Preparation method of polycaprolactone/hydroxyapatite composite biological ceramic material

A technology of composite bioceramics and hydroxyapatite, applied in medical science, prosthesis and other directions, can solve the problems of low interface strength, uneven particle distribution, low relative density, etc., to improve mechanical strength, high bioavailability, The effect of low reaction temperature

Inactive Publication Date: 2015-03-04
SUZHOU COSMETIC MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The melt blending method is simple and convenient to operate, but due to the certain viscosity of the polymer, it is difficult to fully disperse the filler particles inside the substrate, resulting in uneven particle distribution and low interface strength; the in-situ composite method can better improve the interface strength, but it is easy to Residual reaction impurities affect product performance; the solution casting method is to select a suitable solvent, add nano-inorganic particles to the polymer bulk solution, and remove the solvent after sufficient dispersion. The obtained composite material has good dispersion, but the relative density is low and the performance not guaranteed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Dissolve 10 g of polycaprolactone, 5 g of propylene glycol monolaurate and 1 g of n-butanol into 50 mL of toluene to prepare an oil phase solution of polycaprolactone, and seal it for later use;

[0022] (2) Add 2 mL of 6 mol / L calcium nitrate solution dissolved with 0.1 g NaOH and 2 mL of 3 mol / L dipotassium hydrogen phosphate solution to 25 mL of the oil phase solution prepared in step (1) respectively to form calcium ion emulsion and Phosphate ion emulsion, mix calcium ion emulsion and phosphate ion emulsion, and react at 30°C for 24 hours to form a mixed emulsion of polycaprolactone / hydroxyapatite;

[0023] (3), volatilize the toluene in the mixed emulsion prepared in step (2) in a fume hood, wash with water, dry, put the obtained powder into a spark plasma sintering chamber, apply an axial pressure of 20 MPa at both ends, and pump the powder. Vacuum, when the pressure in the sintering chamber reaches 60Pa, the heating starts, and the heating rate is 30℃ / min. Wh...

Embodiment 2

[0025] (1) Dissolve 30 g of polycaprolactone, 8 g of sorbitan sesquioleate and 1 g of n-amyl alcohol into 100 mL of chloroform to prepare an oil phase solution of polycaprolactone, and seal it for later use;

[0026] (2) Add 6 mL of 6 mol / L calcium nitrate solution dissolved with 0.5 g NaOH and 6 mL of 3 mol / L dipotassium hydrogen phosphate solution respectively into 50 mL of the oil phase solution prepared in step (1) to prepare calcium ion emulsion and Phosphate ion emulsion, mix calcium ion emulsion and phosphate ion emulsion, and react at 40°C for 32 hours to form a mixed emulsion of polycaprolactone / hydroxyapatite;

[0027] (3), volatilize the chloroform in the mixed emulsion prepared in step (2) in a fume hood, wash with water, dry, put the obtained powder into a spark plasma sintering chamber, apply an axial pressure of 30 MPa at both ends, and pump Vacuum, when the pressure of the sintering chamber reaches 60Pa, the heating starts, and the heating rate is 50℃ / min. When...

Embodiment 3

[0029] (1) Dissolve 60 g of polycaprolactone, 12 g of sodium dioctyl succinate sulfonate and 1 g of n-propanol into 200 mL of dichloromethane to prepare an oil phase solution of polycaprolactone, and seal it for later use;

[0030] (2) Add 12 mL of 6 mol / L calcium nitrate solution dissolved with 1 g NaOH and 12 mL of 3 mol / L dipotassium hydrogen phosphate solution to 100 mL of the oil phase solution prepared in step (1) respectively to form calcium ion emulsion and phosphoric acid. Radical ion emulsion, mix calcium ion emulsion and phosphate ion emulsion, react at 50 ℃ for 40 hours to form a mixed emulsion of polycaprolactone / hydroxyapatite;

[0031] (3), volatilize the dichloromethane in the mixed emulsion prepared in step (2) in a fume hood, wash with water, dry, put the obtained powder into a spark plasma sintering chamber, and apply an axial pressure of 30 MPa at both ends , vacuumize, start heating when the pressure of the sintering chamber reaches 60Pa, and the heating r...

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PUM

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Abstract

The invention provides a preparation method of a polycaprolactone/hydroxyapatite composite biological ceramic material. The preparation method comprises the following steps: (1) dissolving polycaprolactone, surfactants and cosurfactants in organic solvents to prepare oil phase solutions of polycaprolactone; (2) respectively adding calcium ion solutions and phosphate ion solutions to the oil phase solutions to prepare calcium ion emulsions and phosphate ion emulsions, mixing the calcium ion emulsions with the phosphate ion emulsions, and reacting at 30-60 DEG C for 24-48 hours to form a mixed emulsion of polycaprolactone/hydroxyapatite; (3) volatilizing the organic solvents in the mixed emulsion prepared in the step (2), washing and drying the mixed emulsion, and putting the obtained powder in a spark plasma sintering cavity to be sintered. The prepared composite biological ceramic material has the beneficial effects that the composite biological ceramic material has good dispersibility and high mechanical strength; the reaction temperature is relatively low, and hydroxyapatite can not be degraded, so that the composite biological ceramic material has higher bioavailability and is safer in production.

Description

technical field [0001] The invention relates to the field of biological materials, in particular to a preparation method of a polycaprolactone / hydroxyapatite composite biological ceramic material. Background technique [0002] Bone defects have always been a medical problem. At present, the ideal method is autologous or allogeneic bone transplantation. Autologous bone transplantation is widely regarded as the "gold standard" for measuring bone fusion. Although autologous bone transplantation has many advantages, such as adaptation to the regeneration of surrounding bone tissue, there are still some disadvantages, such as limited donors for autologous bone transplantation, secondary trauma, increased surgical difficulty, and a certain failure rate. Allogeneic bone sometimes fails to stimulate osteogenesis, and often induces adverse reactions. Researching new bone substitute products has become a common problem faced by medical workers and material workers. [0003] Hydroxya...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L27/12A61L27/54A61L27/18C04B35/447C04B35/622
Inventor 欧阳智琨喻国贞全春兰
Owner SUZHOU COSMETIC MATERIALS
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