CN106620866A - Preparation method of collagen-hydroxyapatite bracket containing nano zirconium dioxide - Google Patents
Preparation method of collagen-hydroxyapatite bracket containing nano zirconium dioxide Download PDFInfo
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- CN106620866A CN106620866A CN201610961712.9A CN201610961712A CN106620866A CN 106620866 A CN106620866 A CN 106620866A CN 201610961712 A CN201610961712 A CN 201610961712A CN 106620866 A CN106620866 A CN 106620866A
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- zirconium dioxide
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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
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/446—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with other specific inorganic fillers other than those covered by A61L27/443 or A61L27/46
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- A—HUMAN NECESSITIES
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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
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/46—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with phosphorus-containing inorganic fillers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/62—Encapsulated active agents, e.g. emulsified droplets
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Abstract
The invention relates to a preparation method of a collagen-hydroxyapatite bracket containing nano zirconium dioxide. The preparation method comprises the following steps: carrying out liquid-phase reduction reaction to prepare the nano zirconium dioxide, and unifomrly mixing the nano zirconium dioxide with a collagen-hydroxyapatite solution; freeze-drying with a one-step method and carrying out cross-linking to prepare the collagen-hydroxyapatite bracket, wherein the concentration range of the nano zirconium dioxide is 10mu.g/ml to 50mu.g/ml; the grain diameter of nano zirconium dioxide particles is 10nm to 30nm. According to the bracket provided by the invention, the needed materials are simple, and complicated technical requirements and high-end equipment requirements are not needed; the cost is low and the bracket is easy to popularize; a reasonable nano zirconium dioxide slow releasing system is provided for a wound surface and long-period and effective drug slow release is provided for the wound surface; a drug concentration of the wound surface keeps balanced and is not excessive.
Description
Technical field
The invention belongs to technical field of biological materials, and in particular to a kind of ash of the collagen-hydroxyl phosphorus containing nano zirconium dioxide
The preparation method of stone 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 zirconium dioxide has excellent conductivity of heat, electric conductivity, surface-active and catalytic performance, in optics, catalysis, micro-
The fields such as electronics, bio-sensing, antibacterial have huge using value.The nano zirconium dioxide mealiness of different-shape can be different,
As particle diameter is less, narrow particle size distribution spherical nanometer zirconium dioxide powder has good anti-microbial property and electric conductivity.
Due to the high bioactivity of nano zirconium dioxide, when applying it in organizational project, the surface of a wound or mesh are discharged into
Mark organ, it preferentially can be captured by the GAP-associated protein GAP in wound exudate or tissue, chlorion and group, cause nano zirconium dioxide
Particle is in some position high concentration abnormal aggregations, although can effectively participate in antibacterial, but these superfluous nano zirconium dioxides will be
Aggregation, causes the apoptosis of cell in epidermal cell, macrophage, fibroblast, ultimately results in the disunion of the surface of a wound or prolongs
Healing late.Generally speaking, immoderate use or uncontrolled release nano zirconium dioxide will certainly run counter to desire, to the surface of a wound
Reparation is no advantage.Therefore, safely and effectively using nano zirconium dioxide rational slow-releasing system is needed, for the surface of a wound length is provided
Phase effective medicament slow release, 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 collagen-hydroxyapatite support containing nano zirconium dioxide
Preparation method, is to prepare nano zirconium dioxide by Liquid reduction reaction process, is then well mixed with collagen-hydroxyapatite solution
Afterwards one-step method is freezed and is crosslinked preparation becomes Metal pylon, and the novel nano zirconium dioxide prepared with antibacterial, safety is biological
Material.
The present invention is achieved by the following technical solutions：
(1) adopting zirconium oxychloride and ammoniacal liquor and adding absolute ethyl alcohol carries out Liquid reduction reaction process preparation nanometer two for dispersant
Zirconia sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) heating using microwave in confined conditions of nano zirconium dioxide colloidal sol is reacted, first under 250～350W microwave powers
2～2.5min of reaction, then 2.5～3min is reacted under 100～150W microwave powers, nanometer titanium dioxide zirconium 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 zirconium solution to nanometer titanium dioxide, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the collagen-hydroxyapatite containing nano zirconium dioxide that mass fraction is 0.5%
Solution, by nano zirconium dioxide, collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C,
Then collagen-hydroxyapatite support of the porous containing nano zirconium dioxide for obtaining that thickness is 2mm for 24 hours is freezed.Nano-silica
The concentration range for changing zirconium is 10ug/ml-50ug/ml, and the particle diameter of nano zirconium dioxide 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 zirconium dioxide using microwave-hydrothermal method, with process is simple,
With short production cycle, energy-conserving and environment-protective, the features such as having a safety feature.
2. the nano zirconium dioxide particle 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 zirconium dioxide slow-releasing system for the surface of a wound, provides permanently effective for the surface of a wound
Medicament slow release, keep 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 zirconium dioxide is realized by procedure below
's：
(1) adopting zirconium oxychloride and ammoniacal liquor and adding absolute ethyl alcohol carries out Liquid reduction reaction process preparation nanometer two for dispersant
Zirconia sol；Plus the addition of absolute ethyl alcohol is the 3% of tetra chlorauric acid quality；Reaction temperature is 40 DEG C；
(2) nano zirconium dioxide colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan in Beijing under airtight condition
HX-300A computer microwaves ultrasound combinatorial compound instrument is microwave source), first 2.25min is reacted under 300W microwave powers, then in 120W
2.75min is reacted under microwave power, nanometer titanium dioxide zirconium 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 zirconium solution to nanometer titanium dioxide, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the collagen-hydroxyapatite containing nano zirconium dioxide that mass fraction is 0.5%
Solution, by nano zirconium dioxide, collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C,
Then the collagen-hydroxyapatite support containing nano zirconium dioxide for obtaining that thickness is 2mm for 24 hours is freezed.Nano zirconium dioxide
Concentration range be 10ug/ml-50ug/ml, the particle diameter of nano zirconium dioxide particle is 10-30nm.
Embodiment 2
A kind of preparation method of the collagen-hydroxyapatite support containing nano zirconium dioxide is realized by procedure below
's：
(1) adopting zirconium oxychloride and ammoniacal liquor and adding absolute ethyl alcohol carries out Liquid reduction reaction process preparation nanometer two for dispersant
Zirconia sol；Plus the addition of absolute ethyl alcohol is the 3% of tetra chlorauric acid quality；Reaction temperature is 30 DEG C；
(2) nano zirconium dioxide colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan in Beijing under airtight condition
HX-300A computer microwaves ultrasound combinatorial compound instrument is microwave source), first 2.5min is reacted under 250W microwave powers, then in 150W
2.5min is reacted under microwave power, nanometer titanium dioxide zirconium 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 zirconium solution to nanometer titanium dioxide, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and it is 0.5% containing nano zirconium dioxide, collagen-hydroxyapatite to obtain mass fraction
Solution, by nano zirconium dioxide, collagen-hydroxyapatite solution the mould of 4cm × 4cm is injected, and is freezed 2 hours at -20 DEG C,
Then collagen-hydroxyapatite support of the porous containing nano zirconium dioxide for obtaining that thickness is 2mm for 24 hours is freezed.Nano-silica
The concentration range for changing zirconium is 10ug/ml-50ug/ml, and the particle diameter of nano zirconium dioxide 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 zirconium dioxide, is characterized in that, step is as follows：
(1) zirconium oxychloride and ammoniacal liquor are adopted and is added absolute ethyl alcohol and is carried out Liquid reduction reaction process for dispersant and prepare nanometer titanium dioxide
Zirconium colloidal sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) heating using microwave in confined conditions of nano zirconium dioxide colloidal sol is reacted, is first reacted under 250～350W microwave powers
2～2.5min, then 2.5～3min is reacted under 100～150W microwave powers, nanometer titanium dioxide zirconium solution is obtained；
(3) by ox NTx albumen and shitosan according to 9：1 mass ratio is dissolved in the acetic acid solution of 0.5mol/L, with
10ppm is added to after nanometer titanium dioxide zirconium solution for aimed concn and mixes 4h, be subsequently adding gross mass 0.5% glutaraldehyde simultaneously
Mix, obtain mass fraction be 0.5% containing nano zirconium dioxide, collagen-hydroxyapatite solution, by nano zirconium dioxide,
Collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes at -20 DEG C 2 hours, then freezes and obtains thickness in 24 hours
Spend collagen-hydroxyapatite support of the porous containing nano zirconium dioxide for 2mm.
2. the preparation method of a kind of collagen-hydroxyapatite support containing nano zirconium dioxide according to claim 1, its
It is characterized in that：The concentration range of nano zirconium dioxide is 10ug/ml-50ug/ml, and the particle diameter of nano zirconium dioxide particle is 10-
30nm。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610961712.9A CN106620866A (en) | 2016-11-04 | 2016-11-04 | Preparation method of collagen-hydroxyapatite bracket containing nano zirconium dioxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610961712.9A CN106620866A (en) | 2016-11-04 | 2016-11-04 | Preparation method of collagen-hydroxyapatite bracket containing nano zirconium dioxide |
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| CN106620866A true CN106620866A (en) | 2017-05-10 |
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| CN201610961712.9A Pending CN106620866A (en) | 2016-11-04 | 2016-11-04 | Preparation method of collagen-hydroxyapatite bracket containing nano zirconium dioxide |
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2016
- 2016-11-04 CN CN201610961712.9A patent/CN106620866A/en active Pending
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Application publication date: 20170510 |