JP3987878B1 - Method for producing ZnO antibacterial agent - Google Patents
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- JP3987878B1 JP3987878B1 JP2007010176A JP2007010176A JP3987878B1 JP 3987878 B1 JP3987878 B1 JP 3987878B1 JP 2007010176 A JP2007010176 A JP 2007010176A JP 2007010176 A JP2007010176 A JP 2007010176A JP 3987878 B1 JP3987878 B1 JP 3987878B1
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- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 239000007864 aqueous solution Substances 0.000 claims abstract description 37
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 23
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 17
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 5
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 31
- 238000000034 method Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 230000004075 alteration Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- SDGKUVSVPIIUCF-UHFFFAOYSA-N 2,6-dimethylpiperidine Chemical compound CC1CCCC(C)N1 SDGKUVSVPIIUCF-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 229910014130 Na—P Inorganic materials 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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Abstract
【課題】暗所においても優れた抗菌性能を有するＺｎＯ系抗菌剤の製造方法を提供する。
【解決手段】この発明のＺｎＯ系抗菌剤の製造方法は、ＺｎＯ及び亜鉛イオンを含有した水溶液をオートクレーブ中で水熱処理する工程を含むことを特徴とする。また、この発明の別のＺｎＯ系抗菌剤の製造方法は、ＺｎＯ粉末を所定形状に成形して成形体を得る工程と、前記成形体を、亜鉛イオンを含有した水溶液に浸漬した状態でオートクレーブ中において水熱処理する工程と、前記水熱処理を経た成形体を焼結処理することによってＺｎＯ系多孔質焼結体を得る工程と、を含むことを特徴とする。
【選択図】なしA method for producing a ZnO-based antibacterial agent having excellent antibacterial performance even in a dark place is provided.
A method for producing a ZnO antibacterial agent according to the present invention includes a step of hydrothermally treating an aqueous solution containing ZnO and zinc ions in an autoclave. Further, another method for producing a ZnO-based antibacterial agent according to the present invention includes a step of forming a ZnO powder into a predetermined shape to obtain a molded body, and an autoclave in which the molded body is immersed in an aqueous solution containing zinc ions. And a step of obtaining a ZnO-based porous sintered body by sintering the formed body that has undergone the hydrothermal treatment.
[Selection figure] None
Description
この発明は、暗所においても優れた抗菌性能を有するＺｎＯ系抗菌剤の製造方法に関する。 The present invention relates to a method for producing a ZnO-based antibacterial agent having excellent antibacterial performance even in a dark place.
ＺｎＯは、光触媒作用によって抗菌性を示すことが知られており、例えばこのＺｎＯの粉末を含有した分散液を、金属物品、ガラス物品等の物品の表面に塗布して表面コート層を形成することによって、物品に抗菌性能を付与できることが知られている（特許文献１参照）。
しかしながら、上記従来技術では、抗菌性能を発揮させるためにはＺｎＯに光が照射されていることが必要であり、暗所においては抗菌性能が殆ど得られないか又は全く得られないという問題があった。例えば、水の浄化装置内にこのようなＺｎＯを配置せしめることで微生物の繁殖を抑制又は防止しようとしても、浄化装置内には光が入ってこないためにこのＺｎＯにより抗菌を行うことはできなかった。 However, the above prior art requires that ZnO be irradiated with light in order to exhibit antibacterial performance, and there is a problem that little or no antibacterial performance is obtained in the dark. It was. For example, even if an attempt is made to suppress or prevent the growth of microorganisms by arranging such ZnO in a water purification device, no light enters the purification device, so that antibacterial activity cannot be performed with this ZnO. It was.
この発明は、かかる技術的背景に鑑みてなされたものであって、暗所においても優れた抗菌性能を有するＺｎＯ系抗菌剤の製造方法を提供することを目的とする。 This invention is made | formed in view of this technical background, Comprising: It aims at providing the manufacturing method of the ZnO type | system | group antibacterial agent which has the outstanding antibacterial performance also in the dark place.
前記目的を達成するために、本発明は以下の手段を提供する。 In order to achieve the above object, the present invention provides the following means.
［１］ＺｎＯ及び亜鉛イオンを含有した水溶液をオートクレーブ中で水熱処理する工程を含むことを特徴とするＺｎＯ系抗菌剤の製造方法。 [1] A method for producing a ZnO antibacterial agent, comprising a step of hydrothermally treating an aqueous solution containing ZnO and zinc ions in an autoclave.
［２］ＺｎＯ粉末及び亜鉛イオンを含有した水溶液をオートクレーブ中で水熱処理する工程と、
前記水熱処理を経たＺｎＯ粉末を所定形状に成形して成形体を得る工程と、
前記成形体を焼結処理することによってＺｎＯ系多孔質焼結体を得る工程と、を含むことを特徴とするＺｎＯ系抗菌剤の製造方法。
[2] a step of hydrothermally treating an aqueous solution containing ZnO powder and zinc ions in an autoclave;
A step of obtaining a molded body by molding the hydrothermally treated ZnO powder into a predetermined shape;
And a step of obtaining a ZnO-based porous sintered body by subjecting the molded body to a sintering treatment, and a method for producing a ZnO-based antibacterial agent.
［３］ＺｎＯ粉末を所定形状に成形して成形体を得る工程と、
前記成形体を、亜鉛イオンを含有した水溶液に浸漬した状態でオートクレーブ中において水熱処理する工程と、
前記水熱処理を経た成形体を焼結処理することによってＺｎＯ系多孔質焼結体を得る工程と、を含むことを特徴とするＺｎＯ系抗菌剤の製造方法。
[3] A step of forming a ZnO powder into a predetermined shape to obtain a molded body;
Hydrothermally treating the molded body in an autoclave while being immersed in an aqueous solution containing zinc ions;
And a step of obtaining a ZnO-based porous sintered body by sintering the molded body that has undergone the hydrothermal treatment.
［４］前記焼結処理を４００〜６００℃で１〜１０時間行うことを特徴とする前項２または３に記載のＺｎＯ系抗菌剤の製造方法。 [4] The method for producing a ZnO-based antibacterial agent according to item 2 or 3, wherein the sintering treatment is performed at 400 to 600 ° C. for 1 to 10 hours.
［５］前記オートクレーブ中での水熱処理を１．２〜１０気圧、１１０〜１８０℃の処理条件で行う前項１〜４のいずれか１項に記載のＺｎＯ系抗菌剤の製造方法。 [5] The method for producing a ZnO-based antibacterial agent according to any one of items 1 to 4, wherein the hydrothermal treatment in the autoclave is performed under a treatment condition of 1.2 to 10 atm and 110 to 180 ° C.
［６］前記亜鉛イオンを含有した水溶液として、硝酸亜鉛を含有した水溶液を用いる前項１〜５のいずれか１項に記載のＺｎＯ系抗菌剤の製造方法。 [6] The method for producing a ZnO-based antibacterial agent according to any one of items 1 to 5, wherein an aqueous solution containing zinc nitrate is used as the aqueous solution containing zinc ions.
［７］前記水溶液中における硝酸亜鉛の濃度が０．５〜５モル／Ｌである前項６に記載のＺｎＯ系抗菌剤の製造方法。 [7] The method for producing a ZnO-based antibacterial agent according to item 6 above, wherein the concentration of zinc nitrate in the aqueous solution is 0.5 to 5 mol / L.
［８］前記ＺｎＯ粉末として粒径が０．０１〜０．３０μｍであるものを用いる前項１〜７のいずれか１項に記載のＺｎＯ系抗菌剤の製造方法。 [8] The method for producing a ZnO-based antibacterial agent according to any one of items 1 to 7, wherein the ZnO powder has a particle size of 0.01 to 0.30 μm.
［１］の発明では、ＺｎＯ及び亜鉛イオンを含有した水溶液をオートクレーブ中で水熱処理するので、得られたＺｎＯ系抗菌剤は、暗所においても優れた抗菌性能を有したものとなる。なお、得られたＺｎＯ系抗菌剤では、光が当たる条件下ではさらに優れた抗菌性能が発揮され得る。 In the invention of [1], since an aqueous solution containing ZnO and zinc ions is hydrothermally treated in an autoclave, the obtained ZnO antibacterial agent has excellent antibacterial performance even in a dark place. In addition, in the obtained ZnO type | system | group antibacterial agent, the further outstanding antibacterial performance may be exhibited on the conditions which light strikes.
［２］の発明では、ＺｎＯ粉末及び亜鉛イオンを含有した水溶液をオートクレーブ中で水熱処理した後、ＺｎＯ粉末を所定形状に成形して得た成形体を焼結処理するので、暗所においても優れた抗菌性能を有したＺｎＯ系多孔質焼結体を製造することができる。なお、得られたＺｎＯ系多孔質焼結体は、光が当たる条件下ではより優れた抗菌性能を発揮する。 In the invention of [2], an aqueous solution containing ZnO powder and zinc ions is hydrothermally treated in an autoclave, and then the molded product obtained by molding the ZnO powder into a predetermined shape is sintered, so that it is excellent even in the dark. A ZnO-based porous sintered body having antibacterial performance can be produced. In addition, the obtained ZnO type porous sintered body exhibits more excellent antibacterial performance under the condition of being exposed to light.
［３］の発明では、ＺｎＯ成形体を、亜鉛イオンを含有した水溶液に浸漬した状態でオートクレーブ中において水熱処理した後、焼結処理を行うので、暗所においても優れた抗菌性能を有したＺｎＯ系多孔質焼結体を製造することができる。本製造方法では、ＺｎＯをオートクレーブ中で水熱処理する際にはＺｎＯは既に所定形状に成形されており、水熱処理時のハンドリング性に優れていると共に、ＺｎＯ粉末を所定形状に成形することで水熱処理時のＺｎＯの処理量を増大でき処理効率を向上させることができるから、生産効率を顕著に向上できる利点がある。この点において、この［３］の発明の製造方法は、前記［２］の発明の製造方法よりも好適である。なお、得られたＺｎＯ系多孔質焼結体は、光が当たる条件下ではより優れた抗菌性能を発揮する。 In the invention of [3], since the ZnO molded body is hydrothermally treated in an autoclave in a state of being immersed in an aqueous solution containing zinc ions, and then subjected to a sintering treatment, ZnO having excellent antibacterial performance even in a dark place A porous sintered body can be produced. In this production method, when hydrothermally treating ZnO in an autoclave, the ZnO is already formed into a predetermined shape, which is excellent in handling properties during hydrothermal treatment and is formed by forming ZnO powder into a predetermined shape. Since the throughput of ZnO during the heat treatment can be increased and the processing efficiency can be improved, there is an advantage that the production efficiency can be remarkably improved. In this respect, the manufacturing method of the invention of [3] is more preferable than the manufacturing method of the invention of [2]. In addition, the obtained ZnO type porous sintered body exhibits more excellent antibacterial performance under the condition of being exposed to light.
［４］の発明では、焼結処理を４００〜６００℃で１〜１０時間行うから、より優れた抗菌性能を確保しつつ、多孔質焼結体として十分な強度を確保できる。 In the invention of [4], since the sintering treatment is performed at 400 to 600 ° C. for 1 to 10 hours, sufficient strength as a porous sintered body can be ensured while ensuring superior antibacterial performance.
［５］の発明では、オートクレーブ中での水熱処理を１．２〜１０気圧、１１０〜１８０℃の処理条件で行うので、変質を生じさせることなく、十分な水熱処理を行うことができる。 In the invention of [5], since the hydrothermal treatment in the autoclave is performed under the treatment conditions of 1.2 to 10 atm and 110 to 180 ° C., sufficient hydrothermal treatment can be performed without causing alteration.
［６］の発明では、亜鉛イオンを含有した水溶液として、硝酸亜鉛を含有した水溶液を用いるので、暗所における抗菌性能をさらに向上させたものを製造できると共に、水中等で繰り返し使用しても抗菌性能が低下しない耐久性に優れた抗菌剤を製造できる。 In the invention of [6], since an aqueous solution containing zinc nitrate is used as an aqueous solution containing zinc ions, an antibacterial performance further improved in a dark place can be produced, and even if it is repeatedly used in water, the antibacterial property can be obtained. An antibacterial agent excellent in durability that does not deteriorate in performance can be produced.
［７］の発明では、水溶液中における硝酸亜鉛の濃度が０．５〜５モル／Ｌであるから、より一層暗所での抗菌性能に優れたＺｎＯ系抗菌剤を製造できる。 In the invention of [7], since the concentration of zinc nitrate in the aqueous solution is 0.5 to 5 mol / L, a ZnO-based antibacterial agent having further excellent antibacterial performance in a dark place can be produced.
［８］の発明では、原料として用いるＺｎＯ粉末の粒径が０．０１〜０．３０μｍであるから、暗所における抗菌性能を十分に有したＺｎＯ系抗菌剤を製造できる。 In the invention of [8], since the particle diameter of the ZnO powder used as a raw material is 0.01 to 0.30 μm, a ZnO antibacterial agent having sufficient antibacterial performance in a dark place can be produced.
この発明に係るＺｎＯ系抗菌剤の製造方法は、ＺｎＯ（粉末、成形体等）及び亜鉛イオンを含有した水溶液をオートクレーブ中で水熱処理する工程を含むことを特徴とする。このように、ＺｎＯ（粉末、成形体等）を、亜鉛イオンを含有した水溶液中でオートクレーブにより水熱処理することによって得られたＺｎＯ系抗菌剤は、暗所においても優れた抗菌性能を有している。勿論、このＺｎＯ系抗菌剤は、光が当たる条件下では、より優れた抗菌性能が発揮されるものとなる。 The method for producing a ZnO-based antibacterial agent according to the present invention includes a step of hydrothermally treating an aqueous solution containing ZnO (powder, molded body, etc.) and zinc ions in an autoclave. Thus, the ZnO antibacterial agent obtained by hydrothermally treating ZnO (powder, molded body, etc.) with an autoclave in an aqueous solution containing zinc ions has excellent antibacterial performance even in the dark. Yes. Of course, this ZnO-based antibacterial agent exhibits more excellent antibacterial performance under the condition of being exposed to light.
ＺｎＯ系抗菌剤として所定形状に成形されたものを製造する場合には、次の第１製造方法または第２製造方法を採用するのが好ましい。 When manufacturing what was shape | molded by the predetermined shape as a ZnO type | system | group antibacterial agent, it is preferable to employ | adopt the following 1st manufacturing method or the 2nd manufacturing method.
［第１製造方法］
ＺｎＯ粉末及び亜鉛イオンを含有した水溶液をオートクレーブ中で水熱処理する工程と、前記水熱処理を経たＺｎＯ粉末を所定形状に成形して成形体を得る工程と、前記成形体を焼結処理することによってＺｎＯ系多孔質焼結体を得る工程と、を含むことを特徴とする。
[First production method]
By hydrothermally treating an aqueous solution containing ZnO powder and zinc ions in an autoclave, molding the ZnO powder subjected to the hydrothermal treatment into a predetermined shape to obtain a molded body, and sintering the molded body And a step of obtaining a ZnO-based porous sintered body.
［第２製造方法］
ＺｎＯ粉末を所定形状に成形して成形体を得る工程と、前記成形体を、亜鉛イオンを含有した水溶液に浸漬した状態でオートクレーブ中において水熱処理する工程と、前記水熱処理を経た成形体を焼結処理することによってＺｎＯ系多孔質焼結体を得る工程と、を含むことを特徴とする。
[Second production method]
A step of forming a ZnO powder into a predetermined shape to obtain a molded body, a step of hydrothermally treating the molded body in an autoclave while being immersed in an aqueous solution containing zinc ions, and a step of firing the molded body that has undergone the hydrothermal treatment. And a step of obtaining a ZnO-based porous sintered body by performing a sintering process.
この発明において、前記ＺｎＯ粉末の粒径は０．０１〜０．３０μｍであるのが好ましい。０．３０μｍを超えると、得られるＺｎＯ系抗菌剤の抗菌性能が十分に得られ難くなるので、好ましくない。 In the present invention, the ZnO powder preferably has a particle size of 0.01 to 0.30 μm. If it exceeds 0.30 μm, the antibacterial performance of the obtained ZnO-based antibacterial agent becomes difficult to obtain sufficiently, which is not preferable.
前記オートクレーブ中で水熱処理する時の圧力は１．２〜１０気圧に設定するのが好ましい。１．２気圧以上に設定することで水熱処理を十分に行うことができると共に、１０気圧以下に設定することで変質を防止することができる。 The pressure during hydrothermal treatment in the autoclave is preferably set to 1.2 to 10 atmospheres. Hydrothermal treatment can be sufficiently performed by setting the pressure to 1.2 atmospheres or more, and alteration can be prevented by setting the pressure to 10 atmospheres or less.
また、前記オートクレーブ中で水熱処理する時の温度は１１０〜１８０℃に設定するのが好ましい。１１０℃以上であることで水熱処理を十分に行うことができると共に、１８０℃以下に設定することで変質を防止することができる。中でも、前記オートクレーブ中で水熱処理する時の温度は１１５〜１２５℃に設定するのが特に好ましい。 Moreover, it is preferable to set the temperature at the time of hydrothermal treatment in the autoclave to 110 to 180 ° C. Hydrothermal treatment can be sufficiently performed when the temperature is 110 ° C. or higher, and alteration can be prevented by setting the temperature to 180 ° C. or lower. Especially, it is especially preferable to set the temperature at the time of hydrothermal treatment in the autoclave to 115 to 125 ° C.
また、前記オートクレーブ中での水熱処理の処理時間は３〜１０時間に設定するのが好ましい。３時間以上であることで水熱処理を十分に行うことができると共に、１０時間以下であることで暗所における抗菌性能をさらに向上させることができる。中でも、前記オートクレーブ中での水熱処理の処理時間は６〜８時間に設定するのが特に好ましい。 The treatment time for hydrothermal treatment in the autoclave is preferably set to 3 to 10 hours. When it is 3 hours or more, hydrothermal treatment can be sufficiently performed, and when it is 10 hours or less, the antibacterial performance in the dark can be further improved. Especially, it is especially preferable to set the processing time of the hydrothermal treatment in the autoclave to 6 to 8 hours.
前記亜鉛イオンを含有した水溶液としては、特に限定されるものではないが、例えば硝酸亜鉛を含有した水溶液、塩化亜鉛を含有した水溶液、酢酸亜鉛を含有した水溶液等が挙げられる。これらの中でも、硝酸亜鉛を含有した水溶液を用いるのが好ましく、この場合には暗所における抗菌性能がさらに向上したＺｎＯ系抗菌剤を製造できる。 The aqueous solution containing zinc ions is not particularly limited, and examples thereof include an aqueous solution containing zinc nitrate, an aqueous solution containing zinc chloride, and an aqueous solution containing zinc acetate. Among these, it is preferable to use an aqueous solution containing zinc nitrate. In this case, a ZnO antibacterial agent having further improved antibacterial performance in a dark place can be produced.
前記水溶液中における硝酸亜鉛の濃度は０．５〜５モル／Ｌに設定するのが好ましい。０．５モル／Ｌ以上であることで十分に優れた暗所での抗菌性能を付与できると共に、５モル／Ｌ以下であることでＺｎＯ表面の過度の変質を防止できる。中でも、前記水溶液中における硝酸亜鉛の濃度は２〜４モル／Ｌに設定するのが特に好ましい。 The concentration of zinc nitrate in the aqueous solution is preferably set to 0.5 to 5 mol / L. When it is 0.5 mol / L or more, sufficiently excellent antibacterial performance in a dark place can be imparted, and when it is 5 mol / L or less, excessive deterioration of the ZnO surface can be prevented. Among these, the concentration of zinc nitrate in the aqueous solution is particularly preferably set to 2 to 4 mol / L.
前記焼結処理に供する成形体としては、ハンドリングを行い得る程度の強度を少なくとも備えていれば良い。 The molded body to be subjected to the sintering process only needs to have at least a strength that allows handling.
前記焼結処理の処理温度は４００〜６００℃に設定するのが好ましい。４００℃以上であることで成形体として十分な強度を確保できると共に、６００℃以下であることで暗所における抗菌性能をさらに向上させることができる。中でも、前記焼結処理の処理温度は４５０〜５５０℃に設定するのが特に好ましい。 The processing temperature of the sintering process is preferably set to 400 to 600 ° C. When the temperature is 400 ° C. or higher, sufficient strength as a molded body can be secured, and when the temperature is 600 ° C. or lower, antibacterial performance in a dark place can be further improved. Especially, it is especially preferable to set the processing temperature of the sintering process to 450 to 550 ° C.
また、前記焼結処理の処理時間は１〜１０時間に設定するのが好ましい。１時間以上であることで成形体として十分な強度を確保できると共に、１０時間以下であることで暗所における抗菌性能をさらに向上させることができる。中でも、前記焼結処理の処理時間は３〜７時間に設定するのが特に好ましい。 The processing time for the sintering process is preferably set to 1 to 10 hours. When it is 1 hour or longer, sufficient strength as a molded article can be secured, and when it is 10 hours or shorter, antibacterial performance in a dark place can be further improved. Especially, it is especially preferable to set the processing time of the sintering process to 3 to 7 hours.
前記焼結処理は、１段階で行っても良いし、或いは２段階以上の複数段階で行っても良い。例えば、４５０℃×１時間、４７０℃×１時間、４８５℃×１時間、５００℃×２時間の順で４段階（計５時間）で行っても良い。 The sintering process may be performed in one stage, or may be performed in two or more stages. For example, it may be performed in four steps (total 5 hours) in the order of 450 ° C. × 1 hour, 470 ° C. × 1 hour, 485 ° C. × 1 hour, and 500 ° C. × 2 hours.
次に、この発明の具体的実施例について説明するが、本発明はこれら実施例のものに特に限定されるものではない。 Next, specific examples of the present invention will be described, but the present invention is not particularly limited to these examples.
＜実施例１＞
粒径０．０２μｍのＺｎＯ粉末（堺化学工業株式会社製、「ＮＡＮＯＦＩＮＥ Ｐ−２」、純度９８．５％、比表面積５２．０ｇ／ｍ2）を９８ＭＰａで一軸加圧金型成形することによって円盤状の成形体（１６ｍｍφ×厚さ１０ｍｍ）を得た。この成形体を、３モル／Ｌの硝酸亜鉛水溶液に浸漬し、この浸漬状態でオートクレーブ中において水熱処理した。前記オートクレーブでの水熱処理は、２気圧、１２０℃の処理条件で７時間行った。次いで、前記水熱処理を経た成形体を空気雰囲気下５００℃で５時間焼結処理することによって、ＺｎＯ系多孔質焼結体を得た。
<Example 1>
By uniaxially press-molding a ZnO powder (manufactured by Sakai Chemical Industry Co., Ltd., “NANOFINE P-2”, purity 98.5%, specific surface area 52.0 g / m 2 ) at 98 MPa with a particle size of 0.02 μm A disk-shaped molded body (16 mmφ × 10 mm thickness) was obtained. This molded body was immersed in a 3 mol / L zinc nitrate aqueous solution and hydrothermally treated in an autoclave in this immersed state. The hydrothermal treatment in the autoclave was carried out for 7 hours under the treatment conditions of 2 atm and 120 ° C. Next, the compact subjected to the hydrothermal treatment was sintered at 500 ° C. for 5 hours in an air atmosphere to obtain a ZnO-based porous sintered body.
＜実施例２＞
水熱処理時間を１０時間にした以外は、実施例１と同様にして、ＺｎＯ系多孔質焼結体を得た。
<Example 2>
A ZnO-based porous sintered body was obtained in the same manner as in Example 1 except that the hydrothermal treatment time was 10 hours.
＜実施例３＞
硝酸亜鉛水溶液として、濃度が１モル／Ｌのものを用いた以外は、実施例１と同様にして、ＺｎＯ系多孔質焼結体を得た。
<Example 3>
A ZnO-based porous sintered body was obtained in the same manner as in Example 1 except that a zinc nitrate aqueous solution having a concentration of 1 mol / L was used.
＜実施例４＞
３モル／Ｌの硝酸亜鉛水溶液に代えて１モル／Ｌの酢酸亜鉛水溶液を用い、水熱処理時間を１０時間にした以外は、実施例１と同様にして、ＺｎＯ系多孔質焼結体を得た。
<Example 4>
A ZnO-based porous sintered body was obtained in the same manner as in Example 1 except that a 1 mol / L zinc acetate aqueous solution was used in place of the 3 mol / L zinc nitrate aqueous solution and the hydrothermal treatment time was 10 hours. It was.
＜実施例５＞
粒径０．０２μｍのＺｎＯ粉末に代えて、粒径０．１０μｍのＺｎＯ粉末を用いた以外は、実施例１と同様にして、ＺｎＯ系多孔質焼結体を得た。
<Example 5>
A ZnO-based porous sintered body was obtained in the same manner as in Example 1 except that a ZnO powder having a particle size of 0.10 μm was used instead of the ZnO powder having a particle size of 0.02 μm.
＜比較例１＞
３モル／Ｌの硝酸亜鉛水溶液に代えて、イオン交換水を用いて水熱処理を行った以外は、実施例１と同様にして、ＺｎＯ系多孔質焼結体を得た。
<Comparative Example 1>
A ZnO-based porous sintered body was obtained in the same manner as in Example 1 except that hydrothermal treatment was performed using ion-exchanged water instead of the 3 mol / L zinc nitrate aqueous solution.
上記のようにして得られたＺｎＯ系多孔質焼結体について下記評価法に基づいて抗菌性の評価を行った。評価結果を表１に示す。 The antibacterial property was evaluated based on the following evaluation method for the ZnO-based porous sintered body obtained as described above. The evaluation results are shown in Table 1.
＜抗菌性評価法＞
Ｎａ−Ｐバッファー液（組成：ＫＨ2ＰＯ4１．３６ｇ、１Ｎ−ＮａＯＨ７．９ｍＬ、Ｈ2Ｏ４９２ｍＬ）に、大腸菌が入った水溶液を添加して、菌数をコロニーカウント法により測定した後、ここに滅菌処理が施されたＺｎＯ系多孔質焼結体を入れ、暗室において３６℃で２４時間静置し、この２４時間経過後の菌数（個／ｍＬ）をコロニーカウント法により測定した。
<Antimicrobial evaluation method>
An aqueous solution containing Escherichia coli was added to Na-P buffer solution (composition: KH 2 PO 4 1.36 g, 1N-NaOH 7.9 mL, H 2 O 492 mL), and the number of bacteria was measured by the colony count method. The sterilized ZnO-based porous sintered body was put in the plate, allowed to stand at 36 ° C. for 24 hours in a dark room, and the number of bacteria (cells / mL) after the lapse of 24 hours was measured by the colony count method.
表１から明らかなように、この発明の製造方法で製造された実施例１〜５のＺｎＯ系多孔質焼結体（ＺｎＯ系抗菌剤）では、暗所において３６℃で２４時間静置後、菌が確認されず、これら焼結体は、暗所においても抗菌性能に優れていた。 As is clear from Table 1, in the ZnO-based porous sintered bodies (ZnO-based antibacterial agents) of Examples 1 to 5 manufactured by the manufacturing method of the present invention, after standing at 36 ° C. for 24 hours in the dark, Bacteria were not confirmed, and these sintered bodies were excellent in antibacterial performance even in the dark.
これに対し、イオン交換水中で水熱処理した比較例１のＺｎＯ系多孔質焼結体では、暗所において３６℃で２４時間静置後、菌が非常に多く存在しており、暗所における抗菌性能は殆ど認められなかった。 In contrast, in the ZnO-based porous sintered body of Comparative Example 1 hydrothermally treated in ion-exchanged water, there were very many bacteria after standing at 36 ° C. for 24 hours in the dark, and antibacterial in the dark. Little performance was observed.
この発明の製造方法で得られたＺｎＯ系抗菌剤は、例えば水の浄化装置内に配置される抗菌剤や抗菌フィルター等として好適に用いられるが、特にこのような用途に限定されるものではない。 The ZnO-based antibacterial agent obtained by the production method of the present invention is suitably used as an antibacterial agent or an antibacterial filter disposed in, for example, a water purification device, but is not particularly limited to such applications .
Claims (8)
前記水熱処理を経たＺｎＯ粉末を所定形状に成形して成形体を得る工程と、
前記成形体を焼結処理することによってＺｎＯ系多孔質焼結体を得る工程と、を含むことを特徴とするＺｎＯ系抗菌剤の製造方法。 Hydrothermally treating an aqueous solution containing ZnO powder and zinc ions in an autoclave;
A step of obtaining a molded body by molding the hydrothermally treated ZnO powder into a predetermined shape;
And a step of obtaining a ZnO-based porous sintered body by subjecting the molded body to a sintering treatment, and a method for producing a ZnO-based antibacterial agent.
前記成形体を、亜鉛イオンを含有した水溶液に浸漬した状態でオートクレーブ中において水熱処理する工程と、
前記水熱処理を経た成形体を焼結処理することによってＺｎＯ系多孔質焼結体を得る工程と、を含むことを特徴とするＺｎＯ系抗菌剤の製造方法。 Forming a ZnO powder into a predetermined shape to obtain a molded body;
Hydrothermally treating the molded body in an autoclave while being immersed in an aqueous solution containing zinc ions;
And a step of obtaining a ZnO-based porous sintered body by sintering the molded body that has undergone the hydrothermal treatment.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010042953A (en) * | 2008-08-12 | 2010-02-25 | Takeshi Hirota | METHOD FOR PRODUCING POROUS CERAMIC-ZnO-BASED ANTIBACTERIAL COMPOSITE BODY |
| CN115572413A (en) * | 2021-07-06 | 2023-01-06 | 天津碧海蓝天水性高分子材料有限公司 | Nano-boehmite zinc-loaded inorganic composite antibacterial agent and preparation method thereof |
| CN117819954A (en) * | 2024-01-04 | 2024-04-05 | 廊坊瑞耀建筑装饰工程有限公司 | High-performance antibacterial domestic ceramic and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010042953A (en) * | 2008-08-12 | 2010-02-25 | Takeshi Hirota | METHOD FOR PRODUCING POROUS CERAMIC-ZnO-BASED ANTIBACTERIAL COMPOSITE BODY |
| CN115572413A (en) * | 2021-07-06 | 2023-01-06 | 天津碧海蓝天水性高分子材料有限公司 | Nano-boehmite zinc-loaded inorganic composite antibacterial agent and preparation method thereof |
| CN117819954A (en) * | 2024-01-04 | 2024-04-05 | 廊坊瑞耀建筑装饰工程有限公司 | High-performance antibacterial domestic ceramic and preparation method and application thereof |
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