CN115105592A - Preparation and application of vanadium-containing MXene antibacterial material - Google Patents
Preparation and application of vanadium-containing MXene antibacterial material Download PDFInfo
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 51
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
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- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 8
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- 229910010272 inorganic material Inorganic materials 0.000 claims 1
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- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 15
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
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- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 229960003165 vancomycin Drugs 0.000 description 1
- MYPYJXKWCTUITO-LYRMYLQWSA-N vancomycin Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C2C=C3C=C1OC1=CC=C(C=C1Cl)[C@@H](O)[C@H](C(N[C@@H](CC(N)=O)C(=O)N[C@H]3C(=O)N[C@H]1C(=O)N[C@H](C(N[C@@H](C3=CC(O)=CC(O)=C3C=3C(O)=CC=C1C=3)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)O2)=O)NC(=O)[C@@H](CC(C)C)NC)[C@H]1C[C@](C)(N)[C@H](O)[C@H](C)O1 MYPYJXKWCTUITO-LYRMYLQWSA-N 0.000 description 1
- MYPYJXKWCTUITO-UHFFFAOYSA-N vancomycin Natural products O1C(C(=C2)Cl)=CC=C2C(O)C(C(NC(C2=CC(O)=CC(O)=C2C=2C(O)=CC=C3C=2)C(O)=O)=O)NC(=O)C3NC(=O)C2NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(CC(C)C)NC)C(O)C(C=C3Cl)=CC=C3OC3=CC2=CC1=C3OC1OC(CO)C(O)C(O)C1OC1CC(C)(N)C(O)C(C)O1 MYPYJXKWCTUITO-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
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- A41—WEARING APPAREL
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- A41D31/00—Materials specially adapted for outerwear
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Abstract
The invention discloses a preparation method of a vanadium-containing MXene antibacterial material and application of the vanadium-containing MXene antibacterial material in the field of biology. Specifically, the vanadium-containing MXene material is prepared by using a vanadium-containing MAX phase precursor through a one-step method, so that the antibacterial property of MXene is enhanced. The preparation method is simple, and the obtained vanadium-containing MXene material has excellent antibacterial performance and can effectively inhibit the growth of escherichia coli. The vanadium-containing antibacterial MXene disclosed by the invention has wide application in the biological field, including but not limited to medical dressings, antibacterial masks and tumor treatment.
Description
Technical Field
The invention relates to the technical field of nano materials and the field of nano medical treatment, including but not limited to medical dressings, antibacterial masks and cancer treatment.
Background
Overuse and abuse of antibiotics has led to the development of resistance to antibacterial drugs. Antibiotic-resistant bacteria, such as methicillin-resistant staphylococcus aureus and vancomycin-resistant enterococcus, are difficult or even impossible to treat with existing antibiotics, resulting in nearly 100 million worldwide deaths per year. If the trend is followed, the number will rise sharply to 1000 ten thousand by 2050. In addition to developing antibiotic resistance, bacteria can also form biofilms, leading to many persistent infections. The antibiotic cannot penetrate the dense outer shell of the bacterial surface, resulting in limited therapeutic effect. Therefore, there is an urgent need to develop a new method to combat antibiotic-resistant bacteria and disrupt bacterial biofilms.
In recent years, two-dimensional materials have attracted a wide attention in the biomedical field. Some two-dimensional materials, such as graphene, have demonstrated antimicrobial properties and greatly reduced bacterial resistance. The antibacterial mechanism of the 2D material: 1) physical damage to the bacterial membrane caused by the sharp edges of the 2D material, resulting in loss of its integrity; 2) chemical damage by oxidative stress or charge transfer. The antibacterial mechanisms of physical and chemical damage greatly reduce the ability of bacteria to develop resistance to drugs.
MXene is a group of compounds having M n+1 X n T x The material system is composed of elements, wherein M represents an early transition metal element, X represents C or N, T represents a group/modifier on the surface of the two-dimensional material, and N usually has a value ranging from 1 to 3. Thus, the MXene family has a rich chemical makeup, numerous members, and is still expanding. MXene has excellent electrical and optical properties and has a great number of applications in energy storage and electromagnetism. In recent years, MXene materials have been increasingly developed for use in the biological field.
At present, multiple researches report the antibacterial and anticancer effects of MXene materials. The study by Mahmoud et al showed that Ti 3 C 2 T x A typical MXene material has antibacterial effects on gram-negative escherichia coli and gram-positive bacillus subtilis, the antibacterial activity of the material is dose-dependent, and the antibacterial efficiency of the material is higher than that of graphene oxide. Like graphene, Ti 3 C 2 T x Bacteria are inhibited by the destruction of cell membranes and the production of Reactive Oxygen Species (ROS). However, some areBacteria can counteract oxidant-based clearance mechanisms by producing antioxidants. Thus, antibacterial mechanisms involving oxidative stress may be less effective or even ineffective against these bacteria. By utilizing the high photo-thermal conversion efficiency of MXene materials, photo-thermal treatment (PPT) synergistic antibiosis is used by Hongweili and the like. Ti (titanium) 3 C 2 MXene can rapidly kill bacteria under near infrared irradiation by photothermal effect, is effective on 15 detection bacteria (including gram-positive bacteria, gram-negative bacteria and antibiotic-resistant bacteria), and has broad-spectrum antibacterial effect. In addition, the MXene material has excellent biocompatibility and biodegradability, and a large amount of ROS are efficiently generated through Fenton-like reaction in a tumor microenvironment to kill tumor cells. Ti prepared by the micro-explosion method of the pottery groggery and the like 3 C 2 T x MXene quantum dots efficiently catalyze H under tumor acidic condition 2 O 2 The growth of the tumor of the HeLa-bearing mouse is obviously inhibited by the generation of a large amount of OH and the synergistic photothermal therapy, and no obvious toxic or side effect is shown.
Vanadium has great potential in the aspects of antibiosis and tumor treatment. Vanadium, like Ti, reduces H by catalysis 2 O 2 、O 2 Generating a large amount of OH or O 2 ·- And further kill bacteria or tumor cells. However, the current biological field application of vanadium is mainly limited to vanadium oxide nanoparticles, and the application of vanadium-based MXene materials in the biological field is not reported.
Disclosure of Invention
The vanadium-containing MXene two-dimensional nanomaterial prepared by the invention has a remarkable inhibiting effect on gram-negative escherichia coli, and the medical antibacterial mask which can realize MXene combined PTT and can be reused is prepared. In addition, the invention provides a method for treating tumors by combining vanadium-containing MXene materials with PTT, and the vanadium-containing MXene two-dimensional nano materials can be prepared by the following two methods.
The vanadium-containing MXene two-dimensional nano material can be prepared by a hydrochloric acid/lithium fluoride etching method, and specifically comprises the following steps:
the method comprises the following steps: preparation of vanadium-containing MXene two-dimensional material: 1g of lithium fluoride (LiF) is dissolved in 20mL of hydrochloric acid (HCl) at room temperature (V) Concentrated HCl :V H2O = 1: 1) a LiF/HCl mixture was prepared. 1g of vanadium-containing MAX phase precursor is immersed in 20mL of LiF/HCl solution, and stirred and reacted for 72 h at room temperature to obtain multilayer vanadium-containing MXene. After etching, the resulting suspension was washed with deionized water and centrifuged to separate the powder from the supernatant. After several washes, the pH was brought above 6 and dried in vacuo. Wherein, the vanadium-containing MAX phase is a type of MAX phase with a chemical general formula of M n+1 AX n The ternary layered compound of (1), wherein M is an early transition metal such as Ti, V, Zn, Ga, Ge, Cr, etc.; a is a group III or IV element, X is C or N, N represents 1, 2, 3, etc.;
step two: and adding deionized water into the multilayer MXene to disperse the MXene, and performing ultrasonic treatment for 2 hours to obtain suspension, namely the vanadium-containing MXene solution.
The vanadium-containing MXene two-dimensional nano material can be prepared by a hydrogen fluoride etching method, and specifically comprises the following steps:
the method comprises the following steps: preparing a vanadium-containing MXene two-dimensional material: 1g of vanadium-containing MAX phase precursor was immersed in 10mL of HF solution (55 wt.%) and reacted at 35 ℃ with stirring for 92h to obtain multilayered vanadium-containing MXene. After etching, the resulting suspension was washed with deionized water and centrifuged to separate the powder from the supernatant. After several times of washing, the pH value is made to be more than 6, and vacuum drying is carried out, wherein, the MAX phase containing vanadium is a chemical general formula M n+1 AX n The ternary layered compound of (1), wherein M is an early transition metal such as Ti, V, Zn, Ga, Ge, Cr, etc.; a is a group III or IV element, X is C or N, and N represents 1, 2, 3, etc.
Step two: adding 1g of the vanadium-containing multilayer MXene prepared in the first step into 10mL of intercalator tetrabutylammonium hydroxide (TBA-OH), stirring for 24h, performing suction filtration by using a vacuum filtration device to remove the intercalated MXene, performing suction filtration and cleaning by using deionized water until the pH value is more than 6, and drying in a vacuum drying oven at 60 ℃ for 24h to obtain solid powder, namely the single-layer MXene-based nano material.
Drawings
FIG. 1 is SEM image of multilayer vanadium-containing MXene nanosheets
FIG. 2 is a TEM image of monolayer vanadium-containing MXene nanosheets
FIG. 3 is a graph showing the growth of Escherichia coli on LB solid medium after a monolayer of vanadium-containing MXene for 4 hours
FIG. 4 shows an antibacterial artificial lens coated with vanadium-containing MXene-based nano-material
FIG. 5 is a medical antibacterial gauze dip-coated with the vanadium-containing MXene-based nano material.
Detailed Description
Hereinafter, the present invention will be described in more detail by way of specific examples, which are provided for illustrative purposes only and are not intended to limit the present invention.
Example 1:
(1) 10mL of deionized water, 10mL of hydrochloric acid at a concentration of 12M, and 1g of lithium fluoride were mixed in a high-density polyethylene bottle having a capacity of 60mL, stirred, and heated to 35 ℃. Then adding 1g of TiVAlC phase precursor, stirring for 72 hours, carrying out suction filtration and cleaning by using deionized water until the pH value is more than 6, and placing the obtained precipitate in a vacuum drying oven to dry for 24 hours at 60 ℃;
(2) dispersing the multilayer TiVC precipitate into 100mL of deionized water, performing ultrasonic filtration for 2h, and performing suction filtration by using a vacuum suction filtration device to remove the intercalated TiVC, wherein the suspension in a suction filtration bottle is the single-layer TiVC-based nano material.
Example 2:
(1) adding 1g of TiVAlC phase precursor into 10mL of hydrogen fluoride (55 wt.%), stirring for 92h at 35 ℃, performing suction filtration and washing with deionized water until the pH is more than 6, and drying the obtained precipitate for 24h at 60 ℃ in a vacuum drying oven;
(2) adding 1g of multilayer TiVC into 10ml LTBA-OH, stirring for 24h, performing suction filtration by using a vacuum filtration device, removing the intercalated TiVC, performing suction filtration and cleaning by using deionized water until the pH value is more than 6, and drying in a vacuum drying oven at 60 ℃ for 24h to obtain solid powder, namely the single-layer TiVC-based nano material.
Example 3:
(1) 10mL of deionized water, 10mL of hydrochloric acid at a concentration of 12M, and 1g of lithium fluoride were mixed in a high-density polyethylene bottle having a capacity of 60mL, stirred, and heated to 35 ℃. Followed byThen 1g of V is added 2 Stirring the AlC phase precursor for 72 hours, then carrying out suction filtration and cleaning by using deionized water until the pH value is more than 6, and drying the obtained precipitate for 24 hours at 60 ℃ in a vacuum drying oven;
(2) a plurality of layers V 2 Dispersing the C precipitate into 100mL deionized water, performing ultrasonic treatment for 2h, and performing suction filtration by using a vacuum suction filtration device to remove the intercalation V 2 C, the suspension in the suction flask is a monolayer V 2 C-based nano material.
Example 4:
(1) will be 1g V 2 Adding an AlC phase precursor into 10mL of hydrogen fluoride (55 wt.%), stirring for 92h at 35 ℃, performing suction filtration and washing by using deionized water until the pH is more than 6, and drying the obtained precipitate for 24h at 60 ℃ in a vacuum drying oven;
(2) 1g of a multilayer V 2 Adding C into 10mL of intercalator TBA-OH, stirring for 24h, vacuum filtering with a vacuum filtration device, and removing intercalation V 2 C, using deionized water to perform suction filtration and washing until the pH value is more than 6, placing the mixture in a vacuum drying oven, and drying the mixture for 24 hours at the temperature of 60 ℃ to obtain solid powder, namely single-layer V 2 C-based nanomaterials.
Example 5:
(1) 10mL of deionized water, 10mL of hydrochloric acid at a concentration of 12M, and 1g of lithium fluoride were mixed in a high-density polyethylene bottle having a capacity of 60mL, stirred, and heated to 35 ℃. Then adding 1g of VCrAlC phase precursor, stirring for 72 hours, carrying out suction filtration and cleaning by using deionized water until the pH value is more than 6, and placing the obtained precipitate in a vacuum drying oven to dry for 24 hours at the temperature of 60 ℃;
(2) dispersing the multilayer VCrC precipitate into 100mL of deionized water, performing ultrasonic filtration for 2h, and performing suction filtration by using a vacuum filtration device to remove the intercalated VCrC, wherein the suspension in a filter flask is the single-layer VCrC-based nano material.
Example 6:
(1) adding 1g of VCrAlC phase precursor into 10mL of hydrogen fluoride (55 wt.%), stirring for 92h at 35 ℃, carrying out suction filtration and cleaning by using deionized water until the pH is more than 6, and drying the obtained precipitate for 24h at 60 ℃ in a vacuum drying oven;
(2) 1g of a multilayer V 2 C to 10mL insertStirring the layered agent TBA-OH for 24 hours, then carrying out suction filtration by using a vacuum filtration device to remove the intercalated VCrC, carrying out suction filtration and cleaning by using deionized water until the pH value is more than 6, and drying in a vacuum drying oven at 60 ℃ for 24 hours to obtain solid powder, namely the single-layer VCrC-based nano material.
Example 7:
(1) 10mL of deionized water, 10mL of hydrochloric acid at a concentration of 12M, and 1g of lithium fluoride were mixed in a high-density polyethylene bottle having a capacity of 60mL, stirred, and heated to 35 ℃. Followed by addition of 1g of Ti 2 VAlC 2 Stirring the precursor for 72 hours, then carrying out suction filtration and cleaning by using deionized water until the pH is more than 6, and drying the obtained precipitate for 24 hours at the temperature of 60 ℃ in a vacuum drying oven;
(2) a plurality of layers of Ti 2 VC 2 Dispersing the precipitate into 100mL of deionized water, performing ultrasonic treatment for 2 hours, and performing suction filtration by using a vacuum suction filtration device to remove the intercalated Ti 2 VC 2 The suspension in the suction flask is a monolayer of Ti 2 VC 2 And (3) a base nanomaterial.
Example 8:
(1) mixing 1g of Ti 2 VAlC 2 Adding the phase precursor into 10mL of hydrogen fluoride (55 wt.%), stirring for 92h at 35 ℃, performing suction filtration and washing by using deionized water until the pH is more than 6, and drying the obtained precipitate for 24h at 60 ℃ in a vacuum drying oven;
(2) 1g of a multilayer V 2 Adding C into 10mL of intercalator TBA-OH, stirring for 24h, vacuum filtering with a vacuum filtration device, and removing intercalated Ti 2 VC 2 Filtering and cleaning with deionized water until pH is greater than 6, and drying in a vacuum drying oven at 60 deg.C for 24 hr to obtain solid powder as single-layer Ti 2 VC 2 And (3) a base nanomaterial.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, which is for the purpose of enabling those skilled in the art to practice the invention. It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (5)
1. The preparation method of the vanadium-doped MXene antibacterial material is characterized in that the vanadium-containing MAX phase precursor comprises but is not limited to TiVAlC, V 2 AlC，V 2 PC，V 2 ZnC，V 2 GaC，VCrAlC，V 2 GeC，Ti 2 VAlC 2 Any one or a combination of two or more MAX phase ceramics in VCrAlC.
2. The preparation of the vanadium-doped MXene antibacterial material as claimed in claim, wherein the prepared vanadium-containing MXene material includes but is not limited to TiVC, Ti 2 VC 2 ，V 4 C 3 ，V 2 C，V 3 C 2 ，V 4 N 3 And one or more of CrVC.
3. The method as claimed in claim one or two, wherein the prepared vanadium-containing MXene material comprises any one or more of vanadium-containing MXene powder, vanadium-containing MXene liquid and vanadium-containing MXene composite material.
4. The preparation of the vanadium-doped MXene antibacterial material as claimed in claim three, wherein the vanadium-containing MXene composite material comprises but is not limited to the compounding of vanadium-containing MXene with any one or more than two of inorganic materials, organic materials, metal materials and polymer materials.
5. The method as claimed in one to four claims, wherein the prepared vanadium-containing MXene antibacterial material or vanadium-containing MXene composite material is applied to vanadium-containing MXene antibacterial bandages, vanadium-containing MXene antibacterial dressings, vanadium-containing MXene antibacterial lenses, vanadium-containing MXene antibacterial contact lenses, vanadium-containing MXene antibacterial eyedrops, vanadium-containing MXene anticancer drugs and other vanadium-containing MXene antibacterial and anticancer platforms.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116726229A (en) * | 2023-06-25 | 2023-09-12 | 四川大学 | Nanofiber wound repair material and preparation method and application thereof |
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