CN115252890B - Copper ferrite-MXene polymer composite antibacterial tracheal stent and preparation method thereof - Google Patents
Copper ferrite-MXene polymer composite antibacterial tracheal stent and preparation method thereof Download PDFInfo
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- CN115252890B CN115252890B CN202210886483.4A CN202210886483A CN115252890B CN 115252890 B CN115252890 B CN 115252890B CN 202210886483 A CN202210886483 A CN 202210886483A CN 115252890 B CN115252890 B CN 115252890B
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- mxene
- copper ferrite
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 122
- 239000010949 copper Substances 0.000 title claims abstract description 122
- 239000002131 composite material Substances 0.000 title claims abstract description 101
- 229920000642 polymer Polymers 0.000 title claims abstract description 79
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 102
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 15
- -1 iron ions Chemical class 0.000 claims abstract description 14
- 238000000110 selective laser sintering Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007943 implant Substances 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 238000010907 mechanical stirring Methods 0.000 claims description 9
- 239000002064 nanoplatelet Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 239000002135 nanosheet Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229960003280 cupric chloride Drugs 0.000 claims description 5
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000000149 argon plasma sintering Methods 0.000 claims description 3
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 3
- 239000004626 polylactic acid Substances 0.000 claims description 3
- 229920000954 Polyglycolide Polymers 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229920002463 poly(p-dioxanone) polymer Polymers 0.000 claims description 2
- 229920001610 polycaprolactone Polymers 0.000 claims description 2
- 239000004632 polycaprolactone Substances 0.000 claims description 2
- 239000000622 polydioxanone Substances 0.000 claims description 2
- 239000004633 polyglycolic acid Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 229910052596 spinel Inorganic materials 0.000 claims description 2
- 239000011029 spinel Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 7
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001431 copper ion Inorganic materials 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 230000003848 cartilage regeneration Effects 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 abstract 1
- 229920001432 poly(L-lactide) Polymers 0.000 description 23
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 12
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 230000002349 favourable effect Effects 0.000 description 6
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 description 6
- 239000004310 lactic acid Substances 0.000 description 6
- 235000014655 lactic acid Nutrition 0.000 description 6
- 229920002521 macromolecule Polymers 0.000 description 6
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 208000035143 Bacterial infection Diseases 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 230000001580 bacterial effect Effects 0.000 description 4
- 208000022362 bacterial infectious disease Diseases 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 208000015181 infectious disease Diseases 0.000 description 4
- 108010024636 Glutathione Proteins 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229960003180 glutathione Drugs 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 206010059866 Drug resistance Diseases 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 108090000765 processed proteins & peptides Proteins 0.000 description 2
- 102000004196 processed proteins & peptides Human genes 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 210000003437 trachea Anatomy 0.000 description 2
- 208000032170 Congenital Abnormalities Diseases 0.000 description 1
- 206010010356 Congenital anomaly Diseases 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Natural products OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- 206010039203 Road traffic accident Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000033115 angiogenesis Effects 0.000 description 1
- 230000002924 anti-infective effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000021164 cell adhesion Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000004962 mammalian cell Anatomy 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000001126 phototherapy Methods 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003642 reactive oxygen metabolite Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- 241000894007 species Species 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000017423 tissue regeneration Effects 0.000 description 1
- 210000005092 tracheal tissue Anatomy 0.000 description 1
Classifications
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
- A61F2/02—Prostheses implantable into the body
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- A61F2/02—Prostheses implantable into the body
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- A61F2210/00—Particular material properties of prostheses classified in groups A61F2/00 - A61F2/26 or A61F2/82 or A61F9/00 or A61F11/00 or subgroups thereof
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- A61F2240/00—Manufacturing or designing of prostheses classified in groups A61F2/00 - A61F2/26 or A61F2/82 or A61F9/00 or A61F11/00 or subgroups thereof
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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
- A61L2300/40—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
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Abstract
The invention discloses a copper ferrite-MXene polymer composite antibacterial tracheal stent and a preparation method thereof, comprising the following steps: copper grows ferrite on MXene in situ to prepare copper ferrite-MXene heterojunction composite powder, the prepared copper ferrite-MXene heterojunction composite powder is added into ethanol to prepare ethanol suspension, the ethanol suspension is ultrasonically mixed with high polymer ethanol suspension, centrifugal drying is carried out to obtain copper ferrite-MXene and high polymer composite powder, and finally the copper ferrite-MXene high polymer composite antibacterial air tube bracket is prepared through a selective laser sintering technology. The copper ferrite-MXene polymer composite antibacterial tracheal stent prepared by the invention can generate local high temperature and a large amount of active oxygen under the excitation of near infrared light as a novel tracheal implant material, thereby playing a good bactericidal role, and simultaneously, copper ions and iron ions released by the copper ferrite-MXene polymer composite antibacterial tracheal stent also have the function of promoting tracheal cartilage regeneration.
Description
Technical Field
The invention belongs to the technical field of preparation of compound materials, and particularly relates to a copper ferrite-MXene polymer composite antibacterial tracheal stent and a preparation method thereof.
Background
Segmental tracheal defects are often caused by congenital deformities, traffic accidents, tumors, and infections. When the defect length of the adult exceeds 6 cm or 1/3 of the child's trachea, normal tracheal structure and function cannot be restored by conventional surgery. In general, long segment tracheal defects require implantation of a suitable artificial airway stent. The occurrence of poly-L-lactic acid (macromolecule) biodegradable stent can overcome the limitation of permanently implanted stent, macromolecule can be naturally degraded in vivo, and lactic acid produced by degradation can be completely metabolized by human body. However, the macromolecule degradation can make the local microenvironment of the human body acidic, and meanwhile, the trachea is directly communicated with the external environment, so that bacterial infection is easily caused, and the clinical restoration effect is seriously affected. Therefore, developing a polymer composite airway stent with excellent, durable and safe antibacterial functions has important significance for treating implantation-related infections.
In order to solve the problem of bacterial infection caused by implants, various agents including antibiotics, heavy metal ions and their oxides, antibacterial peptides, quaternary ammonium salt compounds, etc. have been proved to be a good sterilization strategy. Among them, antibiotics are potent antibacterial drugs, but their widespread abuse has led to bacterial resistance, which has become a serious problem in the medical field and our living environment. Heavy metals/oxides have long been widely used in the field of sterilization as antibacterial agents. However, they have toxic side effects on specific types of mammalian cells. Antibacterial peptides are novel efficient antibacterial agents, but their application is limited due to the difficulty in synthesis and high cost. The quaternary ammonium salt compound is an efficient and convenient antibacterial agent, but can also generate drug resistance after long-term use.
With the development of light responsive materials, phototherapy has proven to be a promising therapeutic option in the antibacterial field because of its high efficiency, better selectivity, minimal invasiveness and side effects. Recently, copper ferrite (copper ferrite) nanoparticles have received a great deal of attention in the fields of photocatalysis and antibacterial because of their good chemical stability, high catalytic ability, wide near infrared light absorption and excellent Fenton reaction ability. In addition, copper ions and iron ions released from copper ferrite can oxidize glutathione inside bacteria and be reduced to monovalent copper ions and divalent iron ions. Subsequently, due to the high concentration of hydrogen peroxide in the bacterial infection microenvironment, the monovalent copper ions and divalent iron ions are able to further convert endogenous hydrogen peroxide into hydroxyl radicals and be oxidized into divalent copper ions and trivalent iron ions, eventually achieving a self-circulating effect. Self-circulation of these ions can dramatically deplete glutathione within the bacteria, thereby increasing endogenous reactive oxygen species levels. In addition, copper and iron ions can promote tracheal regeneration, which is critical for regeneration of tracheal tissue after anti-infection. However, the narrow band gap easily causes rapid recombination of photo-generated carriers of copper ferrite, and seriously affects the antibacterial effect thereof.
Ti 3 C 2 T x The (MXene) is a novel environment-friendly two-dimensional nanomaterial, has strong near infrared absorption, high photo-thermal conversion efficiency and high conductivity, and can adjust the bandwidth of a semiconductor. Meanwhile, the surface end of MXene may be modified with various functional groups, which provides a large number of active sites for semiconductors. When the copper ferrite forms heterojunction with the carrier surface, the separation of photo-generated carriers can be accelerated, thereby generating more active oxygen. However, in the prior art, there is no study of preparing a tracheal stent by compounding copper ferrite with MXene and incorporating the copper ferrite into a polymer.
Because bacterial infection is easy to be caused after the tracheal stent is transplanted, bacterial drug resistance is easy to be caused by traditional antibiotic treatment, and although some heavy metals and oxides thereof have good antibacterial performance, toxic and side effects of organisms are caused. Based on the above problems, there is an urgent need to develop a safer, longer and more efficient antimicrobial pattern to cope with infection associated with tracheal stent graft.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a copper ferrite-MXene polymer composite antibacterial tracheal stent, which is prepared by growing copper ferrite on MXene in situ to prepare copper ferrite-MXene heterojunction composite powder, adding the prepared copper ferrite-MXene heterojunction composite powder into ethanol to prepare ethanol suspension, mixing with ethanol suspension of polymer, centrifuging, drying to obtain copper ferrite-MXene and polymer composite powder, and finally preparing the copper ferrite-MXene polymer composite antibacterial tracheal stent by selective laser sintering technology.
Preferably, the copper ferrite is spinel copper ferrite, and the polymer is at least one of polylactic acid, polyglycolic acid, polylactic acid-hydroxy glycolic acid copolymer, polycaprolactone, and polydioxanone.
Preferably, in the copper ferrite-MXene/polymer composite antibacterial tracheal stent, the mass fraction of the copper ferrite-MXene heterojunction composite powder is 2-10wt%, the mass fraction of the polymer is 90-98wt%, the particle size of the polymer is 40-60 μm, and the particle size of the copper ferrite-MXene heterojunction composite powder is 1-4 μm.
The preparation method of the copper ferrite-MXene/polymer composite antibacterial tracheal stent comprises the following steps:
firstly, completely dissolving lithium fluoride in concentrated hydrochloric acid, wherein the mass-volume ratio of the lithium fluoride to the concentrated hydrochloric acid is 1g:20mL, and then adding Ti 3 AlC 2 Slowly adding Ti into the reaction solution 3 AlC 2 The mass ratio of the lithium fluoride to the lithium fluoride is 1:1, and stirring is carried out for a first preset time at a first temperature; then centrifuging the product until the pH value reaches above a first preset pH value, and freeze-drying the product overnight to obtain etched Ti 3 C 2 (MXene) nanoplatelets;
step two, preparing the prepared Ti 3 C 2 (MXene) nanosheets dissolved in deionized water, ti 3 C 2 The mass-to-volume ratio of the (MXene) nanosheets to the deionized water is 1g to 2mL, and the nanosheets are subjected to ultrasonic treatment for a second preset time; then adding ferric chloride hexahydrate, cupric chloride dihydrate and Ti in a first mass ratio and stirring for a third preset time 3 C 2 (MXene) nanoplateletsThe mass ratio is 0.7:0.35:0.05; then adjusting the pH value to a second preset pH value by sodium hydroxide, continuously stirring for a fourth preset time at a second preset temperature, transferring the obtained solution into a polytetrafluoroethylene autoclave, and heating for a fifth preset time at a third preset temperature; finally, the obtained product is centrifugally washed by deionized water at a high speed, and dried to obtain copper ferrite-MXene heterojunction composite powder; weighing a certain amount of copper ferrite-MXene heterojunction composite powder and high polymer powder according to a second preset mass ratio, adding the copper ferrite-MXene heterojunction composite powder and the high polymer powder into a flask containing an absolute ethyl alcohol solution, uniformly dispersing the copper ferrite-MXene heterojunction composite powder and the high polymer powder through mechanical stirring and ultrasonic dispersion to obtain a mixed solution, and centrifugally drying the mixed solution to obtain the copper ferrite-MXene/high polymer composite powder;
and fourthly, placing the copper ferrite-MXene/polymer composite powder into a selective laser sintering system, sintering layer by layer according to a pre-established three-dimensional model, and removing unsintered powder after sintering is finished to obtain the copper ferrite-MXene polymer composite antibacterial air pipe bracket.
Preferably, in the first step, the particle diameter of the lithium fluoride powder is 200-400 nm, and the concentration of the concentrated hydrochloric acid is 9mol/L.
Preferably, in the first step, the first temperature is 35 ℃, the first preset time is 24 hours, and the first preset pH value is 6.
Preferably, in the second step, the second preset time is 30min, the ultrasonic power is 500W, and the first mass ratio is 2:1, wherein the third preset time is 1h, the concentration of the added sodium hydroxide solution is 1mol/L, the second preset pH value is 11, the second preset temperature is 85 ℃, the fourth preset time is 8h, the third preset temperature is 120 ℃, and the fifth preset time is 12h;
in the third step, the second preset mass ratio is 2-10: 90-98 g of copper ferrite-MXene heterojunction composite powder and polymer powder with the total mass of 1g correspond to 20mL of absolute ethanol solution.
Preferably, in the fourth step, in the laser sintering process, the laser power of the selective laser sintering system is 1-2W, the scanning speed is 100-300 mm/s, the scanning interval is 0.08-0.12 mm, the spot diameter is 0.3-1.0 mm, the thickness of the powder layer corresponding to the copper ferrite-MXene/polymer composite powder is 0.1mm, and the preheating temperature of the corresponding powder bed is 140-160 ℃.
Preferably, the copper ferrite-MXene/polymer composite antibacterial tracheal stent is applied to a novel tracheal implant material.
The invention at least comprises the following beneficial effects: the invention relates to a 3D printing copper ferrite-MXene/polymer composite antibacterial tracheal stent and a preparation method thereof, wherein the copper ferrite-MXene/polymer composite tracheal stent is prepared by a selective laser sintering technology, and has the characteristics of favorable porosity, favorable nutrient substance transmission, angiogenesis and tissue regeneration, favorable cell adhesion, favorable bioactivity and biocompatibility, safer and more efficient photoresponse antibacterial performance, favorable cartilage regeneration promoting capacity and the like due to favorable porosity. Meanwhile, the material has good degradation capacity and does not need to be taken out twice by operation.
In summary, the copper ferrite-MXene/polymer composite powder prepared by the invention, the used selective laser sintering technology and the copper ferrite-MXene content in the composite material are crystallized through multiple experiments and creative efforts of the inventor, and the copper ferrite-MXene/polymer composite bracket is prepared by controlling the content of the copper ferrite-MXene and adjusting the technological parameters of a laser sintering system so as to solve the problems of related infection of implants and the like, and is expected to be applied to the biomedical field.
The copper ferrite-MXene polymer composite antibacterial tracheal stent prepared by the invention is used as a novel tracheal implant material, the copper ferrite-MXene polymer composite antibacterial tracheal stent is prepared from copper ferrite-MXene/polymer composite powder based on a 3D printing technology, wherein polylactic acid has excellent biodegradability and biocompatibility, the copper ferrite-MXene composite can generate local temperature rise and a large amount of active oxygen under the irradiation of near infrared light, the copper ferrite-MXene composite can have good sterilization effect on staphylococcus aureus and pseudomonas aeruginosa, the antibacterial rate of the prepared copper ferrite-MXene/polymer composite tracheal stent reaches more than 90%, and released copper ions and iron ions have good cartilage differentiation promoting capability.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a scanning electron microscope image of the copper ferrite-MXene polymer compound powder prepared in example 1 of the present invention;
FIG. 2 is a schematic diagram of a copper ferrite-MXene polymer composite antibacterial tracheal stent prepared in example 1 of the present invention;
FIG. 3 shows a copper ferrite-MXene Polymer composite antibacterial airway stent (CFOM/PLLA) and PLLA (poly-L-lactic acid), MXene/PLLA, cuFe prepared by example 1 of the present invention 2 O 4 Schematic of antibacterial test results performed on PLLA material tracheal stent.
Detailed Description
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
The embodiment provides a preparation method of a copper ferrite-MXene polymer composite antibacterial tracheal stent, which comprises the following steps:
firstly, 1g of lithium fluoride with the grain diameter of 200-400 nm is completely dissolved in 20mL of concentrated hydrochloric acid with the concentration of 9mol/L, and then 1g of Ti is dissolved 3 AlC 2 Slowly adding the mixture into the reaction solution, and stirring the mixture for 24 hours at a first temperature; then centrifuging the product until the pH reaches above 6, and freeze drying overnight to obtain etched productTi 3 C 2 (MXene) nanoplatelets;
step two, 10mg of prepared Ti 3 C 2 (MXene) nanoplatelets were dissolved in 20mL deionized water and sonicated for 30min; subsequently, 140mg of ferric chloride hexahydrate and 70mg of cupric chloride dihydrate were added respectively and stirred for 1 hour; then the pH was adjusted to 11 with sodium hydroxide and stirring was continued for 8 hours at 85℃and then the resulting solution was transferred to a polytetrafluoroethylene autoclave and heated at 120℃for 12 hours; finally, the obtained product is centrifugally washed by deionized water at a high speed, and dried to obtain copper ferrite-MXene heterojunction composite powder;
respectively weighing copper ferrite-MXene heterojunction composite powder and poly-left lactic acid powder according to the mass ratio of 2:98, adding the copper ferrite-MXene heterojunction composite powder and the poly-left lactic acid powder into a flask containing 20mL of absolute ethyl alcohol solution, wherein the total mass of the copper ferrite-MXene heterojunction composite powder and the poly-left lactic acid powder is 1g, the particle size of the poly-left lactic acid powder is 40-60 mu m, the particle size of the copper ferrite-MXene heterojunction composite powder is 1-4 mu m, uniformly dispersing the copper ferrite-MXene heterojunction composite powder and the poly-left lactic acid powder by mechanical stirring and ultrasonic dispersing, obtaining a mixed solution with the mechanical stirring rate of 800r/min, and centrifugally drying the mixed solution to obtain the copper ferrite-MXene/macromolecule composite powder;
and fourthly, placing the copper ferrite-MXene/polymer composite powder in a selective laser sintering system, wherein the laser power is 1W, the scanning speed is 100mm/s, the scanning interval is 0.08mm, the light spot diameter is 0.3mm, performing layer-by-layer sintering according to a pre-established three-dimensional model, wherein the thickness of a powder layer corresponding to the copper ferrite-MXene/polymer composite powder is 0.1mm, the preheating temperature of a corresponding powder bed is 140 ℃, and removing unsintered powder after sintering is completed, so that the copper ferrite-MXene polymer composite antibacterial air pipe bracket is obtained.
The copper ferrite-MXene polymer composite antibacterial tracheal stent prepared by the embodiment is applied to a novel tracheal implant material, an electron microscope scanning diagram of the copper ferrite-MXene polymer composite powder obtained in the preparation process is shown in figure 1, the copper ferrite uniformly grows on the surface of MXene, and the copper ferrite-MXene heterojunction can be seen from the diagramSuccessfully synthesizing; the tracheal stent model prepared in this example is shown in fig. 2. Copper ferrite-MXene high polymer composite antibacterial tracheal stent (CFOM/PLLA) and PLLA (poly-L-lactic acid), MXene/PLLA and CuFe prepared in example 1 of the invention are used respectively 2 O 4 The PLLA material bracket is used for carrying out an antibacterial experiment, and the antibacterial experiment operation is as follows: staphylococcus aureus (s.aureus, atcc.25923) was selected as the experimental strain.
First, 1×10 is selected 6 Bacterial species were cultured on different tracheal stents at 37℃for 24 hours. Then, the sample was irradiated under near infrared light for 15 minutes, the scaffold was removed and gently washed with PBS, 1ml of bacterial medium was added and shaken for 10 minutes. The resulting bacterial suspension was diluted 10000 times, and 100. Mu.L of the liquid was then taken out and dropped onto an agar plate, and the mixture was spread with a spreader. Then, the plate was incubated at 37℃for 24 hours, an image of the colony of the agar plate was taken with a digital camera, and the colony count was calculated with image J. The antibacterial ratio was calculated according to the following formula:
antibacterial ratio= (colony count control-colony count experiment)/colony count control×100%
The antibacterial rate data of the obtained tracheal stents made of the materials are shown in fig. 3, and can be seen from fig. 3: in the no-light group (NIR-), all groups showed no antibacterial properties, whereas inside the light group (nir+), the MXene/PLLA group showed some antibacterial properties, possibly due to the locally high temperature of MXene/PLLA,
the copper ferrite-MXene polymer composite antibacterial tracheal stent (CFOM/PLLA) prepared in the embodiment shows the best antibacterial capability in all groups, and the antibacterial rate of the copper ferrite-MXene polymer composite antibacterial tracheal stent to staphylococcus aureus reaches 96.49% respectively, because the CFOM has better photo-thermal, photo-catalytic and glutathione consumption capabilities.
Example 2
The embodiment provides a preparation method of a copper ferrite-MXene polymer composite antibacterial tracheal stent, which comprises the following steps:
first, 1g of lithium fluoride having a particle diameter of 200 to 400nm was completely dissolved in 20mL of concentrated hydrochloric acid having a concentration of 9mol/L, followed by 1g of Ti 3 AlC 2 Slowly adding into the reaction solution at a first temperatureStirring for 24 hours at the same temperature; subsequently, centrifuging the product until the pH reaches above 6, and freeze-drying it overnight to obtain etched Ti 3 C 2 (MXene) nanoplatelets;
step two, 10mg of prepared Ti 3 C 2 (MXene) nanoplatelets were dissolved in 20mL deionized water and sonicated for 30min; subsequently, 140mg of ferric chloride hexahydrate and 70mg of cupric chloride dihydrate were added respectively and stirred for 1 hour; then the pH was adjusted to 11 with sodium hydroxide and stirring was continued for 8 hours at 85℃and then the resulting solution was transferred to a polytetrafluoroethylene autoclave and heated at 120℃for 12 hours; finally, the obtained product is centrifugally washed by deionized water at a high speed, and dried to obtain copper ferrite-MXene heterojunction composite powder;
step three, according to 5:95, respectively weighing copper ferrite-MXene heterojunction composite powder and poly-L-lactic acid powder according to the mass ratio, adding the copper ferrite-MXene heterojunction composite powder and the poly-L-lactic acid powder into a flask containing 20mL of absolute ethyl alcohol solution, wherein the total mass of the copper ferrite-MXene heterojunction composite powder and the poly-L-lactic acid powder is 1g, the particle size of the poly-L-lactic acid powder is 40-60 mu m, the particle size of the copper ferrite-MXene heterojunction composite powder is 1-4 mu m, uniformly dispersing the copper ferrite-MXene heterojunction composite powder and the poly-L-lactic acid powder by mechanical stirring and ultrasonic dispersing, obtaining a mixed solution with the mechanical stirring rate of 900r/min, and centrifugally drying the mixed solution to obtain copper ferrite-MXene/macromolecule composite powder;
and fourthly, placing the copper ferrite-MXene/polymer composite powder in a selective laser sintering system, wherein the laser power is 1.5W, the scanning speed is 200mm/s, the scanning interval is 0.10mm, the light spot diameter is 0.7mm, performing layer-by-layer sintering according to a pre-established three-dimensional model, the thickness of a powder layer corresponding to the copper ferrite-MXene/polymer composite powder is 0.1mm, the preheating temperature of a corresponding powder bed is 150 ℃, and removing unsintered powder after sintering is completed, so that the copper ferrite-MXene polymer composite antibacterial air pipe bracket is obtained.
Example 3
The embodiment provides a preparation method of a copper ferrite-MXene polymer composite antibacterial tracheal stent, which comprises the following steps:
firstly, 1g of lithium fluoride with the grain diameter of 200-400 nm is completely dissolved in 20mL of concentrated hydrochloric acid with the concentration of 9mol/L, and then 1g of Ti is dissolved 3 AlC 2 Slowly adding the mixture into the reaction solution, and stirring the mixture for 24 hours at a first temperature; subsequently, centrifuging the product until the pH reaches above 6, and freeze-drying it overnight to obtain etched Ti 3 C 2 (MXene) nanoplatelets;
step two, 10mg of prepared Ti 3 C 2 (MXene) nanoplatelets were dissolved in 20mL deionized water and sonicated for 30min; subsequently, 140mg of ferric chloride hexahydrate and 70mg of cupric chloride dihydrate were added respectively and stirred for 1 hour; then the pH was adjusted to 11 with sodium hydroxide and stirring was continued for 8 hours at 85℃and then the resulting solution was transferred to a polytetrafluoroethylene autoclave and heated at 120℃for 12 hours; finally, the obtained product is centrifugally washed by deionized water at a high speed, and dried to obtain copper ferrite-MXene heterojunction composite powder;
step three, according to 10:90 mass ratio, respectively weighing copper ferrite-MXene heterojunction composite powder and poly-L-lactic acid powder, adding the copper ferrite-MXene heterojunction composite powder and the poly-L-lactic acid powder into a flask containing 20mL of absolute ethyl alcohol solution, wherein the total mass of the copper ferrite-MXene heterojunction composite powder and the poly-L-lactic acid powder is 1g, the particle size of the poly-L-lactic acid powder is 40-60 mu m, the particle size of the copper ferrite-MXene heterojunction composite powder is 1-4 mu m, uniformly dispersing the copper ferrite-MXene heterojunction composite powder and the poly-L-lactic acid powder by mechanical stirring and ultrasonic dispersing, obtaining a mixed solution with the mechanical stirring rate of 1000r/min, and centrifugally drying the mixed solution to obtain copper ferrite-MXene/macromolecule composite powder;
and fourthly, placing the copper ferrite-MXene/polymer composite powder in a selective laser sintering system, wherein the laser power is 2W, the scanning speed is 300mm/s, the scanning interval is 0.12mm, the light spot diameter is 1.0mm, performing layer-by-layer sintering according to a pre-established three-dimensional model, the thickness of a powder layer corresponding to the copper ferrite-MXene/polymer composite powder is 0.1mm, the preheating temperature of a corresponding powder bed is 160 ℃, and after sintering is completed, removing unsintered powder, thereby obtaining the copper ferrite-MXene polymer composite antibacterial air pipe bracket.
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (5)
1. The preparation method of the copper ferrite-MXene/polymer composite antibacterial tracheal stent is characterized in that copper ferrite is grown on MXene in situ to prepare copper ferrite-MXene heterojunction composite powder, the prepared copper ferrite-MXene heterojunction composite powder is added into ethanol to prepare ethanol suspension, the ethanol suspension and the ethanol suspension of a polymer are ultrasonically mixed, centrifugally dried to obtain copper ferrite-MXene and polymer composite powder, and finally, the copper ferrite-MXene polymer composite antibacterial tracheal stent is prepared by a selective laser sintering technology;
the method specifically comprises the following steps:
firstly, completely dissolving lithium fluoride in concentrated hydrochloric acid, wherein the mass-volume ratio of the lithium fluoride to the concentrated hydrochloric acid is 1g:20mL, and then adding Ti 3 AlC 2 Slowly adding Ti into the reaction solution 3 AlC 2 The mass ratio of the lithium fluoride to the lithium fluoride is 1:1, and stirring is carried out for a first preset time at a first temperature; then centrifuging the product until the pH value reaches above a first preset pH value, and freeze-drying the product overnight to obtain etched Ti 3 C 2 (MXene) nanoplatelets;
step two, preparing the prepared Ti 3 C 2 (MXene) nanosheets dissolved in deionized water, ti 3 C 2 The mass-to-volume ratio of the (MXene) nanosheets to the deionized water is 1g to 2mL, and the nanosheets are subjected to ultrasonic treatment for a second preset time;then adding ferric chloride hexahydrate, cupric chloride dihydrate and Ti in a first mass ratio and stirring for a third preset time 3 C 2 The mass ratio of the (MXene) nanosheets is 0.7:0.35:0.05; then adjusting the pH value to a second preset pH value by sodium hydroxide, continuously stirring for a fourth preset time at a second preset temperature, transferring the obtained solution into a polytetrafluoroethylene autoclave, and heating for a fifth preset time at a third preset temperature; finally, the obtained product is centrifugally washed by deionized water at a high speed, and dried to obtain copper ferrite-MXene heterojunction composite powder;
weighing a certain amount of copper ferrite-MXene heterojunction composite powder and high polymer powder according to a second preset mass ratio, adding the copper ferrite-MXene heterojunction composite powder and the high polymer powder into a flask containing an absolute ethyl alcohol solution, uniformly dispersing the copper ferrite-MXene heterojunction composite powder and the high polymer powder through mechanical stirring and ultrasonic dispersion to obtain a mixed solution, and centrifugally drying the mixed solution to obtain the copper ferrite-MXene/high polymer composite powder;
step four, placing the copper ferrite-MXene/polymer composite powder in a selective laser sintering system, sintering layer by layer according to a pre-established three-dimensional model, and removing unsintered powder after sintering is completed to obtain the copper ferrite-MXene polymer composite antibacterial air pipe bracket;
in the first step, the first temperature is 35 ℃, the first preset time is 24 hours, and the first preset pH value is 6;
in the second step, the second preset time is 30min, the ultrasonic power is 500W, and the first mass ratio is 2:1, wherein the third preset time is 1h, the concentration of the added sodium hydroxide solution is 1mol/L, the second preset pH value is 11, the second preset temperature is 85 ℃, the fourth preset time is 8h, the third preset temperature is 120 ℃, and the fifth preset time is 12h;
in the third step, the second preset mass ratio is 2-10: 90-98, wherein the total mass of the copper ferrite-MXene heterojunction composite powder and the polymer powder is 1g, and the mechanical stirring speed is 800-1000 r/min, wherein the total mass of the copper ferrite-MXene heterojunction composite powder and the polymer powder corresponds to 20mL of absolute ethanol solution;
in the fourth step, in the laser sintering process, the laser power of the selective laser sintering system is 1-2W, the scanning speed is 100-300 mm/s, the scanning interval is 0.08-0.12 mm, the spot diameter is 0.3-1.0 mm, the thickness of a powder layer corresponding to the copper ferrite-MXene/polymer composite powder is 0.1mm, and the preheating temperature of a corresponding powder bed is 140-160 ℃.
2. The method for preparing the copper ferrite-MXene/polymer composite antibacterial tracheal stent according to claim 1, wherein the copper ferrite is spinel copper ferrite, and the polymer is at least one of polylactic acid, polyglycolic acid, polylactic acid-glycolic acid copolymer, polycaprolactone and polydioxanone.
3. The preparation method of the copper ferrite-MXene/polymer composite antibacterial tracheal stent according to claim 1, wherein the copper ferrite-MXene/polymer composite antibacterial tracheal stent comprises 2-10wt% of copper ferrite-MXene heterojunction composite powder, 90-98wt% of polymer, and 40-60 μm of polymer particle size, and 1-4 μm of copper ferrite-MXene heterojunction composite powder particle size.
4. The method for preparing the copper ferrite-MXene/polymer compound antibacterial tracheal stent according to claim 1, wherein in the first step, the particle size of the lithium fluoride powder is 200-400 nm, and the concentration of the concentrated hydrochloric acid is 9mol/L.
5. The method for preparing the copper ferrite-MXene/polymer compound antibacterial tracheal stent according to claim 1 or 2, wherein the copper ferrite-MXene/polymer compound antibacterial tracheal stent is applied to a novel tracheal implant material.
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| 3D打印气管支架植入成功;本刊讯;《中国医疗器械杂志》;第38卷(第4期);300 * |
| Fabrication of novel CuFeO/MXene hierarchical heterostructures for enhanced photocatalytic degradation of sulfonamides under visible light;Cao Y, et al;《Journal of Hazardous Materials》;2-3 * |
| Synthesis, characterization, photocatalytic and antibacterial properties of copper Ferrite/MXene (CuFe2O4/Ti3C2) nanohybrids;Ibrahim A. Alsafari et al;《Ceramics International 》;47(20);28875-28877 * |
| 自供电袭击骨支架的激光增材制造及其性能研究;刘国峰;硕士学位论文;全文 * |
| 载银纳米铁酸铜抗菌剂的制备及抗菌性能;廖辉伟;穆兰;童云;;有色金属(01);44-47 * |
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