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Preparation of amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing material

A technology of hydroxyapatite and polyaryletherketone, which is applied in the direction of additive processing, etc., can solve problems such as single method, poor solubility of PEEK, and unsatisfactory uniformity

Active Publication Date: 2021-11-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are no polar groups on the PEEK molecular chain, the interaction with bioactive fillers is weak, and the solubility of crystalline PEEK is poor, so hydroxyapatite can only be blended by high temperature melting, which is a single and blending method. The uniformity is not ideal

Method used

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  • Preparation of amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing material
  • Preparation of amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing material
  • Preparation of amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing material

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preparation example Construction

[0008] The invention discloses a method for preparing an amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing material, the method comprising:

[0009] Step 1: taking amorphous polyarylether ketone and / or amorphous polyarylether sulfone powder and hydroxyapatite co-dissolved in a polar aprotic solvent to form a viscous liquid, then stirring, and ultrasonic treatment at the same time;

[0010] Step 2: Precipitate the viscous liquid obtained in Step 1 in a solution with a volume ratio of ethanol to water of 5: (1-10) (preferably 5: (4-6)), and filter and pulverize the precipitate , and repeatedly boiled and washed with deionized water 5 to 10 times (preferably 6 to 8 times), dried in a vacuum oven at 100 to 160°C (preferably 120 to 150°C) for 10 to 24h (preferably 18 to 24h), That is, the amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing composite material after preliminary blending is obtained;

[0011] Step 3: Melt and extrude the amorphous poly...

Embodiment 1

[0024] Add phenolphthalein (the structure is shown in (a) above, the same below) (400mmol), 2,6-dichlorobenzonitrile (280mmol), 4,4'-difluorobenzophenone (120mmol), 4 - Fluorobenzophenone (12mmol), potassium carbonate (480mmol), sulfolane (600g), toluene (120ml), under the protection of nitrogen, heat the above mixture to 150°C while stirring to azeotropically remove water, keep the temperature for 3h, remove Toluene and water, continue to heat to 210 ° C for 3.5 hours, stop heating, transfer the reactant to a solution with a volume ratio of ethanol and water of 1:1 for precipitation, the precipitate is filtered, crushed, and repeatedly boiled and washed with deionized water Inorganic salts and residual solvents were removed six times, and dried in a vacuum oven at 150°C for 24 hours to obtain a polymer powder with the structure (II), which was verified by H NMR and IR spectroscopy.

[0025] Take 100g of amorphous polyaryletherketone (structure as shown in formula II) powder, ...

Embodiment 2

[0030] Take 100 g of amorphous polyarylether ketone (structure as shown in formula II) powder prepared in Example 1 and 5 g of hydroxyapatite, dissolve them in 500 ml of N,N-dimethylacetamide, stir, and make a viscous Thick liquid, then high-speed stirring at 8000rpm, and ultrasonic vibration at 60KHz frequency at the same time, the processing time is 60min. Then the obtained viscous liquid is precipitated in a solution with a volume ratio of ethanol and water of 1:1, the precipitate is filtered, crushed, and repeatedly boiled and washed with deionized water for 6 times to remove the residual solvent, and then heated in a vacuum oven at 150°C After drying for 24 hours, the amorphous polyaryletherketone-hydroxyapatite 3D printing composite material after preliminary blending was obtained; then, the composite material powder obtained by the solution method was melt-extruded in a twin-screw at 350 °C, and the screw speed was 100rpm, and under the action of the traction device, a ...

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Abstract

The invention discloses a preparation method of an amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing composite material, a blending mode of combining a solution method and a melting method is adopted, the method comprises the following steps: firstly, co-dissolving a polyaryletherketone (sulfone)-hydroxyapatite mixture in a polar aprotic solvent, and carrying out high-speed stirring and ultrasonic concussion on the mixture, peforming post-treatment to obtain composite material powder and then performing twin-screw melt extrusion so that hydroxyapatite is more uniformly distributed in a resin matrix. The cyano group has strong polarity, so that the acting force between matrix resin and hydroxyapatite can be enhanced, and the compatibility between the composite materials is improved. According to the preparation method of the amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing composite material, the biocompatibility between the resin matrix and the inorganic filler is enhanced, and the biological activity of the resin is improved.

Description

technical field [0001] The invention discloses a method for preparing an amorphous polyaryletherketone (sulfone)-hydroxyapatite 3D printing composite material, belonging to the technical field of 3D printing composite materials. Background technique [0002] In recent years, 3D printing technology has been more and more widely used in the medical field, especially in the field of artificial bone manufacturing, with its advantages of fast forming speed, high precision, high strength, and individualization. The high-performance resin polyaryletherketone has the advantages of excellent wear resistance, biocompatibility, chemical stability, and mechanical properties close to human bone. It is an ideal artificial bone replacement material and is suitable for long-term implantation in the human body. [0003] Among them, polyetheretherketone (PEEK) is a relatively mature 3D printing artificial bone material. However, the bioactivity and biocompatibility of PEEK resin itself are p...

Claims

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Application Information

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IPC IPC(8): C08L71/10C08L81/06C08K3/32B33Y70/10
CPCC08K3/32B33Y70/00C08K2003/325C08L71/00C08L81/06
Inventor 周光远王红华张兴迪王志鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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