CN112522803A - Dental floss containing graphene and preparation method thereof - Google Patents
Dental floss containing graphene and preparation method thereof Download PDFInfo
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- CN112522803A CN112522803A CN202011484642.5A CN202011484642A CN112522803A CN 112522803 A CN112522803 A CN 112522803A CN 202011484642 A CN202011484642 A CN 202011484642A CN 112522803 A CN112522803 A CN 112522803A
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C15/00—Devices for cleaning between the teeth
- A61C15/04—Dental floss; Floss holders
- A61C15/041—Dental floss
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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- D01D5/12—Stretch-spinning methods
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/448—Yarns or threads for use in medical applications
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- D10B2321/042—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons polymers of fluorinated hydrocarbons, e.g. polytetrafluoroethene [PTFE]
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Abstract
The invention provides a dental floss containing graphene and a preparation method thereof, wherein the dental floss containing graphene comprises the following raw materials in percentage by mass: 90-99% of polytetrafluoroethylene, 0.01-8% of graphene, 0.01-9% of polyvinylpyrrolidone and 0.01-7% of liquid paraffin. The invention also comprises a preparation method of the dental floss containing the graphene. The dental floss obtained by the invention has good antibacterial, bacteriostatic and anti-inflammatory effects and good biocompatibility, effectively solves the problems of single function, easy drug resistance generation by adding drugs, low mechanical strength, high cost and the like of the dental floss in the prior art, and is convenient for popularization and use.
Description
Technical Field
The invention belongs to the technical field of dental floss preparation, and particularly relates to a dental floss containing graphene and a preparation method thereof.
Background
Bacterial biofilms are a natural component of the oral environment and are compatible with the body in healthy, balanced conditions. When biofilm accumulates for a certain time on the teeth or gum tissue and is combined with other factors, it can lead to dental caries or periodontal disease, two of the most common chronic diseases of the oral cavity, and is also the main cause of tooth loss worldwide.
Dental floss is a common cleaning tool used by modern people, and people have been trying to find a method for cleaning teeth from a long distance, as is confirmed by the latest archaeological data, and ancient people have used chewing gum, branches, bird feathers and animal bones to clean teeth.
The american dentist liviet pamley first reported flossing the teeth. Since the 19 th century, people began using floss made of silk, and after world war ii, nylon floss began to be marketed. A convenient dental floss stick was invented later. Currently, most dental floss is made using polymer fibers.
The Polytetrafluoroethylene (PTFE) is a high polymer formed by polymerizing Tetrafluoroethylene (TFE) monomers, has the relative molecular mass of millions generally, has the melting temperature of 320 ℃ plus 342 ℃, has excellent heat resistance and cold resistance, and can be used for a long time at the temperature of minus 180 ℃ plus 260 ℃; the special spiral conformation of the polytetrafluoroethylene forms a dense protection layer of fluorine atoms outside a carbon chain framework of the polytetrafluoroethylene, so that the polytetrafluoroethylene has excellent chemical stability, corrosion resistance, biocompatibility, high lubrication non-adhesiveness, electric insulation and good ageing resistance. However, polytetrafluoroethylene is an excellent self-lubricating material, and has a low friction coefficient, which is not favorable for removing plaque and food residues in the dental space.
Since the discovery of graphene, graphene has become a research hotspot in the field of carbon materials due to its excellent optical, electrical and mechanical properties. Graphene is also receiving increased attention due to its excellent physical properties, antibacterial properties, and other properties. Graphene is a two-dimensional honeycomb crystal with a monoatomic layer thickness, each smallest structural unit is a hexagon consisting of six carbon atoms, wherein each carbon atom is bound to the adjacent 3 carbon atoms by sp2 hybridization in a sigma bond, and the remaining pi electron orbitals form delocalized large pi bonds with the pi electron orbitals of other carbon atoms. The tensile strength of the graphene is up to 125GPa, and the Young modulus is 1100GPa, so that the graphene is an ideal two-dimensional nano filler.
The existing dental floss generally only has basic functions and single function, and the contact surface between the dental floss and the teeth is increased by changing the shape of the floss body, so that the cleaning efficiency is improved. The existing dental floss is added with medicines such as pseudo-ginseng and the like, so that the dental floss has certain antibacterial and anti-inflammatory effects, but long-term use of the medicines can lead bacteria to generate drug resistance; the dental floss also uses nano silver as an additive component of the dental floss, has good antibacterial and bactericidal effects, but has high cost and is not beneficial to popularization and use; or the silk fiber is modified by chitosan, so that the silk fiber has a certain antibacterial effect, but the mechanical strength is lower.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the dental floss containing the graphene and the preparation method thereof, the obtained dental floss has good antibacterial, bacteriostatic and anti-inflammatory effects and good biocompatibility, the problems of single function, easy generation of drug resistance due to addition of drugs, low mechanical strength, high cost and the like of the dental floss in the prior art are effectively solved, and the dental floss is convenient to popularize and use.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: the dental floss containing graphene is provided and comprises the following raw materials in percentage by mass: 90-99% of polytetrafluoroethylene, 0.01-8% of graphene, 0.01-9% of polyvinylpyrrolidone and 0.01-7% of liquid paraffin.
Further, the dental floss containing graphene comprises the following raw materials in percentage by mass: 96% of polytetrafluoroethylene, 1.5% of graphene, 0.5% of polyvinylpyrrolidone and 2% of liquid paraffin.
Furthermore, the graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a sheet layer of the graphene is 0.4-100nm, and the diameter of the sheet is 0.3-5 μm.
Further, the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass of 1-5 times that of the polytetrafluoroethylene, uniformly mixing, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) melting and blending the premix obtained in the step (1), extruding, forming a trickle in air, cooling, and then sequentially drying, stretching and twisting to obtain the dental floss containing graphene.
Further, in the step (1), the stirring speed is 50-800rpm and lasts for 5-48h during the mixing.
Further, in the step (2), the premix obtained in the step (1) is quantitatively extruded out of a spinneret plate through a screw extruder by a metering pump to carry out melt blending extrusion, wherein the extrusion pressure is 5-90MPa, and the rotating speed of the screw is 15-200 rpm.
Further, in the step (2), drying is carried out for 2-48h, and stretching and twisting are carried out at the temperature of 80-500 ℃, wherein the stretching multiple is 1-80 times.
Further, in the step (2), the titer of each fiber in the obtained graphene-containing dental floss is 2.42D, and each dental floss comprises 30-300 fibers.
Further, in the step (2), the drying is at least one of normal pressure drying, reduced pressure drying, spray drying, boiling drying, freeze drying, infrared drying, microwave drying and moisture absorption drying.
In summary, the invention has the following advantages:
1. according to the invention, the graphene is added into the dental floss, the friction force of fibers can be increased by adding the graphene, so that the dental floss can be used for cleaning dental plaque and dental calculus on the surface of teeth more quickly, conveniently and efficiently, the obtained dental floss has better antibacterial, bacteriostatic and anti-inflammatory effects and good biocompatibility, the problems of single function, easy drug resistance generation by adding medicines, lower mechanical strength, higher cost and the like of the dental floss in the prior art are effectively solved, and the dental floss is convenient to popularize and use. The dental floss has greatly improved dental floss performance, high mechanical strength, excellent antibacterial performance and cleaning ability.
2. The dental floss with a proper graphene adding amount has good antibacterial and bacteriostatic properties, and the antibacterial mechanism of the graphene is derived from physical damage and oxidative stress generated when the graphene is contacted with microorganisms or synergistic effect with an antimicrobial nano material, so that bacteria cannot generate drug resistance to the dental floss; and the graphene can accelerate the healing of the wound and repair the micro wound on the surface of the gum. And the graphene is low in cost and convenient to popularize and use.
3. The good dispersion of the graphene in the polymer matrix can effectively enhance the mechanical strength and the friction resistance of the polytetrafluoroethylene; the fiber surface prepared by compounding with polytetrafluoroethylene has the exposure of the nano-scale graphene microchip, so that the friction coefficient of the dental floss can be increased, the effect of a nano brush can be achieved, and dental plaque, food residues and soft dirt in dental gaps can be cleaned more conveniently and efficiently.
4. After the polytetrafluoroethylene fiber containing the graphene is stretched, the graphene is uniformly dispersed in the polytetrafluoroethylene substrate, but the graphene micro-sheets are mutually overlapped and have a synergistic effect, so that the mechanical property of the fiber is further enhanced.
5. The dental floss containing the graphene prepared by the method has good antibacterial and bacteriostatic properties and good biocompatibility. The dental floss also has the functions of accelerating wound healing and repairing micro-wounds on the surface of the gum. Meanwhile, dental plaque and dental calculus on the surface of the tooth can be cleaned more quickly, conveniently and efficiently by the dental floss, the mechanical performance of the polytetrafluoroethylene fiber is greatly improved, and the application prospect is very wide.
Drawings
FIG. 1 is a schematic view of a mechanical property test of dental floss;
FIG. 2 is a schematic diagram of the dental floss anti-Escherichia coli performance test:
FIG. 3 is a schematic diagram of a dental floss anti-Staphylococcus aureus performance test.
Detailed Description
Example 1
A dental floss containing graphene comprises the following raw materials in percentage by mass: 98% of polytetrafluoroethylene, 1% of graphene, 0.05% of polyvinylpyrrolidone and 1% of liquid paraffin. Wherein the graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a sheet layer of the graphene is 2nm, and the diameter of the sheet is 0.5 mu m; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 170rpm for 5 hours, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) through a metering pump by a screw extruder to form a spinneret plate for melt blending extrusion, wherein the extrusion pressure is 7MPa, the rotating speed of the screw is 20rpm, forming trickle in air, cooling, spray drying for 4h, stretching and twisting at the temperature of 100 ℃, and the stretching multiple is 10 times to obtain the dental floss containing graphene.
Wherein, the spray drying refers to drying the dental floss by adopting a spray dryer under the conditions of the air inlet temperature of 240 ℃, the total solid content of the fed material of 9 percent, the feeding speed of 25ml/min and the pressure of a spray head of 0.3 MPa.
Example 2
A dental floss containing graphene comprises the following raw materials in percentage by mass: 97% of polytetrafluoroethylene, 2% of graphene, 0.5% of polyvinylpyrrolidone and 0.5% of liquid paraffin. The graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a graphene sheet layer is 10nm, and the sheet diameter is 1 mu m; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 195rpm for 10 hours, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) through a metering pump by a screw extruder to form a spinneret plate for melt blending extrusion, wherein the extrusion pressure is 8MPa, the rotating speed of the screw is 30rpm, the premix is formed into trickle in the air and is cooled, the premix is dried under normal pressure, and is stretched and twisted at the temperature of 120 ℃ by 15 times to obtain the dental floss containing graphene.
Wherein, the normal pressure drying refers to that the dental floss is placed in a hot oven under the atmospheric pressure, the temperature is kept at 80 ℃, and the temperature is kept for 12 hours.
Example 3
A dental floss containing graphene comprises the following raw materials in percentage by mass: 96% of polytetrafluoroethylene, 1.5% of graphene, 0.5% of polyvinylpyrrolidone and 2% of liquid paraffin. The graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a graphene sheet layer is 20nm, and the diameter of the graphene sheet layer is 2 microns; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 330rpm for 16 hours, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) through a metering pump by a screw extruder to form a spinneret plate for melt blending extrusion, wherein the extrusion pressure is 20MPa, the rotating speed of the screw is 80rpm, forming trickle in air, cooling, drying under reduced pressure, stretching and twisting at the temperature of 80 ℃, and the stretching multiple is 50 times to obtain the dental floss containing graphene.
Wherein, the decompression drying means that the dental floss is placed in a constant-temperature decompression drying oven, the pressure is below 2.67KPa, the temperature is kept at 60 ℃, and the temperature is kept for 8 h.
Example 4
A dental floss containing graphene comprises the following raw materials in percentage by mass: 92% of polytetrafluoroethylene, 5% of graphene, 0.01% of polyvinylpyrrolidone and 2.99% of liquid paraffin. The graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a graphene sheet layer is 12nm, and the sheet diameter is 2.1 mu m; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 200rpm for 22 hours, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) through a metering pump by a screw extruder to form a spinneret plate for melt blending extrusion, wherein the extrusion pressure is 15MPa, the rotating speed of the screw is 95rpm, the premix is formed into trickle in the air and is cooled, the trickle is boiled and dried, the premix is stretched and twisted at the temperature of 480 ℃, and the stretching multiple is 20 times, so that the dental floss containing graphene is obtained.
Wherein, the boiling drying is that the dental floss is dried and primarily concentrated under normal pressure in a boiling bed dryer, and then is dried by circulating air, the air supply rate is 2/3 of the total air quantity, the drying time is 90min, and the steam pressure is 5.0 MPa.
Example 5
A dental floss containing graphene comprises the following raw materials in percentage by mass: 93% of polytetrafluoroethylene, 5.97% of graphene, 0.03% of polyvinylpyrrolidone and 1% of liquid paraffin. The graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a graphene sheet layer is 40nm, and the sheet diameter is 3 mu m; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, then adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 230rpm for 27 hours, drying, then adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) through a metering pump by a screw extruder to form a spinneret plate for melt blending extrusion, wherein the extrusion pressure is 21MPa, the rotating speed of the screw is 70rpm, forming trickle in air, cooling, freeze-drying, stretching and twisting at the temperature of 420 ℃, and the stretching multiple is 60 times, so that the dental floss containing graphene is obtained.
Wherein the freeze drying is to freeze the dental floss in a freeze dryer at-40 deg.C for 4h, continuously vacuum the freezing chamber until the vacuum value is reduced to below 0.1mbar, adjust the temperature to 20 deg.C, and continuously vacuum for 12 h.
Example 6
A dental floss containing graphene comprises the following raw materials in percentage by mass: 91% of polytetrafluoroethylene, 4.93% of graphene, 0.07% of polyvinylpyrrolidone and 4% of liquid paraffin. Wherein the graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a sheet layer of the graphene is 10nm, and the diameter of the sheet is 0.8 mu m; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 310rpm for 40 hours, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) through a metering pump by a screw extruder to form a spinneret plate for melt blending extrusion, wherein the extrusion pressure is 47MPa, the rotating speed of the screw is 50rpm, the premix is formed into trickle in the air and is cooled, the trickle is dried by infrared rays, the premix is stretched and twisted at the temperature of 300 ℃, and the stretching multiple is 80 times, so that the dental floss containing graphene is obtained.
Wherein the infrared drying refers to baking the dental floss in an infrared drying oven at 110 deg.C for 4 h.
Example 7
A dental floss containing graphene comprises the following raw materials in percentage by mass: 95% of polytetrafluoroethylene, 3.9% of graphene, 0.1% of polyvinylpyrrolidone and 1% of liquid paraffin. The graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a graphene sheet layer is 40nm, and the sheet diameter is 4 microns; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, then adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 230rpm for 48 hours, drying, then adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) out of a spinneret plate through a metering pump through a screw extruder, carrying out melt blending extrusion, wherein the extrusion pressure is 32MPa, the rotating speed of a screw is 100rpm, forming trickle in air, cooling, carrying out microwave drying, stretching and twisting at the temperature of 90 ℃, and the stretching multiple is 70 times to obtain the dental floss containing graphene.
Wherein, the microwave drying means that the dental floss is dried in a microwave dryer under the conditions of 60KPa, 1kw of power, 60 ℃ of upper limit temperature and 3h of drying time.
Example 8
A dental floss containing graphene comprises the following raw materials in percentage by mass: 97% of polytetrafluoroethylene, 2.3% of graphene, 0.2% of polyvinylpyrrolidone and 0.5% of liquid paraffin. The graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a graphene sheet layer is 60nm, and the diameter of the graphene sheet layer is 5 mu m; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 400rpm for 18h, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) out of a spinneret plate through a metering pump through a screw extruder, carrying out melt blending extrusion, wherein the extrusion pressure is 49MPa, the rotating speed of a screw is 60rpm, forming trickle in air, cooling, absorbing moisture, drying, stretching and twisting at the temperature of 210 ℃, and the stretching multiple is 40 times, so as to obtain the dental floss containing graphene.
Wherein, the moisture absorption drying means that the dental floss which is dried at normal temperature and contains certain moisture is placed on a drying cabinet, a large amount of calcium oxide drying agent is placed on the lower layer, the dental floss is vacuumized, the pressure is kept below 2.67KPa, and the dental floss is stored for 24 hours.
Example 9
A dental floss containing graphene comprises the following raw materials in percentage by mass: 96% of polytetrafluoroethylene, 2.1% of graphene, 0.4% of polyvinylpyrrolidone and 1.5% of liquid paraffin. The graphene is non-defective and non-oxidized group biologically safe graphene, the thickness of a graphene sheet layer is 25nm, and the diameter of the graphene sheet layer is 2 microns; the molecular weight of the polytetrafluoroethylene is 300-800 ten thousand.
The preparation method of the dental floss containing graphene comprises the following steps:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass 3 times that of the polytetrafluoroethylene, uniformly mixing, keeping the stirring speed at 300rpm for 25h, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) quantitatively extruding the premix obtained in the step (1) through a metering pump by a screw extruder to form a spinneret plate for melt blending extrusion, wherein the extrusion pressure is 30MPa, the rotating speed of the screw is 90rpm, forming trickle in air, cooling, spray drying, stretching and twisting at the temperature of 320 ℃, and the stretching multiple is 80 times to obtain the dental floss containing graphene.
Wherein, the spray drying refers to drying the dental floss by adopting a spray dryer under the conditions of the air inlet temperature of 240 ℃, the total solid content of the fed material of 9 percent, the feeding speed of 25ml/min and the pressure of a spray head of 0.3 MPa.
Experimental example 1 mechanical Property test
The mechanical properties of the floss containing graphene obtained in examples 1-3 and the floss obtained from a commercial arch floss rod made of polytetrafluoroethylene were measured, and the results are shown in FIG. 1.
The detection method comprises the following steps: and (3) testing by using a universal mechanical testing machine, wherein the gauge length is 10mm, the stretching speed is 20mm/min, each sample is tested for 8 times, and after an obvious error value is removed, the average value is taken.
As can be seen from FIG. 1, the tensile strength and elongation at break of the graphene-containing dental floss obtained by the present invention are much higher than those of ordinary dental floss.
Experimental example 2 antibacterial Property test
The floss obtained in examples 1 to 3 and comprising graphene and the floss obtained in the commercially available bow-shaped floss rod made of polytetrafluoroethylene were subjected to the antibacterial property test, and the results are shown in FIGS. 2 to 3.
The detection method comprises the following steps: samples were tested for in vitro antibacterial activity against the gram-positive bacteria staphylococcus aureus (ATCC 25923) and the gram-negative bacteria escherichia coli (ATCC 25922) in suspension by using a viable cell count method.
Samples were mixed in Phosphate Buffered (PB) solution and a blank prepared with bacteria only in PB solution was used as a control; both solutions were added to 2mL PB microbial suspension and incubated with shaking at 37 ℃ for 18 hours; serial dilution of the samples and mixing with molten Luria-Bertani agar and pouring into sterile petri dishes; after 4 hours of incubation at 37 ℃, the number of bacterial colonies was counted and an average of three replicates was performed for each sample.
Meanwhile, the survival of the bacteria was determined by measuring the growth curve by OD. OD was measured every half hour in 200 μ L of fresh medium using a Synergy MX microtiter plate reader at 600 nm. This process was repeated three times. Statistical analysis (two-sided t-test, 95% confidence interval) was performed to identify whether the OD values of the sample containing the conjugate fibers were significantly different from the control group.
As can be seen from FIGS. 2 to 3, the antibacterial performance of the dental floss containing graphene is far stronger than that of the dental floss of an arched dental floss rod made of a commercial polytetrafluoroethylene material, the antibacterial effect of the dental floss is gradually improved along with the increase of the content of graphene, and the sensitivity of gram-positive bacteria to the dental floss containing graphene is obviously higher than that of gram-negative bacteria.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (10)
1. The dental floss containing graphene is characterized by comprising the following raw materials in percentage by mass: 90-99% of polytetrafluoroethylene, 0.01-8% of graphene, 0.01-9% of polyvinylpyrrolidone and 0.01-7% of liquid paraffin.
2. The graphene-containing dental floss of claim 1, comprising the following raw materials by mass: 96% of polytetrafluoroethylene, 1.5% of graphene, 0.5% of polyvinylpyrrolidone and 2% of liquid paraffin.
3. The graphene-containing dental floss according to claim 1 or 2, wherein the graphene is a defect-free, non-oxidized group biologically safe graphene, and the graphene has a sheet thickness of 0.4-100nm and a sheet diameter of 0.3-5 μm.
4. The graphene-containing dental floss of claim 1 or 2, wherein the polytetrafluoroethylene has a molecular weight of 300-800 ten thousand.
5. The method of preparing a graphene-containing dental floss of any of claims 1-4, comprising the steps of:
(1) respectively weighing polytetrafluoroethylene, graphene and polyvinylpyrrolidone, adding ethanol solution with the mass of 1-5 times that of the polytetrafluoroethylene, uniformly mixing, drying, adding liquid paraffin, and uniformly mixing to obtain premix;
(2) and (2) melting and blending the premix obtained in the step (1), extruding, forming a trickle in air, cooling, and then sequentially drying, stretching and twisting to obtain the dental floss containing graphene.
6. The method for preparing a graphene-containing dental floss according to any one of claims 5, wherein in the step (1), the stirring speed is 50-800rpm for 5-48h during the mixing.
7. The method for preparing a graphene-containing dental floss according to any one of claims 5, wherein in the step (2), the premix obtained in the step (1) is extruded by melt blending through a screw extruder and a metering pump quantitatively extruded out of a spinneret plate, wherein the extrusion pressure is 5-90MPa, and the rotation speed of the screw is 15-200 rpm.
8. The method of preparing a graphene-containing dental floss according to any one of claims 5, wherein in step (2), the floss is dried for 2 to 48 hours, stretched and twisted at a temperature of 80 to 500 ℃, and the stretching ratio is 1 to 80 times.
9. The method for preparing a graphene-containing dental floss according to any one of claims 5, wherein in the step (2), the titer of each fiber in the obtained graphene-containing dental floss is 2.42D, and each dental floss comprises 30-300 fibers.
10. The method of claim 5, wherein in step (2), the drying is at least one of drying under atmospheric pressure, drying under reduced pressure, spray drying, boiling drying, freeze drying, infrared drying, microwave drying, and moisture absorption drying.
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