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Modification method and application of hydroxyapatite

A technology of modification of hydroxyapatite, which is applied in the fields of fibrous fillers, medical science, dyeing and low-molecular-weight organic compounds, etc. It can solve the problems of low hydroxyl activity, low grafting rate, and no increase in flexural strength, etc. problem, to achieve the effect of high bone conduction and simple process

Active Publication Date: 2013-11-13
ZHEJIANG APELOA JIAYUAN BIOMEDICAL MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And the ring-opening polymerization of lactide can be initiated by the hydroxyl group on the surface of hydroxyapatite, so that a small amount of polylactic acid can be grafted on the surface of hydroxyapatite, and then compounded with polylactic acid polymers to obtain better reinforced composite materials. However, due to the low activity of hydroxyl groups on the surface of hydroxyapatite itself, the grafting rate is not high, resulting in unsatisfactory modification effects, especially when the content of hydroxyapatite is as high as 10% or more. The flexural strength is low Polylactic acid polymer matrix material
For this reason, literature reports (Biomacromolecules2005, 6, 1193-1199) react lactic acid with hydroxyapatite first, and then use the hydroxyl groups on lactic acid to indirectly graft lactide, although adding 15wt% of hydroxyapatite can stretch The strength has been improved, but there is no report on its flexural strength enhancement. As a fracture fixation material, the flexural strength is an important indicator to measure whether its mechanical properties meet the clinical requirements.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 5.0g of nano-hydroxyapatite with a particle size of 100-120nm (refer to Materials Research Bulletin48(2013)1233-1238 for the preparation method), disperse it with 100ml of N,N dimethylformamide, add 0.5g of citric acid at 120°C Heat and stir for 6 hours, filter, wash and dry, and ultrasonically disperse in 100ml of xylene for 20 minutes with an ultrasonic power of 200W, and then heat to 100°C. Take D,L-lactide 2.5g, use 25ml xylene in N 2 After heating and dissolving at 120°C under protection, add it to the xylene dispersion of nano-hydroxyapatite, then add 0.0025g stannous octoate catalyst, and continue to 2 Heating and stirring at 120° C. under protection for 6 hours. After the reaction was completed and cooled to room temperature, it was filtered, washed with dichloromethane, and dried. Take 1.0g powder and keep it in a muffle furnace at 700°C for 4h, and the measured grafting rate is 7.3%.

[0029] Take 2.0g of the above-mentioned grafted nano-hydroxyapatite...

Embodiment 2

[0031] Take 5.0g of micron hydroxyapatite with a particle size of 3-5μm, disperse it with 200ml of N,N dimethylformamide, add 3.0g of citric acid, heat and stir at 120°C for 8 hours, filter, wash and dry, and dissolve in 100ml of xylene Ultrasonic dispersion for 30 minutes, the ultrasonic power is 300W, and then heated to 100°C. Take 5.0g of L-lactide, and use 50ml xylene in N 2 After heating and dissolving at 120°C under protection, add the above-mentioned xylene dispersion of micron hydroxyapatite, then add 0.0030g stannous octoate catalyst, and continue to 2 Heating and stirring at 120° C. under protection for 8 hours. After the reaction was completed and cooled to room temperature, it was filtered, washed with dichloromethane, and dried. Take 1.0g of powder and keep it in a muffle furnace at 700°C for 4h, and the measured grafting rate is 8.5%.

[0032] Take 2.0g of the above-mentioned grafted micron hydroxyapatite, add it to poly-L-polylactic acid with a molecular weig...

Embodiment 3

[0034] Take 5.0 g of hydroxyapatite whiskers with a particle size of 10-20 μm, disperse them with 250 ml of N,N dimethylformamide, add 5.0 g of citric acid, heat and stir at 120°C for 6 hours, filter, wash and dry, and then dissolve them in 100 ml of dimethicone Ultrasonic disperse in toluene for 20 minutes, the ultrasonic power is 200W, and then heated to 100°C. Take D, L-lactide 7.5g, use 50ml xylene in N2 After heating and dissolving at 120°C under protection, add it to the xylene dispersion of the above-mentioned hydroxyapatite whiskers, then add 0.0030g of stannous octoate catalyst, and continue to 2 Heating and stirring at 120°C under protection for 10 hours. After the reaction was completed and cooled to room temperature, it was filtered, washed with dichloromethane, and dried. Take 1.0g powder and keep it in a muffle furnace at 700°C for 4h, and the measured grafting rate is 9.5%.

[0035] Take 2.0g of the above-mentioned grafted hydroxyapatite whiskers, add it to L-...

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Abstract

The invention discloses a modification method and application of hydroxyapatite. The modification method comprises the following steps of: dispersing hydroxyapatite powder in N,N-dimethylformamide, adding citric acid, and heating and stirring for reaction at 100-120 DEG C; filtering and then washing and drying; performing ultrasonic dispersion on the hydroxyapatite treated by use of the citric acid, then adding a xylene solution of lactide, and adding 0.05-0.2% of stannous octoate catalyst; heating to 120-140 DEG C under the protection of N2; continuously heating and stirring for a grafting reaction; and after the reaction, cooling to room temperature and washing and drying. By adopting the modification method disclosed by the invention, the grafting rate of the hydroxyapatite surface can be improved; by compounding the modified hydroxyapatite of high content with a polylactic acid high polymer, a better mechanical enhancement effect still can be realized; and the modified hydroxyapatite can be applied to a fracture fixing material.

Description

technical field [0001] The invention relates to a hydroxyapatite for reinforcing polylactic acid high polymers, and more specifically relates to a modification method and application of the hydroxyapatite. Background technique [0002] At present, in view of the shortcomings of clinically used polylactic acid polymers as internal fixation materials for fractures, such as insufficient mechanical properties, a large amount of acidic degradation products produced during degradation, which are not conducive to fracture healing, and lack of osteogenic activity, it will have good biocompatibility and osteogenic properties. It is a good idea to improve the performance of polylactic acid materials with conductive hydroxyapatite. It can not only achieve the purpose of strengthening and toughening, but also use the slightly alkaline characteristics of hydroxyapatite itself to slow down the polylactic acid. During the degradation process of lactic acid materials, a large amount of acid...

Claims

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Application Information

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IPC IPC(8): C09C1/02C09C3/08C08L67/04C08K9/04C08K3/32A61L31/12A61L31/14
Inventor 蒋柳云华菲蒋立新伍春林吴侃熊成东庞秀炳
Owner ZHEJIANG APELOA JIAYUAN BIOMEDICAL MATERIAL
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