CN114129768A - Anti-infection improved iodine-loaded titanium alloy antibacterial implant and preparation method thereof - Google Patents

Anti-infection improved iodine-loaded titanium alloy antibacterial implant and preparation method thereof Download PDF

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CN114129768A
CN114129768A CN202111311238.2A CN202111311238A CN114129768A CN 114129768 A CN114129768 A CN 114129768A CN 202111311238 A CN202111311238 A CN 202111311238A CN 114129768 A CN114129768 A CN 114129768A
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iodine
titanium alloy
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infective
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CN114129768B (en
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叶招明
叶福林
滕王锶源
方明
朱伟强
虞方磊
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Zhejiang University ZJU
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/04Metals or alloys
    • A61L27/06Titanium or titanium alloys
    • AHUMAN NECESSITIES
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    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/34Macromolecular materials
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54Biologically active materials, e.g. therapeutic substances
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56Porous materials, e.g. foams or sponges
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/026Anodisation with spark discharge
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/106Halogens or compounds thereof, e.g. iodine, chlorite
    • AHUMAN NECESSITIES
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    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/202Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with halogen atoms, e.g. triclosan, povidone-iodine
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404Biocides, antimicrobial agents, antiseptic agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
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    • A61LMETHODS 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
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    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/06Coatings containing a mixture of two or more compounds
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    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/02Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants

Abstract

The invention discloses an anti-infection improved iodine-carrying titanium alloy antibacterial implant and a preparation method thereof. The preparation method of the improved iodine-carrying titanium alloy antibacterial implant mainly applies an electrochemical method to carry out iodine impregnation on the surface of the micro-arc titanium oxide alloy, and comprises two steps of constructing a titanium alloy surface porous structure and carrying iodine through iodine impregnation improvement treatment; the invention improves the prior process of carrying iodine on the surface of the titanium alloy, so that the production process of the material is more controllable, and the surface bacteriostatic component is more stable. The process is simple, the reaction conditions are appropriate, the advantages of high efficiency and short production period are achieved, and the obtained titanium alloy implant has a very obvious antibacterial effect.

Description

Anti-infection improved iodine-loaded titanium alloy antibacterial implant and preparation method thereof
Technical Field
The invention relates to the technical field of medical biomaterials, in particular to an anti-infection improved iodine-carrying titanium alloy antibacterial implant and a preparation method thereof.
Background
Despite the rapid development of orthopedic surgical techniques over the past decade, infection of the deep tissues of the surgical site remains a relatively delicate complication that medical personnel must face. Endoprosthesis-associated infections are the major manifestation of deep infections. More than half of these endoprosthesis-related infections are caused by staphylococcus epidermidis and staphylococcus aureus. In its pathogenesis, the formation of biofilms is a critical component that makes treatment of such infections difficult. The formation of a biofilm provides a protective barrier for bacteria to have the ability to resist antibiotics and the body's autoimmune defense response. Based on the above theory, the scholars propose that the surface modification of the implant material can endow the material with the capability of inhibiting or hindering the formation of the biofilm, and finally achieve the purpose of preventing the infection related to the internal implant.
The povidone iodine is a compound of polyvinylpyrrolidone and triiodide ions, and has a broad-spectrum antibacterial effect and good biological safety. At present, the povidone iodine is widely used for disinfection of wounds and repair and healing of wounds. In povidone-iodine, iodine forms a complex with the synthetic carrier polymer povidone, which itself has no bactericidal activity. In the aqueous medium, free iodine is released from the povidone-iodine complex into the solution and an equilibrium is established, and as the antibacterial process continues, the consumed free iodine is continuously replenished from the povidone-iodine complex to maintain the equilibrium of bound iodine and free iodine. The ratio of povidone-bound iodine to free iodine is in a concentration and temperature dependent balance that minimizes safety and tolerability issues associated with elemental iodine formulations at the early stages of skin contact.
Disclosure of Invention
The invention aims to provide an iodine-carrying titanium alloy implant with simplified technology and a preparation method thereof, aiming at the problem of implant infection caused by using a titanium alloy medical material in the field of orthopedic surgery.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: an anti-infectious improved iodine-loaded titanium alloy antibacterial implant comprises a titanium alloy material, wherein a porous micro-nano structure is constructed on the surface of the titanium alloy material, and povidone iodine is deposited and attached to the surface of the porous micro-nano structure to form an antibacterial coating.
As an improvement, the porous micro-nano structure is a porous film structure, and the thickness range of the film is 5-25 μm.
As an improvement, the thickness of the antibacterial coating is 10-20 mu m, and the iodine content on the surface is 0.1-1 wt%.
A preparation method of an anti-infection improved iodine-carrying titanium alloy antibacterial implant mainly applies an electrochemical method to carry out iodine impregnation on the surface of a micro-arc titanium oxide alloy, and comprises two steps of constructing a titanium alloy surface porous structure and carrying iodine through iodine impregnation improvement treatment, wherein the specific process flow is as follows:
the method for constructing the porous structure on the surface of the titanium alloy comprises the following steps:
after the surface base material is pretreated, the titanium alloy base material is immersed into an electrolytic cell for electrochemical treatment to form a porous film structure.
The pretreatment mainly comprises the impurity removal step, and the operation flow is as follows: the material is washed by solutions such as acetone, glycol, ultrapure water and the like in sequence to remove impurities, and then the material is subjected to acid washing to remove impurities and finally ultrasonic cleaning.
In the pretreatment process, the concentration of acetone is more than or equal to 99.5 percent, and the concentration of glycol is more than or equal to 99.5 percent;
in the acid washing process, the solution comprises: HF (not less than 40%), HNO3 (65.0-68.0%), H3PO4 (85%), and the acid washing time is 5-25 min;
in the ultrasonic cleaning process, the material is placed in ultrapure water for cleaning for 5 min/time, and the circulation is carried out for 3 times.
The electrochemical treatment is anodic oxidation or micro-arc oxidation, the voltage is maintained within the range of 100-500V, the current frequency is 200-1000Hz, and the temperature of the electrolyte is 10-50 DEG C
The electrolytic cell solution is an acidic electrolytic cell (sulfuric acid-phosphoric acid-hydrogen peroxide-water system) or an alkaline electrolytic cell (sodium hydroxide-potassium nitrate-water system) as an electrolyte. For example in a sulfuric acid-phosphoric acid-hydrogen peroxide-water system.
The improved treatment method for iodine impregnation on the surface of the titanium alloy material comprises the following steps:
and (3) placing the material with the surface porous structure in an iodine-containing solution, performing surface iodine impregnation by an electrochemical method, washing with purified water for 3 times to remove impurities, and drying.
In the operation of electrochemical iodine modification, the material is required to be placed on a titanium-based hook or a mesh basket on the anode side under the conditions of light shielding, constant pressure of 100-200V, and initial current density of 0.3-1.0A/dm2, wherein the cathode side is a pure titanium substrate, the distance between the cathode and the anode is 10-20cm, and the reaction time is 2-60 min; and then connecting the titanium-based hook or the basket on the side of the original anode with the negative electrode of a power supply, connecting the pure titanium substrate on the side of the original anode with the positive electrode of the power supply, and reacting for 30-60min under the same reaction conditions of voltage, initial current density, cathode-anode spacing and solution temperature, thereby completing a reaction cycle. Repeating the circulation for 3-10 times, washing the materials with purified water, blow-drying, and sterilizing for use.
The iodine-containing solution is an aqueous solution containing 2-5g/L of potassium iodide, 0.5-2g/L of povidone iodine and 1-8g/L of beta-cyclodextrin.
In the drying process, the temperature is 10-50 ℃, the drying time is 10-24h, and light shielding is required.
Compared with the prior art, the invention has the advantages that: the invention improves the prior process of carrying iodine on the surface of the titanium alloy, so that the production process of the material is more controllable, and the surface bacteriostatic component is more stable. The process is simple, the reaction conditions are appropriate, the advantages of high efficiency and short production period are achieved, and the obtained titanium alloy implant has a very obvious antibacterial effect.
Drawings
Fig. 1 is a surface electron microscope representation of the improved iodine-carrying titanium alloy, wherein: A. anodizing the porous substrate material; B. an improved iodine-carrying titanium alloy material (the magnification is 5 hundred times); c and D are respectively high power under-lens visual field (magnification is 2 ten thousand times) of corresponding area in B, the iodine content is 0-0.18 wt% by energy spectrum detection of area C, and the iodine content is 0.37-0.63 wt% by energy spectrum detection of area D.
FIG. 2 is a graph showing the results of control and experimental group materials CCK8 experiments 1d and 3 d.
FIG. 3 is a diagram of the result of the detection of the bacteriostatic property of the material, wherein: a is a control group, common titanium alloy; and B is the titanium alloy of the experimental group and the improved coating.
Detailed Description
The improved iodine-carrying titanium alloy antibacterial implant for resisting infection and the preparation method thereof are further described in detail with reference to the accompanying drawings 1-3.
The invention relates to an anti-infection improved iodine-carrying titanium alloy antibacterial implant and a preparation method thereof, wherein the specific implementation process of the anti-infection improved iodine-carrying titanium alloy antibacterial implant comprises the following steps:
1. the titanium alloy base material with the roughness Ra of 0-0.4 mu m (provided by Zhejiang Uhui medical instruments Co., Ltd.) is pretreated by acetone (not less than 99.5%), ethylene glycol (not less than 99.5%), ultrapure water and the like in sequence, then the material is put into a solution system containing HF (not less than 40%, 20ml/L), HNO3 (65.0-68.0%, 80ml/L) and H3PO4 (85%, 15ml/L) for acid cleaning for 15min, and finally ultrasonic cleaning is carried out for 3 times and blow drying is carried out.
2. Carrying out anodic oxidation operation on the material treated in the step 1, wherein the specific steps are as follows: dissolving 95.0-98.0 wt% of sulfuric acid (CAS #7664-93-9, 35 ml/; L, national drug group chemical agents Co., Ltd.), 85 wt% of phosphoric acid (aladdin, CAS #7664-38-2, 25ml/L) and 30-31% of hydrogen peroxide (aladdin, CAS #7722-84-1, 10ml/L) in water to prepare an electrolyte, fixing the material on an anode side, wherein the distance between the anode side and the cathode side is 10-20cm, and the reaction conditions are as follows: the voltage is 150V, the frequency is 1000HZ, the water temperature is controlled at 30-50 ℃, and the reaction time is 5 min; and finally, placing the sample subjected to the oxidation operation in an aqueous solution for ultrasonic immersion cleaning for 3min, and repeating the cleaning operation for 3 times.
3. The material treated in step 2 was placed in a reaction solution containing 3g/L potassium iodide (Aladdin, CAS #7681-11-0), 2.5g/L beta-cyclodextrin (Michelin, CAS #7585-39-9), and 1g/L povidone-iodine powder (Roen reagent CAS # 25655-41-8). The material is firstly fixed on the anode side, the distance between the anode and the cathode is kept between 10 cm and 20cm under the conditions of constant pressure of 120V, initial current density of 0.5A/dm2 and light shielding, and the temperature of the reaction liquid is kept between 20 ℃ and 50 ℃ for reaction for 5 min; then the positions of the cathode and anode electrified joints are exchanged, and the reaction is carried out for 5min under the reaction conditions, thus completing a reaction cycle. Repeating the circulation for 5 times, washing the materials with purified water, blow-drying, and sterilizing by irradiation for later use.
4. The modified iodine-carrying material is subjected to a CCK-8 experiment, and the experimental result shows that the three batches of materials subjected to repeated experiments have no obvious cell proliferation activity difference in the group on the 1 st day and the 3 rd day of cell co-culture. Therefore, we can consider that the improved iodine-carrying titanium alloy material has no obvious cytotoxicity (as shown in fig. 2, the experimental group is a titanium alloy containing silver and iodine elements on the surface, the control group is a common titanium alloy, and the results are shown in the figure that the human-derived bone marrow mesenchymal stem cells are cultured in vitro on the material surface for 24h and 72 h).
5. The improved iodine-carrying material has the antibacterial effect and stability test: dividing the titanium alloy sample into a control group (A group) and a B group; the group A samples are prepared into iodine-carrying titanium alloy sample wafers according to the prior art (the preparation process refers to Chinese patent document CN 102416202A); and preparing the group B samples according to the steps 1-3 to obtain the improved iodine-carrying sample. The samples of group A and group B are placed in an environment with natural illumination and room temperature of 20-30 ℃ for 24h and 72h, the obtained sample wafer is subjected to bacteriostasis detection, the obtained result is shown in figure 3, the bacteria in the sample wafer of group B are far less than that in group A, and the improved iodine-carrying material has a remarkable bacteriostasis effect.
The present invention and its embodiments have been described above, and the description is not intended to be limiting, and the drawings are only one embodiment of the present invention, and the actual structure is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. An anti-infective improvement type carries antibiotic implant of iodine titanium alloy, includes titanium alloy material, its characterized in that: a porous micro-nano structure is constructed on the surface of the titanium alloy material, and povidone iodine is deposited and attached to the surface of the porous micro-nano structure to form an antibacterial coating.
2. The improved anti-infective titanium-iodine-carrying alloy antibacterial implant as claimed in claim 1, wherein: the porous micro-nano structure is a porous film structure, and the thickness range of the film is 5-25 mu m.
3. The improved anti-infective titanium-iodine-carrying alloy antibacterial implant as claimed in claim 1, wherein: the thickness of the antibacterial coating is 10-20 mu m, and the iodine content on the surface is 0.1-1 wt%.
4. The method for preparing an anti-infective improved iodine-carrying titanium alloy antibacterial implant as claimed in claim 1, wherein the method comprises the following steps: the method comprises the following steps:
step 1, constructing a porous micro-nano structure on the surface of a titanium alloy material;
step 2, povidone iodine is deposited and attached to the surface of the porous micro-nano structure through improved electrochemical treatment to form a coating with an antibacterial effect;
5. the method for preparing an anti-infective improved iodine-carrying titanium alloy antibacterial implant according to claim 4, wherein the method comprises the following steps: the porous micro-nano structure is a porous film structure formed after anodic oxidation or micro-arc oxidation treatment, and the thickness range of the film is 5-25 mu m.
6. The method for preparing an anti-infective improved iodine-carrying titanium alloy antibacterial implant according to claim 5, wherein the method comprises the following steps: the anodic oxidation or micro-arc oxidation treatment is electrolytic treatment which adopts an acid electrolytic cell or an alkaline electrolytic cell as electrolyte, applies a current of 200-1000Hz to the titanium alloy substrate in the electrolyte, maintains the voltage within the range of 100-500V, and has the electrifying time of 3-6min and the electrolyte temperature of 10-50 ℃.
7. The method for preparing an anti-infective improved iodine-carrying titanium alloy antibacterial implant according to claim 4, wherein the method comprises the following steps: the improved electrochemical treatment is realized by utilizing cathode-anode circulation alternation in a reaction liquid system of iodine-containing solution under the condition of keeping out of the sun.
8. The method for preparing an anti-infective improved iodine-carrying titanium alloy antibacterial implant according to claim 7, wherein the method comprises the following steps: the cathode and anode cycle alternation process comprises the following steps: the material is firstly fixed on a titanium-based hook or a basket on the anode side, and the reaction is carried out for 2-60min at the constant pressure of 100-200V, the initial current density of 0.5A/dm2, the distance between the anode and the cathode is kept at 10-20cm, and the temperature of the reaction liquid is in the range of 10-50 ℃; and then interchanging lead connectors connected with the anode and the cathode of the power supply, and reacting for 2-10min under the reaction conditions of the same voltage, initial current density, cathode-anode distance and solution temperature, thus completing a reaction cycle. Repeating the circulation for 3-10 times, washing the materials with purified water, and blow-drying.
9. The method for preparing an anti-infective improved iodine-carrying titanium alloy antibacterial implant according to claim 7, wherein the method comprises the following steps: the iodine-containing solution is an aqueous solution containing potassium iodide, povidone iodine and beta-cyclodextrin.
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WO2023077953A1 (en) * 2021-11-08 2023-05-11 浙江大学 Anti-infection improved iodine-loaded titanium alloy antibacterial implant and production method therefor

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