CN114959933A - Electroactive antibacterial dental floss and preparation method thereof - Google Patents
Electroactive antibacterial dental floss and preparation method thereof Download PDFInfo
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- CN114959933A CN114959933A CN202210806838.4A CN202210806838A CN114959933A CN 114959933 A CN114959933 A CN 114959933A CN 202210806838 A CN202210806838 A CN 202210806838A CN 114959933 A CN114959933 A CN 114959933A
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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
- 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
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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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- 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
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- 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
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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 material of the piezoelectric polymer matrix is selected from at least one of polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene and polyvinylidene fluoride-hexafluoropropylene; the piezoelectric ceramic particles are selected from at least one of barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate. The application provides an antibiotic dental floss of electroactive can produce piezoelectric effect in the use, not only can clean residue and tartar, can also produce good antibiotic performance through bacterial growing in the electrified function suppression tooth of dental floss.
Description
Technical Field
The application relates to the technical field of dental floss, in particular to an electroactive antibacterial dental floss and a preparation method thereof.
Background
Maintaining clean teeth is critical to oral health, and the lesions of periodontal and gingival inflammation are mostly located on interproximal and interproximal spaces between teeth. Thus, cleaning of the interproximal and interproximal teeth is an important aspect of oral self care. Dental floss is used as a cleaning tool that can penetrate through the interproximal spaces of teeth to clean interproximal areas of teeth, subgingival spaces, and debris and tartar from misaligned teeth.
At present, the dental floss is generally made of nylon threads, silk threads, polyester threads and the like, mainly removes residues and tartar of teeth through a mechanical cleaning principle, and cannot remove and inhibit bacteria and dental plaque on the adjacent surfaces of the teeth, so that the risks of caries and periodontal diseases are increased.
Disclosure of Invention
The application aims to provide an electroactive antibacterial dental floss which generates a piezoelectric effect in a using process and has good antibacterial performance while cleaning residues in gaps between teeth. The specific technical scheme is as follows:
the application provides an electroactive antibacterial dental floss, which comprises the following components in percentage by volume:
piezoelectric polymer matrix 70-100%
Piezoelectric ceramic particles 0-30%;
wherein, the material of the piezoelectric polymer matrix is selected from at least one of polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene and polyvinylidene fluoride-hexafluoropropylene;
the piezoelectric ceramic particles are selected from at least one of barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate.
In some embodiments, an electroactive antimicrobial dental floss comprising the following components in percent by volume:
piezoelectric polymer matrix 70-90%
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 antimicrobial 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 dental floss 33 Is 1.5pC/N-9.3 pC/N.
In some embodiments, the electroactive antimicrobial dental floss has a maximum output voltage of 0.3V to 1.0V.
In some embodiments, the electrically active antimicrobial dental floss has an antimicrobial rate of 66% to 91%.
A second aspect of the present invention provides a motorized flosser including the electrically active antimicrobial floss of any one of the preceding embodiments.
In a third aspect of the present invention, there is provided a method for preparing an electrically active antibacterial dental floss, comprising the steps of:
(1) adding a piezoelectric polymer matrix and piezoelectric ceramic particles into a solvent 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 a dental floss;
(4) the dental floss is obtained by stretching, annealing and/or corona polarization treatment of the dental floss.
The fourth aspect of the invention provides a preparation method of an electroactive antibacterial dental floss, which comprises the following steps:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and adding the mixture into a double-screw extruder for granulation to form material particles;
(2) adding the material particles into a melt injection molding machine, and performing melt injection molding to form the dental floss wires;
(3) the dental floss is obtained by stretching, annealing and/or corona polarization treatment of the dental floss.
The fifth aspect of the present invention provides a method for preparing an electrically active antibacterial dental floss, comprising the steps of:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and filling the mixture into a high-molecular three-dimensional printer for three-dimensional printing by a fusion method to form a dental floss wire;
(2) the dental floss is obtained by stretching, annealing and/or corona polarization treatment of the dental floss.
The invention provides a preparation method of an electroactive antibacterial dental floss, which comprises the following steps:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, adding the mixture into a double-screw extruder for granulation to form material particles, adding the material particles into an extrusion spinning machine, and performing melt spinning to form dental filaments; or
(1') adding a piezoelectric polymer matrix into an extrusion spinning machine, and carrying out melt spinning to form a dental thread;
(2) the dental floss is subjected to drawing, 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 is uniform in distribution, stable in performance, good in flexibility and strong in operability; the application provides an antibiotic dental floss of electroactive produces the piezoelectricity effect through rubbing with the adjacent face contact of tooth in the use, and the output signal of telecommunication when clean residue and tartar, can also restrain bacterial growing in the tooth through electrified performance, produces good antibacterial property, effectively prevents the caries, reduces the probability that gingivitis appears etc..
Of course, it is not necessary for any product or method of the present application to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions in the present application or the prior art, the drawings needed for describing the embodiments or the prior art are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and other embodiments can be obtained by those skilled in the art according to the drawings.
FIG. 1 is a schematic representation of the electroactive antimicrobial dental floss prepared according to examples 1, 9, comparative examples 1 and 2 of the present application;
FIG. 2 is a graph showing the static piezoelectric constant d of the electroactive antibacterial dental floss prepared in examples 1 and 9, comparative examples 1 and 2 of the present application 33 A test result chart of (1);
FIG. 3 is a graph showing the dynamic piezoelectric signal test of the electroactive antibacterial flosses prepared in examples 1 and 9, comparative example 1 and comparative example 2 under the action of external force;
fig. 4 is a result of a bacteriostatic performance test of the electrically active antibacterial dental floss prepared in example 1, example 9, comparative example 1 and comparative example 2 of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the description herein are intended to be within the scope of the present disclosure.
In a first aspect of the present application, there is provided an electrically active antibacterial dental floss comprising the following components in percentage by volume:
piezoelectric polymer matrix 70-100%
Piezoelectric ceramic particles 0-30%;
wherein, the material of the piezoelectric polymer matrix is selected from at least one of polyvinylidene fluoride, polyvinylidene fluoride-trifluoroethylene and polyvinylidene fluoride-hexafluoropropylene;
the piezoelectric ceramic particles are selected from at least one of barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate.
In the present application, among the materials of the piezoelectric polymer matrix, the piezoelectric constants d of polyvinylidene fluoride (PVDF), polyvinylidene fluoride-trifluoroethylene (P (VDF-TrFE)), and polyvinylidene fluoride-hexafluoropropylene (P (VDF-HFP)) are 33 Respectively 18 pC/N-35 pC/N, 30 pC/N-40 pC/N, and 30 pC/N-40 pC/N; piezoelectric constant d of barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate in piezoelectric ceramic particles 33 185 and 195pC/N respectively; 139-149 pC/N; 187-197 pC/N; 120-130 pC/N; the piezoelectric polymer matrix and the piezoelectric ceramic particles have large dielectric constants and strong piezoelectricity, 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 in the present application as long as the object of the present application can be achieved, and for example, the weight average molecular weight of the polyvinylidene fluoride (PVDF), polyvinylidene fluoride-trifluoroethylene (P (VDF-TrFE)), and polyvinylidene fluoride-hexafluoropropylene (P (VDF-HFP)) is 50 to 60 ten thousand, 40 to 50 ten thousand, and 40 to 50 ten thousand 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 200-280 ℃, 110-217 ℃ and 110-180 ℃ 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 within the range, the electroactive antibacterial dental floss with certain piezoelectric performance can be formed, and the dental floss wire has appropriate flexibility and toughness and strong operability. The piezoelectric ceramic particles are used as inorganic piezoelectric materials, and when the volume percentage of the piezoelectric ceramic particles is within the range, the piezoelectric ceramic particles can 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:
piezoelectric polymer matrix 70-90%
10-30% of piezoelectric ceramic particles.
The application provides an electro-active antibacterial dental floss, through the content of control electric pressure polymer base member and piezoceramics granule in the anti-bacterial dental floss of electro-active, can make the anti-antibiotic of electro-activeThe floss has piezoelectric function, so that piezoelectric effect is generated in the using process of the electroactive antibacterial floss, for example, the floss is wrapped around the adjacent surfaces of teeth in a C shape in the using process, and ultrasonic or pressure is applied to promote the upper and lower lifting and friction, so that the friction-piezoelectric composite effect is realized, and the floss has good antibacterial performance under the combined action of friction and piezoelectric. In particular, the piezoelectric constant d 33 1.5pC/N-9.3pC/N, and the highest output voltage is 0.3V-1.0V. Under the action of the piezoelectric effect, the electroactive antibacterial dental floss can better clean residues and tartar in teeth and can bring good antibacterial performance. In some embodiments of the present application, the electroactive antimicrobial dental floss is at least one of straight wire, beaded, and wavy in shape. The formation of the dental filaments into the above-described shape can be controlled by adjusting the electrospinning parameters and the post-processing process.
In some embodiments of the present 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 range, the dispersibility of the piezoelectric ceramic particles in the piezoelectric polymer matrix is high, the mixing uniformity of the dental floss material is high, and the performance stability of the prepared electroactive antibacterial dental floss is good.
In some embodiments of the present application, the electroactive antimicrobial 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 present application, the piezoelectric constant d of the electroactive antimicrobial dental floss 33 Is 1.5pC/N-9.3 pC/N. The electroactive antibacterial dental floss provided by the application has certain piezoelectric performance.
In some embodiments, the electroactive antimicrobial dental 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 present application, the antimicrobial rate of the electrically active antimicrobial dental floss is between 66% and 91%. The electroactive antibacterial dental floss provided by the application has good antibacterial performance. The electrically active antibacterial dental floss generates a piezoelectric effect after being stimulated by external force in the using process, so that the electrically active antibacterial dental floss is electrified, the breeding of bacteria in dental gaps can be inhibited, the formation of dental plaque is prevented, the symptoms such as periodontitis and the like are relieved, and meanwhile, the growth and the propagation of the bacteria on the electrically active antibacterial dental floss can be reduced, so that the antibacterial performance of the dental floss is improved.
A second aspect of the present invention provides a motorized flosser comprising the electrically active antimicrobial dental floss of any one of the previous embodiments, the resulting motorized flosser having a piezoelectric effect and good antimicrobial and bacteriostatic properties. The present application is not particularly limited to motorized flossers, so long as the objectives of the present application are achieved. For example, motorized flossers are ultrasonically driven. This application antibiotic dental floss of electroactive can install in electronic dental floss ware, can replace through dismantling the mode, sanitary safety, convenient and fast.
In a third aspect of the present invention, there is provided a method for preparing an electrically active antibacterial dental floss, comprising the steps of:
(1) adding a piezoelectric polymer matrix and 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 a dental floss;
(4) the dental floss is obtained by stretching, annealing and/or corona polarization treatment of the dental floss.
In the step (1), the solvent is not particularly limited as long as the object of the present invention can be achieved, and the solvent may be at least one selected from 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 content of the piezoelectric polymer matrix and the piezoelectric ceramic particles added is 15 wt% to 20 wt% based on the mass of the solvent. By controlling the proportion of the solvent to the piezoelectric polymer matrix and the piezoelectric ceramic particles, the piezoelectric material can form uniform dispersion liquid, and electrostatic spinning can be operated. When the addition ratio of the solvent 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 electrostatic spinning is not achievable.
In the step (2), the electrostatic spinning machine is not particularly limited, and any electrostatic spinning machine known in the art may be used as long as the object of the present invention can be achieved, and the present invention is not limited thereto. The working parameters of the electrostatic spinning machine are not particularly limited as long as the purpose of the present invention is achieved. For example, the parameters of electrospinning can be: the voltage is 16kV, the injection rate is 0.7ml/h, the receiving distance is 15cm, the rotating speed of a receiving roller is 900rpm, the spinning temperature is normal temperature, the humidity is 30%, and the spinning time is 6 h. The electrostatic spinning method is adopted, the surface appearance of the dental floss, such as a porous structure, can be changed by controlling the proportion of different solvents, the piezoelectric performance can be better exerted, and the friction coefficient is increased.
In the step (3), the cutting of the fiber cloth is not particularly limited as long as the object of the present invention can be achieved. For example, with a cutting knife, cut precisely to a determined floss width or cut quantitatively with automated equipment. When the prepared dental floss is finally processed into a dental floss roll, the fiber cloth needs to be cut first and then wound so as to realize the dental floss roll.
In the step (4), the drawing is not particularly limited as long as the object of the invention can be achieved. For example, the draft can be at a multiple of 2 to 3.5. When the dental filament is subjected to drawing, annealing and corona polarization treatment, the present application does not specifically limit the order of annealing and corona polarization treatment as long as the object of the present application is achieved. For example, the annealing treatment may be performed first, followed by the corona polarization treatment, or the corona polarization treatment may be performed first, followed by the annealing treatment. The annealing temperature can be 120-150 ℃, the annealing time can be 2-3 h, the voltage of corona polarization can be 10-50 kV, the distance can be 10-50 mm, the temperature can be 25-50 ℃, and the time can be 10-60 min.
The fourth aspect of the invention provides a preparation method of an electroactive antibacterial dental floss, which comprises the following steps:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and adding the mixture into a double-screw extruder for granulation to form material particles;
(2) adding the granules into a melt injection molding machine, and performing melt injection molding to form the dental floss wires;
(3) the dental floss is obtained by stretching, annealing and/or corona polarization treatment of the dental floss.
The twin-screw extruder and the melt injection molding 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 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 twin-screw extruder are not particularly limited by the present application as long as the object of the present application can be achieved. For example, the extrusion temperature can be 200-300 ℃, and the working pressure can be 7-15 MPa. The working parameters of the melt injection molding 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 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 can be at a multiple of 2 to 3.5. When the dental filament is subjected to drawing, annealing and corona polarization treatment, the present application does not specifically limit the order of annealing and corona polarization treatment as long as the object of the present application is achieved. For example, the annealing treatment may be performed first, followed by the corona polarization treatment, or the corona polarization treatment may be performed first, followed by the annealing treatment. The annealing temperature can be 120-150 ℃, the annealing time can be 2-3 h, the voltage of corona polarization can be 10-50 kV, the distance can be 10-50 mm, the temperature can be 25-50 ℃, and the time can be 10-60 min.
The fifth aspect of the present invention provides a method for preparing an electrically active antibacterial dental floss, comprising the steps of:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and filling the mixture into a high-molecular three-dimensional printer for three-dimensional printing by a fusion method to form a dental floss wire;
(2) the dental floss is obtained by stretching, annealing and/or corona polarization treatment of the dental floss.
The polymer three-dimensional printer is not particularly limited in the present application, 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 three-dimensional printing by the fusion method are not particularly limited as long as the purpose of the present application can be achieved. For example, the operating parameters for three-dimensional printing by the fusion method may include: the layer thickness is 0.01mm-0.015mm, the wall thickness is 0.01mm-0.015mm, the printing speed is 0.1-0.2mm/s, and the printing temperature is 200-. The present application is not particularly limited as long as the object of the present application can be achieved. For example, the draft can be at a multiple of 2 to 3.5. When the dental filament is subjected to drawing, annealing and corona polarization treatment, the present application does not specifically limit the order of annealing and corona polarization treatment as long as the object of the present application is achieved. For example, the annealing treatment may be performed first, followed by the corona polarization treatment, or the corona polarization treatment may be performed first, followed by the annealing treatment. The annealing temperature can be 100-150 ℃, the annealing time can be 1-3 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 10min-60 min.
The invention provides a preparation method of an electroactive antibacterial dental floss, which comprises the following steps:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, adding the mixture into a double-screw extruder for granulation to form material particles, adding the material particles into an extrusion spinning machine, and performing melt spinning to form dental filaments; or
(1') adding a piezoelectric polymer matrix into an extrusion spinning machine, and carrying out melt spinning to form a dental thread;
(2) the dental floss is subjected to drawing, 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 herein, and those known in the art can be used as long as the object of the present application can be achieved. The working parameters of the twin-screw extruder are not particularly limited by the present application as long as the object of the present application can be achieved. For example, the extrusion temperature can be 200-300 ℃, and the working pressure can be 7-15 MPa. The working parameters of melt spinning are not particularly limited as long as the object of the present invention can be achieved. For example, the melt spinning temperature 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 can be at a multiple of 2 to 3.5. When annealing and corona polarization treatment are adopted, the sequence of annealing and corona polarization treatment is not particularly limited, so long as the purpose of the invention can be achieved. For example, the annealing treatment may be performed first, followed by the corona polarization treatment, or the corona polarization treatment may be performed first, followed by the annealing treatment. The annealing temperature can be 120-150 ℃, the annealing time can be 1-3 h, the voltage of corona polarization can be 10-50 kV, the distance can be 10-50 mm, the temperature can be 25-50 ℃, and the time can be 10-60 min. When the volume percentage of the piezoelectric polymer matrix in the raw material of the electric active antibacterial dental floss is not 100 percent, forming a dental wire by adopting the preparation method in the step (1); and (2) when the volume percentage of the piezoelectric polymer matrix in the raw materials of the electric active antibacterial dental floss is 100 percent and the volume percentage of the piezoelectric ceramic particles is 0 percent, forming the dental floss wire by adopting the preparation method in 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 is uniform in distribution, stable in performance, good in flexibility and strong in operability; the application provides an electro-active antibacterial dental floss produces piezoelectric effect through the adjacent face contact friction with the tooth in the use, and the output signal of telecommunication when clean residue and tartar, can also restrain bacterial growing in the tooth, produces good antibacterial property, effectively alleviates periodontitis, prevents symptoms such as carious.
Test methods and apparatus:
and (3) testing dynamic piezoelectric performance:
cutting the electroactive antibacterial dental floss into a length of 10cm, clamping the electroactive antibacterial dental floss by using a clamp to enable the electroactive antibacterial dental floss to be in a tense state and enable the surface of the electroactive antibacterial dental floss to be tightly attached to a prepared in-vitro tooth, adhering conductive adhesive and electrodes at two ends, respectively connecting the electrodes connected with the two ends to a Gishley electrometer (Keithley 6514), controlling the electroactive antibacterial dental floss to regularly slide on the tooth surface (1 time/second) by using a stepper (three-friend Delley mechanical processing factory), 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 sciences, Chinese academy of sciences) for measuring piezoelectric constant d of electroactive antibacterial dental floss 33 The edge of the electroactive antibacterial dental floss material is gently clamped by a pair of tweezers, the electroactive antibacterial dental floss material is placed between two measuring electrodes of the quasistatic instrument, the upper button is gently rotated to enable the two electrodes to be gently contacted, screen display data are recorded, and 5 points are measured by each electroactive antibacterial dental floss to obtain an average value as a final test result.
Static strength test:
static Strength test the static strength test was carried out according to the national Standard ISO2815:2018 dental Integrated handle dental floss.
And (3) tensile test:
tensile test tests were performed according to the national standard ISO2815:2018 dental integrated handle dental floss.
And (3) testing antibacterial performance:
(1) preparation of brain heart infusion medium (BHI liquid medium): weighing 7.4g BHI powder (200.0g medulla bovis Seu Bubali, 250.0g Cor bovis Seu Bubali extract 10.0g peptone, 2.0g glucose, 5.0g NaCl, 20.0g agar), adding 400ml deionized water, mixing, and keeping at 120 deg.C under high pressure; preparing a solid culture medium: adding 2% agar powder into the dissolved liquid culture medium, autoclaving, cooling to 70 deg.C, pouring into a 9cm culture dish in a super clean bench, cooling, inverting, sealing, and storing in a refrigerator at 4 deg.C;
(2) selecting Streptococcus mutans ua159 as experimental strain, inoculating the experimental strain on solid culture medium, recovering, inoculating at 37 deg.C and 5% CO 2 Culturing for 24 hours in an incubator, selecting partial colonies, observing the morphology of the colonies under an optical microscope after gram staining, and performing partial subculture for later use after confirming no pollution;
(3) the electroactive antibacterial dental floss in each example and comparative example is sterilized by absolute ethyl alcohol and then is co-cultured with streptococcus mutans in a BHI liquid culture medium for 24 hours;
(4) preparing a dyeing liquid: the fluorescent stain comprises two SYT09 stains and a PI stain, and can enable live bacteria to emit green fluorescence and dead bacteria to emit red fluorescence. Before dyeing, respectively mixing SYT09 dye and dye reagent in equal proportion in the same centrifugal tube (Ep tube) under the condition of keeping out of the sun, oscillating and uniformly mixing, and keeping out of the sun for later use;
(5) co-culturing the electrically active antibacterial dental floss and the streptococcus mutans in a BHI liquid culture medium for 24 hours, sucking a supernatant by using a pipette, carefully washing the supernatant with sterile normal saline for 1 time, and washing off suspended bacteria;
(6) the plaque biofilm surface was incubated with a proper amount of staining solution dropwise in a dark room at room temperature for 15min, carefully rinsed with PBS buffer to remove excess dye and the electroactive antibacterial dental floss in each of the examples and comparative examples was placed on a glass slide, photographed by observation using a laser confocal microscope (CLSM), and red fluorescence intensity and green fluorescence intensity were obtained.
The inhibition ratio was red fluorescence intensity/(red fluorescence intensity + green fluorescence intensity) × 100%.
3h absorbance (OD value) test:
co-culturing streptococcus mutans and the electroactive antibacterial dental floss for 24 hours, removing a bacterial liquid by suction, washing the streptococcus mutans and the electroactive antibacterial dental floss for 3 times by using phosphate buffered saline (PBS buffer), adding a fresh BHI liquid culture medium, continuously culturing for 3 hours, taking out 100 mu L of bacterial suspension, putting each sample into a 96-well plate, arranging 5 repeated wells, reading an OD value at a wavelength of 630nm in an enzyme-labeling instrument for 3-hour absorbance (OD value).
The time for continuous culture after adding fresh BHI liquid culture medium is changed to 0h, 6h and 12h, and the absorbance (OD value) of 0h, the absorbance (OD value) of 6h and the absorbance (OD value) of 12h can be obtained in sequence. Wherein, the smaller the OD value is, the better the antibacterial performance of the toothbrush filament is.
Example 1
(1) PVDF was added to the solvent N, N-dimethylformamide according to the composition of the raw materials in Table 1, mixed by magnetic stirring until a homogeneous mixture was formedA homogeneously dispersed liquid, wherein the mass ratio of PVDF to solvent is 18:100, the weight average molecular weight of PVDF is 55 ten thousand, the piezoelectric constant d 33 30pC/N and 235 ℃ of melting temperature;
(2) loading the dispersion into an injector in an electrostatic spinning machine for electrostatic spinning to form fiber cloth with the thickness of 130 mu m; the parameters of electrostatic spinning are as follows: the voltage is 16kV, the injection rate is 0.7ml/h, the receiving distance is 15cm, the rotating speed of a receiving roller is 900rpm, the spinning temperature is normal temperature, the humidity is 30 percent, and the spinning time is 6 h;
(3) cutting the fiber cloth to form a dental floss wire, wherein the cutting width is 2 mm;
(4) drawing the dental floss wire by 2 times, and annealing at 120 deg.C for 2h to obtain the electrically active antibacterial dental floss with thickness of 130 μm and width of 1 mm.
Example 2
(1) Uniformly mixing PVDF and potassium-sodium niobate according to the raw material composition in Table 1, adding the mixture into a double-screw extruder for granulation to form granules, wherein the weight-average molecular weight of PVDF is 55 ten thousand, the melting temperature is 235 ℃, the piezoelectric constant is 30pC/N, the piezoelectric constant of potassium-sodium niobate is 125pC/N, the temperature for extrusion granulation is 235 ℃, and the pressure is 10 MPa;
(2) adding the material particles into a melt injection molding machine, heating to the melting temperature of 235 ℃, after the material particles are completely melted, extruding, molding and winding the material particles through a spinneret to form a dental thread;
(3) drawing the dental floss by 2 times, and annealing at 120 deg.C for 1.5h to obtain the final product with thickness of 120 μm and width of 1 mm.
Example 3
(1) According to the raw material composition in table 1, P (VDF-TrFE) is loaded into a polymer three-dimensional printer for melt three-dimensional printing to form a dental floss filament, and the working parameters of the melt three-dimensional printing are as follows: the thickness of the layer is 0.01mm, the printing speed is 0.1mm/s, the printing temperature is 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 35 pC/N;
(2) the dental floss is stretched 2 times, and then 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 ℃, the time is 30min, the thickness of the electroactive antibacterial dental floss is 60 mu m, and the width of the electroactive antibacterial dental floss is 1 mm.
Example 4
(1) Adding P (VDF-HFP) into an extrusion spinning machine according to the raw material composition in the table 1, heating to the melting temperature of material particles of 235 ℃, after the material particles are completely melted, extruding, spinning and winding through a spinning nozzle to form the dental floss, wherein the weight average molecular weight of the 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 stretched 2 times, and then 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 of the electroactive antibacterial dental floss is 1 mm.
Examples 5 to 10
The procedure was as in example 1 except that the relevant parameters were adjusted as shown in Table 1.
Comparative example 1
The procedure was as in example 1 except that the relevant 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 shown in Table 1. Wherein the weight average molecular weight of the nylon is 1.5 ten thousand.
The parameter settings of each example and comparative example are shown in table 1, and the performance test data are shown in table 2.
TABLE 1
Note: the "/" in table 1 indicates that there is no corresponding parameter; among the annealing treatment process parameters, "120 ℃,2 h" means that the annealing temperature is 120 ℃ and the annealing time is 2 h; among the polarization treatment parameters, "10 kV,20mins,50 mm" means a voltage of 20kV, a time of 30min, and a distance of 50mm for corona polarization.
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 electroactive antibacterial dental floss prepared by using the raw material formulation of the electroactive antibacterial dental floss provided by the present application has good piezoelectric properties and certain antibacterial properties, and particularly, the piezoelectric and antibacterial properties of the dental floss in the examples of the present application are significantly improved compared to the dental floss prepared by using a nylon material without piezoelectric properties (comparative example 2). Piezoelectric constant d of the electroactive antibacterial dental floss of examples 1 to 10 33 The highest output voltage is higher than 0.38V and is larger than that of the comparative example 2 between 1.5pC/N and 9.3pC/N, which shows that the electroactive antibacterial dental floss prepared by using the raw materials of the application has excellent piezoelectric performance. Meanwhile, the tensile force of the electroactive antibacterial dental floss in examples 1 to 10 of the present application is greater than 11N, the static strength is not broken and removed, and the antibacterial rate is greater than 65.3%, while the static strength of the dental floss in comparative examples 1 and 2 is broken and removed, and the antibacterial rate is lower, which indicates that the electroactive antibacterial dental floss prepared by using the raw material ratio of the present application has excellent strength and antibacterial property. Specifically, as shown in fig. 2 and 4, the piezoelectric constant d of the electroactive antibacterial dental floss in the static state of the example 1 and the example 9 33 7.5pC/N and 9.3pC/N, respectively, and 3h OD values of 0.05 and 0.046, respectively, while the piezoelectric constant d of the electroactive antibacterial dental floss of comparative example 1 and comparative example 2 33 4.2pC/N and 0, respectively, and 3h OD values of 0.052 and 0.131, respectively. It can be seen that the piezoelectric constant d of the electroactive antibacterial dental floss in the examples of the present application is comparable to that of the dental floss in the comparative example 33 The capability of inhibiting the breeding of bacteria is improved correspondingly. Specifically, as shown in fig. 3, under the action of external force (equivalent to the process of using dental floss), the output voltages of example 1 and example 9 are 0.65V and 0.8V, respectively, and the bacteriostatic rate reaches 78.9% and 90.8%, while the comparative example 2 has no voltage output and has bacteriostatic effectThe rate is only 10.3, which shows that the electroactive antibacterial dental floss prepared by the method has voltage output under the action of dynamic external force and good antibacterial performance.
Referring to table 2, it can be seen from example 1 and comparative example 1 that the raw material composition of the electroactive antibacterial dental floss is the same, but the treatment manner of the dental floss wires is different, so that the maximum output voltage, the 3h OD value, and the antibacterial rate of the obtained electroactive antibacterial dental floss are greatly different, and the piezoelectric performance of the electroactive antibacterial dental floss in example 1 is superior to that of comparative example 1. Therefore, the dental floss is annealed and/or corona-polarized within the range of the application, so that the electroactive antibacterial dental floss with the piezoelectric effect can be obtained, and the electroactive antibacterial dental floss has an excellent antibacterial effect, can effectively inhibit the growth of bacteria in dental gaps during the use process, and can reduce the formation of dental plaque. 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 prepared in the examples 1, 9, 1 and 2 of the present application, respectively, and the dark gray part is the background, in the antibacterial performance test, the higher the OD value of the culture solution, the faster the streptococcus mutans grows, the higher the concentration per unit volume, and the worse the antibacterial performance of the dental floss. As shown in Table 2, the OD values of the cultured solutions of the dental floss of examples 1 to 10 after being cultured with Streptococcus mutans for 3 hours in the antibacterial property test were all lower than those of comparative example 1, thereby demonstrating that the toothbrush filaments prepared by the preparation method provided by the present application have good antibacterial property.
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.
All the embodiments in the present specification are described in a related manner, and the same and similar parts among the embodiments may be referred to each other, and each embodiment focuses on the differences from the other embodiments.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (12)
1. An electroactive antibacterial dental floss, which comprises the following components in percentage by volume:
piezoelectric polymer matrix 70-100%
Piezoelectric ceramic particles 0-30%;
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 selected from at least one of barium titanate, barium strontium titanate, lithium niobate and potassium sodium niobate.
2. The electroactive antimicrobial dental floss of claim 1, comprising the following components in percent by volume:
piezoelectric polymer matrix 70-90%
10-30% of piezoelectric ceramic particles.
3. The electrically active antimicrobial dental floss of claim 1, wherein the piezoelectric ceramic particles have a particle size of 50nm-30 μ ι η.
4. The electroactive antimicrobial dental floss of claim 1, wherein the electroactive antimicrobial dental floss has a width of 50 μ ι η to 3mm and a thickness of 50 μ ι η to 150 μ ι η.
5. The electroactive antimicrobial dental floss of claim 1, wherein the electroactive antimicrobial dental floss has a piezoelectric constant d 33 Is 1.5pC/N-9.3 pC/N.
6. The electrically active antimicrobial dental floss of claim 1, wherein the electrically active antimicrobial dental floss has a maximum output voltage of 0.3V-1.0V.
7. The electrically active antimicrobial dental floss of claim 1, wherein the antimicrobial rate of the electrically active antimicrobial dental floss is between 66% and 91%.
8. A motorized flosser comprising the electrically active antimicrobial dental floss of any one of claims 1-7.
9. A method of preparing an electrically active antimicrobial dental floss according to any of the claims 1-7, comprising the steps of:
(1) adding a piezoelectric polymer matrix and piezoelectric ceramic particles into a solvent 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 a dental floss wire;
(4) the dental floss is subjected to drawing, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
10. A method of preparing an electrically active antimicrobial dental floss according to any of the claims 1-7, 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 granulation to form material particles;
(2) adding the material particles into a melt injection molding machine, and performing melt injection molding to form the dental floss wires;
(3) the dental floss is subjected to drawing, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
11. A method of preparing an electrically active antimicrobial dental floss according to any of the claims 1-7, comprising the steps of:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, and filling the mixture into a high-molecular three-dimensional printer for three-dimensional printing by a fusion method to form a dental floss wire;
(2) the dental floss is subjected to drawing, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
12. A method of preparing an electrically active antimicrobial dental floss according to any of the claims 1-7, comprising the steps of:
(1) uniformly mixing a piezoelectric polymer matrix and piezoelectric ceramic particles, adding the mixture into a double-screw extruder for granulation to form material particles, adding the material particles into an extrusion spinning machine, and performing melt spinning to form dental filaments; or
(1') adding a piezoelectric polymer matrix into an extrusion spinning machine, and carrying out melt spinning to form a dental thread;
(2) the dental floss is subjected to drawing, annealing and/or corona polarization treatment to obtain the electroactive antibacterial dental floss.
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| CN202210806838.4A CN114959933B (en) | 2022-07-08 | 2022-07-08 | Electroactive antibacterial dental floss and preparation method thereof |
| CN202310911721.7A CN116949589A (en) | 2022-07-08 | 2022-07-08 | Electroactive antibacterial dental floss and preparation method thereof |
| PCT/CN2023/115427 WO2024008213A1 (en) | 2022-07-08 | 2023-08-29 | Electrically active antibacterial dental floss and preparation method therefor |
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| CN115286883A (en) * | 2022-09-30 | 2022-11-04 | 北京大学口腔医学院 | Method for regulating antibacterial activity and application |
| CN115381574A (en) * | 2022-10-27 | 2022-11-25 | 北京大学口腔医学院 | Antibacterial electric toothbrush based on pulse ultrasonic piezoelectric response principle and antibacterial method |
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| CN115634159A (en) * | 2022-12-16 | 2023-01-24 | 北京大学口腔医学院 | Antibacterial toothpaste |
| CN115634158A (en) * | 2022-12-21 | 2023-01-24 | 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 |
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| CN116270727A (en) * | 2022-12-23 | 2023-06-23 | 北京大学口腔医学院 | Oral antibacterial composition, preparation method and application |
| 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 |
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| CN115286883A (en) * | 2022-09-30 | 2022-11-04 | 北京大学口腔医学院 | Method for regulating antibacterial activity and application |
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| WO2024087434A1 (en) * | 2022-10-27 | 2024-05-02 | 北京大学口腔医学院 | Antibacterial electric toothbrush based on pulsed 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 |
| CN115634159A (en) * | 2022-12-16 | 2023-01-24 | 北京大学口腔医学院 | Antibacterial toothpaste |
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| CN115957137A (en) * | 2022-12-23 | 2023-04-14 | 北京大学口腔医学院 | Compositions and methods for long-acting anti-bacterial adhesion |
| CN116270727A (en) * | 2022-12-23 | 2023-06-23 | 北京大学口腔医学院 | Oral antibacterial composition, preparation method and application |
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| CN114959933B (en) | 2023-08-15 |
| WO2024008213A1 (en) | 2024-01-11 |
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