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Method for preparing nano-phase hydroxyapatite/fimbrin composite material

A technology of phase hydroxyapatite and silk fibroin, which is applied in the field of preparation of nanophase hydroxyapatite/silk fibroin composite materials, can solve the problems of salt discharge, time consumption, water consumption, etc., and achieve low equipment requirements, The effect of compounding is sufficient and good, and the preparation process is simple

Inactive Publication Date: 2008-08-06
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in the process of filtration-dialysis-concentration of the silk fibroin solution, this preparation method consumes water and time, and also discharges a large amount of salt, which is in line with the development direction of energy saving, emission reduction and green processing. does not match

Method used

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  • Method for preparing nano-phase hydroxyapatite/fimbrin composite material
  • Method for preparing nano-phase hydroxyapatite/fimbrin composite material
  • Method for preparing nano-phase hydroxyapatite/fimbrin composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The fully degummed silk fibroin fiber of 2.78g is dissolved in 27.68g CaCl 2 , 35.98g C 2 h 5 OH, 28.60g H 2 In the ternary system solvent composed of O, stir and dissolve at 75±2°C, and obtain a light yellow liquid after 0.5h; put the obtained light yellow liquid in a 1L three-neck round bottom flask, and then put the flask into In the constant temperature water bath, install a stirrer, a normal pressure dropping funnel and a pH indicator; weigh (NH 4 )HPO 4 19.80g, dissolved in 500ml of water, adjust the pH value to 10.5 with ammonia water to obtain a diammonium hydrogen phosphate solution; start the stirrer, then evenly drop the obtained diammonium hydrogen phosphate solution at a speed of 2.4ml / min, compound reaction 3.5 h, the temperature in the first 2 hours of the composite reaction is controlled at 30°C, and the temperature in the last 0.5h is controlled at 60°C; after the reaction is completed, after vacuum filtration, washing, infrared drying, and grinding...

Embodiment 2

[0030] The fully degummed silk fiber of 4.41g is dissolved in 27.68g CaCl 2 , 35.98g C 2 h 5 OH, 28.60gH 2 In the ternary system solvent composed of O, stir and dissolve at 72±2°C, and obtain a light yellow liquid after 0.5h; put the obtained light yellow liquid in a 1L three-neck round bottom flask, and then put the flask into In the constant temperature water bath, install a stirrer, a normal pressure dropping funnel and a pH indicator; weigh (NH 4 )HPO 4 19.80g, dissolve in 500ml of water, adjust the pH value to 11 with ammonia water, and obtain the diammonium hydrogen phosphate solution; start the stirrer, then add the obtained diammonium hydrogen phosphate solution evenly at a speed of 2.4ml / min, compound reaction for 4h , the temperature is controlled at 30°C for the first 3h of the composite reaction, and 60°C for the next 1h; after the reaction is completed, the composite material in powder form can be obtained after vacuum filtration, washing, infrared drying, and...

Embodiment 3

[0037] The difference between this embodiment and embodiment 2 is that the added amount of silk fibroin fiber is 6.25g. Remaining with embodiment 2.

[0038] The composite material that this implementation obtains has the following characteristics after being identical with the detection of embodiment 1:

[0039] The calcium-phosphorus ratio is 1.6698, which is consistent with the calcium-phosphorus ratio in standard hydroxyapatite;

[0040] The internal two-phase composite is uniform and good, with a network structure, needle-shaped or columnar grains; the grain size is less than 50nm, and belongs to the hexagonal crystal system, and the unit cell parameters are a=b=9.0319×10 -10 m, c=7.0148×10 -10 m, the average grain size along the c-axis direction is 227.7282×10 -10 m;

[0041] Contains the respective functional groups of hydroxyapatite and silk fibroin, and does not contain new chemical functional groups;

[0042] The silk fibroin content in the composite was 20% (w / ...

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Abstract

The invention relates to a preparation process of nano-hydroxyapatite / silk fibroin composite material, which comprises choosing CaC1 2-C 2 H5 OH-H2O ternary system with molar ratio of 1:2:8 as solution, adding silk fibroin fiber which has fully been degelatinized according to the proportion that mass fraction is 3-14.68 (w / w) under the temperature of 75+-5 DEG C, dissolving 0.5h to obtain silk fibroin solution whose mass fraction is 3-14.68 (w / w), adding diammonium phosphate in silk fibroin solution according to the molar ration that calcium: phosphorus=10:6 under the condition of uniform stirring, finishing the dripping within 2-5h, then continuing compound reaction for 2-3h, wherein the temperature in former 2-4h is 30-60 DEG C, and the temperature of the latter 2-4h is 60-100 DEG C in the whole 4-8h reaction process, paying attention to the change of pH value of reaction system, regulating the pH value to 9-12 with ammonial solution which is diluted, and obtaining the composite material through filtering, fully repeatedly scouring and filtering after finished reaction.

Description

technical field [0001] The invention relates to composite material preparation technology, specifically a preparation method of nano-phase hydroxyapatite / silk fibroin composite material. The prepared composite material can be applied to the repair and replacement of bone defects. The international patent classification number is intended to be Int .Cl.A61L 27 / 12 (2006.01). Background technique [0002] Hydroxyapatite (referred to as HA, the chemical formula is Ca 10 (OH) 2 (PO 4 ) 6 ) is a typical biomaterial with excellent biocompatibility and bioactivity. It can come into contact with blood without coagulation, with only slight tissue reactions in soft tissues and bones. The composition of hydroxyapatite contains elements such as calcium and phosphorus that can be replaced by the normal metabolic pathway of the human body; it also contains groups such as hydroxyl that can bond with human tissues, and achieve complete affinity through bond bonding, thereby It is an ex...

Claims

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Application Information

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IPC IPC(8): C08L89/00C08K3/32C08J3/21A61L27/46A61L27/12
Inventor 姚金波王刚赵海洋
Owner TIANJIN POLYTECHNIC UNIV
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