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Preparation method of cross-linked polycaprolactone material

A technology of polycaprolactone and caprolactone is applied in the field of preparation of cross-linked polycaprolactone materials, which can solve the problem of the complexity of cross-linked polycaprolactone, the limitation of application of crystallization speed of cross-linked polycaprolactone, and the regulation of cross-linking. Polycaprolactone and other problems, to achieve the effect of inhibiting the crystallization rate

Active Publication Date: 2020-07-17
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there have been reports in the literature on the method of regulating the crystallization rate of linear polycaprolactone, but cross-linked polycaprolactone is more complicated than linear polycaprolactone, and the cross-linking structure of cross-linked polycaprolactone has a great influence on certain regulation. The crystallization speed of cross-linked polycaprolactone and the agent and cross-linked polycaprolactone are all affected, so it is not possible to directly refer to the crystallization speed of linear polycaprolactone to regulate the crystallization speed of cross-linked polycaprolactone, that is, how to regulate the crystallization speed of cross-linked polycaprolactone The crystallization rate of the
However, the crystallization speed of cross-linked polycaprolactone is too fast, which also limits its application.

Method used

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preparation example Construction

[0029] In order to effectively control the crystallization rate of cross-linked polycaprolactone material, the application provides a preparation method of cross-linked polycaprolactone material, the preparation method is due to the introduction of styrene-acrylonitrile copolymer (SAN), and by Electron beam irradiation can effectively regulate the crystallization speed of cross-linked polycaprolactone. Specifically, the embodiment of the present invention discloses a preparation method of a cross-linked polycaprolactone material, comprising the following steps:

[0030] Melt-blending polycaprolactone and styrene-acrylonitrile copolymer with a crosslinking agent, and then melt-blending to obtain polycaprolactone blend pellets;

[0031] Compressing the polycaprolactone composite pellets to obtain a polycaprolactone sheet;

[0032] The polycaprolactone sheet is irradiated with an electron beam to obtain a cross-linked polycaprolactone material.

[0033] In the process of prepar...

Embodiment 1

[0040] Put the PCL pellets and SAN pellets in a vacuum dryer at 40°C and 80°C for 12 hours, respectively; melt and blend the dried PCL and SAN in an internal mixer at 200°C and 40rpm at a mass ratio of 100:0 After 2 minutes, add 1.75% cross-linking agent TAIC, continue to melt and blend for 3 minutes, and discharge to obtain polycaprolactone blend pellets; press the blend pellets into a sheet with a thickness of 1 mm in a film pressing machine , the film pressing temperature is 120°C, melting for 2 minutes, depressurizing 3 times, and keeping the pressure at 10MPa for 1 minute; put the pressed sheet into a polyethylene bag, and irradiate it with electron beams, and the irradiation dose is 20KGy. Cross-linked polycaprolactone material.

Embodiment 2

[0042] The preparation process is the same as in Example 1, except that the mass ratio of PCL to SAN is 95:5, and the irradiation dose is 50KGy.

[0043] figure 1 The DSC curve of the cross-linked polycaprolactone material prepared for embodiment 1 and embodiment 2 is cooled at 7.65°C / min after melting; the crystallization peak temperature corresponding to the cooling curve in the figure is an important index reflecting the crystallization behavior of polycaprolactone, The crystallization peak temperature of the crosslinked polycaprolactone material (adding 5% SAN) prepared in embodiment 2 is lower than the crystallization peak temperature of embodiment 1 (pure PCL), illustrating that adding SAN can slow down the crystallization of crosslinked polycaprolactone Crystallization speed.

[0044] figure 2 The DSC curve of the cross-linked polycaprolactone material prepared for Example 1 and Example 2 isothermal crystallization at 38°C; through the isothermal crystallization test...

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Abstract

The invention provides a preparation method of a cross-linked polycaprolactone material, wherein the preparation method comprises the following steps: carrying out melt blending on polycaprolactone and a styrene-acrylonitrile copolymer, mixing with a cross-linking agent, and carrying out melt blending to obtain polycaprolactone blend granules; pressing the polycaprolactone blend granules to obtaina polycaprolactone sheet material; and carrying out electron beam irradiation on the polycaprolactone sheet to obtain the cross-linked polycaprolactone material. The styrene-acrylonitrile copolymer is introduced, so that the crystallization speed of the cross-linked polycaprolactone can be remarkably inhibited; furthermore, the crystallization speed and the crosslinking degree of the crosslinkedpolycaprolactone material can be further regulated and controlled by regulating the content of the styrene-acrylonitrile copolymer, the content of the crosslinking agent and the irradiation dose.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of a cross-linked polycaprolactone material. Background technique [0002] Polycaprolactone (PCL) is a new type of degradable polymer material. Polycaprolactone is widely used in various fields of the national economy because of its good biocompatibility, biodegradability, and compatibility with other polymers. Polycaprolactone has the characteristics of excellent mechanical properties, non-toxicity and biocompatibility, and it has great application value in biomedical fields such as drug delivery, surgical sutures, and porous tissue engineering scaffolds. [0003] It is well known that the crystallization behavior of polymers is closely related to the properties of polymers. If the crystallization speed is too slow and the performance requirements cannot be met within the expected time, it will consume time, waste financial resources, material re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/24C08J3/28C08J5/18C08L67/04C08L25/12C08K5/3492
CPCC08J3/24C08J3/246C08J3/28C08J5/18C08J2367/04C08J2425/12C08K5/34924
Inventor 王志刚徐翠张娟王学会
Owner UNIV OF SCI & TECH OF CHINA
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