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Sheet hydroxyapatite/polylactic acid nanometer composite prepared through in-situ intercalation method

A technology of hydroxyapatite and nano-hydroxyapatite, which is applied in the field of biomedical materials, can solve problems such as the contradiction between strength and toughness, complicated preparation steps, and difficult dispersion of nanoparticles, and achieve good biocompatibility and simple preparation process , the effect of excellent interfacial compatibility

Inactive Publication Date: 2016-02-03
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems in the process of preparing nano-hydroxyapatite / polylactic acid composite materials by the traditional blending method, such as complicated preparation steps, difficult dispersion of nanoparticles, and contradiction between strength and toughness, the invention provides a method for preparing nano-hydroxyapatite / polylactic acid composite materials using in-situ composite intercalation technology. A new method for layered nano-hydroxyapatite / polylactic acid composite materials. The technical principle of the present invention is to improve the mechanical properties of composite materials by imitating the organic-inorganic layered alternating microstructure in natural shells and natural bones. The specific technical scheme is : Using the template method to prepare long-range ordered nano-layer flake hydroxyapatite, using lactide monomer as raw material, through in-situ polymerization intercalation technology, the lactide molecules are ring-opened and polymerized between the hydroxyapatite layers into polylactic acid to form an organic-inorganic nanocomposite with a shell-like structure

Method used

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  • Sheet hydroxyapatite/polylactic acid nanometer composite prepared through in-situ intercalation method
  • Sheet hydroxyapatite/polylactic acid nanometer composite prepared through in-situ intercalation method
  • Sheet hydroxyapatite/polylactic acid nanometer composite prepared through in-situ intercalation method

Examples

Experimental program
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Effect test

Embodiment 1

[0019] (1) Dissolve 1.88mmol of lauric acid and 50mmol of calcium nitrate tetrahydrate in 60ml of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1), and stir evenly at 37°C.

[0020] (2) Weigh 30mmol of diammonium hydrogen phosphate and add it to 60ml of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1), pour the prepared diammonium hydrogen phosphate solution into a constant pressure dropping funnel, and place it at 37°C under magnetic force Slowly add dropwise at a speed of 2ml / min into the mixed solution of calcium nitrate tetrahydrate and lauric acid under stirring.

[0021] (3) After the above mixed solution was stirred for 0.5 hours, 40ml of 2M sodium hydroxide ethanol aqueous solution (the volume ratio of ethanol to water was 1:1) was added dropwise, reacted at 37°C for 2 hours, heated in water at 100°C for 8h, and mixed with ethanol and After washing with hot water and suction filtration for 3 times, dry it.

[0022] (4) Take ...

Embodiment 2

[0025] (1) Dissolve 3.76mmol of lauric acid and 50mmol of calcium nitrate tetrahydrate in 60ml of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1), and stir evenly at 37°C.

[0026] (2) Weigh 30mmol of diammonium hydrogen phosphate and add it to 60ml of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1), pour the prepared diammonium hydrogen phosphate solution into a constant pressure dropping funnel, and place it at 37°C under magnetic force Slowly add dropwise at a speed of 3ml / min into the mixed solution of calcium nitrate tetrahydrate and lauric acid under stirring.

[0027] (3) After the above mixed solution was stirred for 1 hour, 40ml of 2M sodium hydroxide ethanol aqueous solution (the volume ratio of ethanol to water was 1:1) was added dropwise, reacted at 37°C for 4 hours, heated in water at 100°C for 12h, and mixed with ethanol and After washing with hot water and suction filtration for 4 times, dry.

[0028] (4) Take 100 p...

Embodiment 3

[0031] (1) Dissolve 18.8mmol of lauric acid and 50mmol of calcium nitrate tetrahydrate in 60ml of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1), and stir evenly at 37°C.

[0032] (2) Weigh 30mmol of diammonium hydrogen phosphate and add it to 60ml of ethanol aqueous solution (the volume ratio of ethanol to water is 1:1), pour the prepared diammonium hydrogen phosphate solution into a constant pressure dropping funnel, and place it at 37°C under magnetic force Slowly add dropwise at a speed of 4ml / min into the mixed solution of calcium nitrate tetrahydrate and lauric acid under stirring.

[0033] (3) After the above mixed solution was stirred for 1 hour, 40ml of 2M sodium hydroxide ethanol aqueous solution (the volume ratio of ethanol to water was 1:1) was added dropwise, reacted at 37°C for 6 hours, heated in water at 100°C for 24h, and mixed with ethanol and After washing with hot water and suction filtration for 5 times, dry.

[0034] (4) Take 100 p...

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Abstract

The invention provides a new method for preparing a sheet nanometer hydroxyapatite / polylactic acid composite through an in-situ compound intercalation method for solving the problems that a traditional blending method is complex in preparation step, poor in nanoparticle dispersion, contradictory in strength and toughness and the like. The method includes the steps of preparing long-range orderly nanometer sheet hydroxyapatite with lauric acid as template agent, conducting ring opening polymerization on lactide molecules between layers of hydroxyapatite to form polylactic acid through the in-situ polymerization intercalation method with lactide monomers as the raw material, and forming the organic and inorganic nanometer composite of a nacre-like structure. Breakthrough is achieved on the aspects of strength and toughness of the composite at the same time, the tensile strength of the composite with addition amount of 5% is increased by 40% compared with that of pure polylactic acid, and the elongation at break is increased by 30%. The preparation process is simple, surface treatment does not need to be conducted on hydroxyapatite, no substances with biological toxicity are introduced in the whole process, and biological compatibility is high.

Description

technical field [0001] The invention belongs to the field of biomedical materials, and in particular relates to an in-situ intercalation method for preparing a layered hydroxyapatite / polylactic acid nanocomposite material. Background technique [0002] Due to its good biocompatibility, bioactivity and osteoinductivity, hydroxyapatite has been widely used as an excellent artificial bone material and tissue material, but due to its low strength, toughness and poor mechanical properties The disadvantages limit its wide application, and it can only be used for non-bearing small implants, such as ear bones, artificial dentary bones, filling bone defects, etc., which greatly limits its wide use as human biomaterials. Polylactic acid is a biodegradable material with good biocompatibility and biodegradability. However, its hydrophilicity is not enough, and its adhesion to cells is weak, and the degraded products are easy to cause inflammation. Combining hydroxyapatite and polylact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08K3/32A61L27/40A61L27/50C01B25/32B82Y30/00
Inventor 左桂福孙海娜陈菲王宇璐沈毅
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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