CN115252890A - 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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- CN115252890A CN115252890A CN202210886483.4A CN202210886483A CN115252890A CN 115252890 A CN115252890 A CN 115252890A CN 202210886483 A CN202210886483 A CN 202210886483A CN 115252890 A CN115252890 A CN 115252890A
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- mxene
- copper ferrite
- powder
- polymer composite
- copper
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 115
- 239000010949 copper Substances 0.000 title claims abstract description 115
- 239000002131 composite material Substances 0.000 title claims abstract description 100
- 229920000642 polymer Polymers 0.000 title claims abstract description 78
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 91
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000000110 selective laser sintering Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 26
- 229920001432 poly(L-lactide) Polymers 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 13
- 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
- -1 polytetrafluoroethylene Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 239000002135 nanosheet Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000010907 mechanical stirring Methods 0.000 claims description 7
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims description 6
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 6
- 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 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002064 nanoplatelet Substances 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
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 238000000149 argon plasma sintering Methods 0.000 claims description 3
- 239000007943 implant Substances 0.000 claims description 3
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 3
- 239000004626 polylactic acid Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229920000954 Polyglycolide Polymers 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 229920000117 poly(dioxanone) Polymers 0.000 claims description 2
- 229920001610 polycaprolactone Polymers 0.000 claims description 2
- 239000004632 polycaprolactone Substances 0.000 claims description 2
- 239000004633 polyglycolic acid Substances 0.000 claims description 2
- 229910052596 spinel Inorganic materials 0.000 claims description 2
- 239000011029 spinel Substances 0.000 claims description 2
- 238000002513 implantation Methods 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
- 230000001954 sterilising effect Effects 0.000 abstract description 3
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 3
- 210000000845 cartilage Anatomy 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 abstract 1
- 230000005284 excitation Effects 0.000 abstract 1
- 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
- 229910052742 iron Inorganic materials 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 5
- 229910001431 copper ion Inorganic materials 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 208000015181 infectious disease Diseases 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
- 208000022362 bacterial infectious disease Diseases 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 108010024636 Glutathione Proteins 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 230000001580 bacterial effect Effects 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
- 239000007789 gas Substances 0.000 description 3
- 229960003180 glutathione Drugs 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 210000003437 trachea Anatomy 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 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
- 239000004065 semiconductor Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000017423 tissue regeneration Effects 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 206010010356 Congenital anomaly Diseases 0.000 description 1
- 206010059866 Drug resistance Diseases 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
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 230000003848 cartilage regeneration Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000021164 cell adhesion Effects 0.000 description 1
- 229940068911 chloride hexahydrate Drugs 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- VOAPTKOANCCNFV-UHFFFAOYSA-N hexahydrate;hydrochloride Chemical compound O.O.O.O.O.O.Cl VOAPTKOANCCNFV-UHFFFAOYSA-N 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
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- 230000036244 malformation Effects 0.000 description 1
- 210000004962 mammalian cell Anatomy 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 235000015097 nutrients Nutrition 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 239000003642 reactive oxygen metabolite Substances 0.000 description 1
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- 210000005092 tracheal tissue Anatomy 0.000 description 1
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Abstract
The invention discloses a copper ferrite-MXene polymer composite antibacterial tracheal stent and a preparation method thereof, wherein the preparation method comprises the following steps: the method comprises the steps of growing 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 the ethanol suspension with high-molecular ethanol suspension in an ultrasonic mode, conducting centrifugal drying to obtain copper ferrite-MXene and high-molecular composite powder, and finally obtaining the copper ferrite-MXene high-molecular composite antibacterial air pipe support through a selective laser sintering technology. The copper ferrite-MXene polymer composite antibacterial tracheal stent prepared by the method is used as a novel tracheal implantation material, can generate local high temperature and a large amount of active oxygen under the excitation of near infrared light, thereby playing a good sterilization role, and simultaneously zinc ions released by the copper ferrite-MXene polymer composite antibacterial tracheal stent also have the function of promoting the regeneration of tracheal cartilage.
Description
Technical Field
The invention belongs to the technical field of compound material preparation, 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 malformations, traffic accidents, tumors, and infections. When the length of the adult defect exceeds 6 cm or 1/3 of the trachea of the child, the normal trachea structure and function can not be recovered through the conventional operation. In general, long-length tracheal defects require the implantation of a suitable artificial airway stent. The occurrence of the poly-L-lactic acid (macromolecule) biodegradable stent can overcome the limitation of permanently implanting the stent, the macromolecule can be naturally degraded in vivo, and the lactic acid generated by degradation can be completely metabolized by the human body. However, the degradation of the polymer can make the local microenvironment of the human body acidic, and meanwhile, the trachea is directly communicated with the external environment, which is easy to cause bacterial infection and seriously affects the clinical repair effect. Therefore, the development of the polymer composite airway stent with excellent, durable and safe antibacterial functions has important significance for treating implantation-related infection.
In order to solve the problem of bacterial infection caused by implants, various medicaments, including antibiotics, heavy metal ions and oxides thereof, antibacterial peptides, quaternary ammonium salt compounds and the like, have been proved to be good sterilization strategies one by one. Among them, antibiotics are effective antibacterial drugs, but extensive abuse thereof has resulted in bacterial resistance, which has become a serious problem in the medical field and our living environment. Heavy metals/oxides have long been used extensively in the germicidal arts as antimicrobial agents. However, they have toxic side effects on specific types of mammalian cells. Antibacterial peptides are a new type of highly effective antibacterial agents, but their use is limited due to the difficulty and cost of synthesis. Quaternary ammonium compounds are highly effective, convenient antimicrobial agents, but also develop resistance to drugs after long-term use.
With the development of light responsive materials, phototherapy has proven to be a promising therapeutic option in the antibacterial field due to its high efficiency, better selectivity, minimal invasiveness and side effects. Recently, copper ferrite nanoparticles have received much attention in the fields of photocatalysis and antibacterium due to 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 by copper ferrite can oxidize glutathione inside bacteria and be reduced into monovalent copper ions and divalent iron ions. Subsequently, due to high concentrations of hydrogen peroxide in the microenvironment of bacterial infection, monovalent copper ions and divalent iron ions can further convert endogenous hydrogen peroxide into hydroxyl radicals and be oxidized into divalent copper ions and trivalent iron ions, and finally, a self-circulation effect is achieved. The self-circulation of these ions can significantly deplete glutathione from within the bacteria, thereby increasing endogenous reactive oxygen species levels. In addition, copper and iron ions can also promote tracheal regeneration, which is important for tracheal tissue regeneration after infection. However, the narrow band gap easily causes the fast recombination of the photo-generated carriers of the copper ferrite, and the antibacterial effect of the copper ferrite is seriously influenced.
Ti3C2Tx(MXene) is a novel environment-friendly two-dimensional nano material, has strong near infrared absorption, photo-thermal conversion efficiency and high conductivity, and can adjust the bandwidth of a semiconductor. Meanwhile, the surface terminal of MXene can be modified by various functional groups, which provides a large number of active sites for semiconductors. When the copper ferrite forms a heterojunction with the surface of the carrier, the separation of the photogenerated carriers can be accelerated, thereby generating more active oxygen. However, in the prior art, the research of preparing the tracheal stent by compounding and doping the copper ferrite with MXene into high polymer is not available.
Because the tracheal stent is easy to cause bacterial infection after being transplanted, the traditional antibiotic treatment is easy to cause bacterial drug resistance, and some heavy metals and oxides thereof have good antibacterial performance but can cause toxic and side effects of organisms. Based on the problems, a safer, long-lasting and efficient antibacterial mode is urgently needed to be developed to treat the infection related to the tracheal stent transplantation.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
In order to realize the purposes and other advantages according to the invention, the copper ferrite-MXene polymer composite antibacterial gas pipe support is provided, wherein copper ferrite grows 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 polymer ethanol suspension, centrifugal drying is carried out to obtain copper ferrite-MXene and polymer composite powder, and finally the copper ferrite-MXene polymer composite antibacterial gas pipe support is prepared by a selective laser sintering technology.
Preferably, the copper ferrite is spinel type copper ferrite, and the polymer is at least one of polylactic acid, poly-L-lactic acid, polyglycolic acid, polylactic acid-glycolic acid copolymer, polycaprolactone and poly-p-dioxanone.
Preferably, in the copper ferrite-MXene/polymer composite antibacterial tracheal stent, the mass fraction of the copper ferrite-MXene heterojunction composite powder is 2-10 wt%, the mass fraction of the polymer is 90-98 wt%, 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.
A preparation method of a 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 1g3AlC2Slowly added to the reaction solution, ti3AlC2Stirring the mixture and lithium fluoride at a first temperature for a first preset time, wherein the mass ratio of the mixture to the lithium fluoride is 1; subsequently, the product is centrifuged until the pH reaches above a first predetermined pH and freeze-dried overnight to obtain etched Ti3C2(MXene) nanoplatelets;
step two, the prepared Ti3C2Dissolving (MXene) nanosheets in deionized water, ti3C2The mass-volume ratio of the (MXene) nanosheets to the deionized water is 1g, 2mL, and the ultrasonic treatment is carried out for a second preset time; then adding ferric chloride hexahydrate and copper chloride dihydrate in a first mass ratio and stirring for a third preset timeFerric chloride hexahydrate, cupric chloride dihydrate and Ti3C2The mass ratio of the (MXene) nanosheets is 0.7; then adjusting the pH value to a second preset pH value by using sodium hydroxide, continuously stirring for a fourth preset time at a second preset temperature, then transferring the obtained solution into a polytetrafluoroethylene high-pressure kettle, and heating for a fifth preset time at a third preset temperature; finally, the obtained product is washed by deionized water in a high-speed centrifugal mode and dried, and finally copper ferrite-MXene heterojunction composite powder is obtained; step three, weighing a certain amount of copper ferrite-MXene heterojunction composite powder and polymer powder according to a second preset mass ratio, adding the copper ferrite-MXene heterojunction composite powder and the polymer powder into a flask containing absolute ethanol solution, uniformly dispersing the copper ferrite-MXene heterojunction composite powder and the polymer powder through mechanical stirring and ultrasonic dispersion to obtain a mixed solution, and then centrifugally drying the mixed solution to obtain the copper ferrite-MXene/polymer composite powder;
and 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 finished to obtain the copper ferrite-MXene polymer composite antibacterial gas pipe support.
Preferably, in the first step, the particle size of the lithium fluoride powder is 200 to 400nm, 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, the third preset time is 1 hour, 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 8 hours, the third preset temperature is 120 ℃, and the fifth preset time is 12 hours;
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 implantation 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 hydrophilicity, favorable cell adhesion, favorable bioactivity and biocompatibility, safer and more efficient photoresponse antibacterial performance, favorable cartilage regeneration promoting capability and the like due to favorable porosity and favorable generation of nutrient substances, blood vessels and tissue regeneration. Meanwhile, the degradable biological material has good degradation capability and does not need to be taken out again after operation.
In conclusion, the copper ferrite-MXene/polymer composite powder prepared by the method, the used selective laser sintering technology and the copper ferrite-MXene content in the composite material are crystallized through multiple experiments and creative labor of the inventor, and the copper ferrite-MXene/polymer composite stent prepared by the method disclosed by the invention is expected to be applied to the field of biomedicine and can solve the problems of implant-related infection and the like by controlling the content of the copper ferrite-MXene and adjusting the process parameters of a laser sintering system.
The copper ferrite-MXene polymer composite antibacterial tracheal stent prepared by the method is used as a novel tracheal implantation material, and 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, a good sterilization effect is shown on staphylococcus aureus and pseudomonas aeruginosa, the antibacterial rate of the prepared copper ferrite-MXene/polymer composite tracheal stent reaches over 90%, and the 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 composite powder prepared in example 1 of the present invention;
fig. 2 is a schematic model diagram of a copper ferrite-MXene polymer composite antibacterial tracheal stent prepared in example 1 of the present invention;
FIG. 3 shows the copper ferrite-MXene polymer composite antibacterial tracheal stent (CFOM/PLLA) and PLLA (poly-L-lactic acid), MXene/PLLA, cuFe prepared in example 1 of the present invention2O4A schematic diagram of the results of antibacterial experiments carried out on PLLA material tracheal stents.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
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, completely dissolving 1g of lithium fluoride with the particle size of 200-400 nm in 20mL of concentrated hydrochloric acid with the concentration of 9mol/L, and then dissolving 1g of Ti3AlC2Slowly adding the mixture into the reaction solution, and stirring the mixture for 24 hours at the first temperature; then will produceCentrifuging until pH reaches above 6, and freeze drying overnight to obtain etched Ti3C2(MXene) nanoplatelets;
step two, the prepared 10mg Ti3C2Dissolving the (MXene) nanosheets in 20mL of deionized water, and performing ultrasonic treatment for 30min; then 140mg of ferric chloride hexahydrate and 70mg of copper chloride dihydrate are respectively added and stirred for 1 hour; then adjusting the pH to 11 with sodium hydroxide and stirring continuously at 85 ℃ for 8h, then transferring the obtained solution to a polytetrafluoroethylene autoclave and heating at 120 ℃ for 12h; finally, centrifugally washing the obtained product at a high speed by using deionized water, and drying to obtain copper ferrite-MXene heterojunction composite powder;
step three, respectively weighing copper ferrite-MXene heterojunction composite powder and poly-L-lactic acid powder according to the mass ratio of 2;
and step four, 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 spot diameter is 0.3mm, carrying out layer-by-layer sintering according to a pre-established three-dimensional model, the powder layer thickness 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 finished, thus obtaining the copper ferrite-MXene polymer composite antibacterial air pipe support.
The copper ferrite-MXene polymer composite antibacterial tracheal stent prepared in this example is applied to a novel tracheal implantation material, and an electron microscope scanning image of the copper ferrite-MXene polymer composite powder obtained in the preparation process is shown in FIG. 1, which is shown in the figureThe copper ferrite can be uniformly grown on the surface of MXene, and the copper ferrite-MXene heterojunction is successfully synthesized; the model of the tracheal stent prepared in this example is shown in fig. 2. The copper ferrite-MXene polymer composite antibacterial tracheal stent (CFOM/PLLA) and PLLA (poly-L-lactic acid), MXene/PLLA and CuFe prepared in the embodiment 1 of the invention are respectively used2O4The 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 species.
First, 1 × 10 is selected6The bacterial species were cultured on different tracheal scaffolds at 37 ℃ for 24 hours. Then, the sample was irradiated under near infrared light for 15 minutes, the scaffold was taken out and gently washed with PBS, 1ml of a bacteria culture medium was added and shaken for 10 minutes. The resulting bacterial suspension was diluted 10000 times, and 100. Mu.L of the liquid was dropped onto an agar plate and spread with an applicator. Subsequently, the plate was incubated at 37 ℃ for 24 hours, and the colony number was counted by taking an image of the colony on the agar plate with a digital camera and using the image J. The antibacterial rate was calculated according to the following formula:
antibacterial rate = (colony count control-colony count experiment)/colony count control × 100%
The obtained antibacterial rate data of each material of the tracheal stent is shown in fig. 3, and can be seen from fig. 3: in the non-illuminated group (NIR-), all groups showed no antibacterial properties, while inside the illuminated group (NIR +), the MXene/PLLA group showed some antibacterial properties, probably due to the local high temperature of MXene/PLLA,
the copper ferrite-MXene polymer composite antibacterial tracheal stent (CFOM/PLLA) prepared by the embodiment shows the best antibacterial capability in all groups, and the antibacterial rates to staphylococcus aureus respectively reach 96.49%, because 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 size of 200 to 400nm was completely dissolved in 20mL of 9mol/L concentrated hydrochloric acid,followed by mixing 1g of Ti3AlC2Slowly adding the mixture into the reaction solution, and stirring the mixture for 24 hours at a first temperature; the product was then centrifuged until a pH of above 6 was reached and freeze dried overnight to obtain etched Ti3C2(MXene) nanoplatelets;
step two, the prepared 10mg Ti3C2Dissolving the (MXene) nanosheets in 20mL of deionized water, and ultrasonically treating for 30min; then 140mg of ferric chloride hexahydrate and 70mg of copper chloride dihydrate are respectively added and stirred for 1 hour; then adjusting the pH to 11 with sodium hydroxide, continuously stirring at 85 ℃ for 8h, then transferring the obtained solution to a polytetrafluoroethylene autoclave, and heating at 120 ℃ for 12h; finally, the obtained product is washed by deionized water in a high-speed centrifugal mode and dried, and finally copper ferrite-MXene heterojunction composite powder is obtained;
step three, according to 5:95, respectively weighing copper ferrite-MXene heterojunction composite powder and poly-L-lactic acid powder, adding the copper ferrite-MXene heterojunction composite powder and poly-L-lactic acid powder into a flask containing 20mL of absolute ethanol 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 dispersion, wherein the mechanical stirring speed is 900r/min to obtain a mixed solution, and then centrifugally drying the mixed solution to obtain the copper ferrite-MXene/high polymer composite powder;
and step four, 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 spot diameter is 0.7mm, carrying out layer-by-layer sintering according to a pre-established three-dimensional model, the powder layer thickness 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 finished, thus obtaining the copper ferrite-MXene polymer composite antibacterial air pipe support.
Example 3
The embodiment provides a preparation method of a copper ferrite-MXene polymer composite antibacterial tracheal stent, which comprises the following steps:
firstly, completely dissolving 1g of lithium fluoride with the particle size of 200-400 nm in 20mL of concentrated hydrochloric acid with the concentration of 9mol/L, and then dissolving 1g of Ti3AlC2Slowly adding the mixture into the reaction solution, and stirring the mixture for 24 hours at the first temperature; the product was then centrifuged until the pH reached above 6 and freeze dried overnight to obtain etched Ti3C2(MXene) nanoplatelets;
step two, the prepared 10mg Ti3C2Dissolving the (MXene) nanosheets in 20mL of deionized water, and ultrasonically treating for 30min; then 140mg of ferric chloride hexahydrate and 70mg of copper chloride dihydrate are respectively added and stirred for 1 hour; then adjusting the pH to 11 with sodium hydroxide and stirring continuously at 85 ℃ for 8h, then transferring the obtained solution to a polytetrafluoroethylene autoclave and heating at 120 ℃ for 12h; finally, centrifugally washing the obtained product at a high speed by using deionized water, and drying to obtain copper ferrite-MXene heterojunction composite powder;
step three, according to 10:90, respectively weighing copper ferrite-MXene heterojunction composite powder and poly-L-lactic acid powder, adding the copper ferrite-MXene heterojunction composite powder and poly-L-lactic acid powder into a flask containing 20mL of absolute ethanol 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, and 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 dispersion at the mechanical stirring speed of 1000r/min to obtain a mixed solution, and then centrifugally drying the mixed solution to obtain the copper ferrite-MXene/high polymer composite powder;
and step four, 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 spot diameter is 1.0mm, carrying out layer-by-layer sintering according to a pre-established three-dimensional model, the powder layer thickness corresponding to the copper ferrite-MXene/polymer composite powder is 0.1mm, the preheating temperature of a corresponding powder bed is 160 ℃, and removing unsintered powder after sintering is finished, thus obtaining the copper ferrite-MXene polymer composite antibacterial air pipe support.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (9)
1. The copper ferrite-MXene/polymer composite antibacterial gas pipe support is characterized in that a copper ferrite in-situ grows on MXene 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 polymer ethanol suspension are subjected to ultrasonic mixing, centrifugal drying is carried out to obtain copper ferrite-MXene and polymer composite powder, and finally the copper ferrite-MXene polymer composite antibacterial gas pipe support is prepared through a selective laser sintering technology.
2. The copper ferrite-MXene/macromolecule composite antibacterial tracheal stent of claim 1, wherein the copper ferrite is spinel type copper ferrite, and the macromolecule is at least one of polylactic acid, poly-L-lactic acid, polyglycolic acid, polylactic acid-glycolic acid copolymer, polycaprolactone and poly-p-dioxanone.
3. The copper ferrite-MXene/polymer composite antibacterial tracheal stent of claim 1, wherein in the copper ferrite-MXene/polymer composite antibacterial tracheal stent, the mass fraction of the copper ferrite-MXene heterojunction composite powder is 2-10 wt%, the mass fraction of the polymer is 90-98 wt%, 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.
4. The preparation method of the copper ferrite-MXene/polymer composite antibacterial tracheal stent according to any one of claims 1-3, comprising 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 1g3AlC2Slowly added to the reaction solution, ti3AlC2Stirring the mixture and lithium fluoride at a first temperature for a first preset time, wherein the mass ratio of the mixture to the lithium fluoride is 1; subsequently, the product is centrifuged until the pH reaches above a first predetermined pH and freeze-dried overnight to obtain etched Ti3C2(MXene) nanoplatelets;
step two, the prepared Ti3C2Dissolving (MXene) nanosheets in deionized water, ti3C2The mass-volume ratio of the (MXene) nanosheets to the deionized water is 1g, 2mL, and the ultrasonic treatment is carried out for a second preset time; then adding ferric chloride hexahydrate and copper chloride dihydrate in a first mass ratio and stirring for a third preset time, wherein ferric chloride hexahydrate, copper chloride dihydrate and Ti3C2The mass ratio of the (MXene) nanosheets is 0.7; then adjusting the pH value to a second preset pH value by using sodium hydroxide, continuously stirring for a fourth preset time at a second preset temperature, then transferring the obtained solution into a polytetrafluoroethylene high-pressure kettle, and heating for a fifth preset time at a third preset temperature; finally, centrifugally washing the obtained product at a high speed by using deionized water, and drying to obtain copper ferrite-MXene heterojunction composite powder;
step three, weighing a certain amount of copper ferrite-MXene heterojunction composite powder and polymer powder according to a second preset mass ratio, adding the weighed copper ferrite-MXene heterojunction composite powder and polymer powder into a flask containing absolute ethanol solution, uniformly dispersing the copper ferrite-MXene heterojunction composite powder and the polymer powder through mechanical stirring and ultrasonic dispersion to obtain mixed solution, and then centrifugally drying the mixed solution to obtain copper ferrite-MXene/polymer composite powder;
and 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 to obtain the copper ferrite-MXene polymer composite antibacterial air pipe support.
5. The method for preparing the copper ferrite-MXene/polymer composite antibacterial tracheal stent of claim 4, 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.
6. The method for preparing the copper ferrite-MXene/polymer composite antibacterial tracheal stent of claim 4, wherein in the first step, the first temperature is 35 ℃, the first preset time is 24h, and the first preset pH value is 6.
7. The preparation method of the copper ferrite-MXene/polymer composite antibacterial tracheal stent of claim 4, wherein in the second step, the second preset time is 30min, the ultrasonic power is 500W, and the first mass ratio is 2:1, the third preset time is 1 hour, 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 8 hours, the third preset temperature is 120 ℃, and the fifth preset time is 12 hours;
in the third step, the second preset mass ratio is 2-10: 90 to 98 portions, wherein the total mass of the copper ferrite-MXene heterojunction composite powder and the polymer powder of 1g corresponds to 20mL of absolute ethanol solution, and the mechanical stirring speed is 800 to 1000r/min.
8. The method for preparing the copper ferrite-MXene/polymer composite antibacterial tracheal stent of claim 4, wherein 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 ℃.
9. The copper ferrite-MXene/polymer composite antibacterial tracheal stent of claim 1 or 2, wherein the copper ferrite-MXene/polymer composite antibacterial tracheal stent is applied to novel tracheal implant materials.
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