WO2010098309A1 - 銀ナノ微粒子含有の組成物、銀ナノ微粒子含有のマスターバッチおよびその成形品 - Google Patents
銀ナノ微粒子含有の組成物、銀ナノ微粒子含有のマスターバッチおよびその成形品 Download PDFInfo
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- WO2010098309A1 WO2010098309A1 PCT/JP2010/052735 JP2010052735W WO2010098309A1 WO 2010098309 A1 WO2010098309 A1 WO 2010098309A1 JP 2010052735 W JP2010052735 W JP 2010052735W WO 2010098309 A1 WO2010098309 A1 WO 2010098309A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0058—Biocides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
Definitions
- the present invention relates to a composition containing antibacterial silver nanoparticles, a synthetic resin masterbatch containing silver nanoparticles, and a molded product thereof.
- Patent Document 1 aims to “provide a method for producing a masterbatch containing an antibacterial agent that does not inactivate silver ions”, and uses soluble glass as a carrier for silver nanoparticles. Yes. Further, Patent Document 2 states that “thermoplastic capable of exhibiting excellent antibacterial properties even when the resin molded body has a bulky shape by effectively utilizing the original antibacterial properties of the inorganic antibacterial agent.
- the purpose of the present invention is to provide a resin molded article.
- inorganic compounds for supporting antibacterial metal ions include inorganic adsorbents such as activated carbon, activated alumina and silica gel, zeolite, hydroxyapatite, phosphorus Inorganic ion exchangers such as zirconium acid, titanium phosphate, potassium titanate, hydrous bismuth, hydrous zirconium, and hydrotalcite are shown.
- inorganic adsorbents such as activated carbon, activated alumina and silica gel, zeolite, hydroxyapatite, phosphorus Inorganic ion exchangers such as zirconium acid, titanium phosphate, potassium titanate, hydrous bismuth, hydrous zirconium, and hydrotalcite are shown.
- Patent Document 3 has an object of “providing an antibacterial coating composition containing 30 PPM nanosilver particles on the surface of an injection preformed article and a coating method of the antibacterial coating”, and in the manufacturing process shown as a solution means, , “Nanosilver particles are dispersed in ethanol at a predetermined concentration to obtain a nanosilver ethanol dispersion liquid”.
- Patent Document 4 discloses a technique for uniformly dispersing silver nanoparticles in a masterbatch without using a dispersant or a carrier.
- a predetermined amount of an ultrafine particle material is mixed in a molding base material, the molding base material is melted or cured to be molded into a predetermined shape, and the ultrafine particle material is formed on the molding surface or surface layer portion.
- the mixed ultrafine particle material is passed from the inside to the surface or surface layer of the molded article through a crosslinked network of the molded base material.
- JP 05-255515 A Japanese Patent Application Laid-Open No. 07-252376 JP 2006-9008 A JP 2007-197707 A
- Patent Documents 1 to 3 have the following problems in addition to the fact that antibacterial properties are not necessarily at a sufficiently satisfactory level. That is, (1) When a dispersant is used, the components of the dispersant remain in the synthetic resin, which may be harmful depending on the dispersant used, and the silver fine particles are uniform in the synthetic resin. Not distributed. (2) And when using a carrier, (A) Since it is difficult to make the particle size of the inorganic particles themselves carrying silver less than or equal to the wavelength of visible light, transparency, which is a feature of the particles, is impaired when blended with a transparent synthetic resin.
- the silver itself necessary for the expression of antibacterial properties is uniformly dispersed in the synthetic resin, and when blended with the transparent synthetic resin, the characteristic transparency is not impaired, and the synthetic resin originally possesses. It is an object of the present invention to provide a masterbatch that does not impair the preferred physical properties, is excellent in economic efficiency, and does not pose a safety problem even when it is a molded article such as synthetic resin tableware. .
- Silver lactate was added to and blended with the pellets of the synthetic resin, kneaded at a temperature at which the synthetic resin melts using a kneading extruder, and extruded into strands to be cut into pellets.
- this synthetic resin pellet is observed under a transmission microscope, silver is found to be very finely dispersed (average particle diameter is about 1 nm to 80 nm) and uniformly dispersed in the obtained synthetic resin. There was found. If the ultrafine silver particles are dispersed and present in the synthetic resin in such a form, the synthetic resin is expected to have sufficient antibacterial properties.
- a small plate-shaped molded product generally called a color plate is molded from the obtained synthetic resin pellets by injection molding, and whether or not the plate-shaped molded product has antibacterial properties.
- antibacterial properties as expected were obtained, and the present invention was achieved.
- silver lactate is mixed with the synthetic resin and kneaded and extruded at a high temperature.
- silver lactate decomposes into lactic acid and silver at a high temperature, and silver ions formed by the decomposition aggregate to form ultrafine silver particles in the synthetic resin.
- the above invention was originally performed using a polypropylene resin as a synthetic resin. However, it is technically expected that the same effect can be sufficiently expected with other thermoplastic resins, and is therefore another general-purpose synthetic resin. Similar investigations were made not only for polyethylene resins, polystyrene resins, ABS resins, etc., but also for polycarbonate resins, polyamide resins, polyethylene terephthalate resins, etc., which are engineering resins. It was found that similar results were obtained.
- the present invention is as follows. That is, the silver nanoparticle-containing composition according to claim 1 of the present application is produced by mixing a predetermined amount of silver lactate and a thermoplastic resin and kneading the thermoplastic resin at a meltable temperature. .
- the master batch containing silver nanoparticles according to claim 2 of the present application is prepared by mixing a predetermined amount of silver lactate and a thermoplastic resin, kneading at a meltable temperature of the thermoplastic resin to obtain a mixed melt, and mixing and melting the mixture. It is characterized by being manufactured by extruding, cooling and chopping.
- the silver nanoparticle-containing masterbatch according to claim 3 of the present application is the silvernanoparticle-containing masterbatch according to claim 2, wherein the silver concentration in the silver lactate with respect to the thermoplastic resin is about 200 ppm to It is characterized by 20,000 ppm.
- the master batch containing silver nanoparticles according to claim 4 of the present application is the master batch containing silver nanoparticles according to claim 2 or claim 3, wherein the silver nanoparticles have a particle size of about 1 nm to 80 nm. It is characterized by that.
- a synthetic resin molded product according to claim 5 of the present application is a thermoplastic resin containing the silver nanoparticle-containing masterbatch according to any one of claims 2 to 4 added and mixed to melt the thermoplastic resin. It is characterized by being melted and molded at a possible temperature.
- the raw material used to make silver exist as ultrafine particles in the synthetic resin is a simple chemical product called silver lactate, and it requires a special process other than mixing and heating with the synthetic resin.
- a sufficient antibacterial effect can be exhibited even when the amount of silver lactate used is as small as 200 ppm to 20,000 ppm. Therefore, for example, the cost is lower than that of a conventional method in which silver is supported on zeolite or the like described in Patent Document 2 and the amount used is at least 2 to 3% or more.
- the synthetic resin (master batch containing silver nanoparticle) in which ultrafine particles (so-called nanosize) of silver obtained in the present invention are dispersed may be a transparent synthetic resin such as polystyrene resin or polycarbonate resin.
- the transparency of the synthetic resin is not impaired because the size of the silver particles is smaller than the wavelength of visible light.
- the content of silver nanoparticles is 200 ppm to 20,000 ppm, usually about 500 ppm to 5,000 ppm. The physical properties inherent to the synthetic resin are not impaired.
- FIG. 1 is a photograph of an internal structure observed with a transmission electron microscope of a masterbatch containing silver nanoparticles using polypropylene as a synthetic resin raw material pellet according to the present invention
- FIG. 1 (B) is a photograph of a PP substrate containing 4,000 ppm of silver nanoparticles according to the present invention
- FIG. 2 is a production flow diagram of a masterbatch containing silver nanoparticles according to the present invention.
- reference numeral 1 is a master batch containing silver nanoparticles according to the present invention (hereinafter referred to as “master batch (1) containing silver nanoparticles)”
- reference numeral 3 is a synthetic resin raw material pellet
- reference numeral 5 is Silver lactate.
- the predetermined amount is such that the silver concentration in the silver lactate (5) is about 200 ppm to 20,000 ppm with respect to the synthetic resin raw material pellet (3).
- the amount of silver lactate (5) added to the synthetic resin raw material pellet (3) is preferably about 200 ppm to 20,000 ppm with respect to the pellet because the obtained pellet is desirably used as a master batch.
- the concentration of silver becomes too low when used as a master batch, and the antibacterial effect is difficult to be obtained.
- concentration is 20,000 ppm or more, the cost is increased and the practicality is lost.
- liquid paraffin or the like it is desirable to add and mix a small amount in advance as a so-called spreading agent.
- a lubricant such as magnesium stearate so that the silver nanoparticles are more uniformly dispersed in the synthetic resin.
- preparation of the aqueous solution of silver lactate was based on the following procedures. 1. 30 g of powdered silver lactate silver lactate powder is dissolved in 970 g of distilled water. 2. Insoluble particles are filtered through a glass filter. 2 is a schematic view of granular silver lactate (5) stuck to the surface of granular synthetic resin raw material pellet (3).
- the set temperature of the cylinder at the time of melting and kneading extrusion by the kneading extruder for masterbatch production is set to a temperature suitable for each synthetic resin, but usually 170 ° C to 290 ° C is used. For example, about 170 ° C. to 180 ° C. is used for polyethylene resin, and about 270 ° C. to 290 ° C. is used for polycarbonate resin.
- the kneading extruder for producing the master batch is preferably a twin screw extruder, but it has been confirmed that there is no particular problem even with a single screw extruder.
- [Cooling and shredding step: S4] The extruded molded product is cooled and further cut into a master batch (1) containing silver nanoparticles.
- the figure described in [Cooling and Shredding Step] in FIG. 2 is a schematic diagram of a master batch (1) containing silver nanoparticles.
- PP base material a master batch (hereinafter referred to as “PP base material”) containing silver nanoparticles produced through the above process using polypropylene resin pellets as synthetic resin raw material pellets will be described.
- FIG. 1 is a photograph of an internal structure observed with a transmission electron microscope of a masterbatch containing silver nanoparticles using polypropylene as a synthetic resin raw material pellet according to the present invention
- FIG. FIG. 1 (B) is a photograph of a PP substrate containing 4,000 ppm of silver nanoparticles according to the present invention.
- the black dots in the part surrounded by black circles in FIG. 1B are silver nanoparticles, but it can be seen from the photograph that silver nanoparticles having a particle size of less than 10 nm are evenly distributed.
- Table 1 shows the specifications of the PP base material containing the silver nanoparticles.
- non-blended PP substrate refers to a PP substrate that does not contain silver nanoparticles
- silver nanoparticle PP substrate refers to a PP substrate that contains silver nanoparticles.
- the “antibacterial activity value” in Table 2 is a numerical value representing the antibacterial performance. Therefore, the two samples shown in Table 2 are both “antibacterial performance”.
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Abstract
Description
(1)分散剤を使用する場合には、合成樹脂中に分散剤の成分が残留するため、使用する分散剤によっては、有害となる場合がある上に、合成樹脂中に銀の微粒子が均一に分散していない。
(2)そして、担持体を介する場合には、
(a)銀が担持された無機の粒子そのものの粒径を可視光線の波長以下にすることが難しいため、透明合成樹脂に配合した時にその特長である透明性を損なってしまう。
(b)無機の粒子に銀を担持させるため、その工程に費用が掛かって銀担持無機粒子のコストが高くなり、結果的にマスターバッチのコスト高を招く。
(c)銀を合成樹脂中に配合するために、抗菌性付与には何ら寄与しない無機粒子を余分に配合することになり、合成樹脂が本来保有している好ましい物性(例えば衝撃強度)を損なう場合がある。
そこで、これを確認するために、得られた合成樹脂ペレットから射出成形でカラープレートと一般的にいわれる小さい板状の成形品を成形し、この板状成形品に抗菌性があるかどうかを標準的な方法で評価したところ、期待通りの抗菌性が得られることが判明し、本発明に至ったものである。なお、乳酸銀を合成樹脂に混ぜ、高温下で混練押出しをすれば、何故合成樹脂中に銀のナノサイズの超微粒子が存在するようになるのかについては、現在のところ充分に解明をしてはいないが、乳酸銀が高温下で乳酸と銀とに分解し、この分解されてできた銀イオンが凝集して銀の超微粒子を合成樹脂中に形成したものと推定している。
上記発明は、当初、合成樹脂としてポリプロピレン樹脂を用いて行われたが、技法的には他の熱可塑性樹脂でも同様の効果が充分期待されると予想されたので、他の汎用合成樹脂であるポリエチレン樹脂、ポリスチレン樹脂、ABS樹脂等のみならず、エンジニアリング系樹脂であるポリカーボネ―ト樹脂、ポリアミド樹脂、ポリエチレンテレフタレート樹脂等についても同様の検討を行ったところ、これらの合成樹脂についても、ポリプロピレン樹脂の場合と同様の結果が得られることが判明した。
本願請求項1に係る銀ナノ微粒子含有の組成物は、所定量の乳酸銀および熱可塑性樹脂を混合し、該熱可塑性樹脂の溶融可能温度で混練して製造される、ことを特徴としている。
また、本願請求項2に係る銀ナノ微粒子含有のマスターバッチは、所定量の乳酸銀および熱可塑性樹脂を混合し、該熱可塑性樹脂の溶融可能温度で混練して混合溶融物とし、該混合溶融物を押出して冷却し細断することにより製造される、ことを特徴としている。
そして、本願請求項3に係る銀ナノ微粒子含有のマスターバッチは、請求項2に記載の銀ナノ微粒子含有のマスターバッチであって、前記熱可塑性樹脂に対する前記乳酸銀中の銀濃度が略200ppmないし20,000ppmである、ことを特徴としている。
さらに、本願請求項4に係る銀ナノ微粒子含有のマスターバッチは、請求項2または請求項3に記載の銀ナノ微粒子含有のマスターバッチであって、銀ナノ微粒子の粒径は略1nmないし80nmである、ことを特徴としている。
また、本願請求項5に係る合成樹脂成形品は、熱可塑性樹脂に請求項2ないし請求項4のいずれかに記載の銀ナノ微粒子含有のマスターバッチを加えて混合し、該熱可塑性樹脂の溶融可能温度で溶融せしめて成形した、ことを特徴としている。
また、本発明で得られる銀の超微粒子(いわゆるナノサイズ)が分散した合成樹脂(銀ナノ微粒子含有のマスターバッチ)は、たとえば、ポリスチレン樹脂、ポリカーボネート樹脂のような透明系の合成樹脂の場合でも、銀の粒子の大きさが可視光線の波長より小さいために、合成樹脂の本来有する透明性を損なわない。
さらに、本発明による銀ナノ微粒子含有のマスターバッチから得られる合成樹脂成形品の物性は、銀ナノ微粒子の含有量が200ppmないし20,000ppm、通常は500ppmないし5,000ppm程度と極めて少ないために、その合成樹脂が本来有する物性を損なうことがない。
粉末状の乳酸銀(5)または乳酸銀(5)の水溶液と合成樹脂原料ペレット(3)とを所定量計量した後、ヘンシェル型ミキサー等で混合し、その原料混合物を2軸押出機等のマスターバッチ製造用混練押出機に送り込む。なお、この所定量は乳酸銀(5)中の銀濃度を合成樹脂原料ペレット(3)に対して略200ppmないし20,000ppmとするものであるが、実施例においては、質量比で乳酸銀「2」に対して合成樹脂原料ペレット「250」としている。
合成樹脂原料ペレット(3)に添加する乳酸銀(5)の添加量は、得られるペレットをマスターバッチとして使用することが望ましいので、対ペレットで200ppmないし20,000ppm程度が適当である。すなわち、200ppm以下ではマスターバッチとして希釈して使った場合に銀の濃度が低くなり過ぎて抗菌性の効果が出難くなり、20,000ppm以上では結果的に高コストとなり実用性がなくなるからである。
また、合成樹脂原料ペレット(3)と乳酸銀(5)を混合する際に、乳酸銀(5)の細かい粉末を合成樹脂原料ペレット(3)の表面に均一に付着させるために、流動パラフィン等をいわゆる展着剤として事前に少量添加して混合しておくことが望ましい。また合成樹脂の種類にもよるが、銀ナノ微粒子が合成樹脂中でより均一に分散するように、ステアリン酸マグネシウム等の潤滑剤を添加・使用することも好ましい。
1.粉末状の乳酸銀乳酸銀粉末30gを蒸留水970gに溶かす。
2.これをガラスフィルターで不溶の粒を濾す。
なお、図2の[原料の混合工程]に記載の図は、粒状の合成樹脂原料ペレット(3)の表面に張り付いた粒状の乳酸銀(5)の模式図である。
マスターバッチ製造用混練押出機内では、加熱により原料混合物中の合成樹脂原料ペレット(3)が溶融し、乳酸銀(5)は攪拌されて均一に混合されるとともに、乳酸銀(5)中の銀イオンが還元して、ナノサイズの粒径を有する銀ナノ微粒子に変わる。
なお、銀ナノ微粒子は、加工温度によって乳酸銀中の銀イオンが凝集されて作られるものと推察されるが、銀ナノ微粒子含有のマスターバッチ製造時の熱や温度の加減によって粒径の調節を図ることができる。また、マスターバッチ製造用混練押出機による溶融・混練押出し時のシリンダーの設定温度は、それぞれの合成樹脂に適した温度を設定するが、通常は170℃ないし290℃が使われる。たとえば、ポリエチレン樹脂では170℃ないし180℃程度、ポリカーボネート樹脂では270℃ないし290℃程度が使われる。また、マスターバッチ製造用混練押出機は2軸押出機が望ましいが、単軸の押出機でも特に問題はないことを確認している。
再加熱した原料混合物をノズルから押出してストランド状に成形する。
押出した成形物を冷却し、さらに、細断することにより銀ナノ微粒子含有のマスターバッチ(1)とする。
なお、図2の[冷却および細断工程]に記載の図は、銀ナノ微粒子含有のマスターバッチ(1)の模式図である。
試験方法は、JIS Z 2801(フィルム密着法)によりおこない、試験菌株は、大腸菌 E. coli NBRC 3972 を使用した。その結果を表2に示す。なお、表中、「非配合PP基材」とは、銀ナノ微粒子を含有しないPP基材をいい、「銀ナノ粒子PP基材」とは、銀ナノ微粒子を含有するPP基材をいう。
3 合成樹脂原料ペレット
5 乳酸銀
Claims (5)
- 所定量の乳酸銀および熱可塑性樹脂を混合し、該熱可塑性樹脂の溶融可能温度で混練して製造される、ことを特徴とする銀ナノ微粒子含有の組成物。
- 所定量の乳酸銀および熱可塑性樹脂を混合し、該熱可塑性樹脂の溶融可能温度で混練して混合溶融物とし、該混合溶融物を押出して冷却し細断することにより製造される、ことを特徴とする銀ナノ微粒子含有のマスターバッチ。
- 前記熱可塑性樹脂に対する前記乳酸銀中の銀濃度が略200ppmないし20,000ppmである、ことを特徴とする請求項2に記載の銀ナノ微粒子含有のマスターバッチ。
- 銀ナノ微粒子の粒径は略1nmないし80nmである、ことを特徴とする請求項2または請求項3に記載の銀ナノ微粒子含有のマスターバッチ。
- 熱可塑性樹脂に請求項2ないし請求項4のいずれかに記載の銀ナノ微粒子含有のマスターバッチを加えて混合し、該熱可塑性樹脂の溶融可能温度で溶融せしめて成形した、ことを特徴とする合成樹脂成形品。
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JP2020199438A (ja) * | 2019-06-07 | 2020-12-17 | 株式会社アイセル | コーティング液貯蔵体の製造方法 |
CN115521536A (zh) * | 2022-10-10 | 2022-12-27 | 山东诺森塑胶有限公司 | 一种抗菌型塑料色母粒配方的制备工艺 |
JP2023007326A (ja) * | 2021-06-30 | 2023-01-18 | 南亞塑膠工業股▲分▼有限公司 | 抗菌・防カビのポリエステル材料 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2020199438A (ja) * | 2019-06-07 | 2020-12-17 | 株式会社アイセル | コーティング液貯蔵体の製造方法 |
JP2023007326A (ja) * | 2021-06-30 | 2023-01-18 | 南亞塑膠工業股▲分▼有限公司 | 抗菌・防カビのポリエステル材料 |
JP7414788B2 (ja) | 2021-06-30 | 2024-01-16 | 南亞塑膠工業股▲分▼有限公司 | 抗菌・防カビのポリエステル材料 |
US11968980B2 (en) | 2021-06-30 | 2024-04-30 | Nan Ya Plastics Corporation | Antibacterial and antifungal polyester material |
CN115521536A (zh) * | 2022-10-10 | 2022-12-27 | 山东诺森塑胶有限公司 | 一种抗菌型塑料色母粒配方的制备工艺 |
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