Biomimetic calcium phosphate fiber composite bracket material and preparation method thereof

A stent material, fiber composite technology, applied in medical science, prosthesis, coating and other directions, can solve the problems of volatile, no three-dimensional stent structure, difficult to maintain regeneration space, etc., to improve strength and toughness, optimize the preparation process, The effect of high crystallinity

Active Publication Date: 2010-09-08
BEIJING UNIV OF CHEM TECH
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AI Technical Summary

Problems solved by technology

Combining sol-gel with electrospinning technology, the organic / inorganic composite precursor sol solution is formed by electrospinning, and a variety of inorganic nanofibers with continuous phases can be prepared by high-temperature sintering, such as Xiaoshu Dai et al. Sol-gel electrospinning technology, through the hydrolysis of phosphate, the preparation of precursor sol, and the electrospinning after adding polymer spinning aids, prepared nano / micro HA fiber materials (Materials Letters 61(2007) 2735-2738, Material Science and Engineering C 28 (2008) 336-340), and propose to use this nano / micro HA fiber material can be used for bone repair scaffold material, but this nano / micro HA fiber has the following problems: 1, in the preparation In the process of sol precursor, the hydrolysis of phosphate ester is incomplete and volatile, and there are a large amount of calcium oxide heterophase in the obtained nano / micro HA fibers, which has an adverse effect on the regeneration of bone tissue; The nano / micro fibers obtained from silk are in the form of a film, which does not have a three-dimensional scaffold structure. It is difficult to maintain a regeneration space after being implanted in the human body. It needs to be formed into a three-dimensional structure scaffold material by winding, pressing and other processes
At the same time, due to the low sintering temperature, the crystallinity of the prepared HA fiber material is not high
In addition, the nano / micro ceramic fibers prepared by the general sol-gel-electrospinning method are extremely brittle, and it is difficult to meet the strength requirements of bone scaffold materials, so the nano / micro HA fibers themselves cannot be directly used as bone repair scaffold materials.
At present, there is no report on the preparation of biomimetic composite scaffold materials for bone repair by electrospun calcium phosphate fibers

Method used

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  • Biomimetic calcium phosphate fiber composite bracket material and preparation method thereof
  • Biomimetic calcium phosphate fiber composite bracket material and preparation method thereof
  • Biomimetic calcium phosphate fiber composite bracket material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Mix 3.643g of triethyl phosphate, 2.76g of ethanol and 1.08g of deionized water to form a solution, and add nitric acid dropwise to adjust the pH of the solution to 2, and stir vigorously at 80°C for 48 hours to hydrolyze, according to the stoichiometry of Ca / P=1.0 Slowly add 2 mol / L calcium nitrate ethanol solution dropwise, stir the mixed solution for 2 hours, and then place it in the environment of -18°C for 7 days to age. The spinning solution was prepared according to the mass ratio of sol: water = 3: 1, and PVP (Mn = 1300,000) was added as a spinning aid, and the concentration of PVP was 4%wt. Electrospinning process parameters are as follows: ambient temperature 40°C, humidity below 30%, spinning solution flow rate 0.5mL / h, electrostatic voltage -18kV, distance between spinneret and fiber receiver 15cm, fiber receiving The surface temperature of the device was 80°C. After spinning for 10 hours, a white cotton-like hybrid fiber material was obtained. The obtaine...

Embodiment 2

[0040] Mix 4.554g of triethyl phosphate, 3.45g of ethanol and 1.35g of deionized water to form a solution, stir vigorously at 50°C for 48 hours, and slowly add 3mol / L of calcium nitrate dropwise according to the stoichiometric ratio of Ca / P=1.5 Ethanol solution, continue to stir for 2 hours after the dropwise addition, and age at -18°C for 7 days. The spinning solution was prepared according to the mass ratio of sol: water = 5: 1, and PVA (Mn = 100,000) was added as a spinning aid, and the concentration of PVA was 8%wt. Electrospinning process parameters are as follows: ambient temperature 40°C, humidity below 30%, spinning solution flow rate 0.8mL / h, electrostatic voltage -22kV, distance between spinneret and fiber receiver 15cm, fiber receiving The surface temperature of the device was 80°C. After electrospinning for 10 hours, a white, cotton-like nanofiber material was obtained, as shown in figure 2 As shown, its microstructure is as image 3 The SEM photographs are sho...

Embodiment 3

[0042] Mix 2.802g of trimethyl phosphate, 1.84g of methanol and 0.72g of deionized water to form a solution, add ammonia water dropwise to adjust the pH of the solution to 9, stir vigorously at 50°C for 48 hours, and follow the stoichiometry of Ca / P=1.5 Slowly add 2 mol / L calcium nitrate ethanol solution dropwise, stir the mixed solution for 2 hours, and then place it in the environment of -18°C for 7 days to age. The spinning solution was prepared according to the mass ratio of sol:water=6:1, and high molecular weight PEO was added as a spinning aid, and the concentration of PEO was 10%wt. Electrospinning process parameters are as follows: ambient temperature 40°C, humidity below 30%, spinning solution flow rate 0.8mL / h, electrostatic voltage -10kV, distance between spinneret and fiber receiver 10cm, fiber receiving The surface temperature of the device was 80°C. After electrospinning for 10 h, white cotton-like nanofibers were obtained. The obtained hybrid fibers were trea...

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Abstract

The invention provides a biomimetic calcium phosphate fiber composite bracket material and a preparation method thereof. The bracket material has similar component and structure as natural reticulated bone and consists of nanometer/micron calcium phosphate fiber substrate and biological polymer coating on the surface, wherein the calcium phosphate fiber is lapped on each other to form a three-dimensional reticulated bone structure, the porosity is not lower than 80% and thickness of the polymer coating is from 100 to 1000 nm. The preparation method comprises the following steps of: dripping solution containing calcium ions into hydrolyzed phosphate solution; adjusting the PH value of the phosphate solution between 1 and 10 and the calcium-phosphorus ratio between 1.0 and 1.6; aging at low temperature to obtain precursor collosol and adding polymer spinning improver into the collosol to perform electrostatic spinning to obtain continuous three-dimensional nanometer/micron fiber; post-processing for shaping, sintering at high temperature, soaking and drying to obtain the biomimetic calcium phosphate fiber composite bracket material.

Description

technical field [0001] The invention belongs to the preparation of biocomposite materials, and relates to a calcium phosphate fiber composite support material and a preparation method. The composite support material can be used as bone defect filling material, bone tissue engineering support material, drug slow-release carrier and the like. Background technique [0002] Calcium phosphate bioceramics mainly include hydroxyapatite (HAP), tricalcium phosphate (α-TCP, β-TCP), calcium pyrophosphate (CPPD), tetracalcium phosphate (TTCP), octacalcium phosphate pentahydrate (OCP), Brushite (DCPD), anhydrous dicalcium phosphate (DCPA) and amorphous calcium phosphate (ACP) and their mixtures, etc. In the current scientific research and clinical application of tissue replacement biomaterials, calcium phosphate bioceramic materials account for a large proportion. From the perspective of the microstructure of natural bone, bone is a continuous multiphase complex composed of nano calcium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L27/42A61L27/56A61L27/58A61L27/10A61L27/34
Inventor 杨小平张歆张慎蔡晴邓旭亮
Owner BEIJING UNIV OF CHEM TECH
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