CN116377616A - Graphene micro-nano structural fiber with antibacterial activity and preparation method thereof - Google Patents
Graphene micro-nano structural fiber with antibacterial activity and preparation method thereof Download PDFInfo
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to a graphene micro-nano structural fiber with antibacterial activity and a preparation method thereof, wherein the graphene fiber is prepared by adopting graphite to prepare graphene oxide solution through an improved Hummers method, and then preparing a reduced graphene oxide fiber material with excellent broad-spectrum antibacterial activity by utilizing an in-situ confined hydrothermal method heating reduction technology. The micro-nano structure is a micro-oriented strip structure. The product prepared by the method has a good structure, the graphene nano-sheets have a strip structure which is arranged along the axial direction of the fiber, the micron-sized dimension of the oriented structure is 80 microns, the nano-sized dimension is 500 nanometers, and the antibacterial activity on escherichia coli and staphylococcus aureus can reach more than 99.5 percent. The method is simple, easy to control and convenient to produce.
Description
Technical field:
the invention relates to a graphene microstructure fiber with antibacterial activity and a preparation method thereof.
The background technology is as follows:
in the 21 st century, the improvement of life quality of people has become a major problem to be solved by bacterial infection, people pay more attention to the health of people, and the requirement of the quality of antibacterial materials is also improved. Bacteria is a microorganism which not only robs the body of a large amount of nutrients, but also discharges a large amount of exotoxins in the proliferation process and adheres to normal cells of the human body; releasing endotoxin, causing debilitation, typhoid fever, pneumonia and even causing serious diseases such as pulmonary tuberculosis. The antibacterial materials commonly used at present are classified into organic and inorganic materials. Organic antibacterial materials such as antibacterial peptides, antibiotics; inorganic antibacterial materials, such as metals and their oxides (Ag ions), photocatalytic antibacterial materials (TiO 2 ) Etc. However, the antibacterial materials have certain defects, organic antibacterial materials are easy to hydrolyze, the effective period is short, and bacteria have drug resistance to the antibacterial materials; inorganic antibacterial materials need to consider the cost and human health problems. The antibacterial materials are mainly used for water treatment (disinfectant is added in the water purification process to prevent the occurrence of water borne infection), textile fabric (the textile fabric has antibacterial effect by coating padding, spraying and other methods), biomedical (bacteria are inhibited or killed by blocking pathogenic microorganisms) and the like.
In 2004, new materials, graphene, were isolated from graphite by micro-mechanical exfoliation, taught by andersoid lamb and Constant noose Wo Xiao, university of Manchester. Graphene is formed by passing sp through carbon atoms 2 The hybridized two-dimensional honeycomb structure material and the graphene have better physical and chemical properties. Physical properties, such as mechanical properties (theoretical Young's modulus up to 1.0TPa, tensile strength of about 130 GPa), electron mobility (about 15000cm 2 /(v·s)), thermal properties (thermal conductivity of single-layer graphene up to 5000 w/mk), etc.; chemical properties such as biocompatibility, oxidizing (reactive with active metals), etc. By virtue of the excellent properties, the graphene is widely applied to the aspects of new energy batteries, sea water desalination, aerospace, biomedical and the like. With the intensive research, important derivatives of Graphene Oxide (GO) and reduced graphene oxide (rGO) are also applied to various aspects.
Since 2010, huang et al at Shanghai applied physical research institute of China academy of sciences reported for the first time that GO and rGO have an effect of inhibiting the growth of Escherichia coli, and graphene is substantially free of cytotoxicity compared with traditional antibacterial agents. Scientists at home and abroad research the antibacterial activity of the GO and rGO membranes, GO and rGO solutions, and composite materials of GO and rGO and other materials, such as chitosan and Ag ions. Researchers found that GO and rGO in different states have different antibacterial effects. For example, lu et al reported in 2017 that the GO film of vertically aligned GO nanoplatelets has better antimicrobial properties. From studies by scientists, it is found that the antibacterial mechanism of graphene-based materials is largely divided into physical and chemical methods. The physical method is to puncture a bacterial membrane through the sharp edge of the graphene nano sheet, extract phospholipid and kill bacteria; it is also considered that the graphene nanoplatelets encapsulate bacteria, which lose external nutrients, thus inhibiting their growth. Chemical methods are believed to destroy bacteria by oxidizing bacterial nucleic acids, membrane lipids, proteins to produce ROS, disrupting the bacteria's original ROS level balance.
No research report has been made on the antibacterial activity of reduced graphene oxide fibers (rgfs). rGOFs is an assembly of GO nano-sheets in a one-dimensional limited space, and has the advantages of high specific surface area, excellent electric conduction, mechanical property, easiness in functionalization and the like. rGOFs were first prepared in 2011 by the high professor team using wet spun GO liquid crystals. Then, a dry spinning method, a Chemical Vapor Deposition (CVD) method and a one-step one-dimensional fixed hydrothermal method are developed. Among them, the dry spinning process is an industrially viable strategy for the manufacture of continuous rGOFs; unlike wet mill process, graphene oxide is extruded from a dry spinning spinneret to form fiber directly, so that the trouble of using a coagulating bath is avoided, and the graphene oxide is collected in air. Dry-spun rgfs have poor mechanical strength due to the presence of a large number of micropores and core-shell structures. The CVD method uses a graphene film as a raw material, and pulls out graphene fibers on a plane. The CVD graphene film may generate defects, grain boundaries and wrinkles during the preparation process, and the surface contamination and damage may be caused during the preparation and transfer processes, thus limiting its further application. The GOFs are directly prepared from GO solution by taking GO nano sheets as an organization module, so that the pollution and damage to the outside in the preparation process are avoided, meanwhile, the GOFs are prepared in a limited space, and the shape and structure of the GOFs can be regulated and controlled by changing the structure of a limited space mold, so that the GOFs prepared by the method have the advantage of high flexibility.
In summary, graphene and its derivative materials have good antibacterial activity, and most of current research reports show solution, coating and three-dimensional self-supporting film or porous material states. The patent provides a graphene micro-nano structure fiber material with excellent broad-spectrum antibacterial activity. The graphene fiber has good mechanical, electrical and mammalian cell compatibility, and can be widely applied to the fields of composite materials, energy sources, sensors and biomedicine.
The invention comprises the following steps:
the invention provides a graphene micro-nano structural fiber with antibacterial activity and a preparation method thereof, wherein the fiber has a micro-nano structure which is arranged along the axial direction of the fiber, the micron-sized size is 80 mu m, the nanometer-sized size is 500nm, and the antibacterial rate of reduced graphene oxide is over 99.5 percent through a plate colony counting method test. The graphene micro-nano structural fiber with the antibacterial activity is obtained for the first time, and the preparation method has the advantages that the graphene micro-nano structural fiber with the excellent antibacterial activity can be obtained through a limited-domain hydrothermal method by selecting a proper graphene oxide nano sheet precursor, and the preparation method of the graphene micro-nano structural fiber is simple, low in cost and strong in process repeatability.
The preparation method of the graphene micro-nano structural fiber with antibacterial activity comprises the following specific steps:
1) Preparing graphene oxide colloid by using a modified Hummers method;
2) Obtaining graphene oxide colloid with high oxidation degree by changing oxidation time;
3) Obtaining a graphene oxide solution of a small sheet layer through centrifugation;
4) Preparing graphene oxide solution into a certain concentration;
5) Injecting the solution into the capillary glass tube, and sealing both ends;
6) The solution sealed in the capillary glass tube is reduced by a hydrothermal method and dried to prepare the reduced graphene oxide fiber.
In the invention, the graphene oxide colloid in the step 1) is prepared, and the concentration of the graphene oxide colloid is calculated after sampling and drying.
In the present invention, the oxidation time in step 2) was 12 hours.
In the present invention, the oxidizing solution in step 2) is used to prepare a platelet solution.
In the present invention, the solution of step 4) was prepared as 8 mg/ml.
In the invention, the length of the capillary glass tube in the step 5) is 100mm, the inner diameter is 0.9-1.1mm, and the wall thickness is 0.10-0.15mm.
In the invention, the reduction temperature in the step 6) is 200 ℃, the reduction time is 2 hours, the drying temperature is 60 ℃, and the drying time is 12 hours.
The preparation of the reduced graphene oxide fiber material is characterized in that the fiber material is prepared by combining X-ray diffraction (XRD) test; the reduced graphene oxide sheets are uniformly distributed through observation of a Scanning Electron Microscope (SEM), the particle size is 20nm to 50nm, and the bacteriostasis rate of the reduced graphene oxide is over 99.5 percent through a plate colony counting method test.
Description of the drawings:
fig. 1 is an X-ray diffraction pattern of graphene oxide in an example of implementation.
Fig. 2 is an X-ray diffraction pattern of a reduced graphene oxide fiber material in an example implementation.
Fig. 3 is an SEM image of the surface morphology of the reduced graphene oxide fiber material at 1000 x magnification in the example.
FIG. 4 is a blank of E.coli in the bacteriostasis test in the example.
FIG. 5 is a graph showing the results of the test of the bacteriostasis rate of the co-culture of reduced graphene oxide fibers with E.coli in the example.
Fig. 6 is a blank of staphylococcus aureus in the bacteria inhibition test of the examples.
FIG. 7 is a graph showing the results of co-culturing reduced graphene oxide fibers with Staphylococcus aureus in the bacteriostasis rate test of the example.
Figure 8 is a statistic of the results of the bacteriostatic rate test in the example.
The specific embodiment is as follows:
implementation example:
experimental conditions and parameters for preparing the reduced graphene oxide fiber material are as follows:
1) 2g NaNO in a Erlenmeyer flask 3 Dissolving in 96ml of concentrated sulfuric acid, adding 2g of graphite, and uniformly stirring; placing in ice water bath, slowly adding KMnO for thirty minutes 4 12g, continuing the ice-water bath for 1.5 hours; heating to 45 ℃ and preserving heat for 12 hours; cooling to room temperature, adding 200ml of ice water, and diluting uniformly; dropwise adding 10ml hydrogen peroxide until no bubble is generated in the solution and the color of the solution becomes bright yellow; standing for 24 hours, washing and centrifuging with diluted hydrochloric acid (hydrochloric acid: water 1:2) for 3 times, and washing and centrifuging with water until the pH=7; obtaining a small-sheet graphene oxide colloid; carrying out ultrasonic treatment for 1h to obtain a small-sheet graphene oxide solution;
2) Drying the solution to obtain graphene oxide, and calculating the concentration of the graphene oxide solution, wherein the concentration is 15.66mg/ml;
3) Preparing graphene oxide solution into 8mg/ml; injecting the solution into a capillary glass tube with the length of 100mm, the diameter of 1mm and the wall thickness of 0.1-0.15mm, and heating to ensure that two ends of the glass tube are sealed; and (3) placing the glass tube into a vacuum drying oven at 200 ℃ for heat preservation for 2 hours, taking out the glass tube, breaking off two ends of the glass tube, controlling water, and placing the glass tube into a drying oven at 60 ℃ for drying for 12 hours to obtain the reduced graphene oxide fiber.
According to the method of the invention, the reduced graphene oxide fiber material can be prepared, and is characterized in that:
1) The prepared sample is subjected to X-ray diffraction (XRD) analysis, and in combination with a comparison standard diffraction peak PDF card, obvious characteristic diffraction peak positions of the reduced graphene oxide (rGO) material can be seen. And (5) primarily judging that the graphene oxide undergoes a reduction reaction after being heated at 200 ℃.
2) Obtaining the surface morphology features of the reduced graphene oxide fiber material, we performed Scanning Electron Microscope (SEM) analysis on the prepared samples. The result shows that the reduced graphene oxide fiber has a typical fold structure, the nano sheets are uniformly stacked, the fiber thickness is uniform, and the fiber diameter is 70-90 μm.
3) The antibacterial test is carried out on the reduced graphene oxide fiber material, and the antibacterial test is carried out on the sample by a bacteriostasis ring method, so that the result shows that the reduced graphene oxide fiber has excellent antibacterial activity, and the antibacterial rate reaches more than 99.5%.
Claims (8)
1. The graphene micro-nano structural fiber with antibacterial activity is characterized in that the fiber material is reduced graphene oxide according to X-ray diffraction (XRD) test; the reduced graphene oxide sheets are uniformly distributed through observation of a Scanning Electron Microscope (SEM), the particle size is 20nm to 50nm, the fiber has a micro-nano structure which is arranged along the axial direction of the fiber, the micron size is 80um, the nano size is 500nm, and the bacteriostasis rate of the reduced graphene oxide is over 99.5 percent through the test of a plate colony counting method.
2. The preparation method of the graphene micro-nano structural fiber with antibacterial activity is characterized by comprising the following steps of:
1) Preparing graphene oxide colloid by using a modified Hummers method;
2) Obtaining graphene oxide colloid with high oxidation degree by changing oxidation time;
3) Obtaining a graphene oxide solution of a small sheet layer through centrifugation;
4) Preparing graphene oxide solution into a certain concentration;
5) Injecting the solution into the capillary glass tube, and sealing both ends;
6) The solution sealed in the capillary glass tube is reduced by a hydrothermal method and dried to prepare the reduced graphene oxide fiber.
3. The preparation method according to claim 2, wherein the graphene oxide colloid is prepared in step 2), and the concentration of the graphene oxide colloid is calculated after sampling and drying.
4. The process according to claim 2, wherein the oxidation time in step 2) is 12h.
5. The method of claim 2, wherein the 12h oxidation solution in step 2) is used to prepare a platelet graphene oxide nanoplatelet solution.
6. The method of claim 2, wherein in step 4) a solution of 8mg/ml is provided.
7. The method of claim 2, wherein the capillary glass tube in step 5) has a length of 100mm, an inner diameter of 0.9 to 1.1mm, and a wall thickness of 0.10 to 0.15mm.
8. The process according to claim 2, wherein the reduction temperature in step 6) is 200 ℃, the reduction time is 2 hours, the drying temperature is 60 ℃ and the drying time is 12 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110203911A (en) * | 2019-07-10 | 2019-09-06 | 吉林大学 | A kind of graphene fiber and preparation method |
| CN115074865A (en) * | 2022-07-29 | 2022-09-20 | 青岛理工大学 | Graphene fiber preparation method, graphene fiber temperature sensor and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110203911A (en) * | 2019-07-10 | 2019-09-06 | 吉林大学 | A kind of graphene fiber and preparation method |
| CN115074865A (en) * | 2022-07-29 | 2022-09-20 | 青岛理工大学 | Graphene fiber preparation method, graphene fiber temperature sensor and application |
Non-Patent Citations (1)
| Title |
|---|
| 宋长远等: "石墨烯及其衍生物在抗菌纤维中的应用进展", 纺织科技进展, no. 10, 25 October 2017 (2017-10-25), pages 1 - 5 * |
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