CN116949589A - Electroactive antibacterial dental floss and preparation method thereof - Google Patents
Electroactive antibacterial dental floss and preparation method thereof Download PDFInfo
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- CN116949589A CN116949589A CN202310911721.7A CN202310911721A CN116949589A CN 116949589 A CN116949589 A CN 116949589A CN 202310911721 A CN202310911721 A CN 202310911721A CN 116949589 A CN116949589 A CN 116949589A
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Classifications
-
- 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
-
- 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
-
- 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
- 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
-
- 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 application provides an electroactive antibacterial dental floss and a preparation method thereof, wherein the electroactive antibacterial dental floss comprises 70-100% of a piezoelectric polymer matrix and 0-30% of piezoelectric ceramic particles; the piezoelectric polymer matrix is made of at least one of polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene and polyvinylidene fluoride-hexafluoropropylene; the piezoelectric ceramic particles are at least one selected from barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate. The electro-active antibacterial dental floss provided by the application can generate a piezoelectric effect in the use process, not only can clean residues and dental calculus, but also can inhibit bacteria in teeth from breeding through the electrified function of the dental floss, and has good antibacterial performance.
Description
The present application is a divisional application with application number CN202210806838.4, application number 2022, month 07, 08, entitled "an electroactive antibacterial dental floss and method for making same", which is incorporated herein by reference in its entirety.
Technical Field
The application relates to the technical field of dental floss, in particular to electroactive antibacterial dental floss and a preparation method thereof.
Background
Maintaining tooth cleanliness is critical to oral health, and periodontal and gingival inflammation lesions are mostly located in the interproximal areas between teeth and the interproximal spaces between teeth. Thus, cleaning of the interproximal surfaces and spaces of the teeth is an important aspect of oral self-care. The dental floss is used as a cleaning tool capable of penetrating through a tooth gap, and can clean residues and dental calculus at dead angles caused by tooth abutting surfaces, under gum edges and uneven tooth arrangement.
At present, the materials of dental floss generally comprise nylon threads, silk threads, polyester threads and the like, which mainly remove residues and dental calculus of teeth by a mechanical cleaning principle, and cannot remove and inhibit bacteria and dental plaque on the adjacent surfaces of teeth, so that caries and periodontal disease risks are increased.
Disclosure of Invention
The application aims to provide an electroactive antibacterial dental floss, which generates a piezoelectric effect in the use process and simultaneously generates good antibacterial performance when cleaning teeth gap residues. The specific technical scheme is as follows:
the application provides an electroactive antibacterial dental floss, which comprises the following components in percentage by volume:
70-100% of piezoelectric polymer matrix
0-30% of piezoelectric ceramic particles;
wherein the material of the piezoelectric polymer matrix is at least one selected from polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene and polyvinylidene fluoride-hexafluoropropylene;
the piezoelectric ceramic particles are at least one selected from barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate.
In some embodiments, an electroactive antimicrobial dental floss comprises the following components in volume percent:
70-90% of piezoelectric polymer matrix
10-30% of piezoelectric ceramic particles.
In some embodiments, the piezoelectric ceramic particles have a particle size of 50nm to 30 μm.
In some embodiments, the electroactive antibacterial dental floss has a width of 50 μm to 3mm and a thickness of 50 μm to 150 μm.
In some embodiments, the piezoelectric constant d of the electroactive antimicrobial floss 33 1.5pC/N-9.3pC/N.
In some embodiments, the electroactive floss has a maximum output voltage of 0.3V to 1.0V.
In some embodiments, the electroactive antibacterial dental floss has an antibacterial ratio of 66% to 91%.
In a second aspect, the application provides an electrically powered flossing device comprising an electroactive antimicrobial floss according to any of the foregoing embodiments.
In a third aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Adding the piezoelectric polymer matrix and the piezoelectric ceramic particles into a solvent to form uniform dispersion;
(2) Carrying out electrostatic spinning on the dispersion liquid through an electrostatic spinning machine to form fiber cloth;
(3) Cutting the fiber cloth to form dental floss wires;
(4) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
In a fourth aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and adding the mixture into a double-screw extruder for granulating to form material particles;
(2) Adding the material particles into a melt injection molding machine, and performing melt injection molding to form dental floss wires;
(3) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
In a fifth aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and loading the mixture into a high-molecular three-dimensional printer for three-dimensional printing by a fusion method to form dental floss wires;
(2) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
In a sixth aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, adding the mixture into a double-screw extruder for granulating to form granules, and adding the granules into an extrusion spinning machine for melt spinning to form dental floss filaments; or alternatively
(1') adding the piezoelectric polymer matrix into an extrusion spinning machine, and carrying out melt spinning to form dental floss;
(2) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
The application has the beneficial effects that:
the electroactive antibacterial dental floss provided by the application takes the piezoelectric polymer or the compound of the piezoelectric polymer and the piezoelectric ceramic particles as the raw material, and the formed dental floss material has the advantages of uniform distribution, stable performance, good flexibility and strong operability; the electroactive antibacterial dental floss provided by the application generates a piezoelectric effect through contact friction with the adjacent surfaces of teeth in the use process, outputs an electric signal, can inhibit bacteria in teeth from breeding through the electrification performance while cleaning residues and dental calculus, generates good antibacterial performance, effectively prevents caries, reduces the occurrence probability of gingivitis and the like.
Of course, it is not necessary for any one product or method of practicing the application to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the application or the technical solutions of the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it being obvious that the drawings in the description below are only some embodiments of the application, and that other embodiments may be obtained according to these drawings by a person skilled in the art.
FIG. 1 is a physical view showing electroactive antibacterial dental floss prepared in example 1, example 9, comparative example 1 and comparative example 2 according to the present application;
FIG. 2 shows the static piezoelectric constant d of the electroactive antibacterial dental floss prepared in example 1, example 9, comparative example 1 and comparative example 2 according to the present application 33 Is a test result graph of (1);
FIG. 3 is a graph showing the dynamic piezoelectric signal test under the action of external force of the electroactive antibacterial dental floss prepared in example 1, example 9, comparative example 1 and comparative example 2 according to the present application;
fig. 4 shows the antibacterial performance test results of the electroactive antibacterial dental floss prepared in example 1, example 9, comparative example 1 and comparative example 2 according to the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. Based on the embodiments of the present application, all other embodiments obtained by the person skilled in the art based on the present application are included in the scope of protection of the present application.
In a first aspect the present application provides an electroactive antibacterial dental floss comprising the following components in percentage by volume:
70-100% of piezoelectric polymer matrix
0-30% of piezoelectric ceramic particles;
wherein the material of the piezoelectric polymer matrix is at least one selected from polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene and polyvinylidene fluoride-hexafluoropropylene;
the piezoelectric ceramic particles are at least one selected from barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate.
In the application, polyvinylidene fluoride (PVDF) and polyvinylidene fluoride are adopted as the materials of the piezoelectric polymer matrix-piezoelectric constant d of trifluoroethylene (P (VDF-TrFE)), polyvinylidene fluoride-hexafluoropropylene (P (VDF-HFP)) 33 18 pC/N-35 pC/N, 30 pC/N-40 pC/N respectively; piezoelectric constant d of barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate in piezoelectric ceramic particles 33 185-195pC/N respectively; 139-149pC/N;187-197pC/N;120-130pC/N; the piezoelectric polymer matrix and the piezoelectric ceramic particles have large dielectric constant and strong piezoelectricity, and the piezoelectric polymer can be selected to form the electroactive antibacterial dental floss with certain piezoelectric property, and the dental floss wire has proper flexibility and toughness and strong operability; the molecular weight of the piezoelectric polymer is not particularly limited as long as the object of the present application can be achieved, and for example, the weight average molecular weight of the above polyvinylidene fluoride (PVDF), polyvinylidene fluoride-trifluoroethylene (P (VDF-TrFE)), polyvinylidene fluoride-hexafluoropropylene (P (VDF-HFP)) is 50 to 60 tens of thousands, 40 to 50 tens of thousands in this order. The melting temperature of polyvinylidene fluoride (PVDF), polyvinylidene fluoride-trifluoroethylene (P (VDF-TrFE)) and polyvinylidene fluoride-hexafluoropropylene (P (VDF-HFP)) in the piezoelectric polymer matrix is 200 ℃ to 280 ℃, 110 ℃ to 217 ℃ and 110 ℃ to 180 ℃ in sequence.
In the present application, the volume percentage of the piezoelectric polymer matrix may be 70%, 75%, 80%, 85%, 90%, 95%, 100% or a range between any two values therebetween, and the volume percentage of the piezoelectric ceramic particles may be 0%, 5%, 10%, 15%, 20%, 25%, 30% or a range between any two values therebetween. The volume percentage of the piezoelectric polymer matrix is in the range, so that the electroactive antibacterial dental floss with certain piezoelectric property can be formed, and the dental floss has proper flexibility and toughness and strong operability. When the volume percentage of the piezoelectric ceramic particles is in the range, the piezoelectric ceramic particles provide a charging function and simultaneously can improve the strength and the friction strength of the electroactive antibacterial dental floss.
Preferably, the electroactive antibacterial dental floss comprises the following components in percentage by volume:
70-90% of piezoelectric polymer matrix
10-30% of piezoelectric ceramic particles.
According to the electroactive antibacterial dental floss provided by the application, the content of the piezoelectric polymer matrix and the content of the piezoelectric ceramic particles in the electroactive antibacterial dental floss are regulated, so that the electroactive antibacterial dental floss has a piezoelectric function, and a piezoelectric effect is generated in the use process of the electroactive antibacterial dental floss, for example, the dental floss is wrapped on the adjacent surface of teeth in a C-shaped manner in the use process, and the upward and downward lifting friction is promoted by applying ultrasound or pressure, so that a friction-piezoelectric composite effect is realized, and the dental floss has good antibacterial performance under the combined action of friction and piezoelectricity. Specifically, the piezoelectric constant d 33 The maximum output voltage is 0.3V-1.0V and is 1.5pC/N-9.3pC/N. Under the action of piezoelectric effect, the electrically active antibacterial dental floss can clean residues and dental calculus in teeth better, and can bring good antibacterial performance. In some embodiments of the application, the electroactive antibacterial dental floss is in the shape of at least one of a straight wire, a beaded shape, and a wavy shape. The dental floss can be controlled to form the shape by adjusting electrostatic spinning parameters and post-processing technology.
In some embodiments of the application, the piezoelectric ceramic particles have a particle size of 50nm to 30 μm. When the particle size of the piezoelectric ceramic particles is within the above range, the dispersibility of the piezoelectric ceramic particles in the piezoelectric polymer matrix is high, the mixing uniformity of dental floss materials is high, and the prepared electroactive antibacterial dental floss has good performance stability.
In some embodiments of the application, the electroactive antibacterial dental floss has a width of 50 μm to 3mm and a thickness of 50 μm to 150 μm, preferably a width of 100 μm to 1mm and a thickness of 50 μm to 100 μm.
In some embodiments of the application, the piezoelectric constant d of the electroactive antibacterial dental floss 33 1.5pC/N-9.3pC/N. The electroactive antibacterial dental floss provided by the application has certain piezoelectric performance.
In some embodiments, the electroactive antimicrobial floss has a maximum output voltage of 0.3V to 1.0V. The electroactive antibacterial dental floss provided by the application has certain piezoelectric performance.
In some embodiments of the application, the electroactive antibacterial dental floss has an antibacterial ratio of 66% to 91%. The electroactive antibacterial dental floss provided by the application has good antibacterial performance. After the electro-active antibacterial dental floss is stimulated by external force in the use process, the piezoelectric effect is generated, so that the electro-active antibacterial dental floss is electrified, the growth of bacteria in tooth gaps can be inhibited, the formation of dental plaque is prevented, the symptoms such as periodontitis are relieved, and meanwhile, the growth and the reproduction of the bacteria on the electro-active antibacterial dental floss can be reduced, and the antibacterial performance of the dental floss is improved.
In a second aspect the present application provides an electrically powered flossing device comprising an electrically active antimicrobial floss according to any of the previous embodiments, the resulting electrically powered flossing device having a piezoelectric effect and good antimicrobial and antibacterial properties. The present application is not particularly limited as long as the object of the present application can be achieved. For example, motorized flossers are ultrasonically driven. The electro-active antibacterial dental floss can be arranged in an electric dental floss device, can be replaced in a disassembling mode, and is sanitary, safe, convenient and quick.
In a third aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Adding the piezoelectric polymer matrix and the piezoelectric ceramic particles into a solvent, and stirring to form uniform dispersion liquid;
(2) Carrying out electrostatic spinning on the dispersion liquid through an electrostatic spinning machine to form fiber cloth;
(3) Cutting the fiber cloth to form dental floss wires;
(4) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
In the above step (1), the present application is not particularly limited in the kind of the solvent, as long as the object of the present application can be achieved, and the solvent may be at least one selected from the group consisting of N, N-dimethylformamide and acetone. For example, the solvent is N, N-dimethylformamide or N, N-dimethylformamide and acetone are mixed in a volume ratio of 1:2, and the total addition content of the piezoelectric polymer matrix and the piezoelectric ceramic particles is 15wt% to 20wt% based on the mass of the solvent. The application can lead the piezoelectric material to form uniform dispersion liquid by controlling the proportion of the solvent to the piezoelectric polymer matrix and the piezoelectric ceramic particles, and can lead the electrostatic spinning to be operable. When the solvent addition ratio is too small, the piezoelectric material cannot form a uniform dispersion, electrospinning is not operable or the formed fiber cloth has poor stability. When the addition ratio of the solvent is too large, the content of the piezoelectric material in the dispersion is too low, resulting in that electrospinning is not possible.
In the step (2), the present application is not particularly limited to the electrostatic spinning machine, and any electrostatic spinning machine known in the art may be used as long as the object of the present application is achieved, and the present application is not limited thereto. The present application is not particularly limited to the operating parameters of the electrospinning machine, as long as the objects of the present application can be achieved. Parameters such as electrospinning may be: the voltage is 16kV, the push injection rate is 0.7ml/h, the receiving distance is 15cm, the rotating speed of the receiving roller is 900rpm, the spinning temperature is normal temperature, the humidity is 30%, and the spinning time is 6h. The application adopts an electrostatic spinning method, and can change the surface morphology of dental floss, such as a porous structure, by controlling the proportion of different solvents, thereby being beneficial to better exerting the piezoelectric performance and increasing the friction coefficient.
In the step (3), the present application is not particularly limited as long as the object of the present application can be achieved. For example, using a cutter, cutting is performed precisely to a determined floss width or quantitatively using an automated device. When the prepared dental floss is finally processed into a dental floss roll, besides the fiber cloth, the fiber cloth is cut first and then wound so as to realize the dental floss roll.
In the above step (4), the present application is not particularly limited as long as the object of the present application can be achieved. For example, the draft may be 2-3.5 times. When the dental floss wire is subjected to the drawing, annealing and corona polarization treatment, the sequence of the annealing and corona polarization treatment is not particularly limited, so long as the object of the present application can be achieved. For example, the annealing treatment may be performed first, followed by corona polarization treatment, or the corona polarization treatment may be performed first, followed by annealing treatment. The annealing temperature of the application can be 120-150 ℃, the annealing time can be 2-3 h, the voltage of corona polarization can be 10kV-50kV, the distance can be 10mm-50mm, the temperature can be 25-50 ℃, and the time can be 10-60 min.
In a fourth aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and adding the mixture into a double-screw extruder for granulating to form material particles;
(2) Adding the material particles into a melt injection molding machine, and performing melt injection molding to form dental floss wires;
(3) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
The twin screw extruder and the melt injection molding machine are not particularly limited in the present application, and twin screw extruders and melt spinning machines known in the art may be employed as long as the objects of the present application are achieved, and the present application is not limited thereto. The present application is not particularly limited in terms of the operating parameters of the twin-screw extruder as long as the objects of the present application can be achieved. For example, the extrusion temperature may be 200℃to 300℃and the working pressure may be 7MPa to 15MPa. The working parameters of the melt injection molding are not particularly limited in the present application as long as the objects of the present application can be achieved. For example, the temperature of the melt injection molding may be 130℃to 235 ℃. The present application is not particularly limited as long as the object of the present application can be achieved. For example, the draft may be 2-3.5 times. When the dental floss wire is subjected to the drawing, annealing and corona polarization treatment, the sequence of the annealing and corona polarization treatment is not particularly limited, so long as the object of the present application can be achieved. For example, the annealing treatment may be performed first, followed by corona polarization treatment, or the corona polarization treatment may be performed first, followed by annealing treatment. The annealing temperature of the application can be 120-150 ℃, the annealing time can be 2-3 h, the corona polarization voltage can be 10kV-50kV, the distance is 10mm-50mm, the temperature is 25-50 ℃, and the time is 10-60 min.
In a fifth aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and loading the mixture into a high-molecular three-dimensional printer for three-dimensional printing by a fusion method to form dental floss wires;
(2) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
The polymer three-dimensional printer is not particularly limited, and any polymer three-dimensional printer known in the art may be used as long as the object of the present application can be achieved, and the present application is not limited thereto. The working parameters of the fusion method three-dimensional printing are not particularly limited, so long as the purpose of the application can be achieved. Operating parameters for, for example, fusion process three-dimensional printing may include: the thickness of the layer is 0.01mm-0.015mm, the thickness of the wall is 0.01mm-0.015mm, the printing speed is 0.1-0.2mm/s, and the printing temperature is 200-250 ℃. The present application is not particularly limited as long as the object of the present application can be achieved. For example, the draft may be 2-3.5 times. When the dental floss wire is subjected to the drawing, annealing and corona polarization treatment, the sequence of the annealing and corona polarization treatment is not particularly limited, so long as the object of the present application can be achieved. For example, the annealing treatment may be performed first, followed by corona polarization treatment, or the corona polarization treatment may be performed first, followed by annealing treatment. The annealing temperature of the application can be 100-150 ℃, the annealing time can be 1-3 h, the corona polarization voltage can be 10kV-50kV, the distance is 10mm-50mm, the temperature is 25-50 ℃, and the time is 10-60 min.
In a sixth aspect, the present application provides a method of preparing an electroactive antimicrobial dental floss comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, adding the mixture into a double-screw extruder for granulating to form granules, and adding the granules into an extrusion spinning machine for melt spinning to form dental floss filaments; or alternatively
(1') adding the piezoelectric polymer matrix into an extrusion spinning machine, and carrying out melt spinning to form dental floss;
(2) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
The twin-screw extruder and the melt spinning machine are not particularly limited in the present application, and a twin-screw extruder and a melt spinning machine known in the art may be employed as long as the object of the present application is achieved. The present application is not particularly limited in terms of the operating parameters of the twin-screw extruder as long as the objects of the present application can be achieved. For example, the extrusion temperature may be 200℃to 300℃and the working pressure may be 7MPa to 15MPa. The working parameters of the melt spinning are not particularly limited in the present application as long as the object of the present application can be achieved. For example, the temperature of the melt spinning may be 130℃to 235 ℃. The present application is not particularly limited as long as the object of the present application can be achieved. For example, the draft may be 2-3.5 times. When the annealing and corona polarization treatment are adopted, the sequence of the annealing and corona polarization treatment is not particularly limited as long as the object of the present application can be achieved. For example, the annealing treatment may be performed first, followed by corona polarization treatment, or the corona polarization treatment may be performed first, followed by annealing treatment. The annealing temperature of the application can be 120-150 ℃, the annealing time can be 1-3 h, the corona polarization voltage can be 10kV-50kV, the distance is 10mm-50mm, the temperature is 25-50 ℃, and the time is 10-60 min. When the volume percentage of the piezoelectric polymer matrix in the raw materials of the electroactive antibacterial dental floss is not 100%, forming the dental floss by adopting the preparation method of the step (1); when the volume percentage of the piezoelectric polymer matrix in the raw material of the electroactive antibacterial dental floss is 100 percent and the volume percentage of the piezoelectric ceramic particles is 0, the dental floss wire is formed by adopting the preparation method of the step (1').
The electroactive antibacterial dental floss provided by the application takes the piezoelectric polymer or the compound of the piezoelectric polymer and the piezoelectric ceramic particles as the raw material, and the formed dental floss material has the advantages of uniform distribution, stable performance, good flexibility and strong operability; the electroactive antibacterial dental floss provided by the application generates a piezoelectric effect and outputs an electric signal through contact friction with the adjacent surfaces of teeth in the use process, can inhibit bacteria growth in teeth while cleaning residues and dental calculus, generates good antibacterial performance, and effectively relieves periodontitis, prevents caries and other symptoms.
Test method and instrument:
dynamic piezoelectric performance test:
cutting the electroactive antibacterial dental floss to 10cm in length, clamping the electroactive antibacterial dental floss to be in a tight state by using a clamp, tightly attaching the surface of the electroactive antibacterial dental floss to the prepared isolated dental floss, bonding conductive adhesive and electrodes at two ends, respectively connecting the electrodes at the two ends to a Jimmy electrometer (Keithley 6514), controlling the electroactive antibacterial dental floss to regularly slide on the dental floss surface (1 time/second) by using a stepper (Sanyou benefit mechanical processing plant), and receiving voltage output on a screen.
Static piezoelectric performance test:
quasi-static d for electroactive antibacterial dental floss in different examples and comparative examples 33 Measuring instrument (ZJ-6A, institute of acoustic science, department of China) for measuring piezoelectric constant d of electroactive antibacterial dental floss 33 The edge of the electroactive antibacterial dental floss material is gently clamped by using a pair of tweezers, the electroactive antibacterial dental floss material is placed between two measuring electrodes of a quasi-static instrument, the upper button is gently rotated to enable the two electrodes to be in light contact, screen display data are recorded, and the average value of 5 points measured by each electroactive antibacterial dental floss is taken as a final test result.
Static strength test:
static Strength test the test was performed according to the national standard ISO2815:2018 dental integral handle floss.
Tensile test:
tensile test the test was carried out according to the national standard ISO2815:2018 "dental integral handle floss".
Antibacterial performance test:
(1) Preparation of brain heart infusion medium (BHI liquid medium): 7.4g of BHI powder (200.0 g of bovine brain, 250.0g of bovine heart extract 10.0g of peptone, 2.0g of glucose, 5.0g of NaCl and 20.0g of agar) is weighed, 400ml of deionized water is added, and the mixture is uniformly mixed and then subjected to high pressure at 120 ℃ for standby; preparation of a solid culture medium: adding 2% agar powder into the dissolved liquid culture medium, sterilizing under high pressure, cooling to 70deg.C, pouring into 9cm culture dish in an ultra clean bench, cooling, sealing, and storing in a refrigerator at 4deg.C;
(2) The experimental strain is selected from streptococcus mutans ua159 and resuscitatedInoculating on solid culture medium at 37deg.C with 5% CO 2 Culturing in an incubator for 24 hours, picking part of bacterial colonies, observing bacterial colony morphology under an optical microscope after gram staining, and carrying out partial subculture for later use after confirming no pollution;
(3) The electroactive antibacterial dental floss of each example and comparative example was sterilized with absolute ethanol and co-cultured with streptococcus mutans in BHI liquid medium for 24 hours;
(4) Preparing a staining solution: the fluorescent stain comprises two SYT09 stains and PI stains, and can make living bacteria emit green fluorescence and dead bacteria emit red fluorescence. Before dyeing, respectively mixing SYT09 coloring agent and coloring agent reagent in equal proportion under a light-shielding condition, putting into the same centrifuge tube (Ep tube), shaking and mixing uniformly, and keeping out light for later use;
(5) Co-culturing electroactive antibacterial dental floss and streptococcus mutans in a BHI liquid culture medium for 24 hours, sucking the supernatant by a pipetting gun, carefully and lightly washing with sterile normal saline for 1 time, and washing out suspended bacteria;
(6) An appropriate amount of staining solution was added dropwise to the surface of the plaque biofilm, incubated for 15min at room temperature under a dark room, carefully rinsed with PBS buffer to remove excess dye and the electroactive antibacterial dental floss in each example and comparative example was placed on a slide glass, photographed using a laser confocal microscope (CLSM) observation, and red fluorescence intensity and green fluorescence intensity were obtained.
Antibacterial ratio = red fluorescence intensity/(red fluorescence intensity + green fluorescence intensity) ×100%.
Absorbance (OD value) test for 3 h:
the streptococcus mutans and the electroactive antibacterial dental floss are co-cultured for 24 hours, bacteria liquid is sucked, PBS buffer solution is used for washing for 3 times, fresh BHI liquid culture medium is added, the culture is continued for 3 hours, 100 mu L of bacteria suspension is taken out to a 96-well plate, 5 compound wells are arranged for each sample, 3 repeated samples are arranged in each group, OD value is read at 630nm wavelength in an enzyme label instrument, and 3h absorbance (OD value) is obtained.
The time for continuing the culture after adding the fresh BHI liquid medium was changed to 0h, 6h and 12h, and the absorbance at 0h (OD value), the absorbance at 6h (OD value) and the absorbance at 12h (OD value) were obtained in this order. Among them, the smaller the OD value, the better the antibacterial property of the toothbrush filament.
Example 1
(1) PVDF is added into N, N-dimethylformamide as a solvent according to the raw material composition in Table 1, and the mixture is magnetically stirred and mixed until a uniform dispersion is formed, wherein the mass ratio of PVDF to the solvent is 18:100, the weight average molecular weight of PVDF is 55 ten thousand, and the piezoelectric constant d 33 30pC/N with a melting temperature of 235 ℃;
(2) Filling the dispersion liquid into a syringe in an electrostatic spinning machine for electrostatic spinning to form fiber cloth with the thickness of 130 mu m; the parameters of the electrostatic spinning are as follows: voltage 16kV, push rate 0.7ml/h, receiving distance 15cm, receiving roller rotating speed 900rpm, spinning temperature normal temperature, humidity 30%, spinning time 6h;
(3) Cutting the fiber cloth to form dental floss wires, wherein the cutting width is 2mm;
(4) The dental floss is drawn for 2 times and annealed for 2 hours at 120 ℃ to obtain the electroactive antibacterial dental floss, wherein the thickness of the electroactive antibacterial dental floss is 130 mu m, and the width of the electroactive antibacterial dental floss is 1mm.
Example 2
(1) According to the raw material composition in Table 1, PVDF and potassium sodium niobate are uniformly mixed, added into a double screw extruder for granulation to form granules, wherein the PVDF has a weight average molecular weight of 55 ten thousand, a melting temperature of 235 ℃, a piezoelectric constant of 30pC/N, a piezoelectric constant of 125pC/N, and a temperature of 235 ℃ and a pressure of 10MPa for extrusion granulation;
(2) Adding the material particles into a melt injection molding machine, heating to 235 ℃ of the melting temperature of the material particles, extruding, injecting and winding by a spinneret after the material particles are completely melted, and forming dental floss wires;
(3) The dental floss is drawn for 2 times and annealed for 1.5 hours at 120 ℃ to obtain the electroactive antibacterial dental floss, wherein the thickness of the electroactive antibacterial dental floss is 120 mu m, and the width of the electroactive antibacterial dental floss is 1mm.
Example 3
(1) According to the raw material composition in Table 1, P (VDF-TrFE) is loaded into a high molecular three-dimensional printer for three-dimensional printing by a fusion method to form dental floss, and the working parameters of the three-dimensional printing by the fusion method are as follows: a layer thickness of 0.01mm, a wall thickness of 0.01mm, a printing speed of 0.1mm/s, a printing temperature of 235 ℃, wherein the weight average molecular weight of P (VDF-TrFE) is 45 ten thousand, the melting temperature is 126.9 ℃ and the piezoelectric constant is 35pC/N;
(2) The dental floss is drawn for 2 times, and corona polarization treatment is carried out to obtain the electroactive antibacterial dental floss, wherein the voltage of the corona polarization treatment is 20kV, the distance is 30mm, the temperature is 40 ℃ and the time is 30min, and the thickness of the electroactive antibacterial dental floss is 60 mu m and the width is 1mm.
Example 4
(1) Adding P (VDF-HFP) into an extrusion spinning machine according to the raw material composition in Table 1, heating to 235 ℃ of melting temperature of the granules, extruding, spinning and winding by a spinneret after the granules are completely melted to form dental floss, wherein the weight average molecular weight of P (VDF-HFP) is 45 ten thousand, the piezoelectric constant is 35pC/N, and the melting temperature is 126.9 ℃;
(2) The dental floss is drawn for 2 times, and corona polarization treatment is carried out to obtain the electroactive antibacterial dental floss, wherein the voltage of the corona polarization treatment is 50kV, the distance is 50mm, the temperature is 50 ℃, the time is 60min, the thickness of the electroactive antibacterial dental floss is 140 mu m, and the width is 1mm.
Examples 5 to 10
The procedure of example 1 was repeated except that the parameters were adjusted as shown in Table 1.
Comparative example 1
The procedure of example 1 was repeated except that the parameters were adjusted as shown in Table 1.
Comparative example 2
The procedure was as in example 2, except that the relevant parameters were adjusted as in Table 1. Wherein the weight average molecular weight of nylon is 1.5 ten thousand.
The parameter settings for each example and comparative example are shown in table 1 and the performance test data are shown in table 2.
TABLE 1
Note that: the "/" in table 1 indicates that there is no corresponding parameter; the annealing process parameters are 120 ℃ and 2h, wherein the annealing temperature is 120 ℃ and the annealing time is 2h; the "10kV,20mins,50mm" in the polarization treatment parameters represents the voltage of corona polarization of 20kV, the time of 30min and the distance of 50mm.
TABLE 2
Referring to table 2 and fig. 2 to 4, it can be seen from examples 1 to 10 and comparative examples 1 to 2 that the electrically active antibacterial dental floss prepared by using the raw material formulation of the electrically active antibacterial dental floss provided by the present application has good piezoelectric properties and a certain antibacterial property, and particularly, compared with the dental floss prepared by using a nylon material having no piezoelectric function (comparative example 2), the piezoelectric and antibacterial properties of the dental floss of the present application are significantly improved. Examples 1 to 10 have a piezoelectric constant d of the electroactive antibacterial dental floss 33 The highest output voltage between 1.5pC/N and 9.3pC/N, which is higher than 0.38V, is greater than that of comparative example 2, indicating that the electroactive antibacterial dental floss prepared using the raw materials of the present application has excellent piezoelectric properties. Meanwhile, the tensile force of the electroactive antibacterial dental floss in the embodiment 1 to the embodiment 10 is more than 11N, the static strength is not damaged and is removed, the antibacterial rate is more than 65.3%, and the static strength of the dental floss in the comparative example 1 and the comparative example 2 is damaged and removed, and the antibacterial rate is lower, which indicates that the electroactive antibacterial dental floss prepared by adopting the raw material proportion of the application has excellent strength and antibacterial property. Specifically, as shown in fig. 2 and 4, examples 1 and 9 have piezoelectric constants d of electroactive antibacterial dental floss in a static state 33 The 3h OD values were 0.05 and 0.046 for 7.5pC/N and 9.3pC/N, respectively, while the piezoelectric constants d of the electroactive antibacterial dental floss of comparative example 1 and comparative example 2 were 0.05 and 0.046, respectively 33 The OD values were 0.052 and 0.131 for 4.2pC/N and 0.3 h, respectively. It can be seen that the piezoelectric constant d of the electroactive antibacterial dental floss in the examples of the present application is higher than that of the dental floss in the comparative example 33 Is improved and inhibits bacteriaThe breeding capacity is correspondingly enhanced. Specifically, as shown in fig. 3, under the action of external force (equivalent to the process of using dental floss), the output voltages of the embodiment 1 and the embodiment 9 are 0.65V and 0.8V respectively, the antibacterial rate reaches 78.9% and 90.8%, while the comparative example 2 has no voltage output, and the antibacterial rate is only 10.3, which shows that the electroactive antibacterial dental floss prepared by the application has voltage output under the action of dynamic external force and has good antibacterial performance.
Referring to table 2, it can be seen from example 1 and comparative example 1 that the raw material composition in the electrically active antibacterial floss was the same, but the floss was treated differently, so that the highest output voltage, 3h OD value and antibacterial rate of the obtained electrically active antibacterial floss were greatly different, and the piezoelectric performance of the electrically active antibacterial floss in example 1 was superior to that of comparative example 1. Thus, it is demonstrated that annealing and/or corona polarization treatment of dental floss within the above-described range of the present application can provide an electroactive antibacterial dental floss having a piezoelectric effect, and the electroactive antibacterial dental floss has an excellent antibacterial effect, and can effectively inhibit the growth of bacteria in crevices and reduce the formation of dental plaque during use. Specifically, referring to table 2 and fig. 1 to 4, wherein the white part in the middle of fig. 1 is the electroactive antibacterial dental floss object prepared in example 1, example 9, comparative example 1 and comparative example 2 according to the present application, respectively, the dark gray part is background, and in the antibacterial property test, the higher the OD value of the culture solution, the faster the streptococcus mutans grows, the higher the concentration per unit volume thereof, and further the antibacterial property of the dental floss is worse. As shown in Table 2, the OD values of the culture solutions of the dental floss of examples 1 to 10 after 3 hours of cultivation with Streptococcus mutans were lower than that of comparative example 1 in the antibacterial property test, thereby demonstrating that the toothbrush filaments manufactured by the manufacturing method provided by the present application have good antibacterial properties.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or article that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, or article. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method or article comprising such element.
In this specification, each embodiment is described in a related manner, and identical and similar parts of each embodiment are all referred to each other, and each embodiment mainly describes differences from other embodiments.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application are included in the protection scope of the present application.
Claims (10)
1. An electroactive antimicrobial dental floss comprising the following components in percentage by volume:
90-100% of piezoelectric polymer matrix
0-10% of piezoelectric ceramic particles; or alternatively
70-90% of piezoelectric polymer matrix
10-30% of piezoelectric ceramic particles;
wherein the material of the piezoelectric polymer matrix is at least one selected from polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene and polyvinylidene fluoride-hexafluoropropylene;
the piezoelectric ceramic particles are at least one selected from barium titanate, barium strontium titanate, lithium niobate and sodium potassium niobate;
the dental floss is treated by stretching, annealing and/or corona polarization to make the dental floss wire have a piezoelectric constant d 33 1.5pC/N-9.3pC/N.
2. The electroactive antibacterial dental floss of claim 1, wherein the piezoelectric ceramic particles have a particle size of 50nm-30 μm.
3. The electro-active antibacterial dental floss of claim 1, wherein the electro-active antibacterial dental floss has a width of 50 μm-3mm and a thickness of 50 μm-150 μm.
4. The electro-active antibacterial floss of claim 1, wherein the highest output voltage of the electro-active antibacterial floss is 0.3V-1.0V.
5. The electrically active antibacterial floss of claim 1, wherein the antibacterial rate of the electrically active antibacterial floss is 66% -91%.
6. An electrically powered flossing device comprising the electrically active antibacterial floss of any one of claims 1-5.
7. A method of preparing an electroactive antimicrobial dental floss according to any one of claims 1-5 comprising the steps of:
(1) Adding the piezoelectric polymer matrix and the piezoelectric ceramic particles into a solvent to form uniform dispersion;
(2) Carrying out electrostatic spinning on the dispersion liquid through an electrostatic spinning machine to form fiber cloth;
(3) The fiber cloth is cut to form dental floss wires;
(4) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
8. A method of preparing an electroactive antimicrobial dental floss according to any one of claims 1-5 comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and adding the mixture into a double-screw extruder for granulating to form material particles;
(2) Adding the material particles into a melt injection molding machine, and performing melt injection molding to form dental floss;
(3) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
9. A method of preparing an electroactive antimicrobial dental floss according to any one of claims 1-5 comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and loading the mixture into a high-molecular three-dimensional printer for three-dimensional printing by a fusion method to form dental floss wires;
(2) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
10. A method of preparing an electroactive antimicrobial dental floss according to any one of claims 1-5 comprising the steps of:
(1) Uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, adding the mixture into a double-screw extruder for granulating to form granules, and adding the granules into an extrusion spinning machine for melt spinning to form dental floss filaments; or alternatively
(1') adding the piezoelectric polymer matrix into an extrusion spinning machine, and carrying out melt spinning to form dental floss; and
(2) The dental floss silk is subjected to drafting, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115286883A (en) * | 2022-09-30 | 2022-11-04 | 北京大学口腔医学院 | Method for regulating antibacterial activity and application |
| CN115381574B (en) * | 2022-10-27 | 2023-01-24 | 北京大学口腔医学院 | Antibacterial electric toothbrush based on pulse ultrasonic piezoelectric response principle and antibacterial method |
| CN115399906A (en) * | 2022-11-01 | 2022-11-29 | 北京大学口腔医学院 | Electric antibacterial interdental cleaner containing piezoelectric response silk thread and antibacterial method |
| CN115634159B (en) * | 2022-12-16 | 2023-07-07 | 北京大学口腔医学院 | Antibacterial toothpaste |
| CN115634158B (en) * | 2022-12-21 | 2023-04-11 | 北京大学口腔医学院 | Long-acting antibacterial flowing composite resin or pit and fissure sealant composition for dentistry and application |
| CN116270727B (en) * | 2022-12-23 | 2023-11-14 | 北京大学口腔医学院 | Oral antibacterial composition, preparation method and application |
| CN115957137B (en) * | 2022-12-23 | 2023-09-12 | 北京大学口腔医学院 | Compositions and methods for long-acting antibacterial adhesion |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110088367A (en) * | 2017-10-17 | 2019-08-02 | 株式会社村田制作所 | Antimicrobial yarn and antibiotic fabric |
| CN110088366A (en) * | 2016-12-20 | 2019-08-02 | 株式会社村田制作所 | Anti-bacterial fibre |
| CN114058165A (en) * | 2021-11-04 | 2022-02-18 | 四川大学 | Piezoelectric polylactic acid material and preparation method and application thereof |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030075212A (en) * | 2002-03-16 | 2003-09-26 | (주)카마텍 | Dieletric Device Using PVDF and Nano Ceramics Particles, and Method for Fabrication the Same |
| CA3043345A1 (en) * | 2016-11-10 | 2018-05-17 | Polyvalor, Limited Partnership | Piezoelectric composite, ink and ink cartridge for 3d printing, bifunctional material comprising the piezoelectric composite, manufacture and uses thereof |
| CN107233625A (en) * | 2017-06-13 | 2017-10-10 | 北京大学口腔医学院 | A kind of powered composite membrane and preparation method thereof that prevents adhesion for skull repairing |
| US20210047484A1 (en) * | 2018-03-01 | 2021-02-18 | Tepha, Inc. | Medical devices containing poly(butylene succinate) and copolymers thereof |
| CN111819205B (en) * | 2018-03-23 | 2024-01-30 | 科腾聚合物有限责任公司 | Styrene block copolymer with ultrahigh melt fluidity |
| CN108530806B (en) * | 2018-04-08 | 2020-04-10 | 北京科技大学 | Double-layer structure flexible piezoelectric film with high output and preparation and application methods thereof |
| CN114051543B (en) * | 2019-12-20 | 2023-09-29 | 株式会社村田制作所 | Spun yarn, yarn and cloth provided with spun yarn |
| CN112646335A (en) * | 2020-12-04 | 2021-04-13 | 珠海麦得发生物科技股份有限公司 | Tough polyester material and preparation method and application thereof |
| CN113478810B (en) * | 2021-07-26 | 2022-05-03 | 四川大学 | Preparation method of polyvinylidene fluoride-based 3D printed piezoelectric part with porous structure |
| CN114959933B (en) * | 2022-07-08 | 2023-08-15 | 北京大学口腔医学院 | Electroactive antibacterial dental floss and preparation method thereof |
| CN115399906A (en) * | 2022-11-01 | 2022-11-29 | 北京大学口腔医学院 | Electric antibacterial interdental cleaner containing piezoelectric response silk thread and antibacterial method |
-
2022
- 2022-07-08 CN CN202210806838.4A patent/CN114959933B/en active Active
- 2022-07-08 CN CN202310911721.7A patent/CN116949589A/en active Pending
-
2023
- 2023-08-29 WO PCT/CN2023/115427 patent/WO2024008213A1/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110088366A (en) * | 2016-12-20 | 2019-08-02 | 株式会社村田制作所 | Anti-bacterial fibre |
| CN110088367A (en) * | 2017-10-17 | 2019-08-02 | 株式会社村田制作所 | Antimicrobial yarn and antibiotic fabric |
| CN114058165A (en) * | 2021-11-04 | 2022-02-18 | 四川大学 | Piezoelectric polylactic acid material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李军 等: "《检测技术及仪表》", vol. 2, 中国轻工业出版社, pages: 177 - 181 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024008213A1 (en) * | 2022-07-08 | 2024-01-11 | 北京大学口腔医学院 | Electrically active antibacterial dental floss and preparation method therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114959933B (en) | 2023-08-15 |
| WO2024008213A1 (en) | 2024-01-11 |
| CN114959933A (en) | 2022-08-30 |
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