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Silk fibroin/calcium phosphate bone cement composite material and preparation method thereof

A technology of calcium phosphate bone cement and silk fibroin, which is applied in the field of medical biological materials and preparation thereof, can solve the problems that affect the application of silk fibroin, the fibers are not easily dispersed uniformly, and have no injectability, etc., so as to improve the preparation working conditions and reduce the cost. , good biocompatibility

Inactive Publication Date: 2011-02-02
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese invention patent (CN1736492) discloses a silk fibroin hydroxyapatite composite material and its preparation method. Although the composite material obtained in this invention has good mechanical properties, it needs to be dried and solidified at a temperature of 110-130°C. , not injectable, not self-curing, not solidified in the body and accurately molded, it can only be used as an implant material, which greatly affects the application of silk fibroin in bone defect repair; in addition, the mechanical properties of its material are affected by the Influenced by the uniformity of hydroxyapatite distribution, the fiber has the disadvantage that it is not easy to disperse uniformly

Method used

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  • Silk fibroin/calcium phosphate bone cement composite material and preparation method thereof
  • Silk fibroin/calcium phosphate bone cement composite material and preparation method thereof
  • Silk fibroin/calcium phosphate bone cement composite material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0022] The preparation steps of the silk fibroin / calcium phosphate bone cement composite material provided by the present embodiment are as follows:

[0023] (1) Preparation of Tetracalcium Phosphate

[0024] Will (NH 4 ) 2 HPO 4 The solution is added dropwise to the Ca(NO 3 ) 2 4H 2 In the O solution, the pH value is kept above 9 during the dropwise addition. After the dropwise addition, continue to stir the reaction for 3 hours, and let it settle for 24 hours. According to the ratio of the Ca / P molar ratio of the entire system to 2.0, add dropwise to the above suspension at the same time. Ca(NO 3 ) 2 4H 2 O solution and (NH 4 ) 2 CO 3 After the dropwise addition of the solution, the aging reaction was continued for 24 hours and then filtered, and the filter cake was dried in an oven at 110° C. for 12 hours. Place the tetracalcium phosphate precursor synthesized by the above liquid phase reaction method in a high-temperature furnace, raise the temperature to 1500°C ...

Embodiment 2

[0034] The non-water-soluble silk fibroin protein powder was prepared according to the technical scheme of Example 1.

[0035] Will (NH 4 ) 2 HPO 4 The solution was added dropwise to Ca(NO 3 ) 2 4H 2 In the O solution, the pH value was kept above 9 during the dropwise addition. After the dropwise addition, continue to stir and react for 3 hours, and let it settle for 22 hours. According to the ratio of the Ca / P molar ratio of the entire system to 2.0, add dropwise to the above suspension at the same time Ca(NO 3 ) 2 4H 2 O solution and (NH 4 ) 2 CO 3 Solution, after the dropwise addition, continue the aging reaction for 22 hours and then filter, put the filter cake in a 110°C oven to dry for 12 hours, then place it in a high-temperature furnace, raise the temperature to 1500°C at a rate of 360°C / h, and keep it for 8 hours. Into nitrogen gas and quickly cooled to 1300°C and taken out, cooled to 100°C in air, then placed in a dry environment and cooled to room tempera...

Embodiment 3

[0039] The non-water-soluble silk fibroin protein powder was prepared according to the technical scheme of Example 1.

[0040] Will (NH 4 ) 2 HPO 4 The solution was added dropwise to Ca(NO 3 ) 2 4H 2 In the O solution, the pH value was kept above 9 during the dropwise addition. After the dropwise addition, continue to stir and react for 3 hours, and let it settle for 20 hours. According to the ratio of the Ca / P molar ratio of the entire system to 2.0, dropwise add Ca(NO 3 ) 2 4H 2 O solution and (NH 4 ) 2 CO 3 Solution, after the dropwise addition, continue the aging reaction for 24 hours and then filter, put the filter cake in a 110°C oven to dry for 12 hours, then place it in a high-temperature furnace, raise the temperature to 1500°C at a rate of 360°C / h, and keep it for 8 hours. Into nitrogen gas and quickly cooled to 1300°C and taken out, cooled to 102°C in air, then placed in a dry environment and cooled to normal temperature to obtain tetracalcium phosphate, ...

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Abstract

The invention discloses a silk fibroin / calcium phosphate bone cement composite material and a preparation method thereof. In the preparation of the main component of tracalcium phosphate of calcium phosphate bone cement, the tracalcium phosphate is prepared in a mode of cooling by stages after calcining a tracalcium phosphate precursor which is synthesized by adopting a liquid-phase reaction method; composite powder is prepared by adding water-insoluble silk fibroin powder into the calcium phosphate bone cement; and the silk fibroin / calcium phosphate bone cement composite material with a similar structure to a bone is converted by blending the composite powder in a certain liquid-solid ratio to form paste. The silk fibroin / calcium phosphate bone cement composite material has high mechanical property and biocompatibility, is directly injected in a surgical site by using a syringe, and can be molded and cured accurately to serve as a filling material for bone repair; or the composite material can be implanted into a body to be used as an implant material for the bone repair after being self-cured in the in vitro environment. The technical scheme of the invention greatly improves preparation working conditions of the calcium phosphate bone cement, reduces preparation cost, and expands the medical application of silk fibroin.

Description

technical field [0001] The invention relates to a medical biomaterial and a preparation method thereof, in particular to a composite material with calcium phosphate bone cement as a matrix and silk fibroin powder as a reinforcement and a preparation method thereof. Background technique [0002] Calcium phosphate bone cement is generally composed of two or more calcium phosphate salts mixed powder and solidification liquid. When used, the two are evenly blended in a certain proportion, and can be cured and accurately shaped at room temperature or in the human body environment. The final product of the curing reaction of bone cement is mainly hydroxyapatite, which is similar to the composition of human bone, which can conduct bone growth, be gradually absorbed by tissue and produce bone tissue regeneration effect, and has good biocompatibility. It shows the advantages of huge clinical application and broad market prospects. However, the traditional calcium phosphate bone ceme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L27/42
Inventor 谢瑞娟王彪李明忠
Owner SUZHOU UNIV
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