CN104274862B - The preparation method of titanium net surface active medicine controlled-release coating is repaired in a kind of cranium jaw face - Google Patents
The preparation method of titanium net surface active medicine controlled-release coating is repaired in a kind of cranium jaw face Download PDFInfo
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
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- 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
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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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- 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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- 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
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- 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
- A61L2300/106—Halogens or compounds thereof, e.g. iodine, chlorite
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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 present invention provides a kind of new method to repair titanium net surface active medicine controlled-release coating to prepare cranium jaw face, including: the steps such as prepared by titanium net, template crosslinked, prepared by electrolyte, and magnetic field processes, heat treatment.The invention still further relates to cranium jaw face and repair titanium net surface active medicine controlled-release coating and system thereof.Compared with prior art, environmental protection of the present invention, nontoxic, nanotube size is the most controlled, and coating is substantially better than prior art with the adhesion of substrate.
Description
Technical field
The present invention relates to medical instruments field, particularly relate to a kind of cranium jaw face repair titanium net surface drug sustained release system and
Preparation method.
Background technology
When treating the neurosurgery related diseases such as cranium Maxillofacial defect, epilepsy, intracranial tumor, generally require and carry out skull reparation
Operation.Titanium net, due to its higher intensity, excellent biocompatibility, is often used for cranium jaw face and repairs.But,
Cranium jaw face prosthesis especially skull prosthesis danger is higher, and perioperative untoward reaction is more, common
There are hydrocrania, postoperative infection etc., affect therapeutic effect, and the effect of the antibiotic infusion treatment of routine is the most unsatisfactory.
Therefore, if there being a kind of method can be administered at operative region interior orientation, it is possible to alleviate the untoward reaction of perioperative.
Titanium net surface drug sustained release system is a kind of to repair perioperative untoward reaction and design have life for alleviating cranium jaw face
The coating of thing activity, its microstructure is the titania nanotube of rule.The preparation side of titania nanotube coating
Method is mainly anodic oxidation, is characterized in that and is connected with constant current source anode by pure titanium, with platinum electrode as negative electrode,
Solution containing fluorion is energized, carries out anodic oxidation.After sample pretreating certain time, surface forms titanium dioxide
Titanium nanotube coatings.The coating of this structure is initially found to have photovoltaic response effect, may act as a kind of sun
The raw material of energy battery.And research subsequently finds, this structure also has higher osteogenic activity, and according to its structure
Feature, it is also possible to as pharmaceutical carrier, can be as drug sustained release system by control.According to these features and effect,
This coating is repaired most suitable for cranium jaw face.
But, nanotube coatings prepared by this employing anodic oxidation has the obvious disadvantage that: 1, electrolyte solution due to
Containing fluorion, and being acid condition, toxicity and corrosivity are very strong, to operator and the negative effect of environment
The biggest；2, leaving over a large amount of fluorion in this coating, require higher to follow-up cleaning treatment, this is at medical instruments field,
Especially the most disadvantageous for implantation instrument, in order to reduce the toxicity to sick human and environment, required manpower and materials and
Cost is the highest；3, this coating is the most weak with the adhesion of substrate, is very easy to come off, and this in the application of medical field is
The most unallowed.
Therefore, those skilled in the art is devoted to develop a kind of new method to prepare active medicine controlled-release coating, its
Electrolyte is a kind of environmental protection solution, not fluoride ion, and ph value is close to neutral；Prepared coating is big with substrate caking power
Big raising, anti-shearing force reinforcement, difficult drop-off；Not fluoride ion, and after subsequent treatment, remnants can be eliminated
Ion, cleaning problem is easy to solve.
Summary of the invention
Because the drawbacks described above of prior art, the technical problem to be solved is that existing titanium net surface medicine delays
Release system is to the sick toxicity of human and environment, corrosive negative effect, and improves the adhesion of coating and substrate so that it is
Application it is easier in medical field cranium jaw face is repaired.
For achieving the above object, the invention provides a kind of new method and repair titanium net surface active medicine to prepare cranium jaw face
Controlled-release coating, comprises the following steps:
Prepared by step one, titanium net: use titanium net common on market.
Step 2, template crosslinked: the titanium net surface prepared carries out crosslinking Treatment, coat one layer of thin with nano-pore
Film.Mainly include following methods:
Method 1, titanium net surface apply organic membrane, organic membrane is the reticular membrane with different-diameter nano aperture, with
As the template of nanotube, the wherein a diameter of 5-100nm of nano aperture；
Method 2, coat one layer of corundum film with regular microwell array template as nanotube at titanium net surface,
Wherein thickness is 1-5 μm.
Prepared by step 3, electrolyte: preparation electrolyte solution, and described electrolyte includes inorganic ions and organic ion,
Research worker is thought, inorganic ions includes the halogen family ion outside Natural zeolite and hydrogen peroxide ions, sodium ion, phosphoric acid
Radical ion etc..Wherein, major function ion is chloride ion and hydrogen peroxide ions, and wherein the molar concentration of chloride ion is
0.01-1mol/L, preferably 0.3-0.5mol/L；The concentration of hydrogen peroxide is 0.01-2mol/L, preferably 1-1.5mol/L.
Organic ion includes that citrate ion, EDTA, Tris, acetate etc. play the acid ion of slow releasing function, concentration model
Enclose 0.1-1mol/L.The ph value scope of electrolyte solution is 3-9, and preferably ph value is 5-7.
Step 4, being immersed in described electrolyte solution by the titanium net with template, the temperature of electrolyte solution is maintained at 10
Degree Celsius to 80 degrees Celsius, preferably 45 degrees Celsius to 55 degrees Celsius.
Step 5, being placed in stationary magnetic field or alternating magnetic field by the electrolyte solution being soaked with titanium net, magnetic field intensity is
0.1A/m to 5A/m, the frequency of alternating magnetic field is 1-30 minute/time, preferably 5-10 minute/time.Alternating magnetic field
Waveform is square wave or sinusoidal wave form or cosine waveform, preferably square wave, and waveform symmetry is Striking symmetry or asymmetric.
Final angle between magnetic direction and titanium net surface plane is 0-180 degree, and optimum is 90 degree.Magnetic field and alternating magnetic field
Being to be produced by magnetic field generator, the process time is more than 5 minutes, and the optimal processing time is 30 minutes-60 minutes.Titanium
Online generation titania nanotube coating.
Step 6, being taken out from electrolyte solution by the titanium net processed through magnetic field, clean, heat treatment, temperature is
150-450 degree Celsius, temperature retention time 30-60 minute, especially 250 degrees Celsius are preferred.This heat treatment will not be to pure titanium
Microstructure produces internal impact.
Further, use above-mentioned preparation method to obtain cranium jaw face and repair titanium net surface active medicine controlled-release coating, its merit
Can be partly titania nanotube, described nanotube size be controlled by pore size of template.
Further, titanium net surface active medicine slow-released system is repaired in a kind of cranium jaw face, obtains including by above-mentioned preparation method
The titania nanotube coating obtained.
Compared with prior art, the invention have the advantages that
1, electrolyte of the present invention is the electrolyte of nontoxic environmental protection, and only need to slightly make subsequent treatment just can be straight
Running in and put, environmentally friendly, this is the remarkable advantage of the present invention；
2, using template way to control the diameter of titania nanotube, size is the most controlled；
3, prepared coating and substrate have good adhesion, may be up to 50N, and prior art floating coat combines
Power is generally 11N, and coating quality is substantially better than similar techniques.
Below with reference to accompanying drawing, the technique effect of design, concrete structure and the generation of the present invention is described further, with
It is fully understood from the purpose of the present invention, feature and effect.
Accompanying drawing explanation
Fig. 1 is the SEM photograph of the nanotube coatings that the preparation of a preferred embodiment of the present invention completes；Wherein
Caliber shown in a-h is 30nm respectively, 40nm, 60nm, 70nm, 85nm, 100nm, 110nm, 130nm.
Detailed description of the invention
Embodiment 1
(1) prepared by titanium net；
(2) coating the one layer of micropore corundum film template as nanotube at titanium net surface, aperture is 100nm；
(3) electrolyte solution includes 0.3mol/L chloride ion, 1.2mol/L hydrogen peroxide ions, sodium ion and 0.5mol/L
Acetate ion, ph value is 5；
(4) being immersed by the titanium net of step (2) in the electrolyte solution of step (3), temperature is maintained at 50 degrees Celsius；
(5) being placed in Constant charge soil by the electrolyte solution of step (4), the process time is 30 minutes；
(6) being taken out from electrolyte solution by the titanium net of step (5), clean, heat treatment, temperature is 400 Celsius
Degree, temperature retention time 30 minutes.
Above-mentioned steps can generate the titania nanotube coating that aperture is 100nm, after tested, its coating on the net at titanium
Adhesion is 45N.
Embodiment 2
(1) prepared by titanium net；
(2) applying one layer of organic membrane at titanium net surface, organic membrane is the reticular membrane with obstructed diameter hole, and aperture is
50nm；
(3) electrolyte solution includes 0.3mol/L chloride ion, 1.5mol/L hydrogen peroxide ions, sodium ion, phosphoric acid
Radical ion and 1mol/L citrate ion, ph value is 6；
(4) being immersed by the titanium net of step (2) in the electrolyte solution of step (3), temperature is maintained at 55 degrees Celsius；
(5) being placed in alternating magnetic field by the electrolyte solution of step (4), magnetic field intensity is 5A/m, and frequency is 5
Minute/time, square wave, Striking symmetry, final angle is 90 degree, processes 60 minutes time.
(6) being taken out from electrolyte solution by the titanium net of step (5), clean, heat treatment, temperature is 250 Celsius
Degree, temperature retention time 60 minutes.
Above-mentioned steps can generate the titania nanotube coating that aperture is 50nm, after tested, its coating on the net at titanium
Adhesion is 50N.
The preferred embodiment of the present invention described in detail above.Should be appreciated that those of ordinary skill in the art without
Need creative work just can make many modifications and variations according to the design of the present invention.Therefore, all in the art
Technical staff the most on the basis of existing technology can by logical analysis, reasoning, or a limited experiment
With the technical scheme obtained, all should be in the protection domain being defined in the patent claims.
Claims (9)
1. the preparation method of a cranium jaw face reparation titanium net surface active medicine controlled-release coating, it is characterised in that bag
Include following steps；
Prepared by step one, titanium net；
Step 2, template crosslinked: the surface of the above-mentioned titanium net prepared is carried out crosslinking Treatment, coat one layer of band
Having the organic membrane of nano-pore, described organic membrane is the reticular membrane with 5-100nm different-diameter hole, film
Thick 1-5 μm；
Prepared by step 3, electrolyte: described electrolyte includes inorganic ions, organic ion and hydrogen peroxide, its
In, described inorganic ions includes that chloride ion, sodium ion and phosphate anion, described organic ion include lemon
Lemon acid ion, EDTA, Tris and acetate ion, the pH value range of described electrolyte solution is 3-9,
Wherein, the molar concentration of chloride ion is 0.01-1mol/L, and the concentration of hydrogen peroxide is 0.01-2mol/L, institute
The molar concentration stating organic ion is 0.1-1mol/L；
In step 4, the electrolyte solution that the described titanium net immersion step 3 with template is prepared, described electrolysis
The temperature of liquor is maintained at 10 degrees Celsius to 80 degrees Celsius；
Step 5, the electrolyte solution being soaked with described titanium net is placed in stationary magnetic field or alternating magnetic field, described
The intensity in magnetic field is 0.1A/m to 5A/m, and the frequency of described alternating magnetic field is 1-30 minute/time, described magnetic
Final angle between field direction and described titanium net surface plane is 0-180 degree, and the magnetic field process time is 5
More than minute；
Step 6, the described titanium net processed through described magnetic field is taken out from described electrolyte solution, cleans,
Heat treatment, wherein heat treatment temperature is 150-450 degree Celsius, and temperature retention time is 30-60 minute.
2. preparation method as claimed in claim 1, it is characterised in that chloride ion described in step 3 mole dense
Degree is preferably 0.3-0.5mol/L, and the molar concentration of described hydrogen peroxide is preferably 1-1.5mol/L, described electricity
The pH value solving liquor is preferably 5-7.
3. preparation method as claimed in claim 1, it is characterised in that the temperature of electrolyte solution described in step 4
Degree is preferably 45 degrees Celsius to 55 degrees Celsius.
4. preparation method as claimed in claim 1, it is characterised in that the frequency of alternating magnetic field described in step 5
It is preferably 5-10 minute/time；The waveform of described alternating magnetic field is square wave, sinusoidal wave form or cosine waveform, institute
The symmetry stating waveform is Striking symmetry or asymmetric.
5. preparation method as claimed in claim 4, it is characterised in that described alternating magnetic field is preferably square wave.
6. preparation method as claimed in claim 1, it is characterised in that magnetic direction described in step 5 is with described
Final angle optimum between titanium net surface plane is 90 degree, and it is 30 points that described magnetic field processes time optimal
Clock-60 minutes.
7. preparation method as claimed in claim 1, it is characterised in that described in step 6, heat treatment temperature is preferred
It it is 250 degrees Celsius.
8. titanium net surface activity is repaired in the cranium jaw face prepared according to the preparation method described in any one of claim 1-7
Medicament controlled-release coating, it is characterised in that the adhesion of described controlled-release coating is 40-50N, its funtion part
Being titania nanotube, the size of described nanotube is by the pore size control of described template.
9. include that titanium net surface drug sustained release system is repaired in the cranium jaw face of the controlled-release coating described in claim 8.
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| CN201410474920.7A CN104274862B (en) | 2014-09-17 | 2014-09-17 | The preparation method of titanium net surface active medicine controlled-release coating is repaired in a kind of cranium jaw face |
| CN201610209579.1A CN105903074B (en) | 2014-09-17 | 2014-09-17 | Repair the preparation method of titanium net surface active drugs controlled-release coating in cranium jaw face |
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| WO2006104644A2 (en) * | 2005-03-29 | 2006-10-05 | Warsaw Orthopedic, Inc. | Implants incorporating nanotubes and methods for producing the same |
| CN101311329A (en) * | 2008-02-20 | 2008-11-26 | 福建师范大学 | Method for preparing titanium oxide nanotube array bone repair biomaterial with biological activity |
| CN101671840A (en) * | 2008-09-10 | 2010-03-17 | 中国科学院金属研究所 | Method for generating nanotube array oxide film on medical titanium and titanium alloy surface |
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| CN105903074A (en) | 2016-08-31 |
| CN105903074B (en) | 2018-09-14 |
| CN104274862A (en) | 2015-01-14 |
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