CN115559109A - Breathable antibacterial nano composite fiber material and preparation method and application thereof - Google Patents
Breathable antibacterial nano composite fiber material and preparation method and application thereof Download PDFInfo
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- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical group C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 3
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- 231100000206 health hazard Toxicity 0.000 description 1
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- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Engineering & Computer Science (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a breathable antibacterial nano composite fiber material and a preparation method and application thereof, belonging to the technical field of functional materials. The invention provides a breathable antibacterial nano composite fiber material, which is prepared by dispersing a modified MXenes composite material in a solvent to prepare a soaking solution, soaking cotton fabrics in the soaking solution and then drying; the modified MXenes composite material is MXenes with tannic acid connected on the surface. The composite fiber material has excellent antibacterial performance and good stability. Can overcome the defects that MXenes materials are easy to oxidize and unstable in water-oxygen environment, prolongs the service life of the antibacterial material, and has good application prospect in the fields of medical and civil materials and the like.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a breathable antibacterial nano composite fiber material as well as a preparation method and application thereof.
Background
The cotton fiber is a material commonly used in life, and is very easy to attach bacteria due to the characteristics of large surface area, good hygroscopicity and the like. This not only affects the usability of the cotton fibers, but also is a health hazard to the user. If the antibacterial cotton fiber can be prepared, the antibacterial cotton fiber has important significance for expanding the application of the cotton fiber.
MXenes is a new two-dimensional material, being a two-dimensional transition metal carbide, nitride or carbonitride. MXenes are obtained mainly by extracting weakly bonded A site elements (e.g., al atoms) from the MAX phase with HF acid or a mixed solution of hydrochloric acid and fluoride. Wherein, titanium carbide (Ti) 3 C 2 T x ) MXene nanosheets are one of them. MXenes has the characteristics of high specific surface area and high conductivity, has the advantages of flexible and adjustable components, controllable minimum nano-layer thickness and the like, and has great potential in the fields of energy storage, adsorption, sensors, conductive fillers and the like. MXenes two-dimensional materials are also reported in the fields of textile and antibiosis. For example, patent application with publication number CN112941899A discloses an MXenes-AgNPs synergistic antibacterial cotton fabric.
However, MXenes is an unstable material which is susceptible to oxidative failure, especially in a water-oxygen environment, which seriously affects its service life and the antibacterial effect of the modified cotton fabric after washing. How to adopt a simple method to improve the stability of MXenes and provide the antibacterial performance of MXenes modified cotton fabrics needs further research.
Disclosure of Invention
The invention aims to provide a breathable antibacterial nano composite fiber material and a preparation method and application thereof.
The invention provides a breathable antibacterial nano composite fiber material, which is prepared by dispersing a modified MXenes composite material in a solvent to prepare a soaking solution, soaking cotton fabrics in the soaking solution and then drying;
the modified MXenes composite material is MXenes with tannic acid connected on the surface.
Further, the air conditioner is provided with a fan,
the concentration of the modified MXenes composite material in the soaking solution is 0.1%;
and/or the solvent is PBS buffer solution;
and/or, the step of soaking the cotton in the soaking solution and then drying is repeated for 10 times.
Further, the air conditioner is provided with a fan,
the cotton fabric is cotton fiber;
and/or, the temperature of soaking is 25 ℃;
and/or the soaking time is 10min;
and/or the temperature of the drying is 50 ℃;
and/or the drying time is 15min.
In the invention, the cellulose content in the cotton fiber is not less than 50%.
Further, the modified MXenes composite material is prepared from the following raw materials in parts by weight: 10-20 parts of tannic acid and 1 part of MXenes nanosheets.
Further, the MXenes nanosheets are titanium carbide MXenes nanosheets.
Further, the surface of the modified MXenes composite material fixes silver ions through ionic bonds.
Further, the modified MXenes composite material also comprises the following raw materials in parts by weight: 0.33 part of silver ions.
Further, the preparation method of the modified MXenes composite material comprises the following steps:
uniformly mixing tannic acid and MXenes nanosheets in a solvent, reacting, centrifugally cleaning, and drying the precipitate to obtain the tannin/MXenes nanosheets;
the solvent is deionized water;
and/or, adjusting the pH to 8.5 prior to the reaction;
and/or, the reaction is carried out in an inert gas;
and/or, the reaction is carried out under the condition of keeping out light;
and/or the reaction temperature is 25 ℃;
and/or the reaction time is 6h;
and/or, directly centrifugally cleaning after the reaction or adding a compound containing silver ions to continue the reaction and then centrifugally cleaning;
and/or, the centrifugal washing is carried out until the pH value is 6.5.
Further, the air conditioner is provided with a fan,
regulating the pH value by using trihydroxymethyl aminomethane before the reaction;
and/or the temperature of the continuous reaction of adding the silver ion-containing compound is 25 ℃ and the time is 1h.
The invention also provides a preparation method of the breathable antibacterial nano composite fiber material, which comprises the following steps:
dispersing the modified MXenes composite material in a solvent to prepare a soaking solution, soaking the cotton fabric in the soaking solution, and then drying to obtain the modified MXenes composite material;
the modified MXenes composite material is MXenes with tannic acid connected on the surface.
The invention also provides application of the breathable antibacterial nano composite fiber material in preparation of antibacterial materials.
The invention provides a breathable antibacterial nano composite fiber material which is excellent in antibacterial performance and good in stability. The defects that the MXenes material is easy to oxidize and is unstable in a water-oxygen environment can be overcome, the service life of the antibacterial material is prolonged, and the antibacterial material has a good application scene in the fields of medical and civil materials and the like.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 is a graph showing the results of dispersion of the soaking solution after 31 days of storage at room temperature.
FIG. 2 is a graph showing the result of XPS data of the immersion liquid after storage at room temperature for 14 days: wherein, the graph A is an XPS data result graph of MXene stored for 14 days; and the graph B is the XPS data result of TA/MXene stored for 14 days.
Detailed Description
The raw materials and equipment used in the embodiment of the present invention are known products and obtained by purchasing commercially available products.
The MXene nanosheets used in the invention are prepared according to the method described in the document "Flexible Anti-biofoulding MXene/Cellulose fiber Membrane for stable Solar-drive Water Purification" (Xiaoang-Jun Zhua et al, ACS appl. Mater. Interfaces 2019, 11, 36589-36597), and the specific preparation method comprises the following steps:
1g LiF is dissolved in 20mL of 9M HCl solution, and the solution is magnetically stirred for 5min to obtain LiF/HCl solution. Then 1g of Ti 3 AlC 2 The powder was slowly added to the LiF/HCl solution and the mixture was reacted for 24 h at 35 ℃ with magnetic stirring to give a stable suspension. Repeatedly washing the obtained Ti with deionized water 3 C 2 T x The suspension is washed and centrifuged at 3500 rpm for 5 minutes until the pH value is reached>5. Then dried under vacuum at 60 ℃ overnight to obtain Ti 3 C 2 T x Powder (MXene few-layer nanoplatelets).
Example 1 preparation of breathable, antimicrobial nanocomposite fiber Material of the invention
The preparation method of the breathable antibacterial nano composite fiber material comprises the following steps:
weighing 30g of Tannic Acid (TA), 3g of MXene nanosheet and 67g of deionized water, adding into a three-neck flask with a nitrogen valve, filling nitrogen, performing light-shielding treatment, and performing ice-water bath ultrasound for 30min to uniformly mix the MXene nanosheets. Then, adding Tris (hydroxymethyl) aminomethane (Tris) to adjust the pH value to 8.5, continuously stirring for 6h at room temperature (25 ℃) under the condition of keeping out of the sun, centrifugally cleaning the obtained mixed solution by using deionized water under the condition of 12000rpm until the pH value of a supernatant is about 6.5, taking a lower layer of the centrifugal substance, and freeze-drying to obtain the TA/MXene material.
And (3) adding 0.5g of TA/MXene material into 500mL of PBS buffer solution, and performing ultrasonic dispersion for 30min in an ice water bath to obtain a soaking solution. And (3) repeatedly soaking and drying the cotton fibers in the soaking solution for 10 times to obtain the composite fiber material. Soaking at 25 deg.C for 10min; drying at 50 deg.C for 15min.
Example 2 preparation of breathable antimicrobial nanocomposite fiber Material of the invention
Weighing 30g of tannic acid, 1.5g of MXene nanosheet and 67g of deionized water, adding into a three-neck flask with a nitrogen valve, filling nitrogen, performing light-shielding treatment, and performing ice-water bath ultrasound for 30min to uniformly mix the MXene nanosheets. Then, adding Tris (hydroxymethyl) aminomethane (Tris) to adjust the pH value to 8.5, continuously stirring for 6 hours at room temperature (25 ℃) under the condition of keeping out of the sun, then adding 0.5g of silver nitrate, continuously stirring for 1 hour, centrifugally washing the obtained mixed solution by using deionized water under the condition of 12000rpm until the pH value of a supernatant is about 6.5, taking a lower layer of a centrifugal substance, and freeze-drying to obtain the TA/MXene material.
And (3) adding 0.5g of TA/MXene material into 500mL of PBS buffer solution, and ultrasonically dispersing in an ice water bath for 30min to obtain a soaking solution. And (3) repeatedly soaking and drying the cotton fibers in the soaking solution for 10 times to obtain the composite fiber material. Soaking at 25 deg.C for 10min; drying at 50 deg.C for 15min.
Comparative example 1 deionized Water soaked Cotton fibers
Repeatedly soaking cotton fiber in deionized water, drying, and soaking and drying for 10 times. Soaking at 25 deg.C for 10min; drying at 50 deg.C for 15min.
Comparative example 2 preparation of other breathable antibacterial nanocomposite fiber materials
Weighing 3g of MXene nanosheet and 97g of deionized water, adding into a three-neck flask with a nitrogen valve, filling nitrogen, performing light-shielding treatment, and performing ice-water bath ultrasound for 30min to uniformly mix the MXene nanosheets to obtain the MXene soaking solution.
And repeatedly soaking and drying the cotton fibers in the soaking solution for 10 times to obtain the composite fiber material. Soaking at 25 deg.C for 10min; drying at 50 deg.C for 15min.
Comparative example 3 tannin soaked Cotton fibers
Weighing 5g of tannic acid and 95g of deionized water, adding the tannic acid and the deionized water into a three-neck flask with a nitrogen valve, filling nitrogen, performing light-shielding treatment, and performing ice-water bath ultrasound for 30min to obtain a tannic acid soaking solution.
And repeatedly soaking and drying the cotton fibers in the soaking solution for 10 times to obtain the composite fiber material. Soaking at 25 deg.C for 10min; drying at 50 deg.C for 15min.
The beneficial effects of the present invention are demonstrated by specific test examples below.
Test example 1 study on antibacterial Properties of air-permeable antibacterial nanocomposite fiber Material of the present invention
1. Experimental method
The antibacterial performance of the cotton fiber samples prepared in the examples 1 to 2 and the comparative examples 1 to 4 is evaluated, and the specific method comprises the following steps: coli and staphylococcus aureus were cultured overnight in Luria-Bertani broth (LB) medium at 37 ℃. After cultivation, at a rotation speed of 5000 rad min -1 The bacteria were centrifuged down for 5min and then washed repeatedly 3 times with PBS buffer solution to remove residual macromolecules and other growth medium components. The bacteria were then diluted with PBS buffer to a bacterial concentration of about 10 7 Individual Colony Forming Unit (CFU) mL -1 The bacterial liquid of (1). Next, each set of cotton fiber samples (1 cm) 2 ) Putting into a bacterial solution of Escherichia coli and Staphylococcus aureus (10) 7 CFU mL −1 ) Cotton fiber samples were suspended in bacteria solution and incubated at 37 ℃ for 24 hours with constant shaking at 110 rpm. Wherein the bacterium of comparative example 1 served as a negative control.
After incubation, 100. Mu.L of the broth was spread on nutrient agar plates and incubated at 37 ℃ for 12 hours to analyze bacterial viability. The experiment was performed using a triple repeat method, with the average taken as the final result. The antibacterial activity was calculated using the following formula:
wherein,N c the number of colonies after the culture of the cotton fiber of comparative example 1,N m the number of colonies after incubation was for each group of cotton fiber samples.
2. Results of the experiment
The bacteriostatic ratio of each group of cotton fiber samples is shown in table 1.
TABLE 1. Bacteriostatic rate of each group of cotton fiber samples
The results in table 1 show that: the composite fiber material prepared by the invention has excellent antibacterial performance. Meanwhile, according to the comparative example 2, the antibacterial performance of the MXene nanosheet is obviously reduced after 14 days, and the antibacterial performance of the antibacterial material prepared by the method is stable after 28 days, which shows that the composite fiber material prepared by the method has good stability.
Test example 2 research on antioxidant Properties of breathable antibacterial nanocomposite fiber Material according to the present invention
After the soaking solutions prepared in example 1 (TA/MXene) and comparative example 2 (MXene) were stored at room temperature for 31 days, the dispersion of the soaking solutions was observed. And when the sample is stored for 14 days at normal temperature, 5mL of the soak solution is taken respectively to carry out X-ray photoelectron scattering test, and the characteristic peak of Ti is obtained.
After being stored for 31 days, as shown in figure 1, MXene soaking solution is seriously layered, while TA/MXene soaking solution still has good uniformity and is not layered, which indicates that the TA/MXene soaking solution is more stable.
After 14 days of storage, X-ray photoelectron scattering data are shown in fig. 2, and it can be seen that after 14 days of storage, the Ti oxidation peak of the TA modified MXene material is significantly inhibited, which indicates that the TA/MXene has better oxidation resistance.
The results show that the oxidation resistance of the nano composite fiber material is obviously improved, and the stability is good.
In conclusion, the invention provides the breathable antibacterial nano composite fiber material which is excellent in antibacterial performance and good in stability. The defects that the MXenes material is easy to oxidize and is unstable in the water-oxygen environment can be overcome, the service life of the antibacterial material is prolonged, and the antibacterial material has good application scenes in the fields of medical and civil materials and the like.
Claims (10)
1. A breathable antibacterial nano composite fiber material is characterized in that: dispersing a modified MXenes composite material in a solvent to prepare a soaking solution, soaking cotton fabrics in the soaking solution, and then drying to obtain the modified MXenes composite material;
the modified MXenes composite material is MXenes with tannic acid connected to the surface.
2. The breathable, antimicrobial nanocomposite fiber material of claim 1, wherein:
the concentration of the modified MXenes composite material in the soaking solution is 0.1%;
and/or the solvent is PBS buffer solution;
and/or, the step of soaking the cotton fabrics in the soaking solution and then drying is repeated for 10 times.
3. The breathable, antimicrobial nanocomposite fibrous material according to claim 2, characterized in that:
the cotton fabric is cotton fiber;
and/or, the temperature of soaking is 25 ℃;
and/or the soaking time is 10min;
and/or the temperature of the drying is 50 ℃;
and/or the drying time is 15min.
4. The breathable, antimicrobial nanocomposite fiber material of claim 1, wherein: the modified MXenes composite material is prepared from the following raw materials in parts by weight: 10-20 parts of tannic acid and 1 part of MXenes nanosheets.
5. The breathable, antimicrobial nanocomposite fiber material of claim 4, wherein: the MXenes nanosheet is a titanium carbide MXenes nanosheet.
6. The breathable, antimicrobial nanocomposite fibrous material according to claim 1, characterized in that: the surface of the modified MXenes composite material is also fixed with silver ions through ionic bonds.
7. The breathable, antimicrobial nanocomposite fibrous material according to claim 6, characterized in that: the preparation of the modified MXenes composite material also comprises the following raw materials in parts by weight: 0.33 part of silver ions.
8. The air-permeable antibacterial nanocomposite fiber material according to any one of claims 1 to 7, characterized in that: the preparation method of the modified MXenes composite material comprises the following steps:
uniformly mixing tannic acid and MXenes nanosheets in a solvent, reacting, centrifugally cleaning, and drying the precipitate to obtain the tannin/MXenes nanosheets;
the solvent is deionized water;
and/or, adjusting the pH to 8.5 prior to the reaction;
and/or, the reaction is carried out in an inert gas;
and/or, the reaction is carried out under the condition of keeping out light;
and/or the reaction temperature is 25 ℃;
and/or the reaction time is 6h;
and/or, after the reaction, directly centrifugally cleaning or adding a compound containing silver ions to continue the reaction and then centrifugally cleaning;
and/or, the centrifugal washing is carried out until the pH value is 6.5.
9. A method for preparing the air-permeable antibacterial nano composite fiber material according to any one of claims 1 to 8, which is characterized by comprising the following steps: the method comprises the following steps:
dispersing the modified MXenes composite material in a solvent to prepare a soaking solution, soaking the cotton fabric in the soaking solution, and then drying to obtain the modified MXenes composite material;
the modified MXenes composite material is MXenes with tannic acid connected to the surface.
10. Use of the breathable antibacterial nanocomposite fiber material of any one of claims 1 to 8 in the preparation of antibacterial materials.
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