Preparation method of novel hydroxyapatite graft polylactic acid

A technology of hydroxyapatite and polylactic acid, which is applied in medical science, prosthesis and other directions, can solve the problems of easy agglomeration of hydroxyapatite, complex system and high cost, and achieves good biocompatibility, simple post-processing, and method. simple effect

Active Publication Date: 2015-09-23
HENAN INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a new method for preparing hydroxyapatite-grafted polylactic acid for the problems that hydroxyapatite is easy to agglomerate in the polylactic acid matrix, and the system is complicated and the cost is high during the preparation process.

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  • Preparation method of novel hydroxyapatite graft polylactic acid

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Comparison scheme
Effect test

Embodiment 1

[0018] The preparation method of the novel hydroxyapatite grafted polylactic acid of this embodiment is as follows:

[0019] (1) Dissolve 3-aminopropyltriethoxysilane (3.5mL, 0.015mol) in a mixed solution of ethanol and water (350mL), hydrolyze it at room temperature for 0.5h, and then add hydroxyapatite (HA) ( 4g, 0.01mol), stirred and reacted for 6h, then centrifuged the reacted product, dried at 50℃ for 12h, washed the dried product with ethanol, and then vacuum dried the washed product to moisture content <20ppm, get hydroxyapatite (SiHA) with -NH2 on the surface;

[0020] (2) Dissolve polylactic acid (0.9g, 0.01mol) containing terminal carboxyl groups in anhydrous dichloromethane, and then add N,N'-carbonyldiimidazole (CDI) (3.2g, 0.02mol) at 0℃ , The carboxyl group is activated for 0.5h under the condition of stirring speed of 300r / min, and then the hydroxyapatite with amino group on the surface (5.1g, 0.01mol) is added to the polylactic acid solution, and the reaction is 8h....

Embodiment 2

[0023] The preparation method of the novel hydroxyapatite grafted polylactic acid of this embodiment is as follows:

[0024] (1) Dissolve 3-aminopropyltriethoxysilane (4.7mL, 0.02mol) in a mixed solution (470mL) of ethanol and water, hydrolyze at room temperature for 2h, and then dissolve hydroxyapatite (4g, 0.01mol) ) Was added to the mixed solution, stirred and reacted for 8h, then centrifuged the reacted product, dried at 50℃ for 12h, washed the dried product with ethanol, and then vacuum dried the washed product to moisture content <20ppm, get hydroxyapatite (SiHA) with -NH2 on the surface;

[0025] (2) Dissolve polylactic acid (1.8g, 0.02mol) containing terminal carboxyl groups in anhydrous dichloromethane, then add N,N'-carbonyldiimidazole (9.6g, 0.06mol) to the polylactic acid solution, Activate the carboxyl group (activation temperature 0℃, activation time 2h), then add hydroxyapatite (5.1g, 0.01mol) with amino groups on the surface to the polylactic acid solution, stir and...

Embodiment 3

[0027] The preparation method of the novel hydroxyapatite grafted polylactic acid of this embodiment is as follows:

[0028] (1) Dissolve 3-aminopropyltriethoxysilane (5.80mL, 0.025mol) in a mixed solution of ethanol and water (580mL), hydrolyze at room temperature for 1h, and then dissolve hydroxyapatite (4g, 0.01mol) ) Add to the mixed solution, stir and react for 7h, then centrifuge the reacted product, dry at 50℃ for 12h, wash the dried product with ethanol, and then vacuum dry the washed product to moisture content <20ppm, get hydroxyapatite (SiHA) with -NH2 on the surface;

[0029] (2) Dissolve polylactic acid (2.7g, 0.03mol) containing terminal carboxyl groups in anhydrous dichloromethane, then add N,N'-carbonyldiimidazole (19.2g, 0.012mol) into the polylactic acid solution, Activate the carboxyl group (activation temperature 0℃, activation time 1h), and then add hydroxyapatite (5.1g, 0.01mol) with amino groups on the surface to the polylactic acid solution, stir and react a...

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Abstract

The invention discloses a preparation method of a novel hydroxyapatite graft polylactic acid. The preparation method comprises the following steps: (1) adopting 3-aminopropyltriethoxysilane (APTES) to modify -NH2 to the surface of HA; and (2) using N,N'-carbonyl di-imidazole (CDI) to activate an end carboxyl group on a polylactic acid molecular chain so as to form a reaction intermediate, then reacting the modified HA with the polylactic acid to obtain the hydroxyapatite graft polylactic acid (HA-PLLA), and thus effectively solving the problem that hydroxyapatite is easily clustered in a polylactic acid basal body. The process is relatively simple in preparation process, toxic small molecular substances are not introduced, the preparation method has the advantages of being low in cost, short in preparation time, mild in reaction conditions, green, environment-friendly and the like, and the application prospect is wide.

Description

Technical field [0001] The invention relates to a method for preparing a novel hydroxyapatite grafted polylactic acid, and belongs to the technical field of biomedical polymer materials. Background technique [0002] Hydroxyapatite (HA), which has a similar composition and structure to human bone tissue, and has good biocompatibility, is a recognized bone repair material, but it is not degradable and tough in vivo Poor. Polylactic acid (PLA) is a biodegradable material with good mechanical and physical properties. It can be decomposed into small molecules that are harmless to the human body through enzymatic hydrolysis in the organism, and has good biocompatibility. Since the 1980s, HA / PLA composite materials have been considered as ideal materials for bone repair and bone replacement. It combines the excellent properties between the two, thus having good mechanical properties, biocompatibility and degradability performance. [0003] However, through research, it has been found ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08K9/06C08K3/32A61L27/46A61L27/58
Inventor 于翔王延伟王娜杨柳田银彩辛长征魏媛
Owner HENAN INST OF ENG
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