Long-chain branched poly(p-dioxanone) and preparation method thereof

A technology of polydioxanone and p-dioxanone, which is applied in the field of long-chain branched polydioxanone and its preparation, and can solve the problems of polymer high elasticity, impact strength, elongation at break, etc. Reduced mechanical properties, weakened polymer crystallinity, limited improvement of rheological properties, etc., to improve processing performance, easy to promote, and increase interaction effects

Active Publication Date: 2013-06-05
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since this technology uses double-terminal hydroxyl-terminated PPDO and three-arm hydroxyl-terminated PPDO to be prepared by chain extension in the process of preparing branched PPDO, it is easy to produce cross-linking, which causes certain difficulties in its molding process.
On the other hand, the long-chain branched polydioxanone prepared by this method has a limited improvement in rheological properties because the structural main body is a single p-dioxanone unit.
In addition, although increasing the degree of branching is conducive to increasing the melt strength of the polymer, it will also weaken the crystallinity of the polymer, which will reduce the mechanical properties of the polymer such as high elasticity, impact strength, and elongation at break. Will make the product subject to certain restrictions in practical application

Method used

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  • Long-chain branched poly(p-dioxanone) and preparation method thereof
  • Long-chain branched poly(p-dioxanone) and preparation method thereof
  • Long-chain branched poly(p-dioxanone) and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add trimethylolpropane and p-dioxanone in a molar ratio of 1:60 to the reaction vessel, raise the temperature to 80°C for 15 minutes under the protection of an inert gas, and then add the molar ratio of p-dioxanone to 1: 0.002 catalyst stannous octoate, continue to stir and react at 80°C for 48 hours, the crude product obtained after cooling is dissolved in phenol / tetrachloroethane with a volume ratio of 1:1, purified by methanol precipitation and dried to obtain the number average Polydioxanone (a-PPDO) with a molecular weight of 5234 and a star-shaped multi-armed hydroxyl group.

[0038] Add the obtained a-PPDO and benzyl-terminated hydroxyl-terminated polylactic acid with a number-average molecular weight of 2412 in a molar ratio of 1:1 into the reaction vessel, and then under the protection of an inert gas, put them in an oil bath at 150°C until the two are completely melted Afterwards, HDI was added in a ratio of 1:1.4 to a-PPDO and benzyl-terminated hydroxyl-termi...

Embodiment 2

[0040] Add trimethylolethane and p-dioxanone in a molar ratio of 1:10 to the reaction vessel, raise the temperature to 60°C for 20 minutes under the protection of an inert gas, and then add the molar ratio of p-dioxanone 1:0.001 catalyst triethylaluminum, continue to stir and react at 60°C for 24 hours, the crude product obtained after cooling is purified by the method described in Example 1 and then dried to obtain a-PPDO with a number average molecular weight of 1100.

[0041] Add the obtained a-PPDO and methyl-terminated hydroxyl-terminated polyethylene glycol with a number average molecular weight of 500 in a molar ratio of 1:1.2 into the reaction vessel, and then under the protection of an inert gas, in an oil bath at 110°C, wait for both After it is completely melted, add XDI which is 1:0.6 in terms of the number of moles of total hydroxyl groups in a-PPDO and methyl-terminated hydroxyl-terminated polyethylene glycol, and react for 1 hour to obtain long-chain branched pol...

Embodiment 3

[0043] Add pentaerythritol and p-dioxanone in a molar ratio of 1:1000 to the reaction vessel, raise the temperature to 80°C for 30 minutes under the protection of an inert gas, and then add dioxanone in a molar ratio of 1:0.001 Catalyst tetrabutyltitanium, continue to stir and react at 80°C for 48 hours, the crude product obtained after cooling is purified by the method described in Example 1 and then dried to obtain a-PPDO with a number average molecular weight of 100214.

[0044] The obtained a-PPDO and the phenyl-terminated hydroxyl-terminated polymethyl carbonate with a number average molecular weight of 11600 were added to the reaction vessel in a molar ratio of 1:1.5, and then under the protection of an inert gas, they were placed in an oil bath at 170°C for two After it is completely melted, add HMDI with a-PPDO and phenyl-terminated hydroxyl-terminated polydimethylcarbonate whose molar number of total hydroxyl groups is 1:1.2, and react for 1 hour to obtain long-chain b...

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Abstract

Long-chain branched poly(p-dioxanone) disclosed by the invention is prepared from star-branched hydroxyl-terminated poly(p-dioxanone) and monohydroxyl-terminated linear polymer by chain extension reaction with a coupling agent, wherein the star-branched hydroxyl-terminated poly(p-dioxanone) has number average molecular weight of 10<3>-10<5>; the monohydroxyl-terminated linear polymer has the number average molecular weight of 5*10<2>-1.5*10<4>; and the long-chain branched poly(p-dioxanone) has intrinsic viscosity of 0.5-4 dL/g, tensile strength of 25-50 MPa and elongation at break of 290-700%. The invention also discloses a preparation method of the long-chain branched poly(p-dioxanone). According to the long-chain branched poly(p-dioxanone) disclosed by the invention, the processing performance of a polymer is improved by long-chain branching, the problem of shaping processing difficulty caused by cross-linking easily occurring in a preparation process in the prior art is avoided, and the shearing viscosity and mechanical performance of the long-chain branched poly(p-dioxanone) are greatly improved.

Description

technical field [0001] The invention belongs to the technical field of modification of polydioxanone, and in particular relates to a long-chain branched polydioxanone and a preparation method thereof. Background technique [0002] Polydioxanone (PPDO), as an aliphatic polyester with excellent biodegradability and biocompatibility, has been successfully used in orthopedic repair materials, surgical sewing threads, etc., and has potential applications in Value in Drug Delivery Systems. However, the linear PPDO thermoplastics prepared by conventional synthesis methods have poor processability, showing very low melt strength, sensitive to temperature and shear, and difficult to process by methods such as extrusion, blow molding and foaming. To a certain extent, its scope of application is limited. [0003] In order to overcome the above shortcomings, people began to try to introduce long-chain branched structure into linear PPDO to improve its processing performance. Because ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/91C08G63/08
Inventor 陈思翀曾令羲刘明静王玉忠
Owner SICHUAN UNIV
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