiment 3

[0033] 114.1 g of mannitol, phosphazene base (t-BuP 4 ) 5.0g, transferred to the autoclave, heated to 110 DEG C for 1h after nitrogen replacement, and 2336g of 3,3-dimethylol butylene oxide was added dropwise, the pressure in the control reaction process was less than 0.4MPa, and the reaction temperature was set to Set the temperature at 110 °C, the feeding time is 16 h, the internal pressure is 5 h after the feeding is completed, the temperature is lowered after 1 h of monomer removal, and a yellowish liquid is obtained. 8.0 g of the hyperbranched polyether polyol obtained by the reaction, phosphazene base (t-BuP 2 ) 0.34g and ε-caprolactone 72.0g were added to a 200mL eggplant-shaped reaction flask, replaced with nitrogen three times, and sealed with a rubber stopper, and 70mL of anhydrous toluene was added with a syringe, and the reaction flask was placed in an oil bath at 115°C for 14h. After the reaction was completed, the reaction flask was quenched in liquid nitrogen t...

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Abstract

The invention belongs to the technical field of biodegradable materials, and in particular relates to a preparation method of hydrolysis-resistant hyperbranched polycaprolactone. The method comprises the following steps: (1) mixing a hydroxyl-containing compound with a phosphazene catalyst, and then reacting with an epoxy compound to prepare a hyperbranched polyether polyol; (2) using the hyperbranched polyether polyol as a macroinitiator, The ring-opening polymerization of caprolactone is continuously initiated under the action of the nitrile catalyst to prepare hyperbranched polycaprolactone. The synthesis process of the present invention is simple, the reactivity is controllable, and the prepared hyperbranched polycaprolactone has the advantages of no metal residue, excellent processing performance, controllable branching degree and hydrolysis resistance, further broadening the application of polycaprolactone materials in biomedicine field applications.

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 topology, the molecular chain entanglement and disentanglement process is more complex, 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 efficiency is higher when it i...

Claims

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Application Information

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Patent Type & Authority Patents(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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