Preparation method of polyvinyl alcohol/hydroxyapatite (PVA/HA) composite microspheres

A technology of hydroxyapatite and composite microspheres, which is applied in the direction of microsphere preparation, microcapsule preparations, skin care preparations, etc., can solve performance limitations and other problems, and achieve easy operation, high degree of spheroidization, and high dispersion Effect

Inactive Publication Date: 2017-11-24
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of polyvinyl alcohol / hydroxyapatite composite microspheres to solve the problem of performance limitations when PVA and HA are used alone

Method used

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  • Preparation method of polyvinyl alcohol/hydroxyapatite (PVA/HA) composite microspheres
  • Preparation method of polyvinyl alcohol/hydroxyapatite (PVA/HA) composite microspheres
  • Preparation method of polyvinyl alcohol/hydroxyapatite (PVA/HA) composite microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0068] Under the condition of water bath at 90°C, dissolve the PVA124 particles in 10mL deionized water to prepare a 7% PVA solution. After cooling the solution to room temperature, 0.175 g of hydroxyapatite powder and an appropriate amount of concentrated hydrochloric acid were added thereto. Stir well at room temperature to completely dissolve the hydroxyapatite. The resulting solution was added dropwise to 100 mL of soybean oil containing Span 80 as a surfactant for dispersion, followed by adding glutaraldehyde for crosslinking. After 1 hour of cross-linking, an appropriate amount of NaOH solution was added to the emulsion system, and the stirring was continued for 2 hours to regenerate HA and deposit it into the PVA matrix in situ. The obtained product is centrifuged, washed repeatedly with acetone and water, and then placed in the air at room temperature to obtain PVA / HA composite microspheres with a theoretical content of HA of 20%.

Embodiment 2

[0070] Under the condition of water bath at 90°C, dissolve the PVA124 particles in 5mL deionized water to prepare a 6% PVA solution. After the solution was cooled to room temperature, 0.176g of calcium nitrate tetrahydrate, 0.16g of disodium hydrogen phosphate dodecahydrate and concentrated nitric acid were added thereto, and an acidic PVA solution containing calcium ions and phosphate ions was formed after thorough stirring. The resulting solution was added dropwise to 100 mL of liquid paraffin containing Span 85 as a surfactant for dispersion, followed by adding glutaraldehyde for crosslinking. After 2 hours of cross-linking, an appropriate amount of ammonia water was added to the emulsion system, and the stirring reaction was continued for 4 hours, so that HA was generated and deposited into the PVA matrix in situ. The obtained product is centrifuged, washed repeatedly with ethanol and water, and then placed in the air at room temperature to obtain PVA / HA composite microsph...

Embodiment 3

[0072] Dissolve PVA1750 particles in 10 mL of deionized water at 80°C in a water bath to prepare a 10% PVA solution. After the solution was cooled to room temperature, 0.473g of calcium chloride, 0.338g of diammonium hydrogen phosphate and concentrated hydrochloric acid were added thereto, fully stirred to dissolve it completely, and an acidic PVA solution containing calcium ions and phosphate ions was formed. The solution was added dropwise to 100 mL of olive oil containing Span80-Tween 80 (mass ratio 8:2) for dispersion, and then glutaraldehyde was added for cross-linking. After cross-linking for 2 hours, add an appropriate amount of NaOH solution to the emulsion system and continue to stir for 2 hours to generate HA and deposit it into the PVA matrix in situ. The obtained product is centrifuged, washed repeatedly with acetone and water, and then placed in the air at room temperature to obtain a PVA / HA composite microsphere with a theoretical content of HA of 30%.

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Abstract

A preparation method of polyvinyl alcohol/hydroxyapatite (PVA/HA) composite microspheres belongs to preparation methods of composite water-in-oil emulsion system microspheres. PVA and HA precursors are used as raw materials to prepare a clear and transparent mixed solution; the clear and transparent mixed solution is dispersed into an oil phase containing a surfactant to form a homogeneous water-in-oil microemulsion; and the PVA/HA composite microspheres can be finally obtained by successive crosslinking reaction under acid-catalyzed conditions, HA deposition under alkaline conditions, product centrifugation, washing, drying and other processes. The method has the advantages of simple process, good repeatability, low energy consumption and low cost, and effectively solves the problems that inorganic nanoparticles are easy to agglomerate in the microspheres to cause uneven structures and poor comprehensive performances and the like. The composite microspheres prepared by the method have the advantages of regular morphology, high dispersibility, uniform microstructure, good biocompatibility, biological activity and adsorption performance, and can be used as drug carrier materials, bone repair materials, environmental water treatment materials, cosmetics or food additives and the like.

Description

technical field [0001] The invention relates to a preparation method of composite microspheres in a water-in-oil emulsion system, in particular to a preparation method of polyvinyl alcohol / hydroxyapatite composite microspheres. Background technique [0002] Hydroxyapatite (HA) is an inorganic biological material with similar composition, structure and properties to biological hard tissues (bones, teeth), and its chemical formula Ca 10 (PO 4 ) 6 (OH) 2 It has an exact chemical equivalent of Ca / P=1.67. HA material has the characteristics of good bone adhesion, bioactivity and excellent biocompatibility, even if HA degrades, it will not release toxic ions. However, HA materials have defects such as high brittleness, poor mechanical properties and difficult molding when used alone, so they cannot be well applied. [0003] Polyvinyl alcohol (PVA) is a synthetic polymer widely used in various biomedical fields (bone tissue, articular cartilage, artificial cornea, drug deliver...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14B01J20/26B01J20/28C02F1/28A61L27/50A61L27/54A61L27/12A61L27/16A61K8/81A61K8/24A61Q19/00C02F101/30C02F101/20
CPCA61K8/24A61K8/8129A61K2800/10A61L27/12A61L27/16A61L27/50A61L27/54A61L2430/02A61Q19/00B01J13/14B01J20/048B01J20/267B01J20/28021C02F1/288C02F2101/20C02F2101/308C08L29/04
Inventor 滕淑华薛珂
Owner CHINA UNIV OF MINING & TECH
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