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Preparation method for hydroxylapatite hydrogel used for bone regeneration

A technology of hydroxyapatite and hydrogel, which is applied in the fields of medical science and prostheses, can solve the problems of poor stability of hydroxyapatite hydrogel, difficulty in stable and uniform dispersion, and no formation of covalent bonds. The effect of large selection range, low cost, good biocompatibility and toughness

Active Publication Date: 2013-11-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above invention patents only disperse hydroxyapatite in the hydrogel matrix by mixing. This effect is only a weak interaction of physical entanglement of polymer molecular chains, and no covalent bonds are formed, making it difficult to disperse stably and uniformly. in a hydrogel matrix
Chinese patents CN101422632A and CN102020777A disclose a preparation method of hydroxyapatite / sodium alginate nanocomposite materials, calcium hydroxide and phosphoric acid aqueous solution are mixed according to the stoichiometric ratio of calcium / phosphorus in hydroxyapatite, and mixed with alginic acid Sodium hydrogel undergoes in situ composite reaction, and the cross-linking reaction with sodium alginate is achieved by adding calcium chloride, forming a three-dimensional network structure similar to natural bone, although the formation of hydroxyapatite and sodium alginate hydrogel matrix Physical cross-linking, but this physical bonding formed by electrostatic adsorption is easily destroyed, resulting in poor stability of this hydroxyapatite hydrogel
[0004] At present, there is no report of using hydroxyapatite as a cross-linking point to prepare hydrogel materials through chemical covalent bonding, by constructing active functional groups on the surface of hydroxyapatite, and participating in the original free radical polymerization process of monomers Among them, the formation of chemical bonds can effectively enhance the mechanical properties of the hydrogel, so that the prepared hydroxyapatite hydrogel has excellent mechanical toughness, which makes up for the shortcomings of traditional hydroxyapatite, which are brittle and difficult to shape.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add 4g of hydroxyapatite nanoparticles to 80g of petroleum ether, stir at 500 rpm for 30 minutes, add 0.8g of n-propylamine and 4g of vinyltrimethoxysilane, and react at 50°C for 240 minutes; after the reaction, cool to 10°C, wash with petroleum ether, and dry to obtain functional hydroxyapatite nanoparticle powder.

[0027] (2) Add 1g of functional hydroxyapatite nanoparticles obtained in step (1), 4g oligoethylene glycol methyl ether methacrylate, 0.04g potassium persulfate, 0.04g N,N,N',N' - Add tetramethylethylenediamine to 20 g of deionized water, stir and disperse evenly to obtain a hydrogel pre-polymerization solution, and then polymerize at 25° C. for 24 hours to prepare a hydroxyapatite hydrogel with biological activity.

Embodiment 2

[0029] (1) Add 2.5g of hydroxyapatite microparticles to 80g of petroleum ether, stir at 500 rpm for 60 minutes, add 0.5g of n-propylamine and 2.5g of vinyl tris(β-methoxyethoxy ) silane, reacted at 60°C for 210 minutes; after the reaction, cooled to 10°C, washed with petroleum ether, and dried to obtain functional hydroxyapatite micron particle powder.

[0030] (2) Add 1g of functional hydroxyapatite microparticles obtained in step (1), 6g of 2-methyl-2-acrylate-2-(2-methoxyethoxy)ethyl ester, 0.05g of potassium persulfate, Add 0.05g of N,N,N',N'-tetramethylethylenediamine to 20g of deionized water, stir well and disperse evenly to obtain a hydrogel pre-polymerization solution, and then polymerize at 25°C for 48 hours to prepare a bioactive Hydroxyapatite hydrogel.

Embodiment 3

[0032] (1) Add 5 g of hydroxyapatite nanorods to 80 g of cyclohexane, stir at 800 rpm for 45 minutes, add 0.4 g of n-propylamine and 2 g of γ-methacryloxypropyltrimethoxysilane , and reacted at 80° C. for 60 minutes; after the reaction, cooled to 25° C., washed with cyclohexane, and dried to obtain functional hydroxyapatite nanorod powder.

[0033] (2) Add 0.8g of the functional hydroxyapatite nanorods obtained in step (1), 8g of polyethylene glycol diacrylate, 0.03g of sodium persulfate, and 0.06g of sodium thiosulfate into 20g of deionized water, and stir well Disperse evenly to obtain a hydrogel pre-polymerization solution, and then polymerize at 37° C. for 24 hours to prepare a hydroxyapatite hydrogel with biological activity.

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Abstract

The invention relates to a preparation method for a hydroxylapatite hydrogel used for bone regeneration. The preparation method comprises (1) a step of adding hydroxylapatite into an organic solvent, adding n-propylamine and a coupling agent, performing a reaction at 50-80 DEG C for 30-240 min to obtain a hydroxylapatite mixed solution, cooling to 10-30 DEG C after the reaction is finished, washing with washing liquid, and drying to obtain functional hydroxylapatite powder; and (2) a step of homogenously dispersing the functional hydroxylapatite powder, hydrophilic monomers, an initiator and a catalyst into a water solution to obtain hydrogel prepolymerization liquid, and then performing polymerization at 0-40 DEG C for 24-72 h to obtain the hydroxylapatite hydrogel used for bone regeneration. The preparation method is simple in technology and low in cost. The hydroxylapatite is homogenously dispersed in the hydrogel matrix. The hydroxylapatite hydrogel, as a tissue engineering implant material, can induce bone growth and promote bone healing, and has high application value.

Description

technical field [0001] The invention belongs to the field of preparation of functional hydrogels, in particular to a preparation method of hydroxyapatite hydrogels for bone regeneration. Background technique [0002] Hydroxyapatite is the main component of human hard tissues (such as nails, bones, teeth, etc.), has good biocompatibility and osteogenic activity, can form a firm combination with bone tissue, and provide a scaffold or template for bone growth. Therefore, hydroxyapatite is recognized as an excellent bioactive material. However, hydroxyapatite has defects such as fragility and low mechanical strength in application. If hydroxyapatite powder is directly filled in the body as a bone tissue repair material, its strength or toughness cannot meet the requirements of implant materials. Combining hydroxyapatite with polymer hydrogel can not only overcome the shortcomings of hydroxyapatite such as high brittleness and difficulty in forming, but also improve the biocompa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/28C08F222/20C08K9/06C08K9/04C08K3/32C08J3/24C08J3/075A61L27/16A61L27/12A61L27/52
Inventor 朱美芳夏梦阁刘丰维陈少华包爽
Owner DONGHUA UNIV
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