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Preparation method of high-purity polydioxanone

A poly-dioxanone and high-purity technology, which is applied in the field of preparation of high-purity poly-dioxanone, can solve the problems of reduction and high residual amount of PDO monomer, and achieve the effect of reducing residual

Inactive Publication Date: 2019-01-01
南京普立蒙医疗科技有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Purpose of the invention: Aiming at the problem of high residual amount of PDO monomer in PPDO prepared by the existing method, the present invention provides a method for preparing high-purity polydioxanone, which can make the content of PDO monomer in the product PPDO Significant reduction in residue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The p-dioxanone (PDO) monomer and stannous octoate catalyst are mixed in a mass ratio of 300:1, heated to 140°C under the protection of vacuum or inert gas, and after reaction for 48 hours, the temperature is raised to 160°C. After being evacuated for 8 hours under a vacuum of <10 Pa, and then cooled to room temperature, the residual amount of PDO monomer in the PPDO polymer was measured to be 1.5 wt%.

Embodiment 2

[0022] The p-dioxanone (PDO) monomer and stannous octoate catalyst were mixed in a mass ratio of 500:1, heated to 120°C under vacuum or inert gas protection, and after 36 hours of reaction, the temperature was raised to 165°C. After being evacuated under a vacuum of <10 Pa for 10 hours, it was cooled down to room temperature, and the residual amount of PDO monomer in the PPDO polymer was measured to be 3 wt%.

Embodiment 3

[0024] The p-dioxanone (PDO) monomer and stannous octoate catalyst are mixed at a mass ratio of 200:1, and heated to 100°C under the protection of vacuum or inert gas. After 72 hours of reaction, the temperature is raised to 170°C. After evacuating for 10 hours under a vacuum of <10 Pa, it is cooled to room temperature. Take out the reacted PPDO and break it into particle size After fine particles of <2 mm, they were extracted with toluene at 110°C for 10 hours, washed with anhydrous ether, and dried in vacuum for 24 hours. The residual PDO monomer in the PPDO polymer was measured to be 0.5 wt%.

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Abstract

The invention discloses a preparation method of high-purity polydioxanone (PPDO). The preparation method comprises the following steps: (1) mixing a dioxanone monomer and a stannous octoate catalyst;carrying out ring-opening polymerization reaction under the protection of vacuum or inert gas; after raising the temperature, raising the temperature to be higher than a melting point of polydioxanone; carrying out gas pumping treatment in vacuum and cooling to room temperature; (2) taking out a reaction product to obtain the high-purity polydioxanone. In step (2), after the product obtained by reaction is taken out, the product can be crushed into small grains and then is extracted through boiled toluene; after extraction is finished, washing and vacuum drying are carried out. According to the preparation method disclosed by the invention, PPDO purification treatment is carried out for two times in PDO ring-opening polymerization reaction and after the reaction, so that residues of the PDO monomer can be greatly reduced; the residual amount of the PDO monomer in PPDO can be lower than 1 percent and the high-purity PPDO polymer is obtained.

Description

Technical field [0001] The invention relates to a method for preparing high-purity poly(p-dioxanone), which belongs to the field of biomedical polymer materials. Background technique [0002] Poly-p-dioxanone (PPDO) has been widely used in biomedical fields such as surgical sutures, hemostatic clips, and cosmetic lifting threads due to its good strength, biocompatibility and biodegradability. PPDO is prepared by the ring-opening polymerization of dioxycyclohexanone (PDO) monomer. However, due to the high crystallinity of PPDO, PPDO is easy to form crystals during the ring-opening polymerization of PDO, which reduces the conversion rate of PDO monomer. The purity and molecular weight of PPDO decrease. [0003] According to literature reports, with stannous octoate as a catalyst, the monomer conversion rate of PDO ring-opening polymerization under different conditions is only 67% (US patent 5652331, WO9721753) and 79.4% (Macromolecules 2000, 33, 6982-6986). At present, the conversi...

Claims

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Application Information

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IPC IPC(8): C08G63/664C08G63/85C08G63/78C08G63/90
CPCC08G63/664C08G63/78C08G63/823C08G63/90
Inventor 何斌蒲雨吉张译心赵子付谢家银
Owner 南京普立蒙医疗科技有限公司
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