WO2018233317A1 - Self-cleaning degradable chitosan toothbrush and preparation method therefor - Google Patents

Self-cleaning degradable chitosan toothbrush and preparation method therefor Download PDF

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Publication number
WO2018233317A1
WO2018233317A1 PCT/CN2018/077975 CN2018077975W WO2018233317A1 WO 2018233317 A1 WO2018233317 A1 WO 2018233317A1 CN 2018077975 W CN2018077975 W CN 2018077975W WO 2018233317 A1 WO2018233317 A1 WO 2018233317A1
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Prior art keywords
solution
toothbrush
rosin
bristles
handle
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PCT/CN2018/077975
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French (fr)
Chinese (zh)
Inventor
于永臣
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青岛容商天下网络有限公司
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Publication of WO2018233317A1 publication Critical patent/WO2018233317A1/en

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    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46DMANUFACTURE OF BRUSHES
    • A46D1/00Bristles; Selection of materials for bristles
    • A46D1/02Bristles details
    • A46D1/0207Bristles characterised by the choice of material, e.g. metal
    • AHUMAN NECESSITIES
    • A46BRUSHWARE
    • A46DMANUFACTURE OF BRUSHES
    • A46D1/00Bristles; Selection of materials for bristles
    • A46D1/04Preparing bristles
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/08Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances

Definitions

  • the invention relates to the technical field of oral hygiene devices, in particular to a self-cleaning degradable chitosan toothbrush and a preparation method thereof.
  • CN201510060032.5 discloses an ultrasonic toothbrush: the ultrasonic vibration frequency is used to break the food residue and plaque, and the bristles are easily cleaned, thereby achieving the purpose of cleaning the oral cavity, but the toothbrush is expensive and long-term use may cause the human body hurt.
  • CN200710003433.2 discloses a toothbrush which stores a cleaning sterilizing agent with a hollow toothbrush handle: the bristles are hollow and communicate with the cavity of the handle, and the cleaning agent flows to the tooth surface through the hollow lumen of the bristles when brushing; the disadvantage of the toothbrush is that it is usually When the brush is not brushed, the detergent will flow out of the bristles, or the amount of detergent flowing out during brushing is uncontrollable; in addition, the detergent is equivalent to toothpaste, which does not essentially change the limitations of using toothpaste.
  • a disposable toothbrush and a small tube of toothpaste are packaged together, but the toothpaste is often not opened, and the toothpaste tube residue and the disposable toothbrush discarded after use are not degradable, polluting the environment, Wasted resources.
  • the present invention aims to provide a self-cleaning degradable chitosan toothbrush and a preparation method thereof.
  • the toothbrush provided by the invention is convenient to use, environment-friendly and does not need toothpaste during use; the toothbrush of the invention actively wears during the brushing process, and the micro-particles generated during the abrasion process can effectively sterilize and rub;
  • the bristles of the invention have antibacterial and antibacterial effects, and the used bristles are exposed to the air for a long time without reproducing harmful microorganisms such as bacteria, thereby better protecting oral hygiene and having wide application value.
  • the present invention provides a toothbrush comprising a bristles; a raw material component of the bristles comprising a first mixture; and a first mixture comprising a chitosan, a polylactic acid solution and a rosin solution.
  • the mass ratio of the mass of the chitosan to the solute polylactic acid in the polylactic acid solution is (1 to 2.5): 10, and the mass concentration of the polylactic acid solution is 4% to 10%
  • the polylactic acid solution is a solution of polylactic acid in acetic acid; the mass of chitosan is not more than 2% of the mass of the polylactic acid solution; the mass ratio of the solute rosin in the rosin solution to the solute polylactic acid in the polylactic acid solution is 1: (6-15);
  • the rosin solution is a rosin ethanol solution, and the mass percentage of the rosin ethanol solution is 9% to 11%.
  • the raw material component of the bristles further comprises a second mixture; the second mixture comprises dandelion, notoginsenoyl and sodium lauroyl sarcosinate; wherein, dandelion, notoginseng and sodium lauroyl sarcosinate
  • the mass ratio is (1 to 1.5) in order: (0.3 to 0.5): 1.
  • the preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 36h to 48h, turning every 3h, then filtering and collecting the filtrate; wherein, for each kilogram of dandelion, the added mass of water is 18L-22L; S302: adding sodium lauroyl sarcosinate to the filtrate and stirring uniformly to obtain a second mixture.
  • the toothbrush further includes a handle and a brush head; wherein the brush head is disposed at one end of the handle, and the brush head has an arc of 0.5 to 1.0 rad, a length of 2 to 3 cm, and a width of 1.5 to 2cm plate-like structure, and the side of the brush head near the arc center is the front side, and the side away from the arc center is the back side; the bristles are disposed on the front side of the brush head, and the length of the bristles is 0.5-0.8 cm;
  • the arc shape is the same, and the bending direction of the front half of the handle is the same as the bending direction of the brush head.
  • the bending direction of the rear half of the handle is opposite to the bending direction of the brush head.
  • the curvature of the handle is 0.8-1.2 rad and the length is 12-18 cm.
  • the end and back of the brush head are covered with silicone.
  • both the brush head and the handle are made of a degradable material.
  • the present invention provides a method for preparing a toothbrush, comprising the steps of: S101: dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution; and S102: adding a rosin solution to the first intermediate solution and stirring Uniformly, obtaining a second intermediate solution, specifically stirred in a sealed container for 15 min to 60 min; S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution; S104: adding to the third intermediate solution The porogen is then exposed to air for 1 h to obtain a glue solution; S105: the glue is made into a silk and then shaped to obtain bristles.
  • the ratio of the volume of the rosin solution to the volume of the first intermediate solution is 1: (10-20); and the preparation method of the rosin solution comprises: dissolving the rosin after being dissolved in the anhydrous Stir in ethanol and obtain a rosin solution. It will be appreciated by those skilled in the art that since the rosin is susceptible to oxidation, the rosin should not be allowed to stand in air for more than 1 hour after grinding, preferably immediately dissolved in ethanol.
  • the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15%-25 %, and the drop rate per minute is less than 60 drops; in S104, the porogen is sodium chloride and/or potassium chloride; and the porogen is added in an amount of 2 to 3 g per 100 mL of the third intermediate solution.
  • the shaping comprises: S201: forming a glue into a filament by a wire drawing machine, and then drying and shaping the filament to obtain a first original yarn; S202: rinsing the first strand with distilled water to remove the porogen, and then drying to obtain a second strand; S203: soaking the second strand in the second mixture, ultrasonically stirring for 10 min to 20 min, and then hanging indoors until The water is not dripped downward, and then dried at a low temperature of 60 ° C to 65 ° C to remove moisture to obtain a bristled raw material yarn; wherein the mass ratio of the second mixture to the second raw yarn is (800 to 1200): 1; S204 : The bristles are made into a tuft of toothbrushes to obtain bristles.
  • the operating temperature is 20 ° C to 28 ° C; in S201 to S204, the drying temperature is 60 ° C to 65 ° C.
  • the toothbrush provided by the present invention is convenient to use, environmentally friendly, and does not require toothpaste during use; the self-cleaning degradable chitosan toothbrush of the present invention actively wears during brushing, and is worn during wear.
  • the generated micro-particles can play an effective bactericidal and rubbing effect; in addition, the bristles of the present invention have antibacterial and antibacterial effects, and the used bristles are exposed to the air for a long time without reproducing harmful microorganisms such as bacteria, thereby better protecting Oral hygiene has a wide range of applications.
  • the raw material component of the bristles of the invention belongs to natural materials, has no toxic and side effects, and is more friendly to the human body; the rosin can effectively fill the chain break between chitosan and polylactic acid, and significantly enhance the plasticity and elasticity of the bristles. So that it is not easy to break; dandelion can help kill bacteria on the surface of teeth and other parts of the mouth, prevent plaque, dandelion also has anti-tumor effect, effectively prevent the production of oral cancer; Sanqi has the effect of blood, hemostasis, It can effectively prevent or relieve the symptoms of bleeding gums; sodium lauroyl sarcosinate in raw materials can produce foam when brushing teeth, thus replacing traditional toothpaste.
  • the curved brush head of the invention is more in conformity with the human oral structure, so as to be more conformable to the tooth surface; the silica gel covered on the brush head serves as a cushioning function, and reduces the injury and pain caused when the brushing tooth scrapes the gums and the ankle.
  • the length of the bristles of the present invention is 0.5 to 0.8 cm, which avoids the feeling of discomfort when brushing the gums based on the narrow space between the human gums and the inner wall of the oral cavity.
  • the raw material components of the invention are simple and easy to obtain, and the cost is low, and the preparation method has the advantages of stable process, high yield, good quality, low energy consumption, wide raw materials and simple process, and the production can be completed by using existing equipment.
  • the equipment requirements are reduced, and the brush head bristles can be degraded, naturally decomposed after being discarded, and have zero pollution to the environment, thereby having wide application value.
  • Figure 1 is a front elevational view of the self-cleaning degradable chitosan toothbrush of the present invention
  • Figure 2 is a side elevational view of the self-cleaning degradable chitosan toothbrush of the present invention.
  • test materials used in the following examples were purchased from conventional reagent stores.
  • FIG. 1 is a front view of a self-cleaning degradable chitosan toothbrush of the present invention
  • FIG. 2 is a side view of the self-cleaning degradable chitosan toothbrush of the present invention, as shown in FIGS. 1 and 2: the present invention provides a toothbrush.
  • the toothbrush comprises bristles; the raw material component of the bristles comprises a first mixture; the first mixture comprises chitosan, a polylactic acid solution and a rosin solution.
  • the toothbrush further comprises a handle and a brush head; the brush head is disposed at one end of the handle, and the brush head is a plate-like structure having an arc of 0.5 to 1.0 rad, a length of 2 to 3 cm, and a width of 1.5 to 2 cm, and the brush head
  • the side near the center of the arc is the front side, the side away from the center of the arc is the back side; the bristles are disposed on the front side of the brush head, and the length of the bristles is 0.5-0.8 cm;
  • the handle is curved, and the front half of the handle is The bending direction is the same as the bending direction of the brush head, and the bending direction of the rear half of the handle is opposite to the bending direction of the brush head.
  • the curvature of the handle is 0.8 to 1.2 rad and the length is 12 to 18 cm.
  • the brush head and the handle are made of a degradable material.
  • the mass ratio of the mass of the chitosan to the solute polylactic acid in the polylactic acid solution is (1 to 2.5): 10, the mass concentration of the polylactic acid solution is 4% to 10%, and the polylactic acid solution is polylactic acid.
  • the acetic acid solution; the mass ratio of the solute rosin in the rosin solution to the solute polylactic acid in the polylactic acid solution is 1: (6-15); and the rosin solution is a rosin ethanol solution, and the mass percentage concentration of the rosin ethanol solution is 9% ⁇ 11%.
  • the raw material component of the bristles further comprises a second mixture;
  • the second mixture comprises dandelion, notoginsenoyl and sodium lauroyl sarcosinate; wherein the mass ratio of dandelion, notoginsenoyl and sodium lauroyl sarcosinate is (1) ⁇ 1.5): (0.3 ⁇ 0.5): 1;
  • the preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 36h to 48h, then filtering and collecting the filtrate; wherein, per kilogram of dandelion, The water is added in a mass of 18 L to 22 L; S302: sodium lauroyl sarcosinate is added to the filtrate obtained in S301, and stirred uniformly to obtain a second mixture.
  • the present invention specifically designs a preparation method comprising the following steps:
  • S101 Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
  • the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
  • S103 adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution.
  • the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15% to 25%, and the droplet acceleration per minute is less than 60 drop.
  • the porogen is sodium chloride and/or potassium chloride; and the porogen is added in an amount of 2 to 3 g per 100 mL of the third intermediate solution.
  • the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result a porogen, followed by drying to obtain a second strand; S203: immersing the second strand in the second mixture, ultrasonically stirring, and then drying to obtain a bristled raw material yarn; wherein, the second mixture and the second raw yarn The mass ratio is (800 to 1200): 1; S204: the bristle raw material yarn is made into a toothbrush tuft, that is, the bristles are obtained.
  • the operating temperature is 20 ° C to 28 ° C; in the S201 to S204, the drying temperature is 60 ° C to 65 ° C.
  • the operation principle and process of the self-cleaning degradable chitosan toothbrush of the invention are: in the process of brushing, the toothbrush is placed in the mouth after being drowned, and rubbed and rubbed on the surface of the tooth, and the bristles made of chitosan-polylactic acid copolymer are
  • the wear resistance is very poor, so that it is constantly worn and produces tiny particles. The fine particles assist the bristles to rub the food residue and plaque, and clean the teeth and the mouth, replacing the friction agent in the toothpaste.
  • the chitosan polylactic acid copolymer has many micropores inside, and the dandelion extract, the notoginseng extract and the sodium lauroyl sarcosinate are stored in these micropores, and the teeth are slowly released due to the dissolution of water and the impact of water flow during brushing. Come out, play the role of sterilization, hemostasis and foaming agent.
  • the invention provides a self-cleaning degradable chitosan toothbrush, comprising: chitosan, polylactic acid solution and rosin solution.
  • the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 2.5:10
  • the polylactic acid solution is an acetic acid solution of polylactic acid having a mass percentage of 10%
  • the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid is 1:6, and the rosin solution is a rosin ethanol solution having a mass percent concentration of 9%.
  • the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
  • S101 Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
  • the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
  • S103 adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution.
  • the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 20%, and the droplet acceleration per minute is 50 drops.
  • the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result The pore agent is then dried to obtain a second raw yarn; S203: the second raw yarn is immersed in water, ultrasonically stirred for 10 minutes, and then dried to obtain a bristled raw material yarn.
  • the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 60 ° C.
  • the present invention provides a self-cleaning degradable chitosan toothbrush comprising: a chitosan, a polylactic acid solution, and a rosin solution.
  • the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 1:10
  • the polylactic acid solution is an acetic acid solution of polylactic acid having a mass concentration of 4%
  • the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid was 1:15, and the rosin solution was a rosin ethanol solution having a mass percent concentration of 11%.
  • the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
  • S101 Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
  • the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
  • S103 adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution.
  • the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15%, and the droplet acceleration per minute is 50 drops.
  • the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result The pore agent is then dried to obtain a second raw yarn; S203: the second raw yarn is immersed in water, ultrasonically stirred for 20 minutes, and then dried to obtain a bristled raw material yarn.
  • the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 65 ° C.
  • This embodiment is set on the basis of the first embodiment.
  • the invention provides a self-cleaning degradable chitosan toothbrush, comprising: chitosan, polylactic acid solution, rosin solution, dandelion, notoginsenoic acid and sodium lauroyl sarcosinate; wherein dandelion, notoginseng and lauroyl myosine
  • the mass ratio of sodium is 1:0.3:1 in order.
  • the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 2.5:10, the polylactic acid solution is an acetic acid solution of polylactic acid having a mass concentration of 10%; the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid is 1:6, and the rosin solution is a rosin ethanol solution having a mass percent concentration of 9%.
  • the preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 36h, then filtering and collecting the filtrate; wherein, in kilograms of dandelion, the added mass of water is 20L; S302: sodium lauroyl sarcosinate The filtrate was added to the filtrate and stirred well to obtain a second mixture.
  • the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
  • S101 Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
  • the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
  • S103 adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution.
  • the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 20%, and the droplet acceleration per minute is 50 drops.
  • the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, and then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result a porogen, followed by drying to obtain a second raw yarn; S203: immersing the second raw yarn in the second mixture, ultrasonically stirring for 10 minutes, and then drying to obtain a bristled raw material yarn; wherein, the second mixture and the second raw yarn The mass ratio is 1000:1.
  • the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 60 ° C.
  • This embodiment is set on the basis of the second embodiment.
  • the invention provides a self-cleaning degradable chitosan toothbrush, comprising: chitosan, polylactic acid solution, rosin solution, dandelion, notoginsenoic acid and sodium lauroyl sarcosinate; wherein dandelion, notoginseng and lauroyl myosine
  • the mass ratio of sodium is 1.5:0.5:1 in order.
  • the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 1:10
  • the polylactic acid solution is an acetic acid solution of polylactic acid having a mass concentration of 4%
  • the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid was 1:15, and the rosin solution was a rosin ethanol solution having a mass percent concentration of 11%.
  • the preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 48 hours, then filtering and collecting the filtrate; wherein, for each kilogram of dandelion, the added mass of water is 20L; S302: sodium lauroyl sarcosinate The filtrate was added to the filtrate and stirred well to obtain a second mixture.
  • the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
  • S101 Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
  • the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
  • S103 adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution.
  • the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15%, and the droplet acceleration per minute is 50 drops.
  • the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result a pore agent, followed by drying to obtain a second strand; S203: soaking the second strand in water, ultrasonically stirring for 20 min, and then drying to obtain a bristle strand; wherein, the mass ratio of the second mixture to the second strand It is 1000:1.
  • the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 65 ° C.
  • Test strains Staphylococcus aureus, Lactobacillus, Salmonella typhi, Pseudomonas aeruginosa, Streptococcus mutans, and Helicobacter pylori.
  • Preparation of bacterial solution The slanted strain was inoculated into 20% bovine juice culture medium, cultured overnight at 37 ° C, and the bacterial liquid was diluted to 10 cfu/ml with 20% bovine juice culture medium, and immediately inoculated.
  • MIC measurement serial dilution of the liquid tube was used, and a 20% bovine juice medium sample (each obtained by brushing each of the examples) was subjected to serial dilution.
  • the highest dilution for sterile growth is MIC, thereby evaluating the antibacterial effect of the self-cleaning degradable chitosan toothbrush prepared by the present invention on common strains in an in vitro bacteriostatic test with a minimum inhibitory concentration (MIC, mg/mL).
  • the patients are divided into 5 groups of 100 persons, and the self-cleaning degradable chitosan toothbrushes of the first to fourth embodiments are respectively tested in the first group to the fourth group, one time each morning and evening. 5 min each time; the fifth group was brushed with normal Colgate toothpaste.
  • the toothbrush prepared by the self-cleaning degradable chitosan toothbrush provided by the present invention was continuously tested for 20 days, and the symptoms of each volunteer were recorded. The specific data are shown in Table 2.
  • the efficacy is judged as:
  • the toothbrush provided by the invention is convenient to use, environmentally friendly and does not need toothpaste during use; the self-cleaning degradable chitosan toothbrush of the invention actively wears during the brushing process, and the micro-particles generated during the abrasion process can effectively sterilize
  • the bristles of the present invention have antibacterial and antibacterial effects, and the used bristles are exposed to the air for a long time without propagating harmful microorganisms such as bacteria, thereby better protecting oral hygiene and having wide application value.
  • first and second are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated.
  • features defining “first” and “second” may include one or more of the features either explicitly or implicitly.
  • the meaning of "a plurality” is two or more unless specifically and specifically defined.

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Abstract

A self-cleaning degradable chitosan toothbrush and a preparation method therefor. The toothbrush comprises bristles. The raw material components of the bristles comprise chitosan, a polylactic acid solution, and a rosin solution. The toothbrush further comprises a handle and a head; the head is provided at one end of the handle; the handle is arc-shaped; the bending direction of the front half of the handle is the same as that of the head, and the bending direction of the rear half of the handle is opposite to that of the head; the head and the handle are both made of degradable materials. The toothbrush is convenient to use and environmentally friendly, and needs no toothpaste during use; the toothbrush is actively worn in a tooth brushing process, and micro-particles produced in the wear process can achieve efficient bactericidal and frictional effects. In addition, the toothbrush itself has antibacterial and bacteriostatic effects, so that the reproduction of harmful microorganisms such as bacteria is avoided even if the used bristles are exposed to the air for a long time. Therefore, the toothbrush better protects oral hygiene and has a high application value.

Description

自清洁可降解壳聚糖牙刷及其制备方法Self-cleaning degradable chitosan toothbrush and preparation method thereof 技术领域Technical field
本发明涉及口腔卫生装置技术领域,具体涉及一种自清洁可降解壳聚糖牙刷及其制备方法。The invention relates to the technical field of oral hygiene devices, in particular to a self-cleaning degradable chitosan toothbrush and a preparation method thereof.
背景技术Background technique
刷牙作为人们日常生活中的必须活动,旅途、出差或宿营时常常会遇到带了牙刷没带牙膏的情况,因此,一种不需要使用牙膏的牙刷成为一种需要。此外,日常生活中使用的传统牙刷存在严重的安全隐患:刷毛比表面积较大,导致使用过后潮湿且隐藏有食物残渣、牙齿污垢的刷毛在直接暴露于空气中时滋生细菌等微生物,严重损害人体健康;换句话说,传统牙刷无法自行杀灭刷毛上滋生的有害微生物。Brushing your teeth is a must-have activity in people's daily lives. When you travel, travel or camp, you often encounter a toothbrush without a toothpaste. Therefore, a toothbrush that does not require toothpaste becomes a necessity. In addition, the traditional toothbrush used in daily life has serious safety hazards: the bristles have a large specific surface area, which causes the bristles that are wet after use and hides food residue and tooth dirt to breed bacteria and other microorganisms when directly exposed to the air, seriously damaging the human body. Health; in other words, traditional toothbrushes cannot kill the harmful microbes that breed on the bristles.
传统牙刷中,CN201510060032.5公开了一种超声波牙刷:依靠超声波振动频率达到破碎食物残渣和菌斑、方便刷毛清理,从而达到清洁口腔的目的,但该牙刷价格昂贵且长时间使用可能对人体造成伤害。CN200710003433.2公开了一种以中空牙刷柄储存清洁杀菌剂的牙刷:刷毛中空并与刷柄的空腔连通,刷牙时清洁剂通过刷毛的中空管腔流到牙齿表面;该牙刷的缺点在于平时不刷牙的时候清洁剂会流出刷毛,或者刷牙时清洁剂流出的量不可控;此外,清洁剂即相当于牙膏,本质上并未改变使用牙膏的局限性。对于市场上存在的一次性刷牙用具:将一次性牙刷和一小管牙膏包装在一起,但其中的牙膏经常打不开,且使用后抛弃的牙膏管残骸和一次性牙刷不可降解,污染了环境、浪费了资源。In the traditional toothbrush, CN201510060032.5 discloses an ultrasonic toothbrush: the ultrasonic vibration frequency is used to break the food residue and plaque, and the bristles are easily cleaned, thereby achieving the purpose of cleaning the oral cavity, but the toothbrush is expensive and long-term use may cause the human body hurt. CN200710003433.2 discloses a toothbrush which stores a cleaning sterilizing agent with a hollow toothbrush handle: the bristles are hollow and communicate with the cavity of the handle, and the cleaning agent flows to the tooth surface through the hollow lumen of the bristles when brushing; the disadvantage of the toothbrush is that it is usually When the brush is not brushed, the detergent will flow out of the bristles, or the amount of detergent flowing out during brushing is uncontrollable; in addition, the detergent is equivalent to toothpaste, which does not essentially change the limitations of using toothpaste. For disposable brushing appliances on the market: a disposable toothbrush and a small tube of toothpaste are packaged together, but the toothpaste is often not opened, and the toothpaste tube residue and the disposable toothbrush discarded after use are not degradable, polluting the environment, Wasted resources.
基于此,研发一款新型的能够有效杀菌从而防治各种口腔问题的牙刷尤为 重要。Based on this, it is especially important to develop a new type of toothbrush that can effectively sterilize and prevent various oral problems.
发明内容Summary of the invention
针对现有技术中的缺陷,本发明旨在提供一种自清洁可降解壳聚糖牙刷及其制备方法。本发明提供的牙刷使用方便、环境友好且在使用过程中无需牙膏;本发明的牙刷在刷牙过程中主动磨损,且磨损过程中产生的微型颗粒物可以起到有效的杀菌和摩擦作用;此外,本发明的刷毛自身具有抗菌抑菌作用,使用过的刷毛长时间暴露在空气中不会繁殖细菌等有害微生物,从而更好地保护口腔卫生,具有广泛的应用价值。In view of the deficiencies in the prior art, the present invention aims to provide a self-cleaning degradable chitosan toothbrush and a preparation method thereof. The toothbrush provided by the invention is convenient to use, environment-friendly and does not need toothpaste during use; the toothbrush of the invention actively wears during the brushing process, and the micro-particles generated during the abrasion process can effectively sterilize and rub; The bristles of the invention have antibacterial and antibacterial effects, and the used bristles are exposed to the air for a long time without reproducing harmful microorganisms such as bacteria, thereby better protecting oral hygiene and having wide application value.
为此,本发明提供如下技术方案:To this end, the present invention provides the following technical solutions:
第一方面,本发明提供一种牙刷,牙刷包括刷毛;刷毛的原料组分包括第一混合物;第一混合物包括壳聚糖、聚乳酸溶液和松香溶液。In a first aspect, the present invention provides a toothbrush comprising a bristles; a raw material component of the bristles comprising a first mixture; and a first mixture comprising a chitosan, a polylactic acid solution and a rosin solution.
在本发明的进一步实施方式中,壳聚糖的质量与聚乳酸溶液中溶质聚乳酸的质量比为(1~2.5):10,聚乳酸溶液的质量百分浓度为4%~10%,且聚乳酸溶液为聚乳酸的醋酸溶液;壳聚糖的质量不超过聚乳酸溶液质量的2%;松香溶液中溶质松香与聚乳酸溶液中溶质聚乳酸的质量比为1:(6~15);且松香溶液为松香乙醇溶液,且松香乙醇溶液的质量百分浓度为9%~11%。In a further embodiment of the present invention, the mass ratio of the mass of the chitosan to the solute polylactic acid in the polylactic acid solution is (1 to 2.5): 10, and the mass concentration of the polylactic acid solution is 4% to 10%, and The polylactic acid solution is a solution of polylactic acid in acetic acid; the mass of chitosan is not more than 2% of the mass of the polylactic acid solution; the mass ratio of the solute rosin in the rosin solution to the solute polylactic acid in the polylactic acid solution is 1: (6-15); The rosin solution is a rosin ethanol solution, and the mass percentage of the rosin ethanol solution is 9% to 11%.
在本发明的进一步实施方式中,刷毛的原料组分还包括第二混合物;第二混合物包括蒲公英、三七和月桂酰肌氨酸钠;其中,蒲公英、三七和月桂酰肌氨酸钠的质量比依次为(1~1.5):(0.3~0.5):1。第二混合物的制备方法包括以下步骤:S301:将蒲公英和三七用水浸泡36h~48h,每3h翻动依次,之后过滤并收集滤液;其中,每千克蒲公英中,水的加入质量为18L~22L;S302:将月桂酰肌氨酸钠加入滤液中,搅拌均匀,得到第二混合物。In a further embodiment of the invention, the raw material component of the bristles further comprises a second mixture; the second mixture comprises dandelion, notoginsenoyl and sodium lauroyl sarcosinate; wherein, dandelion, notoginseng and sodium lauroyl sarcosinate The mass ratio is (1 to 1.5) in order: (0.3 to 0.5): 1. The preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 36h to 48h, turning every 3h, then filtering and collecting the filtrate; wherein, for each kilogram of dandelion, the added mass of water is 18L-22L; S302: adding sodium lauroyl sarcosinate to the filtrate and stirring uniformly to obtain a second mixture.
在本发明的进一步实施方式中,牙刷还包括刷柄和刷头;其中,刷头设于刷柄的一端,且刷头是弧度为0.5~1.0rad,长度为2~3cm,宽度为1.5~2cm的板状结构,且刷头靠近弧形圆心的一侧为正面,远离弧形圆心的一侧为背面;刷毛设置在刷头的正面,且刷毛的长度为0.5~0.8cm;刷柄为弧形,且刷柄前半部的弯曲方向与刷头的弯曲方向相同,刷柄后半部的弯曲方向与刷头的弯曲方向相反,刷柄的弧度为0.8~1.2rad,长度为12~18cm;刷头的端部和背面覆有硅胶。In a further embodiment of the present invention, the toothbrush further includes a handle and a brush head; wherein the brush head is disposed at one end of the handle, and the brush head has an arc of 0.5 to 1.0 rad, a length of 2 to 3 cm, and a width of 1.5 to 2cm plate-like structure, and the side of the brush head near the arc center is the front side, and the side away from the arc center is the back side; the bristles are disposed on the front side of the brush head, and the length of the bristles is 0.5-0.8 cm; The arc shape is the same, and the bending direction of the front half of the handle is the same as the bending direction of the brush head. The bending direction of the rear half of the handle is opposite to the bending direction of the brush head. The curvature of the handle is 0.8-1.2 rad and the length is 12-18 cm. The end and back of the brush head are covered with silicone.
在本发明的进一步实施方式中,刷头和刷柄均由可降解材料制成。In a further embodiment of the invention, both the brush head and the handle are made of a degradable material.
第二方面,本发明提供一种牙刷的制备方法,包括以下步骤:S101:将壳聚糖溶于聚乳酸溶液中,得到第一中间溶液;S102:向第一中间溶液中加入松香溶液并搅拌均匀,得到第二中间溶液,具体在密封容器中搅拌15min~60min;S103:向第二中间溶液中滴加氢氧化钠溶液,得到第三中间溶液;S104:向所第三中间溶液中加入致孔剂,之后暴露于空气中静置1h,得到胶液;S105:将胶液制成丝后定型,得到刷毛。In a second aspect, the present invention provides a method for preparing a toothbrush, comprising the steps of: S101: dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution; and S102: adding a rosin solution to the first intermediate solution and stirring Uniformly, obtaining a second intermediate solution, specifically stirred in a sealed container for 15 min to 60 min; S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution; S104: adding to the third intermediate solution The porogen is then exposed to air for 1 h to obtain a glue solution; S105: the glue is made into a silk and then shaped to obtain bristles.
在本发明的进一步实施方式中,S102中,松香溶液的体积与第一中间溶液的体积之比为1:(10~20);且松香溶液的制备方法包括:将松香研磨后溶解于无水乙醇中并搅拌均匀,得到松香溶液。本领域技术人员应当知晓:由于松香容易氧化,因此松香研磨后在空气中的放置时间不应超过1h,优选立即溶于乙醇中。In a further embodiment of the present invention, in S102, the ratio of the volume of the rosin solution to the volume of the first intermediate solution is 1: (10-20); and the preparation method of the rosin solution comprises: dissolving the rosin after being dissolved in the anhydrous Stir in ethanol and obtain a rosin solution. It will be appreciated by those skilled in the art that since the rosin is susceptible to oxidation, the rosin should not be allowed to stand in air for more than 1 hour after grinding, preferably immediately dissolved in ethanol.
在本发明的进一步实施方式中,S103中,氢氧化钠溶液中溶质氢氧化钠与第二中间溶液中乙酸的摩尔比为1:1;氢氧化钠溶液的质量百分浓度为15%~25%,且每分钟的滴加速度小于60滴;S104中,致孔剂为氯化钠和/或氯化钾;且每100mL第三中间溶液中,致孔剂的加入量为2~3g。In a further embodiment of the present invention, in S103, the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15%-25 %, and the drop rate per minute is less than 60 drops; in S104, the porogen is sodium chloride and/or potassium chloride; and the porogen is added in an amount of 2 to 3 g per 100 mL of the third intermediate solution.
在本发明的进一步实施方式中,S105中,将胶液制成丝后定型具体包括: S201:利用拉丝机将胶液制成细丝,之后将细丝烘干定型,得到第一原丝;S202:采用蒸馏水冲洗第一原丝以去除致孔剂,之后烘干,得到第二原丝;S203:将第二原丝浸泡在第二混合物中,超声搅拌10min~20min后挂在室内,直至不再往下滴水,然后进行于60℃~65℃下低温烘干以除去水分,得到刷毛原料丝;其中,第二混合物与第二原丝的质量比为(800~1200):1;S204:将刷毛原料丝制成牙刷毛簇,即得到刷毛。In a further embodiment of the present invention, in S105, after the glue is made into a wire, the shaping comprises: S201: forming a glue into a filament by a wire drawing machine, and then drying and shaping the filament to obtain a first original yarn; S202: rinsing the first strand with distilled water to remove the porogen, and then drying to obtain a second strand; S203: soaking the second strand in the second mixture, ultrasonically stirring for 10 min to 20 min, and then hanging indoors until The water is not dripped downward, and then dried at a low temperature of 60 ° C to 65 ° C to remove moisture to obtain a bristled raw material yarn; wherein the mass ratio of the second mixture to the second raw yarn is (800 to 1200): 1; S204 : The bristles are made into a tuft of toothbrushes to obtain bristles.
在本发明的进一步实施方式中,S101至S105中,操作温度均为20℃~28℃;S201至S204中,烘干的温度均为60℃~65℃。In a further embodiment of the present invention, in S101 to S105, the operating temperature is 20 ° C to 28 ° C; in S201 to S204, the drying temperature is 60 ° C to 65 ° C.
本发明提供的上述技术方案具有以下优点:The above technical solution provided by the present invention has the following advantages:
(1)申请人经过大量实验发现:本发明提供的牙刷使用方便、环境友好且在使用过程中无需牙膏;本发明的自清洁可降解壳聚糖牙刷在刷牙过程中主动磨损,且磨损过程中产生的微型颗粒物可以起到有效的杀菌和摩擦作用;此外,本发明的刷毛自身具有抗菌抑菌作用,使用过的刷毛长时间暴露在空气中不会繁殖细菌等有害微生物,从而更好地保护口腔卫生,具有广泛的应用价值。(1) Applicants have found through a large number of experiments that the toothbrush provided by the present invention is convenient to use, environmentally friendly, and does not require toothpaste during use; the self-cleaning degradable chitosan toothbrush of the present invention actively wears during brushing, and is worn during wear. The generated micro-particles can play an effective bactericidal and rubbing effect; in addition, the bristles of the present invention have antibacterial and antibacterial effects, and the used bristles are exposed to the air for a long time without reproducing harmful microorganisms such as bacteria, thereby better protecting Oral hygiene has a wide range of applications.
(2)本发明刷毛的原料组分壳聚糖属于天然材料,无毒副作用,对人体更加友好;松香能够有效填补壳聚糖和聚乳酸之间的断链,显著增强刷毛的塑性和弹性,从而使其不易折断;蒲公英能够辅助杀灭牙齿表面和口腔内其他部位的细菌,防止产生牙菌斑,蒲公英还具有抗肿瘤作用,有效防止口腔癌的产生;三七具有补血、止血的作用,能够有效防止或缓解牙龈出血的症状;原料中的月桂酰肌氨酸钠在刷牙时能够产生泡沫,从而代替传统牙膏。(2) The raw material component of the bristles of the invention belongs to natural materials, has no toxic and side effects, and is more friendly to the human body; the rosin can effectively fill the chain break between chitosan and polylactic acid, and significantly enhance the plasticity and elasticity of the bristles. So that it is not easy to break; dandelion can help kill bacteria on the surface of teeth and other parts of the mouth, prevent plaque, dandelion also has anti-tumor effect, effectively prevent the production of oral cancer; Sanqi has the effect of blood, hemostasis, It can effectively prevent or relieve the symptoms of bleeding gums; sodium lauroyl sarcosinate in raw materials can produce foam when brushing teeth, thus replacing traditional toothpaste.
(3)本发明弧形的刷头更符合人的口腔构造,从而更贴合牙面;刷头上覆盖的硅胶起缓冲作用,减轻刷牙刮戳牙龈和腮部时所产生的伤害和疼痛。本发明刷毛的长度为0.5~0.8cm,避免了基于人体牙龈与口腔内壁之间的空间狭小, 刷牙龈时的不适感。(3) The curved brush head of the invention is more in conformity with the human oral structure, so as to be more conformable to the tooth surface; the silica gel covered on the brush head serves as a cushioning function, and reduces the injury and pain caused when the brushing tooth scrapes the gums and the ankle. The length of the bristles of the present invention is 0.5 to 0.8 cm, which avoids the feeling of discomfort when brushing the gums based on the narrow space between the human gums and the inner wall of the oral cavity.
(4)本发明的各原料组分简单易得、成本低廉,制备方法工艺稳定、产率高、质量好、能耗低、原材料广泛、工序简单节省;采用现有的设备即可完成生产,降低了设备要求,且刷头刷柄刷毛均可降解,在丢弃后自然分解,对环境零污染,从而具有广泛的应用价值。(4) The raw material components of the invention are simple and easy to obtain, and the cost is low, and the preparation method has the advantages of stable process, high yield, good quality, low energy consumption, wide raw materials and simple process, and the production can be completed by using existing equipment. The equipment requirements are reduced, and the brush head bristles can be degraded, naturally decomposed after being discarded, and have zero pollution to the environment, thereby having wide application value.
本发明的附加方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。The additional aspects and advantages of the invention will be set forth in part in the description which follows.
附图说明DRAWINGS
图1为本发明自清洁可降解壳聚糖牙刷的主视图;Figure 1 is a front elevational view of the self-cleaning degradable chitosan toothbrush of the present invention;
图2为本发明自清洁可降解壳聚糖牙刷的侧视图。Figure 2 is a side elevational view of the self-cleaning degradable chitosan toothbrush of the present invention.
具体实施方式Detailed ways
下面将对本发明技术方案的实施例进行详细的描述。以下实施例仅用于更加清楚的说明本发明的技术方案,因此只作为实例,而不能以此来限制本发明的保护范围。The embodiments of the technical solution of the present invention will be described in detail below. The following examples are only intended to illustrate the technical solutions of the present invention more clearly, and thus are not intended to limit the scope of the present invention.
下述实施例中的实验方法,如无特殊说明,均为常规方法。The experimental methods in the following examples are conventional methods unless otherwise specified.
下述实施例中所用的试验材料,如无特殊说明,均为自常规试剂商店购买得到的。The test materials used in the following examples, unless otherwise specified, were purchased from conventional reagent stores.
以下实施例中的定量试验,均设置三次重复实验,数据为三次重复实验的平均值或平均值±标准差。For the quantitative tests in the following examples, three replicate experiments were set up, and the data were the mean or mean ± standard deviation of three replicate experiments.
图1为本发明自清洁可降解壳聚糖牙刷的主视图;图2为本发明自清洁可降解壳聚糖牙刷的侧视图,如图1和图2所示:本发明提供一种牙刷,牙刷包 括刷毛;刷毛的原料组分包括第一混合物;第一混合物包括壳聚糖、聚乳酸溶液和松香溶液。此外,牙刷还包括刷柄和刷头;刷头设于刷柄的一端,且刷头是弧度为0.5~1.0rad,长度为2~3cm,宽度为1.5~2cm的板状结构,且刷头靠近弧形圆心的一侧为正面,远离弧形圆心的一侧为背面;刷毛设置在刷头的正面,且刷毛的长度为0.5~0.8cm;刷柄为弧形,且刷柄前半部的弯曲方向与刷头的弯曲方向相同,刷柄后半部的弯曲方向与刷头的弯曲方向相反,刷柄的弧度为0.8~1.2rad,长度为12~18cm。且刷头和刷柄均由可降解材料制成。1 is a front view of a self-cleaning degradable chitosan toothbrush of the present invention; FIG. 2 is a side view of the self-cleaning degradable chitosan toothbrush of the present invention, as shown in FIGS. 1 and 2: the present invention provides a toothbrush. The toothbrush comprises bristles; the raw material component of the bristles comprises a first mixture; the first mixture comprises chitosan, a polylactic acid solution and a rosin solution. In addition, the toothbrush further comprises a handle and a brush head; the brush head is disposed at one end of the handle, and the brush head is a plate-like structure having an arc of 0.5 to 1.0 rad, a length of 2 to 3 cm, and a width of 1.5 to 2 cm, and the brush head The side near the center of the arc is the front side, the side away from the center of the arc is the back side; the bristles are disposed on the front side of the brush head, and the length of the bristles is 0.5-0.8 cm; the handle is curved, and the front half of the handle is The bending direction is the same as the bending direction of the brush head, and the bending direction of the rear half of the handle is opposite to the bending direction of the brush head. The curvature of the handle is 0.8 to 1.2 rad and the length is 12 to 18 cm. And the brush head and the handle are made of a degradable material.
优选地,壳聚糖的质量与聚乳酸溶液中溶质聚乳酸的质量比为(1~2.5):10,聚乳酸溶液的质量百分浓度为4%~10%,且聚乳酸溶液为聚乳酸的醋酸溶液;松香溶液中溶质松香与聚乳酸溶液中溶质聚乳酸的质量比为1:(6~15);且松香溶液为松香乙醇溶液,且松香乙醇溶液的质量百分浓度为9%~11%。Preferably, the mass ratio of the mass of the chitosan to the solute polylactic acid in the polylactic acid solution is (1 to 2.5): 10, the mass concentration of the polylactic acid solution is 4% to 10%, and the polylactic acid solution is polylactic acid. The acetic acid solution; the mass ratio of the solute rosin in the rosin solution to the solute polylactic acid in the polylactic acid solution is 1: (6-15); and the rosin solution is a rosin ethanol solution, and the mass percentage concentration of the rosin ethanol solution is 9%~ 11%.
优选地,刷毛的原料组分还包括第二混合物;第二混合物包括蒲公英、三七和月桂酰肌氨酸钠;其中,蒲公英、三七和月桂酰肌氨酸钠的质量比依次为(1~1.5):(0.3~0.5):1;其中,第二混合物的制备方法包括以下步骤:S301:将蒲公英和三七用水浸泡36h~48h,之后过滤并收集滤液;其中,每千克蒲公英中,水的加入质量为18L~22L;S302:将月桂酰肌氨酸钠加入S301得到的滤液中,搅拌均匀,得到第二混合物。Preferably, the raw material component of the bristles further comprises a second mixture; the second mixture comprises dandelion, notoginsenoyl and sodium lauroyl sarcosinate; wherein the mass ratio of dandelion, notoginsenoyl and sodium lauroyl sarcosinate is (1) ~1.5): (0.3~0.5): 1; wherein the preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 36h to 48h, then filtering and collecting the filtrate; wherein, per kilogram of dandelion, The water is added in a mass of 18 L to 22 L; S302: sodium lauroyl sarcosinate is added to the filtrate obtained in S301, and stirred uniformly to obtain a second mixture.
另外,针对本发明的牙刷,本发明专门设计了制备方法,包括以下步骤:In addition, with respect to the toothbrush of the present invention, the present invention specifically designs a preparation method comprising the following steps:
S101:将壳聚糖溶于聚乳酸溶液中,得到第一中间溶液。S101: Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
S102:向第一中间溶液中加入松香溶液并搅拌均匀,得到第二中间溶液。其中,松香溶液的制备方法包括:将松香研磨后溶解于无水乙醇中并搅拌均匀,得到松香溶液。S102: adding a rosin solution to the first intermediate solution and stirring uniformly to obtain a second intermediate solution. Wherein, the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
S103:向第二中间溶液中滴加氢氧化钠溶液,得到第三中间溶液。其中, 氢氧化钠溶液中溶质氢氧化钠与第二中间溶液中乙酸的摩尔比为1:1;氢氧化钠溶液的质量百分浓度为15%~25%,且每分钟的滴加速度小于60滴。S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution. Wherein, the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15% to 25%, and the droplet acceleration per minute is less than 60 drop.
S104:向第三中间溶液中加入致孔剂,之后静置,得到胶液。其中,致孔剂为氯化钠和/或氯化钾;且每100mL第三中间溶液中,致孔剂的加入量为2~3g。S104: adding a porogen to the third intermediate solution, and then standing to obtain a glue. Wherein, the porogen is sodium chloride and/or potassium chloride; and the porogen is added in an amount of 2 to 3 g per 100 mL of the third intermediate solution.
S105:将胶液制成丝后定型,得到刷毛。其中,将胶液制成丝后定型具体包括:S201:利用拉丝机将胶液制成丝,之后将丝烘干定型,得到第一原丝;S202:采用蒸馏水冲洗第一原丝以去除致孔剂,之后烘干,得到第二原丝;S203:将第二原丝浸泡在第二混合物中,超声搅拌,之后烘干,得到刷毛原料丝;其中,第二混合物与第二原丝的质量比为(800~1200):1;S204:将所述刷毛原料丝制成牙刷毛簇,即得到所述刷毛。S105: After the glue is made into a wire, the bristles are obtained. Wherein, the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result a porogen, followed by drying to obtain a second strand; S203: immersing the second strand in the second mixture, ultrasonically stirring, and then drying to obtain a bristled raw material yarn; wherein, the second mixture and the second raw yarn The mass ratio is (800 to 1200): 1; S204: the bristle raw material yarn is made into a toothbrush tuft, that is, the bristles are obtained.
优选地,所述S101至所述S105中,操作温度均为20℃~28℃;所述S201至所述S204中,所述烘干的温度均为60℃~65℃。Preferably, in the S101 to the S105, the operating temperature is 20 ° C to 28 ° C; in the S201 to S204, the drying temperature is 60 ° C to 65 ° C.
本发明自清洁可降解壳聚糖牙刷运行原理和过程是:在刷牙过程中,将牙刷蘸水后放入口腔,在牙齿表面往复摩擦,由壳聚糖-聚乳酸共聚物制成的刷毛由于耐磨性很差,从而不断地被磨损并产生微小颗粒,微小颗粒辅助刷毛摩擦食物残渣和菌斑,起到清洁牙齿和口腔的作用,代替了牙膏中的摩擦剂。壳聚糖聚乳酸共聚物内部有许多微孔,蒲公英提取物、三七提取物和月桂酰肌氨酸钠存储在这些微孔中,刷牙时由于水的溶解作用和水流的冲击,会缓慢释放出来,起到杀菌、止血和发泡剂的作用。The operation principle and process of the self-cleaning degradable chitosan toothbrush of the invention are: in the process of brushing, the toothbrush is placed in the mouth after being drowned, and rubbed and rubbed on the surface of the tooth, and the bristles made of chitosan-polylactic acid copolymer are The wear resistance is very poor, so that it is constantly worn and produces tiny particles. The fine particles assist the bristles to rub the food residue and plaque, and clean the teeth and the mouth, replacing the friction agent in the toothpaste. The chitosan polylactic acid copolymer has many micropores inside, and the dandelion extract, the notoginseng extract and the sodium lauroyl sarcosinate are stored in these micropores, and the teeth are slowly released due to the dissolution of water and the impact of water flow during brushing. Come out, play the role of sterilization, hemostasis and foaming agent.
下面结合具体实施方式进行说明:The following describes the specific embodiments:
实施例一Embodiment 1
本发明提供一种自清洁可降解壳聚糖牙刷,包括:壳聚糖、聚乳酸溶液和松香溶液。其中,壳聚糖的质量与聚乳酸溶液中溶质聚乳酸的质量比为2.5:10, 聚乳酸溶液为质量百分浓度为10%的聚乳酸的醋酸溶液;松香溶液中溶质松香与聚乳酸溶液中溶质聚乳酸的质量比为1:6,松香溶液为质量百分浓度为9%的松香乙醇溶液。The invention provides a self-cleaning degradable chitosan toothbrush, comprising: chitosan, polylactic acid solution and rosin solution. Wherein, the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 2.5:10, the polylactic acid solution is an acetic acid solution of polylactic acid having a mass percentage of 10%; the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid is 1:6, and the rosin solution is a rosin ethanol solution having a mass percent concentration of 9%.
按上述原料组分,采用本发明提供的制备方法,制备自清洁可降解壳聚糖牙刷:According to the above raw material component, the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
S101:将壳聚糖溶于聚乳酸溶液中,得到第一中间溶液。S101: Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
S102:向第一中间溶液中加入松香溶液并搅拌15min,得到第二中间溶液。其中,松香溶液的制备方法包括:将松香研磨后溶解于无水乙醇中并搅拌均匀,得到松香溶液。S102: adding a rosin solution to the first intermediate solution and stirring for 15 minutes to obtain a second intermediate solution. Wherein, the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
S103:向第二中间溶液中滴加氢氧化钠溶液,得到第三中间溶液。其中,氢氧化钠溶液中溶质氢氧化钠与第二中间溶液中乙酸的摩尔比为1:1;氢氧化钠溶液的质量百分浓度为20%,且每分钟的滴加速度为50滴。S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution. Wherein, the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 20%, and the droplet acceleration per minute is 50 drops.
S104:向所第三中间溶液中加入致孔剂氯化钠,之后静置,得到胶液。其中,每100mL第三中间溶液中,致孔剂的加入量为2g。S104: adding a porogen sodium chloride to the third intermediate solution, followed by standing to obtain a glue solution. Among them, the porogen was added in an amount of 2 g per 100 mL of the third intermediate solution.
S105:将胶液制成丝后定型,得到刷毛。其中,将胶液制成丝后定型具体包括:S201:利用拉丝机将胶液制成丝,之后将丝烘干定型,得到第一原丝;S202:采用蒸馏水冲洗第一原丝以去除致孔剂,之后烘干,得到第二原丝;S203:将第二原丝浸泡于水中,超声搅拌10min,之后烘干,得到刷毛原料丝。S105: After the glue is made into a wire, the bristles are obtained. Wherein, the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result The pore agent is then dried to obtain a second raw yarn; S203: the second raw yarn is immersed in water, ultrasonically stirred for 10 minutes, and then dried to obtain a bristled raw material yarn.
其中,S101至S105中,操作温度均为25℃;S201至S204中,烘干的温度均为60℃。Among them, in S101 to S105, the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 60 ° C.
实施例二Embodiment 2
本发明提供一种自清洁可降解壳聚糖牙刷,包括:壳聚糖、聚乳酸溶液和 松香溶液。其中,壳聚糖的质量与聚乳酸溶液中溶质聚乳酸的质量比为1:10,聚乳酸溶液为质量百分浓度为4%的聚乳酸的醋酸溶液;松香溶液中溶质松香与聚乳酸溶液中溶质聚乳酸的质量比为1:15,松香溶液为质量百分浓度为11%的松香乙醇溶液。The present invention provides a self-cleaning degradable chitosan toothbrush comprising: a chitosan, a polylactic acid solution, and a rosin solution. Wherein, the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 1:10, the polylactic acid solution is an acetic acid solution of polylactic acid having a mass concentration of 4%; the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid was 1:15, and the rosin solution was a rosin ethanol solution having a mass percent concentration of 11%.
按上述原料组分,采用本发明提供的制备方法,制备自清洁可降解壳聚糖牙刷:According to the above raw material component, the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
S101:将壳聚糖溶于聚乳酸溶液中,得到第一中间溶液。S101: Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
S102:向第一中间溶液中加入松香溶液并搅拌60min,得到第二中间溶液。其中,松香溶液的制备方法包括:将松香研磨后溶解于无水乙醇中并搅拌均匀,得到松香溶液。S102: adding a rosin solution to the first intermediate solution and stirring for 60 minutes to obtain a second intermediate solution. Wherein, the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
S103:向第二中间溶液中滴加氢氧化钠溶液,得到第三中间溶液。其中,氢氧化钠溶液中溶质氢氧化钠与第二中间溶液中乙酸的摩尔比为1:1;氢氧化钠溶液的质量百分浓度为15%,且每分钟的滴加速度为50滴。S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution. Wherein, the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15%, and the droplet acceleration per minute is 50 drops.
S104:向所第三中间溶液中加入致孔剂氯化钾,之后静置,得到胶液。其中,每100mL第三中间溶液中,致孔剂的加入量为3g。S104: adding a porogen potassium chloride to the third intermediate solution, and then standing to obtain a glue. Among them, the porogen was added in an amount of 3 g per 100 mL of the third intermediate solution.
S105:将胶液制成丝后定型,得到刷毛。其中,将胶液制成丝后定型具体包括:S201:利用拉丝机将胶液制成丝,之后将丝烘干定型,得到第一原丝;S202:采用蒸馏水冲洗第一原丝以去除致孔剂,之后烘干,得到第二原丝;S203:将第二原丝浸泡于水中,超声搅拌20min,之后烘干,得到刷毛原料丝。S105: After the glue is made into a wire, the bristles are obtained. Wherein, the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result The pore agent is then dried to obtain a second raw yarn; S203: the second raw yarn is immersed in water, ultrasonically stirred for 20 minutes, and then dried to obtain a bristled raw material yarn.
其中,S101至S105中,操作温度均为25℃;S201至S204中,烘干的温度均为65℃。Among them, in S101 to S105, the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 65 ° C.
实施例三Embodiment 3
本实施例在实施例一的基础上设置而成This embodiment is set on the basis of the first embodiment.
本发明提供一种自清洁可降解壳聚糖牙刷,包括:壳聚糖、聚乳酸溶液、松香溶液、蒲公英、三七和月桂酰肌氨酸钠;其中,蒲公英、三七和月桂酰肌氨酸钠的质量比依次为1:0.3:1。其中,壳聚糖的质量与聚乳酸溶液中溶质聚乳酸的质量比为2.5:10,聚乳酸溶液为质量百分浓度为10%的聚乳酸的醋酸溶液;松香溶液中溶质松香与聚乳酸溶液中溶质聚乳酸的质量比为1:6,松香溶液为质量百分浓度为9%的松香乙醇溶液。第二混合物的制备方法包括以下步骤:S301:将蒲公英和三七用水浸泡36h,之后过滤并收集滤液;其中,每千克蒲公英中,水的加入质量为20L;S302:将月桂酰肌氨酸钠加入滤液中,搅拌均匀,得到第二混合物。The invention provides a self-cleaning degradable chitosan toothbrush, comprising: chitosan, polylactic acid solution, rosin solution, dandelion, notoginsenoic acid and sodium lauroyl sarcosinate; wherein dandelion, notoginseng and lauroyl myosine The mass ratio of sodium is 1:0.3:1 in order. Wherein, the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 2.5:10, the polylactic acid solution is an acetic acid solution of polylactic acid having a mass concentration of 10%; the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid is 1:6, and the rosin solution is a rosin ethanol solution having a mass percent concentration of 9%. The preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 36h, then filtering and collecting the filtrate; wherein, in kilograms of dandelion, the added mass of water is 20L; S302: sodium lauroyl sarcosinate The filtrate was added to the filtrate and stirred well to obtain a second mixture.
按上述原料组分,采用本发明提供的制备方法,制备自清洁可降解壳聚糖牙刷:According to the above raw material component, the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
S101:将壳聚糖溶于聚乳酸溶液中,得到第一中间溶液。S101: Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
S102:向第一中间溶液中加入松香溶液并搅拌15min,得到第二中间溶液。其中,松香溶液的制备方法包括:将松香研磨后溶解于无水乙醇中并搅拌均匀,得到松香溶液。S102: adding a rosin solution to the first intermediate solution and stirring for 15 minutes to obtain a second intermediate solution. Wherein, the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
S103:向第二中间溶液中滴加氢氧化钠溶液,得到第三中间溶液。其中,氢氧化钠溶液中溶质氢氧化钠与第二中间溶液中乙酸的摩尔比为1:1;氢氧化钠溶液的质量百分浓度为20%,且每分钟的滴加速度为50滴。S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution. Wherein, the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 20%, and the droplet acceleration per minute is 50 drops.
S104:向所第三中间溶液中加入致孔剂氯化钠,之后静置,得到胶液。其中,每100mL第三中间溶液中,致孔剂的加入量为2g。S104: adding a porogen sodium chloride to the third intermediate solution, followed by standing to obtain a glue solution. Among them, the porogen was added in an amount of 2 g per 100 mL of the third intermediate solution.
S105:将胶液制成丝后定型,得到刷毛。其中,将胶液制成丝后定型具体包括:S201:利用拉丝机将胶液制成丝,之后将丝烘干定型,得到第一原丝; S202:采用蒸馏水冲洗第一原丝以去除致孔剂,之后烘干,得到第二原丝;S203:将第二原丝浸泡于第二混合物中,超声搅拌10min,之后烘干,得到刷毛原料丝;其中,第二混合物与第二原丝的质量比为1000:1。S105: After the glue is made into a wire, the bristles are obtained. Wherein, the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, and then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result a porogen, followed by drying to obtain a second raw yarn; S203: immersing the second raw yarn in the second mixture, ultrasonically stirring for 10 minutes, and then drying to obtain a bristled raw material yarn; wherein, the second mixture and the second raw yarn The mass ratio is 1000:1.
其中,S101至S105中,操作温度均为25℃;S201至S204中,烘干的温度均为60℃。Among them, in S101 to S105, the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 60 ° C.
实施例四Embodiment 4
本实施例在实施例二的基础上设置而成This embodiment is set on the basis of the second embodiment.
本发明提供一种自清洁可降解壳聚糖牙刷,包括:壳聚糖、聚乳酸溶液、松香溶液、蒲公英、三七和月桂酰肌氨酸钠;其中,蒲公英、三七和月桂酰肌氨酸钠的质量比依次为1.5:0.5:1。其中,壳聚糖的质量与聚乳酸溶液中溶质聚乳酸的质量比为1:10,聚乳酸溶液为质量百分浓度为4%的聚乳酸的醋酸溶液;松香溶液中溶质松香与聚乳酸溶液中溶质聚乳酸的质量比为1:15,松香溶液为质量百分浓度为11%的松香乙醇溶液。第二混合物的制备方法包括以下步骤:S301:将蒲公英和三七用水浸泡48h,之后过滤并收集滤液;其中,每千克蒲公英中,水的加入质量为20L;S302:将月桂酰肌氨酸钠加入滤液中,搅拌均匀,得到第二混合物。The invention provides a self-cleaning degradable chitosan toothbrush, comprising: chitosan, polylactic acid solution, rosin solution, dandelion, notoginsenoic acid and sodium lauroyl sarcosinate; wherein dandelion, notoginseng and lauroyl myosine The mass ratio of sodium is 1.5:0.5:1 in order. Wherein, the mass ratio of chitosan to the solute polylactic acid in the polylactic acid solution is 1:10, the polylactic acid solution is an acetic acid solution of polylactic acid having a mass concentration of 4%; the solute rosin and the polylactic acid solution in the rosin solution The mass ratio of the medium solute polylactic acid was 1:15, and the rosin solution was a rosin ethanol solution having a mass percent concentration of 11%. The preparation method of the second mixture comprises the following steps: S301: soaking dandelion and notoginseng with water for 48 hours, then filtering and collecting the filtrate; wherein, for each kilogram of dandelion, the added mass of water is 20L; S302: sodium lauroyl sarcosinate The filtrate was added to the filtrate and stirred well to obtain a second mixture.
按上述原料组分,采用本发明提供的制备方法,制备自清洁可降解壳聚糖牙刷:According to the above raw material component, the self-cleaning degradable chitosan toothbrush is prepared by the preparation method provided by the invention:
S101:将壳聚糖溶于聚乳酸溶液中,得到第一中间溶液。S101: Dissolving chitosan in a polylactic acid solution to obtain a first intermediate solution.
S102:向第一中间溶液中加入松香溶液并搅拌60min,得到第二中间溶液。其中,松香溶液的制备方法包括:将松香研磨后溶解于无水乙醇中并搅拌均匀,得到松香溶液。S102: adding a rosin solution to the first intermediate solution and stirring for 60 minutes to obtain a second intermediate solution. Wherein, the preparation method of the rosin solution comprises: pulverizing the rosin, dissolving in absolute ethanol and stirring uniformly to obtain a rosin solution.
S103:向第二中间溶液中滴加氢氧化钠溶液,得到第三中间溶液。其中,氢氧化钠溶液中溶质氢氧化钠与第二中间溶液中乙酸的摩尔比为1:1;氢氧化钠溶液的质量百分浓度为15%,且每分钟的滴加速度为50滴。S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution. Wherein, the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15%, and the droplet acceleration per minute is 50 drops.
S104:向所第三中间溶液中加入致孔剂氯化钾和氯化钾,之后静置,得到胶液。其中,每100mL第三中间溶液中,致孔剂氯化钾和氯化钾的加入量均为1.5g。S104: adding a porogen potassium chloride and potassium chloride to the third intermediate solution, followed by standing to obtain a glue. Among them, the porogen potassium chloride and potassium chloride were added in an amount of 1.5 g per 100 mL of the third intermediate solution.
S105:将胶液制成丝后定型,得到刷毛。其中,将胶液制成丝后定型具体包括:S201:利用拉丝机将胶液制成丝,之后将丝烘干定型,得到第一原丝;S202:采用蒸馏水冲洗第一原丝以去除致孔剂,之后烘干,得到第二原丝;S203:将第二原丝浸泡于水中,超声搅拌20min,之后烘干,得到刷毛原料丝;其中,第二混合物与第二原丝的质量比为1000:1。S105: After the glue is made into a wire, the bristles are obtained. Wherein, the shaping of the glue into the wire comprises: S201: forming the glue into a wire by a wire drawing machine, then drying and shaping the wire to obtain a first original yarn; S202: rinsing the first original wire with distilled water to remove the result a pore agent, followed by drying to obtain a second strand; S203: soaking the second strand in water, ultrasonically stirring for 20 min, and then drying to obtain a bristle strand; wherein, the mass ratio of the second mixture to the second strand It is 1000:1.
其中,S101至S105中,操作温度均为25℃;S201至S204中,烘干的温度均为65℃。Among them, in S101 to S105, the operating temperature is 25 ° C; in S201 to S204, the drying temperature is 65 ° C.
另外,将本发明各实施例得到的自清洁可降解壳聚糖牙刷,通过功能学试验来系统评价其功效:In addition, the self-cleaning degradable chitosan toothbrush obtained in each of the examples of the present invention was systematically evaluated for its efficacy by functional tests:
一、抑菌试验First, the bacteriostatic test
测试菌种:金黄色葡萄球菌、乳酸杆菌、伤寒杆菌、绿脓杆菌、乙型链球菌和幽门螺旋杆菌。菌液制备:挑取斜面菌种接种于20%牛浸汁培养基中,37℃培养过夜,再用20%牛浸汁培养基将菌液稀释至10cfu/ml,立即接种。Test strains: Staphylococcus aureus, Lactobacillus, Salmonella typhi, Pseudomonas aeruginosa, Streptococcus mutans, and Helicobacter pylori. Preparation of bacterial solution: The slanted strain was inoculated into 20% bovine juice culture medium, cultured overnight at 37 ° C, and the bacterial liquid was diluted to 10 cfu/ml with 20% bovine juice culture medium, and immediately inoculated.
MIC测定:采用液体试管连续稀释法,用20%牛浸汁培养基样品(分别将各实施例刷毛研磨得到)作连续对倍稀释。将1.0ml加入灭菌试管中,每管加入0.05ml标准新鲜菌液,并设菌株对照及溶媒对照组,37℃培养18~24小时,观 察细菌生长情况,以无菌生长的最高稀释度为MIC,从而在体外抑菌试验中,以最低抑菌浓度(MIC,mg/mL)指标评价本发明制备的自清洁可降解壳聚糖牙刷对常见菌株的抗菌作用。MIC measurement: serial dilution of the liquid tube was used, and a 20% bovine juice medium sample (each obtained by brushing each of the examples) was subjected to serial dilution. Add 1.0ml to the sterilized test tube, add 0.05ml standard fresh bacterial solution to each tube, set up the strain control and the vehicle control group, and incubate at 37 °C for 18-24 hours to observe the growth of the bacteria. The highest dilution for sterile growth is MIC, thereby evaluating the antibacterial effect of the self-cleaning degradable chitosan toothbrush prepared by the present invention on common strains in an in vitro bacteriostatic test with a minimum inhibitory concentration (MIC, mg/mL).
表1 各实施例自清洁可降解壳聚糖牙刷对常见菌株的抗菌作用Table 1 Antibacterial effects of self-cleaning degradable chitosan toothbrush on common strains in each example
Figure PCTCN2018077975-appb-000001
Figure PCTCN2018077975-appb-000001
二、临床试验Second, clinical trials
征集年龄18~60岁的志愿者500名(男女比例为1:1)。各志愿者均伴随有不同程度的口腔问题,如牙龈出血、口气不清新、龋齿导致的牙疼以及上火引起的口腔溃疡等症状。具体地,将患者均分为5组,每组100人,将第一组至第四组分别试用实施例一至实施例四中的自清洁可降解壳聚糖牙刷,每日早晚各1次,每次5min;将第五组采用市售高露洁牙膏正常刷牙。连续试用本发明提供的自清洁可降解壳聚糖牙刷制备得到的牙刷20天,记录各志愿者的症状,具体数据如表2所示。500 volunteers aged between 18 and 60 years old (1:1 male to female) were recruited. Each volunteer was accompanied by different levels of oral problems, such as bleeding gums, unclear breath, toothache caused by dental caries, and oral ulcers caused by fire. Specifically, the patients are divided into 5 groups of 100 persons, and the self-cleaning degradable chitosan toothbrushes of the first to fourth embodiments are respectively tested in the first group to the fourth group, one time each morning and evening. 5 min each time; the fifth group was brushed with normal Colgate toothpaste. The toothbrush prepared by the self-cleaning degradable chitosan toothbrush provided by the present invention was continuously tested for 20 days, and the symptoms of each volunteer were recorded. The specific data are shown in Table 2.
疗效判断为:The efficacy is judged as:
显效:牙龈出血、口气不清新、龋齿导致的牙疼以及上火引起的口腔溃疡 等症状显著改善;好转:牙龈出血、口气不清新、龋齿导致的牙疼以及上火引起的口腔溃疡等症状有所好转;无效:症状无改善。Significant effect: bleeding gums, unsatisfactory breath, toothache caused by dental caries, and oral ulcers caused by burning, significantly improved; improved: bleeding gums, bad breath, toothache caused by dental caries, and oral ulcers caused by fire Improved; invalid: no improvement in symptoms.
表2 各实施例刷毛制备得到的牙刷对口腔问题志愿者的临床疗效Table 2 Clinical effects of toothbrushes prepared from bristles in various examples on oral problems volunteers
Figure PCTCN2018077975-appb-000002
Figure PCTCN2018077975-appb-000002
当然,除了实施例一至实施例四列举的情况,其他原料组分的种类和重量百分比、制备过程中的条件和参数等也是可以的。Of course, in addition to the cases enumerated in the first to fourth embodiments, the kinds and weight percentages of other raw material components, conditions and parameters in the preparation process, and the like are also possible.
本发明提供的牙刷使用方便、环境友好且在使用过程中无需牙膏;本发明的自清洁可降解壳聚糖牙刷在刷牙过程中主动磨损,且磨损过程中产生的微型颗粒物可以起到有效的杀菌和摩擦作用;此外,本发明的刷毛自身具有抗菌抑菌作用,使用过的刷毛长时间暴露在空气中不会繁殖细菌等有害微生物,从而更好地保护口腔卫生,具有广泛的应用价值。The toothbrush provided by the invention is convenient to use, environmentally friendly and does not need toothpaste during use; the self-cleaning degradable chitosan toothbrush of the invention actively wears during the brushing process, and the micro-particles generated during the abrasion process can effectively sterilize In addition, the bristles of the present invention have antibacterial and antibacterial effects, and the used bristles are exposed to the air for a long time without propagating harmful microorganisms such as bacteria, thereby better protecting oral hygiene and having wide application value.
在本发明的描述中,需要理解的是,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的 数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。在本发明的描述中,“多个”的含义是两个以上,除非另有明确具体的限定。In the description of the present invention, it is to be understood that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, features defining "first" and "second" may include one or more of the features either explicitly or implicitly. In the description of the present invention, the meaning of "a plurality" is two or more unless specifically and specifically defined.
在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。In the description of the present specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" and the like means a specific feature described in connection with the embodiment or example. A structure, material or feature is included in at least one embodiment or example of the invention. In the present specification, the schematic representation of the above terms is not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in a suitable manner in any one or more embodiments or examples. In addition, various embodiments or examples described in the specification and features of various embodiments or examples may be combined and combined without departing from the scope of the invention.
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。Although the embodiments of the present invention have been shown and described, it is understood that the above-described embodiments are illustrative and are not to be construed as limiting the scope of the invention. The embodiments are subject to variations, modifications, substitutions and variations.

Claims (10)

  1. 一种牙刷,其特征在于:所述牙刷包括刷毛;A toothbrush, characterized in that the toothbrush comprises bristles;
    所述刷毛的原料组分包括第一混合物;所述第一混合物包括壳聚糖、聚乳酸溶液和松香溶液。The raw material component of the bristles includes a first mixture; the first mixture includes a chitosan, a polylactic acid solution, and a rosin solution.
  2. 根据权利要求1所述的牙刷,其特征在于:A toothbrush according to claim 1 wherein:
    所述壳聚糖的质量与所述聚乳酸溶液中溶质聚乳酸的质量比为(1~2.5):10,所述聚乳酸溶液的质量百分浓度为4%~10%,且所述聚乳酸溶液为聚乳酸的醋酸溶液;The mass ratio of the mass of the chitosan to the solute polylactic acid in the polylactic acid solution is (1 to 2.5): 10, the mass concentration of the polylactic acid solution is 4% to 10%, and the poly The lactic acid solution is an acetic acid solution of polylactic acid;
    所述松香溶液中溶质松香与所述聚乳酸溶液中溶质聚乳酸的质量比为1:(6~15);且所述松香溶液为松香乙醇溶液,且所述松香乙醇溶液的质量百分浓度为9%~11%。The mass ratio of the solute rosin in the rosin solution to the solute polylactic acid in the polylactic acid solution is 1: (6-15); and the rosin solution is a rosin ethanol solution, and the mass percentage of the rosin ethanol solution It is 9% to 11%.
  3. 根据权利要求2所述的牙刷,其特征在于,所述刷毛的原料组分还包括第二混合物;The toothbrush according to claim 2, wherein the raw material component of the bristles further comprises a second mixture;
    所述第二混合物包括蒲公英、三七和月桂酰肌氨酸钠;其中,所述蒲公英、所述三七和所述月桂酰肌氨酸钠的质量比依次为(1~1.5):(0.3~0.5):1;The second mixture comprises dandelion, notoginsenoyl and sodium lauroyl sarcosinate; wherein the mass ratio of the dandelion, the notoginseng and the sodium lauroyl sarcosinate is (1 to 1.5) in order: (0.3 ~0.5):1;
    其中,所述第二混合物的制备方法包括以下步骤:Wherein the preparation method of the second mixture comprises the following steps:
    S301:将蒲公英和三七用水浸泡36h~48h,之后过滤并收集滤液;其中,每千克所述蒲公英中,水的加入质量为18L~22L;S301: immersing dandelion and notoginseng with water for 36h to 48h, then filtering and collecting the filtrate; wherein, for each kilogram of the dandelion, the water is added in a mass of 18L to 22L;
    S302:将月桂酰肌氨酸钠加入所述S301得到的滤液中,搅拌均匀,得到所述第二混合物。S302: adding sodium lauroyl sarcosinate to the filtrate obtained in the above S301, and stirring uniformly to obtain the second mixture.
  4. 根据权利要求1~3任一项所述的牙刷,其特征在于,所述牙刷还包括刷柄和刷头;The toothbrush according to any one of claims 1 to 3, wherein the toothbrush further comprises a handle and a brush head;
    其中,所述刷头设于刷柄的一端,且所述刷头是弧度为0.5~1.0rad,长度为2~3cm,宽度为1.5~2cm的板状结构,且所述刷头靠近弧形圆心的一侧为正面, 远离弧形圆心的一侧为背面;Wherein, the brush head is disposed at one end of the handle, and the brush head is a plate-like structure having an arc of 0.5 to 1.0 rad, a length of 2 to 3 cm, and a width of 1.5 to 2 cm, and the brush head is close to the curved shape. One side of the center of the circle is the front side, and the side away from the center of the arc is the back side;
    所述刷毛设置在所述刷头的正面,且刷毛的长度为0.5~0.8cm;The bristles are disposed on the front side of the brush head, and the length of the bristles is 0.5 to 0.8 cm;
    所述刷柄为弧形,且所述刷柄前半部的弯曲方向与刷头的弯曲方向相同,刷柄后半部的弯曲方向与刷头的弯曲方向相反,刷柄的弧度为0.8~1.2rad,长度为12~18cm。The handle is curved, and the bending direction of the front half of the handle is the same as the bending direction of the brush head, and the bending direction of the rear half of the handle is opposite to the bending direction of the brush head, and the curvature of the handle is 0.8-1.2. Rad, length is 12 ~ 18cm.
  5. 根据权利要求4所述的牙刷,其特征在于:A toothbrush according to claim 4, wherein:
    所述刷头和刷柄均由可降解材料制成。Both the brush head and the handle are made of a degradable material.
  6. 权利要求1~5任一项所述的牙刷的制备方法,其特征在于,包括以下步骤:The method of preparing a toothbrush according to any one of claims 1 to 5, comprising the steps of:
    S101:将壳聚糖溶于所述聚乳酸溶液中,得到第一中间溶液;S101: dissolving chitosan in the polylactic acid solution to obtain a first intermediate solution;
    S102:向所述第一中间溶液中加入松香溶液并搅拌均匀,得到第二中间溶液;S102: adding a rosin solution to the first intermediate solution and stirring uniformly to obtain a second intermediate solution;
    S103:向所述第二中间溶液中滴加氢氧化钠溶液,得到第三中间溶液;S103: adding a sodium hydroxide solution to the second intermediate solution to obtain a third intermediate solution;
    S104:向所述第三中间溶液中加入致孔剂,之后静置,得到胶液;S104: adding a porogen to the third intermediate solution, and then standing to obtain a glue;
    S105:将所述胶液制成丝后定型,得到所述刷毛。S105: Forming the glue into a wire and setting the bristles.
  7. 根据权利要求6所述的牙刷的制备方法,其特征在于:A method of preparing a toothbrush according to claim 6, wherein:
    所述S102中,所述松香溶液的制备方法包括:In the S102, the preparation method of the rosin solution comprises:
    将松香研磨后溶解于无水乙醇中并搅拌均匀,得到松香溶液。The rosin was ground, dissolved in absolute ethanol, and stirred to obtain a rosin solution.
  8. 根据权利要求6所述的牙刷的制备方法,其特征在于:A method of preparing a toothbrush according to claim 6, wherein:
    所述S103中,所述氢氧化钠溶液中溶质氢氧化钠与所述第二中间溶液中乙酸的摩尔比为1:1;所述氢氧化钠溶液的质量百分浓度为15%~25%,且每分钟的滴加速度小于60滴;In the S103, the molar ratio of the solute sodium hydroxide in the sodium hydroxide solution to the acetic acid in the second intermediate solution is 1:1; the mass percentage concentration of the sodium hydroxide solution is 15% to 25% And the drop rate per minute is less than 60 drops;
    所述S104中,所述致孔剂为氯化钠和/或氯化钾;且每100mL所述第三中 间溶液中,致孔剂的加入量为2~3g。In the above S104, the porogen is sodium chloride and/or potassium chloride; and the porogen is added in an amount of 2 to 3 g per 100 mL of the third intermediate solution.
  9. 根据权利要求6所述的牙刷的制备方法,其特征在于:A method of preparing a toothbrush according to claim 6, wherein:
    所述S105中,所述将所述胶液制成丝后定型具体包括:In the S105, the shaping of the glue liquid into a wire comprises:
    S201:利用拉丝机将所述胶液制成丝,之后将所述丝烘干定型,得到第一原丝;S201: forming the glue into a wire by a wire drawing machine, and then drying and shaping the wire to obtain a first original yarn;
    S202:采用蒸馏水冲洗所述第一原丝以去除所述致孔剂,之后烘干,得到第二原丝;S202: rinsing the first strand with distilled water to remove the porogen, and then drying to obtain a second strand;
    S203:将所述第二原丝浸泡在第二混合物中,超声搅拌,之后烘干,得到刷毛原料丝;其中,所述第二混合物与所述第二原丝的质量比为(800~1200):1;S203: soaking the second raw silk in the second mixture, ultrasonically stirring, and then drying to obtain a bristle raw material yarn; wherein the mass ratio of the second mixture to the second raw yarn is (800-1200) ):1;
    S204:将所述刷毛原料丝制成牙刷毛簇,即得到所述刷毛。S204: The bristles are made into a brush tuft to obtain the bristles.
  10. 根据权利要求9所述的牙刷的制备方法,其特征在于:A method of preparing a toothbrush according to claim 9, wherein:
    所述S101至所述S105中,操作温度均为20℃~28℃;所述S201至所述S204中,所述烘干的温度均为60℃~65℃。In the above S101 to S105, the operating temperature is 20 ° C to 28 ° C; in the S201 to S204, the drying temperature is 60 ° C to 65 ° C.
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