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Reversible crosslinked polycaprolactone/polyethylene glycol with shape memory function, and preparation method thereof

A technology of polyethylene glycol and polycaprolactone, which is applied in the field of reversible cross-linked polycaprolactone/polyethylene glycol and its preparation, can solve the problems of limiting the application of reversible cross-linking, and achieve excellent triple shape memory performance , wide application prospects and mild reaction conditions

Inactive Publication Date: 2019-06-04
TIANJIN AGRICULTURE COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the photolytic crosslinking of coumarin compounds can only be realized to a certain extent, which greatly limits the application in the field of reversible crosslinking.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Will be capped with coumarin, the number of arms is 2.7, the relative molecular mass M n It is 1250g / mol polycaprolactone and capped with coumarin, the number of arms is 2, and the relative molecular mass is M n 8000g / mol polyethylene glycol was mixed in a mass ratio of 7:2, vacuumed to 21Pa to remove water and oxygen for 3.6 hours, then add 1,2-dichloroethane with a water content of 51ppm under nitrogen protection, and stir , after forming a homogeneous solution at room temperature, place it in the reactor with a power of 2210mW / cm 2 1. Illuminate for 45 minutes at a wavelength of 250 nm. After the reaction is completed, remove the solvent. The resulting product shape fixation rate R f1 86.9%, R f2 98.2%, shape recovery rate R r1 89.7%, R r2 89.4% after reversible cross-linking R' f1 84.1%, R' f2 96.7%, shape recovery rate R' r1 87.2%, R' r2 was 82.5%.

Embodiment 2

[0031] Will be capped with coumarin, the number of arms is 2, the relative molecular mass M n It is 610g / mol polycaprolactone and end-capped with coumarin, the number of arms is 2, and the relative molecular mass is M n 2000g / mol polyethylene glycol was mixed in a mass ratio of 5:5, vacuumed to 30Pa to remove water and oxygen for 1.0 hour, then added chloroform with a water content of 30ppm under nitrogen protection, stirred, and formed a uniform mixture at room temperature After the solution is placed in the reactor, the power is 1mW / cm 2 1. Illuminate for 60 minutes at a wavelength of 338nm. After the reaction is completed, remove the solvent. The resulting product shape fixation rate R f184.3%, R f2 90.3%, shape recovery rate R r1 87.2%, R r2 95.8% after reversible cross-linking R' f1 81.7%, R' f2 87.9%, shape recovery rate R' r1 82.1%, R' r2 was 80.2%.

Embodiment 3

[0033] Will be capped with coumarin, the number of arms is 2.2, the relative molecular mass M n It is 4190g / mol polycaprolactone and end-capped with coumarin, the number of arms is 2, the relative molecular mass M n 600g / mol polyethylene glycol was mixed at a mass ratio of 1:10, vacuumed to 33Pa to remove water and oxygen for 3.8 hours, and then add 1,2-dichloroethane with a water content of 95ppm under nitrogen protection, and stir , after forming a homogeneous solution at room temperature, place it in the reactor with a power of 790mW / cm 2 1. Illuminate for 80 minutes at a wavelength of 300nm. After the reaction is completed, remove the solvent. The resulting product shape fixation rate R f1 91.3%, R f2 86.7%, the shape recovery rate R r1 95.2%, R r2 93.1% after reversible cross-linking R' f1 90.2%, R' f2 83.0%, shape recovery rate R' r1 93.8%, R' r2 was 88.9%.

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Abstract

The invention discloses a reversible crosslinked polycaprolactone / polyethylene glycol with a shape memory function, and a preparation method thereof. The reversible crosslinked polycaprolactone / polyethylene glycol with the shape memory function is prepared from coumarin-terminated polycaprolactone and coumarin-terminated polyethylene glycol by a photocrosslinking process. The shape fixation rate Rf1 is 84.3-100%, the shape fixation rate Rf2 is 86.7-100%, the shape recovery ratio Rr1 is 87.2-100%, and the shape recovery ratio Rr2 is 86.2-100%; and the shape fixation rate R'f1 after reversible crosslinking is 81.7-98.9%, the shape fixation rate R'f2 after reversible crosslinking is 83.0-98.9%, the shape recovery ratio R'r1 after reversible crosslinking is 82.1-99.0%, and the shape recovery ratio R'r2 after reversible crosslinking is 80.2-98.7%. The invention also discloses the preparation method of the reversible crosslinked polycaprolactone / polyethylene glycol with the shape memory function. The reversible crosslinked polycaprolactone / polyethylene glycol with the shape memory function, prepared by the photocrosslinking process, has the advantages of excellent triple shape memory property, reversible crosslinking property, controllable crosslinking degree and biodegradability; and the preparation method adopting lights as a radiation source in a reaction has the advantages of mild reaction conditions, no need to add an initiator, few byproducts, easily available devices, simplicity in operation, and wide application prospects.

Description

technical field [0001] The invention relates to the technical field of preparation of reversible cross-linked polymers with shape memory function, in particular to reversible cross-linked polycaprolactone / polyethylene glycol with shape memory function and a preparation method thereof. Background technique [0002] With the advent of the era of intelligence, society's requirements for intelligent materials are increasing. As a member of intelligent materials, shape memory polymer materials can sense the external environment (temperature, light, electricity, force, etc.) , magnetic, etc.), and in response to this change, adjust the mechanical parameters in time and return to the original shape, which has important potential application value, and its research is gradually deepening. [0003] In recent years, due to the wide application of shape memory polymers in the biomedical field, especially in minimally invasive surgery and skeleton support, biodegradable shape memory pol...

Claims

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Application Information

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IPC IPC(8): C08L67/04C08L71/02C08J3/24
Inventor 张静静黄治强石军朱华玲
Owner TIANJIN AGRICULTURE COLLEGE
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