CN106620862A - Preparation method of collagen-hydroxyapatite scaffold containing nano silicon nitride - Google Patents
Preparation method of collagen-hydroxyapatite scaffold containing nano silicon nitride Download PDFInfo
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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Abstract
The invention relates to a preparation method of a collagen-hydroxyapatite scaffold containing nano silicon nitride. The preparation method includes the steps of: performing a liquid-phase reduction reaction to prepare the nano silicon nitride, uniformly mixing the nano silicon nitride with a collagen-hydroxyapatite solution, and performing one-step freeze-drying and crosslinking to produce the scaffold, wherein concentration range of the nano silicon nitride is 10-50 [mu]g/ml and particle size of the nano silicon nitride is 10-30 nm. The raw materials of the scaffold are simple. The method is free of complex technology and high-end equipment, is low in cost and is easy to promote. A reasonable nano silicon nitride slow release system is provided for a wound surface, so that long-acting effective slow releasing of a medicine is provided for the wound surface, thereby maintaining the medicine concentration of the wound surface to be balanced and effective without excess.
Description
Technical field
The invention belongs to technical field of biological materials, and in particular to a kind of collagen-hydroxyapatite containing nano-silicon nitride
The preparation method of support.
Background technology
Hydroxyapatite and collagen are topmost inorganic and organic principles in nature bone, and all have good life
Thing characteristic, but there is different defects again when being used alone, it is difficult to meet requirement of the organizational project to biomaterial performance, with
Collagen preferably make use of the caking property of collagen and overcome hydroapatite particles with hydroxyapatite compound
Mobility.
Nano-silicon nitride has excellent conductivity of heat, electric conductivity, surface-active and catalytic performance, in optics, catalysis, micro- electricity
The fields such as son, bio-sensing, antibacterial have huge using value.The nano silicon nitride powders performance of different-shape is different, such as grain
Footpath is less, narrow particle size distribution ball shaped nano silicon nitride powder has good anti-microbial property and electric conductivity.
Due to the high bioactivity of nano-silicon nitride, when applying it in organizational project, the surface of a wound or target are discharged into
Organ, it preferentially can be captured by the GAP-associated protein GAP in wound exudate or tissue, chlorion and group, cause nano silicon nitride silicon grain
In some position high concentration abnormal aggregations, although can effectively participate in antibacterial, but these superfluous nano-silicon nitrides will be thin in epidermis
Born of the same parents, macrophage, the interior aggregation of fibroblast, cause the apoptosis of cell, ultimately result in disunion or the delayed union of the surface of a wound.
Generally speaking, immoderate use or uncontrolled release nano-silicon nitride will certainly run counter to desire, and not have to wound repair
Benefit.Therefore, safely and effectively using nano-silicon nitride rational slow-releasing system is needed, for the surface of a wound permanently effective medicine is provided
Thing is sustained, and keeps the drug concentration of the surface of a wound balanced effective and not superfluous.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of system of the collagen-hydroxyapatite support containing nano-silicon nitride
Preparation Method, is to prepare nano-silicon nitride by Liquid reduction reaction process, is then well mixed with collagen-hydroxyapatite solution latter
Footwork is freezed and is crosslinked preparation becomes Metal pylon, prepares the novel nano silicon nitride biomaterial with antibacterial, safety.
The present invention is achieved by the following technical solutions：
(1) adopting silicon tetrachloride and sodium azide and adding dipotassium hydrogen phosphate carries out Liquid reduction reaction process preparation for dispersant
Nano silicon nitride Ludox；Reaction temperature is 30 DEG C -45 DEG C；
(2) heating using microwave in confined conditions of nano silicon nitride Ludox is reacted, it is first anti-under 250～350W microwave powers
2～2.5min is answered, then 2.5～3min is reacted under 100～150W microwave powers, nano-silicon nitride solution is obtained；
(3) NTx albumen ox heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, added as aimed concn with 10ppm and mix 4h after a certain amount of solution to nano-silicon nitride, be subsequently adding total matter
The glutaraldehyde of the 0.5% of amount is simultaneously mixed, and obtains the solution of collagen-hydroxyapatite containing nano-silicon nitride that mass fraction is 0.5%,
Nano-silicon nitride, collagen-hydroxyapatite solution are injected into the mould of 4cm × 4cm, is freezed 2 hours at -20 DEG C, then frozen
It is dry to obtain within 24 hours collagen-hydroxyapatite support of the porous containing nano-silicon nitride that thickness is 2mm.The concentration of nano-silicon nitride
Scope is 10ug/ml-50ug/ml, and the particle diameter of nano silicon nitride silicon particle is 10-30nm.
Preferably, the condition of heating using microwave reaction is in the step (2)：First react under 300W microwave powers
2.25min, then react 2.75min under 120W microwave powers.
The present invention has the advantages that：
1. the present invention replaces traditional hydro-thermal method to prepare nano-silicon nitride using microwave-hydrothermal method, with process is simple, life
Cycle is short, energy-conserving and environment-protective are produced, the features such as having a safety feature.
2. the nano silicon nitride silicon grain using the method preparation is spherical in shape, uniform in size, good dispersion.
3. the support material requested of the present invention is simple, without the need for complicated technical requirements and high-end device requirement, low cost,
It is easy to spread.
4. support of the present invention provides rational nano-silicon nitride slow-releasing system for the surface of a wound, provides permanently effective for the surface of a wound
Medicament slow release, keeps the drug concentration of the surface of a wound balanced effective and not superfluous.
Specific embodiment
The present invention is further illustrated with reference to embodiment.
Embodiment 1
A kind of preparation method of the collagen-hydroxyapatite support containing nano-silicon nitride is realized by procedure below：
(1) adopting silicon tetrachloride and sodium azide and adding dipotassium hydrogen phosphate carries out Liquid reduction reaction process preparation for dispersant
Nano silicon nitride Ludox；Plus the addition of dipotassium hydrogen phosphate is the 3% of tetra chlorauric acid quality；Reaction temperature is 40 DEG C；
(2) nano silicon nitride Ludox stirring 10min is taken, microwave heating treatment (selects the auspicious swan HX- in Beijing under airtight condition
300A computer microwaves ultrasound combinatorial compound instrument is microwave source), first 2.25min is reacted under 300W microwave powers, then it is micro- in 120W
2.75min is reacted under wave power, nano-silicon nitride solution is obtained；
(3) NTx albumen ox heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, added as aimed concn with 10ppm and mix 4h after a certain amount of solution to nano-silicon nitride, be subsequently adding total matter
The glutaraldehyde of the 0.5% of amount is simultaneously mixed, and obtains the solution of collagen-hydroxyapatite containing nano-silicon nitride that mass fraction is 0.5%,
Nano-silicon nitride, collagen-hydroxyapatite solution are injected into the mould of 4cm × 4cm, is freezed 2 hours at -20 DEG C, then frozen
It is dry to obtain within 24 hours the collagen-hydroxyapatite support containing nano-silicon nitride that thickness is 2mm.The concentration range of nano-silicon nitride
For 10ug/ml-50ug/ml, the particle diameter of nano silicon nitride silicon particle is 10-30nm.
Embodiment 2
A kind of preparation method of the collagen-hydroxyapatite support containing nano-silicon nitride is realized by procedure below：
(1) adopting silicon tetrachloride and sodium azide and adding dipotassium hydrogen phosphate carries out Liquid reduction reaction process preparation for dispersant
Nano silicon nitride Ludox；Plus the addition of dipotassium hydrogen phosphate is the 3% of tetra chlorauric acid quality；Reaction temperature is 30 DEG C；
(2) nano silicon nitride Ludox stirring 10min is taken, microwave heating treatment (selects the auspicious swan HX- in Beijing under airtight condition
300A computer microwaves ultrasound combinatorial compound instrument is microwave source), first 2.5min is reacted under 250W microwave powers, then in 150W microwaves
2.5min is reacted under power, nano-silicon nitride solution is obtained；
(3) NTx albumen ox heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, added as aimed concn with 10ppm and mix 4h after a certain amount of solution to nano-silicon nitride, be subsequently adding total matter
The glutaraldehyde of the 0.5% of amount is simultaneously mixed, obtain mass fraction be 0.5% it is molten containing nano-silicon nitride, collagen-hydroxyapatite
Liquid, by nano-silicon nitride, collagen-hydroxyapatite solution the mould of 4cm × 4cm is injected, freezing 2 hours at -20 DEG C, then
It is lyophilized to obtain within 24 hours collagen-hydroxyapatite support of the porous containing nano-silicon nitride that thickness is 2mm.Nano-silicon nitride it is dense
Degree scope is 10ug/ml-50ug/ml, and the particle diameter of nano silicon nitride silicon particle is 10-30nm.
Although above-mentioned be described to the specific embodiment of the present invention in conjunction with the embodiments, not to present invention protection
The restriction of scope, one of ordinary skill in the art should be understood that on the basis of technical scheme, those skilled in the art
The various modifications made by creative work need not be paid or deformation are still within protection scope of the present invention.
Claims (2)
1. a kind of preparation method of the collagen-hydroxyapatite support containing nano-silicon nitride, is characterized in that, step is as follows：
(1) adopting silicon tetrachloride and sodium azide and adding dipotassium hydrogen phosphate carries out Liquid reduction reaction process preparation nanometer for dispersant
Nitridation Ludox；Reaction temperature is 30 DEG C -45 DEG C；
(2) heating using microwave in confined conditions of nano silicon nitride Ludox is reacted, first reacts 2 under 250～350W microwave powers
～2.5min, then 2.5～3min is reacted under 100～150W microwave powers, nano-silicon nitride solution is obtained；
(3) by ox NTx albumen and shitosan according to 9：1 mass ratio is dissolved into the acetic acid solution of 0.5mol/L, with
10ppm is added to after nano-silicon nitride solution for aimed concn and mixes 4h, is subsequently adding the 0.5% of gross mass glutaraldehyde and mixes
Even, it is 0.5% containing nano-silicon nitride, collagen-hydroxyapatite solution, by nano-silicon nitride, collagen-hydroxyl to obtain mass fraction
Base apatite solution injects the mould of 4cm × 4cm, freezes at -20 DEG C 2 hours, then freezes and obtains within 24 hours thickness for 2mm
Porous containing nano-silicon nitride collagen-hydroxyapatite support.
2. the preparation method of a kind of collagen-hydroxyapatite support containing nano-silicon nitride according to claim 1, it is special
Levying is：The concentration range of nano-silicon nitride is 10ug/ml-50ug/ml, and the particle diameter of nano silicon nitride silicon particle is 10-30nm.
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| CN201610952850.0A CN106620862A (en) | 2016-11-03 | 2016-11-03 | Preparation method of collagen-hydroxyapatite scaffold containing nano silicon nitride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022133908A1 (en) * | 2020-12-24 | 2022-06-30 | 刘晓东 | Ceramic composite coating material, antivirus ceramic composite coating material and preparation method therefor, and coating layer |
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- 2016-11-03 CN CN201610952850.0A patent/CN106620862A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022133908A1 (en) * | 2020-12-24 | 2022-06-30 | 刘晓东 | Ceramic composite coating material, antivirus ceramic composite coating material and preparation method therefor, and coating layer |
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