WO2020045615A1 - Antibacterial product - Google Patents

Antibacterial product Download PDF

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Publication number
WO2020045615A1
WO2020045615A1 PCT/JP2019/034073 JP2019034073W WO2020045615A1 WO 2020045615 A1 WO2020045615 A1 WO 2020045615A1 JP 2019034073 W JP2019034073 W JP 2019034073W WO 2020045615 A1 WO2020045615 A1 WO 2020045615A1
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Prior art keywords
nanodiamond
antibacterial
substrate
charged
product according
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PCT/JP2019/034073
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French (fr)
Japanese (ja)
Inventor
修一 佐々木
和也 柳沢
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株式会社ヤギ
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Priority claimed from PCT/JP2019/027526 external-priority patent/WO2020013282A1/en
Application filed by 株式会社ヤギ filed Critical 株式会社ヤギ
Priority to JP2020505505A priority Critical patent/JPWO2020045615A1/en
Publication of WO2020045615A1 publication Critical patent/WO2020045615A1/en

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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A01N25/10—Macromolecular compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A—HUMAN NECESSITIES
    • A46—BRUSHWARE
    • A46B—BRUSHES
    • A46B9/00—Arrangements of the bristles in the brush body
    • A46B9/02—Position or arrangement of bristles in relation to surface of the brush body, e.g. inclined, in rows, in groups
    • A46B9/04—Arranged like in or for toothbrushes
    • A—HUMAN NECESSITIES
    • A46—BRUSHWARE
    • A46D—MANUFACTURE OF BRUSHES
    • A46D1/00—Bristles; Selection of materials for bristles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/25—Diamond
    • C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery

Definitions

  • the present invention relates to antibacterial products.
  • an object of the present invention is to provide a new antibacterial product.
  • the antimicrobial product of the present invention is characterized in that it contains charged nanodiamond.
  • the antibacterial product of the present invention can suppress bacterial growth by cell division by capturing bacteria by using the charge of the nanodiamonds, and can exhibit persistent antibacterial properties.
  • FIG. 1 is a graph showing the relationship between the voltage applied to the aqueous nanodiamond-containing liquid and the current for each average particle size and concentration of nanodiamond.
  • FIG. 2 is a graph showing the relationship between the concentration of the aqueous solution containing nanodiamonds and the current.
  • FIG. 3 is a schematic diagram of an electric test circuit used for confirming the electric characteristics of the aqueous solution containing nanodiamonds.
  • FIG. 4 is a schematic diagram illustrating the capture of oral bacteria by toothbrush bristles containing nanodiamonds.
  • FIG. 5 is a schematic diagram illustrating an example of a toothbrush on which toothbrush bristles are planted.
  • the antimicrobial product of the present invention contains charged nanodiamonds.
  • the charged nanodiamond can be obtained, for example, by a detonation method.
  • Detonation nanodiamonds can be produced, for example, by detonating a mixed explosive of trinitrotoluene (TNT) and hexogen (RDX) in an inert medium such as carbon dioxide or water.
  • TNT trinitrotoluene
  • RDX hexogen
  • the detonation nanodiamond obtained by this method is a powdery substance having strong cohesion and an average particle diameter of 3 to 50 ⁇ m.
  • an aqueous solution containing nanodiamonds for example, water-soluble A dispersion liquid (a mixture in a liquid state in which nanodiamond (solute) as a solid component is dispersed in an aqueous solvent as a liquid component such as water), and an "aqueous solution”, “aqueous colloid solution”, “aqueous dispersion solution”, “Aqueous solution” and “aqueous dispersion” can be obtained.
  • the average particle diameter can be measured using, for example, a commercially available dynamic light scattering particle size distribution analyzer, and the same applies hereinafter.
  • FIG. 3 is a schematic diagram of an electric test circuit used for confirming the electric characteristics of the aqueous solution containing nanodiamonds.
  • an electrode electrode plate
  • a current flowing on the circuit when a DC voltage is applied is measured.
  • FIG. 1 is a graph showing the relationship between the voltage applied to the aqueous nanodiamond-containing liquid and the current for each average particle size and concentration of nanodiamond. It can be seen from FIG. 1 that when a voltage is applied to the aqueous-containing liquid, the current increases almost linearly.
  • FIG. 2 is a graph showing the relationship between the concentration of the aqueous nanodiamond solution and the current when a DC voltage of 5 V is applied.
  • FIG. 2 shows that the magnitude of the current strongly depends on the concentration of the nanodiamond.
  • the aqueous nanodiamond-containing liquid conducts electricity. This is attributed to the nanodiamond contained in the aqueous-containing liquid, and it can be seen that the nanodiamond has a charge.
  • the nanodiamond may have a positive charge, have a negative charge, or have both a positive charge and a negative charge.
  • nanodiamonds produced by detonation method, the central nuclei SP 3 diamond structure, and then the intermediate layer of the SP 2 + X, and is composed of a graphite layer of SP 2 as an outermost layer, (100) plane is exactly It is reported that the (111) plane has a special crystal structure having a negatively charged spontaneous charge (for example, see paragraph 0014 of Japanese Patent No. 5761597).
  • the present inventors have also confirmed that nanodiamond produced by the detonation method has an outermost shell (outermost layer) covered with graphite oxide.
  • the average particle diameter of primary particles of nanodiamond contained in the aqueous nanodiamond solution is, for example, 1 to 50 nm, 1 to 20 nm, 1 to 10 nm, 1 to 5 nm, 1 to 3.8 nm, and 3 nm or less.
  • the antibacterial product of the present invention is characterized by containing charged nanodiamonds, and other configurations are not particularly limited.
  • the antimicrobial product of the present invention may further include a charged substrate, wherein the nanodiamonds are electrically fixed to the surface of the substrate.
  • the material of the substrate having a charge may be any material as long as the nanodiamond can be electrically fixed to the surface thereof.
  • the substrate includes a charged fiber.
  • the charged fiber may be, for example, a natural fiber or a synthetic fiber made of resin. Certain fibers are known to be partially charged. For example, wool, silk, and nylon have portions having positive and negative charges, and cotton, hemp, rayon, and the like have portions having slightly positive and negative charges. Among these, nylon resin fibers are preferable.
  • the length and thickness (diameter) of the fiber are not particularly limited, and may be appropriately set according to the use of the antibacterial product of the present invention.
  • the base may be, for example, a charged resin, a charged plastic, or the like. Examples of the resin and the plastic include a resin forming the synthetic fiber and a plastic made of the resin.
  • antimicrobial products of the present invention include sanitary articles such as toothbrush bristles, toothbrushes, disposable diapers, incontinence pads, urine absorbing pads, sanitary napkins, panty liners, cotton swabs, and the like; doctor coats, nurse coats, masks, gauze, adhesive plasters , Bandages and other medical supplies; hair brushes, makeup brushes, cosmetic puffs and other cosmetic supplies; socks, shorts, lingerie, and other clothing; pillows, duvets, sheets, and other bedding; car seats, carpets, curtains, cloths, and other interior goods Materials: food packaging bodies such as food packaging wrap films, food packaging bags, food trays (for example, meat and fish); toys such as stuffed animals; and the like.
  • food packaging bodies such as food packaging wrap films, food packaging bags, food trays (for example, meat and fish); toys such as stuffed animals; and the like.
  • the method for manufacturing the antibacterial product of the present invention will be described by taking toothbrush bristles and toothbrushes as examples, but other antibacterial products also have, for example, electric charges contained in them, like the toothbrush bristles and toothbrushes. It can be manufactured by electrically fixing nanodiamond to the surface of a base (for example, a fiber portion, a resin portion, and a plastic portion).
  • a base for example, a fiber portion, a resin portion, and a plastic portion.
  • Toothbrush bristles can be obtained, for example, by immersing a charged fiber (substrate) in an aqueous solution containing nanodiamonds and then washing with water.
  • concentration of nanodiamond in the aqueous solution is, for example, 0.0001 to 5% by mass.
  • the temperature of the aqueous solution during the immersion is not particularly limited, and may be room temperature or high temperature, for example, 15 to 70 ° C.
  • the immersion time of the fiber is also not particularly limited, but is, for example, 10 to 60 minutes. Examples of the water include fresh water, drinkable water, and pure water.
  • the metal and the metal element-containing compound which are impurities at the time of nanodiamond production, are removed by washing with the water (for example, 1 ppm or less based on the total amount of nanodiamonds), the human body and the oral cavity are removed. It is safer against metal allergy and the like.
  • the impurities include an oxidizing agent such as Fe added at the time of detonation, zirconia beads used for wet bead milling in a crushing process, and oxides such as Y, Al, and Hf added thereto as a stabilizer. And the like.
  • an antibacterial product such as toothbrush bristles can be obtained safely and simply without using a special device.
  • the nanodiamond is electrically fixed to the surface of the charged fiber (substrate) by utilizing the electric charge of the nanodiamond.
  • the charge of the nanodiamond it is possible to capture (collect) bacteria in the oral cavity and bacteria attached to the toothbrush hairs.
  • the bacteria can be immobilized on the fiber (substrate), the motor function can be lost, and the division and growth can be suppressed.
  • Reference 1 it is reported that many microorganisms such as bacteria have a negatively charged cell surface in an aqueous solution. For example, Escherichia coli, staphylococci, and Salmonella are negatively charged. It is known.
  • the toothbrush 1 of the present invention is characterized in that the toothbrush bristles 2 of the present invention are implanted in a head portion.
  • the method for implanting the toothbrush bristles 2 is not particularly limited, and for example, a conventionally known method such as a flat-line type implanting method or an in-mold method can be used.
  • the toothbrush 1 of the present invention can be kept clean, suppresses the division and growth of bacteria in the oral cavity, and is effective in preventing cerebral infarction, myocardial infarction, diabetes and the like. Moreover, since the toothbrush 1 of the present invention uses nanodiamonds that are nontoxic to the human body for antibacterial action of the toothbrush bristles 2, it can be used with confidence from infants to cared persons.
  • a charged fiber (nylon fiber made of nylon resin) was immersed in an aqueous solution containing nanodiamond having a primary particle diameter of 3 nm or less manufactured by the detonation method for 40 minutes, and then washed with pure water. After washing, water was removed by natural drying, followed by washing with fresh water. The concentration of nanodiamond in the aqueous solution was 0.01% by mass. The temperature of the aqueous solution at the time of immersion was 40 ° C., and the surface temperature of the nylon fiber was room temperature.
  • the antibacterial activity value A was 0.9, whereas the antibacterial activity value A was 0.9.
  • the antibacterial activity value A was 4.5, which exceeded the “antibacterial activity value of 2.0 or more”, which is considered to exhibit an antibacterial effect.

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Abstract

The purpose of the present invention is to provide a novel antibacterial product. In order to achieve this purpose, an antibacterial product according to the present invention is characterized by containing charged nanodiamonds.

Description

抗菌製品Antibacterial products
　本発明は、抗菌製品に関する。 The present invention relates to antibacterial products.
　近年、巷には、抗菌・除菌を謳った製品があふれている。しかし、そのほとんどが、一応、安全性に関する法律は遵守しているものの、例えば、人体に有害な四級アンモニウム塩、二酸化塩素又は重金属をイオン化させたものであり、長い意味での人体や環境面への影響は万人が認めるところである。 In recent years, products that declare antibacterial and eradication are overflowing. However, although most of them comply with safety laws for the time being, for example, they have ionized quaternary ammonium salts, chlorine dioxide, or heavy metals that are harmful to the human body. The impact on everyone is justified.
　そこで、本発明は、新たな抗菌製品を提供することを目的とする。 Therefore, an object of the present invention is to provide a new antibacterial product.
　前記目的を達成するために、本発明の抗菌製品は、電荷を有するナノダイヤモンドを含むことを特徴とする。 To achieve the above object, the antimicrobial product of the present invention is characterized in that it contains charged nanodiamond.
　本発明の抗菌製品は、ナノダイヤモンドが有する電荷で、細菌を捕菌（集菌）することで、細菌の細胞分裂による増殖を抑制し、持続性のある抗菌性を発揮し得る。 抗菌 The antibacterial product of the present invention can suppress bacterial growth by cell division by capturing bacteria by using the charge of the nanodiamonds, and can exhibit persistent antibacterial properties.
図１は、ナノダイヤモンド水性含有液への印加電圧と電流との関係を、ナノダイヤモンドの平均粒子径及び濃度毎に示したグラフである。FIG. 1 is a graph showing the relationship between the voltage applied to the aqueous nanodiamond-containing liquid and the current for each average particle size and concentration of nanodiamond. 図２は、ナノダイヤモンド水性含有液の濃度と電流との関係を示すグラフである。FIG. 2 is a graph showing the relationship between the concentration of the aqueous solution containing nanodiamonds and the current. 図３は、ナノダイヤモンド水性含有液の電気的特徴の確認に用いた電気実験回路の模式図である。FIG. 3 is a schematic diagram of an electric test circuit used for confirming the electric characteristics of the aqueous solution containing nanodiamonds. 図４は、ナノダイヤモンドを含む歯ブラシ毛による口腔内細菌の捕菌について説明する模式図である。FIG. 4 is a schematic diagram illustrating the capture of oral bacteria by toothbrush bristles containing nanodiamonds. 図５は、歯ブラシ毛が植毛された歯ブラシの一例を示す模式図である。FIG. 5 is a schematic diagram illustrating an example of a toothbrush on which toothbrush bristles are planted.
　以下、本発明について、さらに具体的に説明する。ただし、本発明は、以下の説明により限定されない。 Hereinafter, the present invention will be described more specifically. However, the present invention is not limited by the following description.
　前述のとおり、本発明の抗菌製品は、電荷を有するナノダイヤモンドを含む。 As described above, the antimicrobial product of the present invention contains charged nanodiamonds.
［ナノダイヤモンド］
　電荷を有するナノダイヤモンドは、例えば、爆轟法により得ることができる。爆轟法ナノダイヤモンドは、例えば、トリニトロトルエン（ＴＮＴ）及びヘキソーゲン（ＲＤＸ）の混合火薬を、炭酸ガス又は水等の不活性媒体中で爆轟させることで生成し得る。この方法で得られる爆轟法ナノダイヤモンドは、凝集性が強く、平均粒子径が３～５０μｍの粉状物である。例えば、この粉状物に、ジルコニアビーズを解砕メディアとする湿式摩擦粉砕（湿式ビーズミリング）等の湿式微粉砕処理と、超音波処理を施すことにより、ナノダイヤモンド水性含有液（例えば、水溶性分散液（水等の液体成分である水性溶媒に、固体成分であるナノダイヤモンド（溶質）が分散した液体状態の混合物）であり、「水溶液」、「水性コロイド溶液」、「水性分散溶液」、「水性溶液」、「水性分散液」等とも言える。）が得られる。前記平均粒子径は、例えば、市販の動的光散乱式粒径分布測定装置を用いて測定でき、これ以降において同様である。 [Nano diamond]
The charged nanodiamond can be obtained, for example, by a detonation method. Detonation nanodiamonds can be produced, for example, by detonating a mixed explosive of trinitrotoluene (TNT) and hexogen (RDX) in an inert medium such as carbon dioxide or water. The detonation nanodiamond obtained by this method is a powdery substance having strong cohesion and an average particle diameter of 3 to 50 μm. For example, by subjecting this powdery material to wet fine grinding treatment such as wet friction grinding (wet bead milling) using zirconia beads as a disintegrating medium, and ultrasonic treatment, an aqueous solution containing nanodiamonds (for example, water-soluble A dispersion liquid (a mixture in a liquid state in which nanodiamond (solute) as a solid component is dispersed in an aqueous solvent as a liquid component such as water), and an "aqueous solution", "aqueous colloid solution", "aqueous dispersion solution", "Aqueous solution" and "aqueous dispersion" can be obtained. The average particle diameter can be measured using, for example, a commercially available dynamic light scattering particle size distribution analyzer, and the same applies hereinafter.
　つぎに、このようにして得られたナノダイヤモンド水性含有液の電気的特徴について説明する。図３は、ナノダイヤモンド水性含有液の電気的特徴の確認に用いた電気実験回路の模式図である。図３に示すように、ナノダイヤモンド水性含有液に電極（極板）を配置し、直流電圧を印加したときに回路上に流れる電流を測定する。 Next, the electrical characteristics of the aqueous nanodiamond solution thus obtained will be described. FIG. 3 is a schematic diagram of an electric test circuit used for confirming the electric characteristics of the aqueous solution containing nanodiamonds. As shown in FIG. 3, an electrode (electrode plate) is arranged on the aqueous solution containing nanodiamonds, and a current flowing on the circuit when a DC voltage is applied is measured.
　図１は、ナノダイヤモンド水性含有液への印加電圧と電流との関係を、ナノダイヤモンドの平均粒子径及び濃度毎に示したグラフである。図１から、水性含有液に電圧をかけると、電流がほぼ直線的に増加することがわかる。 FIG. 1 is a graph showing the relationship between the voltage applied to the aqueous nanodiamond-containing liquid and the current for each average particle size and concentration of nanodiamond. It can be seen from FIG. 1 that when a voltage is applied to the aqueous-containing liquid, the current increases almost linearly.
　図２は、直流電圧５Ｖを印加したときの、ナノダイヤモンド水性含有液の濃度と電流との関係を示すグラフである。図２から、電流の大きさが、ナノダイヤモンドの濃度に強く依存することがわかる。 FIG. 2 is a graph showing the relationship between the concentration of the aqueous nanodiamond solution and the current when a DC voltage of 5 V is applied. FIG. 2 shows that the magnitude of the current strongly depends on the concentration of the nanodiamond.
　このように、ナノダイヤモンド水性含有液は、電気を通す。これには、水性含有液に含まれるナノダイヤモンドが寄与しており、ナノダイヤモンドが電荷を有することがわかる。ナノダイヤモンドは、正電荷を有するものでも、負電荷を有するものでも、正電荷及び負電荷の双方を有するものでもよい。なお、爆轟法で製造されたナノダイヤモンドは、中心核がＳＰ３ダイヤモンド構造、ついでＳＰ２＋Ｘの中間層、及び、最外層としてＳＰ２のグラファイト層から構成され、（１００）面は正に、（１１１）面は負に帯電した自発電荷を有する特殊な結晶構造を有することが報告されている（例えば、特許第５７６１５９７号公報の段落００１４参照）。また、本発明者らは、爆轟法で製造されたナノダイヤモンドが、最外殻（最外層）が酸化黒鉛で覆われたものであることを確認している。 Thus, the aqueous nanodiamond-containing liquid conducts electricity. This is attributed to the nanodiamond contained in the aqueous-containing liquid, and it can be seen that the nanodiamond has a charge. The nanodiamond may have a positive charge, have a negative charge, or have both a positive charge and a negative charge. Incidentally, nanodiamonds produced by detonation method, the central nuclei SP 3 diamond structure, and then the intermediate layer of the SP 2 + X, and is composed of a graphite layer of SP 2 as an outermost layer, (100) plane is exactly It is reported that the (111) plane has a special crystal structure having a negatively charged spontaneous charge (for example, see paragraph 0014 of Japanese Patent No. 5761597). The present inventors have also confirmed that nanodiamond produced by the detonation method has an outermost shell (outermost layer) covered with graphite oxide.
　ナノダイヤモンド水性含有液に含まれるナノダイヤモンドの一次粒子の平均粒子径は、例えば、１～５０ｎｍ、１～２０ｎｍ、１～１０ｎｍ、１～５ｎｍ、１～３．８ｎｍ、３ｎｍ以下である。 平均 The average particle diameter of primary particles of nanodiamond contained in the aqueous nanodiamond solution is, for example, 1 to 50 nm, 1 to 20 nm, 1 to 10 nm, 1 to 5 nm, 1 to 3.8 nm, and 3 nm or less.
［抗菌製品］
　本発明の抗菌製品は、電荷を有するナノダイヤモンドを含むことが特徴であって、その他の構成は、特に制限されない。例えば、本発明の抗菌製品は、さらに、電荷を有する基体を含み、前記ナノダイヤモンドが、前記基体の表面に電気的に固着したものであってもよい。 [Antibacterial products]
The antibacterial product of the present invention is characterized by containing charged nanodiamonds, and other configurations are not particularly limited. For example, the antimicrobial product of the present invention may further include a charged substrate, wherein the nanodiamonds are electrically fixed to the surface of the substrate.
［基体］
　電荷を有する基体の材質としては、ナノダイヤモンドがその表面に電気的に固着可能であればいかなるものであってもよい。例えば、前記基体としては、電荷を有する繊維があげられる。前記電荷を有する繊維としては、例えば、天然繊維であっても、樹脂製の合成繊維であってもよい。ある種の繊維は、部分的に電荷を有することが知られている。例えば、羊毛、絹、ナイロンは、正及び負の電荷を帯びている部分があり、木綿、麻、レーヨン等は、僅かに正及び負の電荷を帯びている部分がある。これらの中でも、ナイロン系樹脂製の繊維が好ましい。繊維の長さ及び太さ（径）は、特に限定されず、本発明の抗菌製品の用途に応じて、適宜設定すればよい。前記基体は、例えば、電荷を有する樹脂、電荷を有するプラスチック等であってもよい。前記樹脂及び前記プラスチックとしては、例えば、前記合成繊維を形成する樹脂及び当該樹脂製のプラスチック等があげられる。 [Base]
The material of the substrate having a charge may be any material as long as the nanodiamond can be electrically fixed to the surface thereof. For example, the substrate includes a charged fiber. The charged fiber may be, for example, a natural fiber or a synthetic fiber made of resin. Certain fibers are known to be partially charged. For example, wool, silk, and nylon have portions having positive and negative charges, and cotton, hemp, rayon, and the like have portions having slightly positive and negative charges. Among these, nylon resin fibers are preferable. The length and thickness (diameter) of the fiber are not particularly limited, and may be appropriately set according to the use of the antibacterial product of the present invention. The base may be, for example, a charged resin, a charged plastic, or the like. Examples of the resin and the plastic include a resin forming the synthetic fiber and a plastic made of the resin.
　本発明の抗菌製品の具体例としては、歯ブラシ毛、歯ブラシ、使い捨ておむつ、失禁パッド、尿取りパッド、生理用ナプキン、パンティーライナー、綿棒等の衛生用品；ドクターコート、ナースコート、マスク、ガーゼ、絆創膏、包帯等の医療用品；ヘアブラシ、化粧筆、化粧用パフ等の化粧用品；靴下、ショーツ、ランジェリー等の衣料品；枕、布団、シーツ等の寝具；カーシート、カーペット、カーテン、クロス等の内装用資材；食品包装用ラップフィルム、食品包装用袋、食品用（例えば、肉、魚用等）トレイ等の食品包装体；ぬいぐるみ等の玩具；等があげられる。これ以降、本発明の抗菌製品の製造方法等について、歯ブラシ毛及び歯ブラシを例にあげて説明するが、その他の抗菌製品についても、例えば、歯ブラシ毛及び歯ブラシと同様に、それらが含む電荷を有する基体（例えば、繊維部分、樹脂部分、プラスチック部分）の表面に、ナノダイヤモンドを電気的に固着させることで製造可能である。 Specific examples of the antimicrobial products of the present invention include sanitary articles such as toothbrush bristles, toothbrushes, disposable diapers, incontinence pads, urine absorbing pads, sanitary napkins, panty liners, cotton swabs, and the like; doctor coats, nurse coats, masks, gauze, adhesive plasters , Bandages and other medical supplies; hair brushes, makeup brushes, cosmetic puffs and other cosmetic supplies; socks, shorts, lingerie, and other clothing; pillows, duvets, sheets, and other bedding; car seats, carpets, curtains, cloths, and other interior goods Materials: food packaging bodies such as food packaging wrap films, food packaging bags, food trays (for example, meat and fish); toys such as stuffed animals; and the like. Hereinafter, the method for manufacturing the antibacterial product of the present invention will be described by taking toothbrush bristles and toothbrushes as examples, but other antibacterial products also have, for example, electric charges contained in them, like the toothbrush bristles and toothbrushes. It can be manufactured by electrically fixing nanodiamond to the surface of a base (for example, a fiber portion, a resin portion, and a plastic portion).
［歯ブラシ毛］
　歯ブラシ毛は、例えば、ナノダイヤモンド水性含有液に、電荷を有する繊維（基体）を浸漬した後、水で洗浄することで得ることができる。前記水性含有液におけるナノダイヤモンドの濃度は、例えば、０．０００１～５質量％である。また、前記浸漬時の水性含有液の温度は、特に限定されず、常温であっても、高温としてもよく、例えば、１５～７０℃である。繊維の浸漬時間も特に限定されないが、例えば、１０～６０分である。前記水としては、真水、飲用可能な水、純水等があげられる。なお、前記歯ブラシ毛において、前記水での洗浄により、ナノダイヤモンド製造時由来の不純物である金属及び金属元素含有化合物を除去（例えば、ナノダイヤモンド全量に対し１ｐｐｍ以下）すれば、人体及び口腔内で発生する金属アレルギー等に対して、より安全である。前記不純物としては、例えば、爆轟時に追加されるＦｅ等の酸化剤、解砕処理での湿式ビーズミリングに用いられるジルコニアビーズ及びそれに安定化剤として添加されたＹ、Ａｌ、Ｈｆ等の酸化物等があげられる。このように、本発明によれば、特別な装置を用いることなく、安全簡便に歯ブラシ毛等の抗菌製品を得ることができる。 [Toothbrush hair]
Toothbrush bristles can be obtained, for example, by immersing a charged fiber (substrate) in an aqueous solution containing nanodiamonds and then washing with water. The concentration of nanodiamond in the aqueous solution is, for example, 0.0001 to 5% by mass. The temperature of the aqueous solution during the immersion is not particularly limited, and may be room temperature or high temperature, for example, 15 to 70 ° C. The immersion time of the fiber is also not particularly limited, but is, for example, 10 to 60 minutes. Examples of the water include fresh water, drinkable water, and pure water. In addition, in the toothbrush bristles, if the metal and the metal element-containing compound, which are impurities at the time of nanodiamond production, are removed by washing with the water (for example, 1 ppm or less based on the total amount of nanodiamonds), the human body and the oral cavity are removed. It is safer against metal allergy and the like. Examples of the impurities include an oxidizing agent such as Fe added at the time of detonation, zirconia beads used for wet bead milling in a crushing process, and oxides such as Y, Al, and Hf added thereto as a stabilizer. And the like. As described above, according to the present invention, an antibacterial product such as toothbrush bristles can be obtained safely and simply without using a special device.
　本発明の歯ブラシ毛等の抗菌製品によれば、図４に例示するように、ナノダイヤモンドが有する電荷を利用して、電荷を有する繊維（基体）の表面にナノダイヤモンドを電気的に固着させるとともに、ナノダイヤモンドが有する電荷で、口腔内の細菌や歯ブラシ毛に付着した細菌を捕菌（集菌）可能である。これにより、細菌を繊維（基体）に固定化し、運動機能を失わせ、分裂・増殖を抑制することで、持続性のある抗菌性を発揮し得る。なお、下記参考文献１において、細菌等の微生物の多くは細胞表面が水溶液中で負に帯電していることが報告されており、例えば、大腸菌、ブドウ球菌、サルモネラ菌は、負に帯電していることが知られている。
 
参考文献
１）辻　高弘、森崎　久雄、“微生物付着に及ぼす静電場の影響”、[online]、日本微生物生態学会、[令和１年７月１０日検索]、インターネット<URL：http://dl.ndl.go.jp/view/download/digidepo_10879531_po_ART0008327273.pdf?itemId=info%3Andljp%2Fpid%2F10879531&contentNo=1&alternativeNo=&__lang=en>
  According to the antibacterial product such as the toothbrush bristles of the present invention, as illustrated in FIG. 4, the nanodiamond is electrically fixed to the surface of the charged fiber (substrate) by utilizing the electric charge of the nanodiamond. With the charge of the nanodiamond, it is possible to capture (collect) bacteria in the oral cavity and bacteria attached to the toothbrush hairs. Thereby, the bacteria can be immobilized on the fiber (substrate), the motor function can be lost, and the division and growth can be suppressed. In the following Reference 1, it is reported that many microorganisms such as bacteria have a negatively charged cell surface in an aqueous solution. For example, Escherichia coli, staphylococci, and Salmonella are negatively charged. It is known.

References 1) Takahiro Tsuji, Hisao Morisaki, "Effects of Electrostatic Field on Microbial Adhesion", [online], Japanese Society for Microbial Ecology, [Searched on July 10, 1980], Internet <URL: http: // dl.ndl.go.jp/view/download/digidepo_10879531_po_ART0008327273.pdf?itemId=info%3Andljp%2Fpid%2F10879531&contentNo=1&alternativeNo = & __ lang = en>
［歯ブラシ］
　図５に例示するように、本発明の歯ブラシ１は、ヘッド部分に本発明の歯ブラシ毛２が植毛されていることを特徴とする。歯ブラシ毛２の植毛方法は、特に限定されず、例えば、平線式植毛法、インモールド法等の従来公知の方法を用い得る。 [toothbrush]
As illustrated in FIG. 5, the toothbrush 1 of the present invention is characterized in that the toothbrush bristles 2 of the present invention are implanted in a head portion. The method for implanting the toothbrush bristles 2 is not particularly limited, and for example, a conventionally known method such as a flat-line type implanting method or an in-mold method can be used.
　本発明の歯ブラシ１は、清潔に保持することが可能であり、また、口腔内の細菌の分裂・増殖を抑制し、脳梗塞、心筋梗塞、糖尿病等の予防に有効である。また、本発明の歯ブラシ１は、歯ブラシ毛２の抗菌に人体に対する毒性の無いナノダイヤモンドを用いているため、乳児から被介護者まで安心して使用することができる。 The toothbrush 1 of the present invention can be kept clean, suppresses the division and growth of bacteria in the oral cavity, and is effective in preventing cerebral infarction, myocardial infarction, diabetes and the like. Moreover, since the toothbrush 1 of the present invention uses nanodiamonds that are nontoxic to the human body for antibacterial action of the toothbrush bristles 2, it can be used with confidence from infants to cared persons.
　爆轟法で製造された、一次粒子径が３ｎｍ以下のナノダイヤモンドの水性含有液に、電荷を有する繊維（ナイロン樹脂製のナイロン繊維）を４０分浸漬した後、純水で洗浄した。洗浄後、自然乾燥で水分を除去した後、真水で洗浄した。前記水性含有液におけるナノダイヤモンドの濃度は、０．０１質量％とした。また、前記浸漬時の水性含有液の温度は４０℃、ナイロン繊維の表面温度は常温とした。 電荷 A charged fiber (nylon fiber made of nylon resin) was immersed in an aqueous solution containing nanodiamond having a primary particle diameter of 3 nm or less manufactured by the detonation method for 40 minutes, and then washed with pure water. After washing, water was removed by natural drying, followed by washing with fresh water. The concentration of nanodiamond in the aqueous solution was 0.01% by mass. The temperature of the aqueous solution at the time of immersion was 40 ° C., and the surface temperature of the nylon fiber was room temperature.
　得られた歯ブラシ毛について、検体質量を０．４ｇから０．１ｇに、接種菌液量を０．２ｍＬから０．０５ｍＬに、洗い出し液量を２０ｍＬから５ｍＬに、同一検体数をＮ＝３からＮ＝１に変更した以外は、ＪＩＳ　Ｌ　１９０２－２０１５繊維製品の抗菌性試験方法８．１菌液吸収法に準じて、抗菌活性値を求めた。なお、試験菌株としては、黄色ブドウ球菌Ｓｔａｐｈｙｌｏｃｏｃｃｕｓ　ａｕｒｅｕｓ　ＮＢＲＣ１２７３２を使用し、試験片の滅菌方法は、１２１℃、１５分間のオートクレーブ滅菌、接種後の培養時間は、１８時間、試験接種菌液の濃度は、８．９×１０４、増殖値Ｆ＝３．０（Ｆ≧１．０により試験成立）とした。 For the obtained toothbrush bristles, the sample mass was changed from 0.4 g to 0.1 g, the inoculum solution volume was changed from 0.2 mL to 0.05 mL, the washing solution volume was changed from 20 mL to 5 mL, and the same sample number was changed from N = 3. Except that N was changed to 1, the antibacterial activity value was determined according to JIS L 1902-2015, Antibacterial Test Method for Textile Products, 8.1 Bacterial Solution Absorption Method. In addition, as a test strain, Staphylococcus aureus NBRC12732 was used as a test strain, and the test piece was sterilized by autoclaving at 121 ° C. for 15 minutes, culturing time after inoculation was 18 hours, and the concentration of the test inoculum was , 8.9 × 10 4 , and the proliferation value F = 3.0 (the test was established when F ≧ 1.0).
　ナノダイヤモンドの水性含有液に浸漬していない市販の歯ブラシの歯ブラシ毛（ブランク、比較例）で同様の試験を行うと、抗菌活性値Ａ＝０．９であったのに対し、本実施例の歯ブラシ毛では、抗菌活性値Ａ＝４．５となり、抗菌効果を示すとされる「抗菌活性値２．０以上」を上回った。 When a similar test was performed on the toothbrush bristles (blank, comparative example) of a commercially available toothbrush not immersed in the aqueous solution containing nanodiamonds, the antibacterial activity value A was 0.9, whereas the antibacterial activity value A was 0.9. In the case of toothbrush bristles, the antibacterial activity value A was 4.5, which exceeded the “antibacterial activity value of 2.0 or more”, which is considered to exhibit an antibacterial effect.
　この出願は、２０１８年８月３１日に出願された日本出願特願２０１８－１７４２２６及び国際出願ＰＣＴ／ＪＰ２０１９／２７５２６を基礎とする優先権を主張し、その開示の全てをここに取り込む。 This application claims priority based on Japanese Patent Application No. 2018-174226 filed on Aug. 31, 2018 and International Application PCT / JP2019 / 27526, the entire disclosure of which is incorporated herein.
１　歯ブラシ
２　歯ブラシ毛 1 toothbrush 2 toothbrush bristles

Claims (8)

  1. 電荷を有するナノダイヤモンドを含むことを特徴とする抗菌製品。 An antibacterial product comprising a charged nanodiamond.
  2. さらに、電荷を有する基体を含み、
    前記ナノダイヤモンドが、前記基体の表面に電気的に固着している、
    請求項１記載の抗菌製品。     Furthermore, it includes a substrate having a charge,
    The nanodiamond is electrically fixed to the surface of the substrate,
    An antimicrobial product according to claim 1.
  3. 前記基体が、繊維、樹脂及びプラスチックからなる群から選択される少なくとも一つである、請求項２記載の抗菌製品。 The antimicrobial product according to claim 2, wherein the substrate is at least one selected from the group consisting of a fiber, a resin, and a plastic.
  4. 衛生用品、医療用品、化粧用品、衣料品、寝具、内装用資材、食品包装体及び玩具からなる群から選択される少なくとも一つである、請求項１から３のいずれか一項に記載の抗菌製品。 The antibacterial according to any one of claims 1 to 3, wherein the antibacterial is at least one selected from the group consisting of a sanitary article, a medical article, a cosmetic article, clothing, bedding, an interior material, a food package, and a toy. Product.
  5. 歯ブラシ毛、歯ブラシ、使い捨ておむつ、失禁パッド、尿取りパッド、生理用ナプキン、パンティーライナー、綿棒、ドクターコート、ナースコート、マスク、ガーゼ、絆創膏、包帯、ヘアブラシ、化粧筆、化粧用パフ、靴下、ショーツ、ランジェリー、枕、布団、シーツ、カーシート、カーペット、カーテン、クロス、食品包装用ラップフィルム、食品包装用袋、食品用トレイ及びぬいぐるみからなる群から選択される少なくとも一つである、請求項１から４のいずれか一項に記載の抗菌製品。 Toothbrush hair, toothbrush, disposable diaper, incontinence pad, urine absorption pad, sanitary napkin, panty liner, cotton swab, doctor coat, nurse coat, mask, gauze, adhesive plaster, bandage, hairbrush, makeup brush, makeup puff, socks, shorts The lingerie, a pillow, a futon, a bed sheet, a car seat, a carpet, a curtain, a cloth, a wrap film for food packaging, a food packaging bag, a food tray, and a stuffed animal. The antibacterial product according to any one of claims 1 to 4.
  6. 前記ナノダイヤモンドが、平均粒子径が３ｎｍ以下の一次粒子である、請求項１から５のいずれか一項に記載の抗菌製品。 The antimicrobial product according to any one of claims 1 to 5, wherein the nanodiamond is a primary particle having an average particle size of 3 nm or less.
  7. 前記ナノダイヤモンドが、最外殻が酸化黒鉛で覆われたものである、請求項１から６のいずれか一項に記載の抗菌製品。 The antimicrobial product according to any one of claims 1 to 6, wherein the nanodiamond has an outermost shell covered with graphite oxide.
  8. 爆轟法で製造された、電荷を有するナノダイヤモンドの水性含有液を調製する含有液調製工程と、
    前記ナノダイヤモンドの水性含有液に、電荷を有する基体を浸漬する浸漬工程と、
    を含むことを特徴とする抗菌製品の製造方法。     A liquid-containing preparation step of preparing an aqueous liquid containing charged nanodiamonds produced by the detonation method,
    An immersion step of immersing a charged substrate in the aqueous solution of the nanodiamond,
    A method for producing an antibacterial product, comprising:
PCT/JP2019/034073 2018-08-31 2019-08-30 Antibacterial product WO2020045615A1 (en)

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