JP2015013969A - Nano-order dispersion type antimicrobial coating and production method thereof - Google Patents

Nano-order dispersion type antimicrobial coating and production method thereof Download PDF

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JP2015013969A
JP2015013969A JP2013142209A JP2013142209A JP2015013969A JP 2015013969 A JP2015013969 A JP 2015013969A JP 2013142209 A JP2013142209 A JP 2013142209A JP 2013142209 A JP2013142209 A JP 2013142209A JP 2015013969 A JP2015013969 A JP 2015013969A
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nano
antibacterial
antibacterial paint
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賢史 米田
Satoshi Yoneda
賢史 米田
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AMAKENTECC KK
YONEDA TSUNEMASA
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AMAKENTECC KK
YONEDA TSUNEMASA
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PROBLEM TO BE SOLVED: To provide an antimicrobial coating having long pot life, capable of forming film even in a practical film formation condition, and capable of obtaining a practical film in durability and light resistance.SOLUTION: An emulsion as a base is prepared and then is agitated and dispersed while performing evacuation. Thereby, a nano-order dispersion type antimicrobial coating having long pot life, excellent in film formation, capable of obtaining a film having high hardness, and capable of achieving an antibacterial effect in a long period, in which separation and sediment of the antimicrobial agent is suppressed, is provided. The production method of the nano-order dispersion type antimicrobial coating is also provided.

Description

本発明は、抗菌塗料に関し、特にナノオーダー分散型抗菌塗料、及びこれらナノオーダー分散型抗菌塗料の製造方法に関するものである。   The present invention relates to an antibacterial paint, and more particularly to a nano-order dispersed antibacterial paint and a method for producing these nano-order dispersed antibacterial paints.

塗料の用途は多岐に亘っており、そこで要求される特性も様々である。その中で、抗菌性を有する塗料は病院、介護施設、老健施設、食品加工工場、学校、公共施設等、或いは家電製品等で様々に活用されている。   There are many uses for paints, and the properties required there are also various. Among them, antibacterial paints are used in various ways in hospitals, nursing homes, health facilities, food processing factories, schools, public facilities, and home appliances.

これら多岐に亘る用途の中で、抗菌性能の向上が望まれていた。しかし、金属或いは金属化合物の微粒子を分散した抗菌塗料においては、特に抗菌材料の分離沈降によるポットライフの問題及び塗膜強度の問題から、実用的な抗菌塗料は存在しなかった。   Among these various applications, improvement of antibacterial performance has been desired. However, in the antibacterial paint in which fine particles of metal or metal compound are dispersed, there is no practical antibacterial paint due to the problem of pot life due to separation and sedimentation of the antibacterial material and the problem of coating film strength.

特開2008−56592号公報JP 2008-56592 A 特開2008−308645号公報JP 2008-308645 A 特開2009−1505号公報JP 2009-1505 A 特開2006−29920号公報JP 2006-29920 A 特開2011−94140号公報JP 2011-94140 A 特開2012−255164号公報JP 2012-255164 A 特開2012−224747号公報JP 2012-224747 A

解決しようとする課題は、ポットライフが長く、且つ実用的な塗膜形成条件でもって成膜出来、耐久性及び耐光性に於いても実用的な塗膜が得られる抗菌塗料を実現することである。   The problem to be solved is to realize an antibacterial paint that has a long pot life, can be formed under practical coating film forming conditions, and can provide a practical coating film in terms of durability and light resistance. is there.

これらの課題を解決するため、筆者らは、塗料に抗菌性を持たせるために金属或いは金属化合物の微粒子を添加するにあたり、塗料の調整工程を鋭意検討し、ベースのエマルジョンを調製後減圧脱気を行いながら撹拌分散を行うことにより、抗菌剤の分離沈降が抑制されてポットライフが長く、成膜特性に優れ、硬度の高い塗膜を得られ、さら長期に亘って抗菌効果を実現するナノオーダー分散型抗菌塗料及びナノオーダー分散型抗菌塗料の製造方法を見出し、本発明を完成したのである。   In order to solve these problems, the authors have intensively studied the process of adjusting the paint when adding fine particles of metal or metal compounds to give the paint antibacterial properties, and after preparing the base emulsion, vacuum degassing By stirring and dispersing while performing antibacterial action, the separation and settling of the antibacterial agent is suppressed, the pot life is long, the film forming property is excellent, the coating film with high hardness is obtained, and the antibacterial effect is realized for a longer period of time. The inventors have found a method for producing an order-dispersed antibacterial paint and a nano-order dispersed antibacterial paint, and have completed the present invention.

本発明のナノオーダー分散型抗菌塗料及びナノオーダー分散型抗菌塗料の製造方法は、ポットライフが長く、且つ実用的な塗膜形成条件でもって成膜出来、耐久性及び耐光性に於いても実用的な塗膜が得られ、さらに長期に亘って抗菌効果を実現するという利点があり、もって多岐に亘る用途に活用出来、我が国産業の発展に資するものである。   The nano-order dispersed antibacterial paint and the method for producing the nano-order dispersed antibacterial paint of the present invention have a long pot life, can be formed under practical coating film forming conditions, and are practical in terms of durability and light resistance. It has the advantage of providing antibacterial effects over a long period of time, and can be used in a wide variety of applications, contributing to the development of Japanese industries.

図1は本発明に係るナノオーダー分散型抗菌塗料の製造方法の工程のフローチャートである。FIG. 1 is a flowchart of the steps of a method for producing a nano-order dispersed antibacterial paint according to the present invention. 図2は本発明に係るナノオーダー分散型抗菌塗料の製造に用いる減圧撹拌分散装置の概念図である。FIG. 2 is a conceptual view of a vacuum stirring and dispersing apparatus used for producing a nano-order dispersed antibacterial paint according to the present invention.

本発明は、ナノオーダー分散型抗菌塗料及びナノオーダー分散型抗菌塗料の製造方法において、減圧脱気を行いながら撹拌分散を行うことにより、抗菌剤の分離沈降が抑制されてポットライフが長く、成膜特性に優れ、塗膜の強度が高く、さらに長期に亘って抗菌効果を実現するナノオーダー分散型抗菌塗料及びナノオーダー分散型抗菌塗料の製造方法である。なお、本件特許明細書内で用いる「塗料」には、一般的な塗用のみでなく、所謂ワックスのように床用等に用いられるものも含まれる。   The present invention provides a nano-order dispersed antibacterial paint and a method for producing a nano-order dispersed antibacterial paint, whereby stirring and dispersing are performed while degassing under reduced pressure, so that separation and settling of the antibacterial agent is suppressed and the pot life is increased. This is a nano-order dispersed antibacterial paint and a method for producing a nano-order dispersed antibacterial paint that have excellent film properties, high strength of the coating film, and realize antibacterial effect over a long period of time. The “paint” used in the present patent specification includes not only general application but also one used for floors such as so-called wax.

本発明に係るナノオーダー分散型抗菌塗料の製造方法に於いては、合成樹脂エマルジョンおよび/または樹脂と、少なくとも金属又は金属化合物の微粒子とを含む塗料組成物を混合分散して塗料を構成する工程に於いて、減圧脱気を行いながら撹拌分散を行う工程を含むことによりナノオーダーの分散を行うことを特徴とする。なお、金属又は金属化合物の微粒子を添加する工程は、減圧脱気を行いながら撹拌分散を行う工程の前であっても、かかる工程が完了した後に添加分散を行うのでも、何れでも問題ない。   In the method for producing a nano-order dispersive antibacterial paint according to the present invention, a step of constituting a paint by mixing and dispersing a paint composition containing a synthetic resin emulsion and / or resin and at least metal or metal compound fine particles. In this case, nano-order dispersion is performed by including a step of stirring and dispersing while performing degassing under reduced pressure. The step of adding the metal or metal compound fine particles may be before the step of stirring and dispersing while performing degassing under reduced pressure, or the step of adding and dispersing after the completion of the step.

本発明に係るナノオーダー分散型抗菌塗料に用いる抗菌剤は、金属或いは金属化合物の微粒子を用いる。金属或いは金属化合物の微粒子としては、プラチナ、銀、チタン、酸化銀、酸化チタン等の微粒子などが好適に用いられる。この中でも、平均粒径が1〜10nmのプラチナ微粒子を用いることが特に効果的である。また、これら抗菌剤は、ナノオーダー分散型抗菌塗料に添加する前にコロイド化等の処理を行っても良い。   The antibacterial agent used in the nano-order dispersion type antibacterial paint according to the present invention uses fine particles of metal or metal compound. As fine particles of metal or metal compound, fine particles of platinum, silver, titanium, silver oxide, titanium oxide, etc. are preferably used. Among these, it is particularly effective to use platinum fine particles having an average particle diameter of 1 to 10 nm. These antibacterial agents may be subjected to a treatment such as colloidalization before being added to the nano-order dispersed antibacterial paint.

なお、前記塗料組成物は、さらに増粘剤、分散剤、湿潤剤、消泡剤、抑泡剤、成膜助剤、凍結防止剤、凍結安定剤、防腐剤、沈降防止剤、付着防止剤、乾燥調製剤、或いは熱変換剤・断熱材・遮熱剤などの温度抑制剤、からなる群より選ばれた1種または2種以上の補助剤を含んでもよい。   The coating composition further comprises a thickener, a dispersant, a wetting agent, an antifoaming agent, an antifoaming agent, a film forming aid, an antifreezing agent, a freezing stabilizer, an antiseptic agent, an antisettling agent, and an antiadhesive agent. 1 type, or 2 or more types of adjuvants chosen from the group which consists of drying preparation agents, or temperature control agents, such as a heat conversion agent, a heat insulating material, and a heat shielding agent, may be included.

さらに本発明に係るナノオーダー分散型抗菌塗料は、顔料、蓄光顔料、蛍光顔料或いは再帰反射材を含んでもよい。また、前記各顔料は、それぞれシリカ等によりコーティングされたものであってもよい。   Furthermore, the nano-order dispersed antibacterial paint according to the present invention may include a pigment, a phosphorescent pigment, a fluorescent pigment, or a retroreflective material. Each pigment may be coated with silica or the like.

本発明に係るナノオーダー分散型抗菌塗料の製造方法に於いては、塗料組成物を、減圧脱気を行いながら撹拌分散を行うことによりナノオーダーの分散を行う。
図1は、本発明に係るナノオーダー分散型抗菌蓄光塗料の製造方法の工程のフローチャートである。まず、合成樹脂エマルジョンおよび/または樹脂と、少なくとも金属或いは金属化合物の微粒子を含んでなる抗菌剤とを含む塗料組成物を、合成樹脂エマルジョンおよび/または樹脂を100重量部、抗菌剤を0.1重量部乃至50重量部、水および/またはは溶媒を50重量部乃至200重量部の範囲で混合して塗料組成物原料を調製する。ここで、塗料組成物原料にはさらに増粘剤、分散剤、湿潤剤、消泡剤、抑泡剤、成膜助剤、凍結防止剤、凍結安定剤、防腐剤、沈降防止剤、付着防止剤、乾燥調製剤、或いは熱変換剤・断熱材・遮熱剤などの温度抑制剤、からなる群より選ばれた1種または2種以上の補助剤を含んでもよい。さらに本発明に係るナノオーダー分散型抗菌塗料は、顔料、蓄光顔料、蛍光顔料或いは再帰反射材を含んでもよい。また、前記各顔料は、それぞれシリカ等によりコーティングされたものであってもよい。
In the method for producing a nano-order dispersion type antibacterial paint according to the present invention, nano-order dispersion is carried out by stirring and dispersing the coating composition while performing degassing under reduced pressure.
FIG. 1 is a flowchart of the steps of a method for producing a nano-order dispersed antibacterial phosphorescent paint according to the present invention. First, a coating composition containing a synthetic resin emulsion and / or resin and an antibacterial agent comprising at least metal or metal compound fine particles, 100 parts by weight of the synthetic resin emulsion and / or resin, and 0.1% of the antibacterial agent A coating composition raw material is prepared by mixing 50 parts by weight to 50 parts by weight, water and / or a solvent in the range of 50 parts by weight to 200 parts by weight. Here, the coating composition raw material further includes a thickener, a dispersant, a wetting agent, an antifoaming agent, an antifoaming agent, a film forming aid, an antifreezing agent, a freezing stabilizer, an antiseptic, an antisettling agent, and an anti-adhesion agent. One or two or more auxiliary agents selected from the group consisting of an agent, a drying preparation agent, or a temperature suppressing agent such as a heat conversion agent, a heat insulating material, and a heat shielding agent may be included. Furthermore, the nano-order dispersed antibacterial paint according to the present invention may include a pigment, a phosphorescent pigment, a fluorescent pigment, or a retroreflective material. Each pigment may be coated with silica or the like.

図2は、本発明に係るナノオーダー分散型抗菌塗料の製造に用いる減圧撹拌分散装置の概念図である。本発明に係るナノオーダー分散型抗菌塗料の製造に用いる減圧撹拌分散装置は、フランジを有して容器部と蓋部が開閉出来るようになっており、前記塗料組成物原料を容器部に投入後フランジを密着させて容器部と蓋部を締め付け、容器体内を減圧出来るようになっている。   FIG. 2 is a conceptual diagram of a vacuum stirring and dispersing apparatus used for producing a nano-order dispersed antibacterial paint according to the present invention. The vacuum stirring and dispersing apparatus used for the production of the nano-order dispersion type antibacterial paint according to the present invention has a flange so that the container part and the lid part can be opened and closed, and after the coating composition raw material is put into the container part The container body and the lid part are tightened by closely contacting the flange so that the inside of the container can be decompressed.

前記塗料組成物原料を容器部に投入後してフランジの締め付けを行った後、真空ポンプを作動させて容器体内を減圧し、またプロペラを回転させて撹拌分散を行う。なお、本発明に係るナノオーダー分散型抗菌蓄光塗料の製造方法に於いては、撹拌分散工程中の容器体内の圧力は1Pa乃至50000Paに調整することが望ましい。容器体内の圧力は1Pa乃至5000Paに調整することがさらに望ましく、1Pa乃至500Paに調整することがより望ましい。容器体内に設置されたプロペラを回転させて撹拌分散を行う工程と減圧工程は交互に繰り返して行うか、或いは同時に行われる。   After the raw material of the coating composition is put into the container part and the flange is tightened, the vacuum pump is operated to depressurize the container body, and the propeller is rotated to disperse the mixture. In the method for producing a nano-order dispersion type antibacterial phosphorescent paint according to the present invention, it is desirable to adjust the pressure in the container during the stirring and dispersing step to 1 Pa to 50000 Pa. The pressure in the container body is more preferably adjusted to 1 Pa to 5000 Pa, and more preferably adjusted to 1 Pa to 500 Pa. The step of stirring and dispersing by rotating the propeller installed in the container and the step of reducing pressure are alternately repeated or simultaneously performed.

容器体内に設置されたプロペラは、エマルジョン粒子を切断分散させる形状であることが撹拌分散に有効である。また、撹拌分散工程中のプロペラの回転数は200rpm乃至5000rpmの範囲に維持することが望ましい。減圧及び/又は撹拌分散工程は、トータルで5分以上24時間以下の範囲で行うことが望ましい。減圧及び/又は撹拌分散工程は、トータルで30分以上12時間以下の範囲で行うことがさらに望ましく、1時間以上6時間以下の範囲で行うことがより望ましく、2時間以上4時間以下の範囲で行うことがより望ましい。   It is effective for stirring and dispersing that the propeller installed in the container has a shape in which emulsion particles are cut and dispersed. Moreover, it is desirable to maintain the rotation speed of the propeller during the stirring and dispersing step in a range of 200 rpm to 5000 rpm. The decompression and / or stirring / dispersing step is desirably performed in a total range of 5 minutes to 24 hours. The decompression and / or stirring dispersion step is more preferably performed in a range of 30 minutes to 12 hours in total, more preferably in a range of 1 hour to 6 hours, and more preferably in a range of 2 hours to 4 hours. More desirable to do.

特に好ましいナノ化工程は、減圧工程と撹拌分散工程を交互に繰り返すことである。もちろん、撹拌分散工程中にも圧力を調整した上で減圧を行うことも有効である。この場合、特に低速回転での減圧撹拌分散、高速回転での減圧撹拌分散、の順に工程を繰り返すことがさらに有効である。前記の交互に低速及び高速回転での減圧撹拌分散を行う場合は、低速回転での減圧撹拌分散を1分以上30分以内、高速回転での減圧撹拌分散を5分以上3時間以内の工程を1セットとして繰り返すことがさらに望ましい。   A particularly preferred nanonization step is to alternately repeat the pressure reduction step and the stirring dispersion step. Of course, it is also effective to reduce the pressure after adjusting the pressure during the stirring and dispersing step. In this case, it is more effective to repeat the steps in the order of reduced pressure stirring dispersion at low speed rotation and reduced pressure stirring dispersion at high speed rotation. In the case of alternately performing the reduced pressure stirring dispersion at the low speed and the high speed rotation as described above, the steps of the reduced pressure stirring dispersion at the low speed rotation within 1 minute to 30 minutes and the reduced pressure stirring dispersion at the high speed rotation within 5 minutes to 3 hours. It is more desirable to repeat as one set.

前記の減圧下での撹拌分散工程を経た本発明に係るナノオーダー分散型抗菌塗料は、抗菌剤の分離沈降が抑制されてポットライフが長く、成膜特性に優れ、硬度の高い塗膜を得られ、さら長期に亘って抗菌効果を実現するナノオーダー分散型抗菌塗料を実現するものであった。   The nano-order dispersion type antibacterial coating material according to the present invention that has undergone the stirring and dispersing step under reduced pressure described above has a long pot life, excellent film forming characteristics, and a high hardness coating film because the separation and settling of the antibacterial agent is suppressed. Therefore, the nano-order dispersion type antibacterial coating material that realizes the antibacterial effect for a long time was realized.

以下、本発明に係るナノオーダー分散型抗菌塗料及びナノオーダー分散型抗菌塗料の製造方法を、実施例に基づいて詳細に説明する。   Hereinafter, the nano-order dispersed antibacterial paint and the method for producing the nano-order dispersed antibacterial paint according to the present invention will be described in detail based on examples.

本実施例に於いては、ナノオーダー分散型抗菌蓄光塗料の製造を行った。ここでは、本発明に係るナノオーダー分散型抗菌蓄光塗料の製造方法の例について説明し、同時にナノオーダー分散型抗菌塗料の製造に用いる減圧撹拌分散装置についても説明する。   In this example, a nano-order dispersed antibacterial phosphorescent paint was produced. Here, an example of a method for producing a nano-order dispersed antibacterial phosphorescent paint according to the present invention will be described, and at the same time, a vacuum stirring and dispersing apparatus used for producing a nano-order dispersed antibacterial paint will be described.

本実施例に於いては、ナノオーダー分散型抗菌蓄光塗料の原料エマルジョンとして、アクリル酸エステル共重合体エマルジョンを水に分散させて用いた。なお、本発明に用いられる原料エマルジョンとしては、本実施例に係る材料に限定されるものではなく、各種の合成樹脂エマルジョンおよび/または水溶性樹脂を好適に用いることが出来る。さらに、水に代えて溶媒等を用いる油性の塗料であっても良い。   In this example, an acrylic acid ester copolymer emulsion was dispersed in water as a raw material emulsion for a nano-order dispersion type antibacterial phosphorescent paint. In addition, as raw material emulsion used for this invention, it is not limited to the material which concerns on a present Example, Various synthetic resin emulsions and / or water-soluble resin can be used suitably. Furthermore, an oil-based paint using a solvent or the like instead of water may be used.

本実施例に於いては、上記アクリル酸エステル共重合体エマルジョン100重量部に水110重量部を加え、さらに消泡剤2.5重量部、湿潤剤及び抑泡剤各0.4重量部、乾燥調製剤2.5重量部を加えて撹拌を行った。ここで、添加剤としては求められる塗料の特性により、塗料組成物原料にはさらに増粘剤、分散剤、湿潤剤、消泡剤、抑泡剤、成膜助剤、凍結防止剤、凍結安定剤、防腐剤、沈降防止剤、付着防止剤、乾燥調製剤、或いは熱変換剤・断熱材・遮熱剤などの温度抑制剤、からなる群より選ばれた1種または2種以上の補助剤を含んでもよい。   In this example, 110 parts by weight of water was added to 100 parts by weight of the acrylate copolymer emulsion, and 2.5 parts by weight of an antifoaming agent, 0.4 parts by weight of a wetting agent and an antifoaming agent, 2.5 parts by weight of the dry preparation agent was added and stirred. Here, depending on the properties of the paint required as additives, the coating composition raw materials further include thickeners, dispersants, wetting agents, antifoaming agents, antifoaming agents, film forming aids, antifreeze agents, and freeze stability. 1 type or 2 types or more of auxiliary agents selected from the group consisting of agents, preservatives, anti-settling agents, anti-adhesion agents, drying preparation agents, or temperature inhibitors such as heat conversion agents, heat insulating materials, and heat shielding agents May be included.

かかるエマルジョンに、さらに抗菌剤を加えて撹拌し、抗菌塗料原料を得て、これをさらに減圧撹拌分散工程によりナノ化を行って、ナノオーダー分散型抗菌塗料を得た。本実施例においては、前記エマルジョン100重量部に対して平均粒径が1〜10nmのプラチナ微粒子を抗菌剤として5重量部加えて撹拌することにより、ナノオーダー分散型抗菌塗料を得たが、本発明はこれら材料及びこれらの配合比に限定されるものではない。   An antibacterial agent was further added to the emulsion and stirred to obtain an antibacterial coating material, which was further nano-sized by a vacuum stirring and dispersing step to obtain a nano-order dispersed antibacterial coating. In this example, 5 parts by weight of platinum fine particles having an average particle size of 1 to 10 nm as an antibacterial agent were added to 100 parts by weight of the emulsion and stirred to obtain a nano-order dispersed antibacterial paint. The invention is not limited to these materials and their blending ratios.

本発明に用いる抗菌剤としては金属或いは金属化合物の微粒子としては、プラチナ、銀、チタン、酸化銀、酸化チタン等の微粒子などが好適に用いられる。この中でも、平均粒径が1〜10nmのプラチナ微粒子を用いることが特に効果的である。また、これら抗菌剤は、ナノオーダー分散型水性抗菌塗料に添加する前にコロイド化等の処理を行っても良い。また、配合比も水性エマルジョンに対して任意に設定することが出来る。ここで、本発明は、水に代えて溶媒等を用いる油性の塗料であっても良い。   As the antibacterial agent used in the present invention, fine particles of platinum, silver, titanium, silver oxide, titanium oxide, etc. are suitably used as the fine particles of metal or metal compound. Among these, it is particularly effective to use platinum fine particles having an average particle diameter of 1 to 10 nm. Further, these antibacterial agents may be subjected to a treatment such as colloidalization before being added to the nano-order dispersed aqueous antibacterial coating. Also, the blending ratio can be arbitrarily set with respect to the aqueous emulsion. Here, the present invention may be an oil-based paint using a solvent or the like instead of water.

前記の混合組成物を十分に撹拌混合した後、エマルジョン塗料組成物をナノオーダー分散型抗菌塗料の製造に用いる減圧撹拌分散装置に投入して、減圧撹拌分散を行うことにより、本発明に係るナノオーダー分散型抗菌塗料が得られた。ここで、本発明は、水に代えて溶媒等を用いる油性の塗料であっても良い。   After sufficiently stirring and mixing the above mixed composition, the emulsion coating composition is put into a vacuum stirring and dispersing apparatus used for the production of a nano-order dispersion type antibacterial coating and subjected to vacuum stirring and dispersing, whereby nano according to the present invention is obtained. An order-dispersed antibacterial paint was obtained. Here, the present invention may be an oil-based paint using a solvent or the like instead of water.

本発明に係るナノオーダー分散型抗菌蓄光塗料の製造に用いる減圧撹拌分散装置の概念図が、図2に示される。本発明に係るナノオーダー分散型抗菌塗料の製造に用いる減圧撹拌分散装置は、フランジを有して容器部と蓋部が開閉出来るようになっており、前記塗料組成物原料を容器部に投入後フランジを密着させて容器部と蓋部を締め付け、容器体内を減圧出来るようになっている。   FIG. 2 shows a conceptual diagram of a vacuum stirring and dispersing apparatus used for producing the nano-order dispersion type antibacterial phosphorescent paint according to the present invention. The vacuum stirring and dispersing apparatus used for the production of the nano-order dispersion type antibacterial paint according to the present invention has a flange so that the container part and the lid part can be opened and closed, and after the coating composition raw material is put into the container part The container body and the lid part are tightened by closely contacting the flange so that the inside of the container can be decompressed.

前記塗料組成物原料を容器部に投入後してフランジの締め付けを行った後、真空ポンプを作動させて容器体内を減圧し、またプロペラを回転させて撹拌分散を行った。なお、本発明に係るナノオーダー分散型抗菌塗料の製造方法に於いては、撹拌分散工程中の容器体内の圧力は1Pa乃至50000Paに調整することが望ましい。容器体内の圧力は1Pa乃至5000Paに調整することがさらに望ましく、1Pa乃至500Paに調整することがより望ましい。本実施例においては、工程中でエマルジョン中に残留する空気の量により容器体内の圧力は変動するが、適宜容器体内のエマルジョンの発泡の程度を観察して、バルブにより減圧度を調整した。   After the coating composition raw material was put into the container part and the flange was tightened, the inside of the container was depressurized by operating a vacuum pump, and the propeller was rotated to perform stirring and dispersion. In the method for producing a nano-order dispersion type antibacterial paint according to the present invention, it is desirable to adjust the pressure inside the container during the stirring and dispersing step to 1 Pa to 50000 Pa. The pressure in the container body is more preferably adjusted to 1 Pa to 5000 Pa, and more preferably adjusted to 1 Pa to 500 Pa. In this example, the pressure in the container fluctuated depending on the amount of air remaining in the emulsion during the process, but the degree of foaming of the emulsion in the container was observed as appropriate, and the degree of pressure reduction was adjusted with a valve.

容器体内に設置されたプロペラは、エマルジョン粒子を切断分散させる形状であることが撹拌分散に有効である。また、撹拌分散工程中のプロペラの回転数は200rpm乃至5000rpmの範囲に維持することが望ましい。減圧及び/又は撹拌分散工程は、トータルで5分以上24時間以下の範囲で行うことが望ましい。減圧及び/又は撹拌分散工程は、トータルで30分以上12時間以下の範囲で行うことがさらに望ましく、1時間以上6時間以下の範囲で行うことがより望ましく、2時間以上4時間以下の範囲で行うことがより望ましい。   It is effective for stirring and dispersing that the propeller installed in the container has a shape in which emulsion particles are cut and dispersed. Moreover, it is desirable to maintain the rotation speed of the propeller during the stirring and dispersing step in a range of 200 rpm to 5000 rpm. The decompression and / or stirring / dispersing step is desirably performed in a total range of 5 minutes to 24 hours. The decompression and / or stirring dispersion step is more preferably performed in a range of 30 minutes to 12 hours in total, more preferably in a range of 1 hour to 6 hours, and more preferably in a range of 2 hours to 4 hours. More desirable to do.

容器体内に設置されたプロペラを回転させて撹拌分散を行う工程と減圧工程は交互に繰り返して行うか、或いは同時に行われる。特に好ましいナノ化工程は、減圧工程と撹拌分散工程を交互に繰り返すことである。本実施例においては、まずフランジを密封後、プロペラを1000rpm以下で低速回転させながら10分間の減圧を行い、その後プロペラの回転速度を1500rpm以上に上げて30分間の減圧撹拌分散を行った。その後、再度低速回転で10分間の減圧を行い、さらに高速回転で1時間の減圧撹拌分散を行った。最後に、低速回転で10分間の減圧撹拌分散を行い、ナノオーダー分散型抗菌蓄光塗料を得た。   The step of stirring and dispersing by rotating the propeller installed in the container and the step of reducing pressure are alternately repeated or simultaneously performed. A particularly preferred nanonization step is to alternately repeat the pressure reduction step and the stirring dispersion step. In this example, first, after sealing the flange, pressure reduction was performed for 10 minutes while rotating the propeller at a low speed of 1000 rpm or less, and then the rotation speed of the propeller was increased to 1500 rpm or more for 30 minutes under reduced pressure stirring dispersion. Thereafter, the pressure was reduced again for 10 minutes at a low speed rotation, and further, stirring and dispersing under reduced pressure for 1 hour was performed at a high speed rotation. Finally, the mixture was stirred and dispersed under reduced pressure for 10 minutes at a low speed to obtain a nano-order dispersion type antibacterial phosphorescent paint.

実施例1で用いたエマルジョンベースをワックスエステルに変更することにより、ワックスとして使用可能なナノオーダー分散型抗菌塗料を得た。本実施例に於いては、抗菌剤として酸化チタン微粒子を用いた。実施例1と同様の装置を用い、同様の工程でもって、ナノオーダー分散型抗菌ワックスが得られた   By changing the emulsion base used in Example 1 to a wax ester, a nano-order dispersed antibacterial paint usable as a wax was obtained. In this example, titanium oxide fine particles were used as an antibacterial agent. A nano-order dispersed antibacterial wax was obtained using the same apparatus as in Example 1 and in the same process.

ここで、本発明に係るナノオーダー分散型抗菌塗料は、前記の条件で撹拌分散することによりエマルジョン径を10μm以下としたことにより、沈降速度が小さく、ポットライフが長い抗菌塗料であった。さらに、エマルジョン径を5μm以下にすることが望ましく、エマルジョン径を1μm以下にすることがさらに望ましく、エマルジョン径を0.5μm以下にすることがさらに望ましい。   Here, the nano-order dispersion type antibacterial paint according to the present invention was an antibacterial paint having a low sedimentation rate and a long pot life by setting the emulsion diameter to 10 μm or less by stirring and dispersing under the above conditions. Furthermore, the emulsion diameter is preferably 5 μm or less, more preferably 1 μm or less, and further preferably 0.5 μm or less.

一般の抗菌塗料等に於いては、抗菌剤を含むエマルジョンの径が大きいため沈降し易く、数日から数週間の保管において沈殿を生じて成膜性が悪化する。しかし、本発明に係るナノオーダー分散型抗菌塗料は抗菌剤を含むエマルジョンの径が非常に小さいナノオーダーまで分散されているため、沈降速度が遅く、1年以上の保管期間を経ても十分に成膜性の良い塗料であった。ここで、本発明は、水に代えて溶媒等を用いる油性の塗料であっても良い。   In general antibacterial paints and the like, the emulsion containing an antibacterial agent has a large diameter, so that it easily settles, and precipitates are formed in storage for several days to several weeks, resulting in deterioration of film formability. However, since the nano-order dispersion type antibacterial paint according to the present invention is dispersed to the nano order where the diameter of the emulsion containing the antibacterial agent is very small, the sedimentation rate is slow, and the nano-order dispersion type antibacterial paint is sufficiently formed even after a storage period of one year or more. It was a paint with good film properties. Here, the present invention may be an oil-based paint using a solvent or the like instead of water.

また、本発明に係るナノオーダー分散型抗菌塗料は環境負荷が低く、非常にエコロジカルな抗菌塗料として多様な用途に用いることが出来る。さらに、本発明に係るナノオーダー分散型抗菌塗料は、ナノオーダーの分散を行っているため、長期間に亘って抗菌作用が持続する。   In addition, the nano-order dispersed antibacterial paint according to the present invention has a low environmental load and can be used for various applications as an extremely ecological antibacterial paint. Furthermore, since the nano-order dispersion type antibacterial paint according to the present invention performs nano-order dispersion, the antibacterial action is maintained for a long period of time.

また、本発明に係るナノオーダー分散型抗菌塗料は、ナノオーダーの分散を行っているため、成膜性が良好で、塗布、スプレー等様々な成膜方法に於いて良好な塗膜を得ることが出来る。また、塗膜の付着強度、塗膜自身の強度、耐候性、耐光性等の特性も良好であった。さらに、重ね塗りにより厚膜を得ることも容易で、様々な用途に対応可能な特性を有している。   In addition, the nano-order dispersion type antibacterial paint according to the present invention has a nano-order dispersion, so that the film formability is good, and a good coating film can be obtained by various film forming methods such as coating and spraying. I can do it. Moreover, the characteristics such as the adhesion strength of the coating film, the strength of the coating film itself, the weather resistance, and the light resistance were also good. Furthermore, it is easy to obtain a thick film by overcoating, and it has characteristics that can be used for various applications.

本発明は、ナノオーダー分散型抗菌塗料及びナノオーダー分散型抗菌塗料の製造方法は、ポットライフが長く、且つ実用的な塗膜形成条件でもって成膜出来、耐久性及び耐光性に於いても実用的な塗膜が得られ、さらに長期に亘って抗菌効果を実現するという利点がある。抗菌性を有する塗料は病院、介護施設、老健施設、食品加工工場、学校、公共施設等、或いは家電製品等の多岐に亘る用途に活用出来、我が国産業の発展に資するものである。   The present invention provides a nano-order dispersive antibacterial paint and a method for producing a nano-order dispersive antibacterial paint, which has a long pot life, can be formed under practical coating film forming conditions, and is durable and light resistant. There is an advantage that a practical coating film can be obtained and an antibacterial effect can be realized over a long period of time. Antibacterial paints can be used in a wide variety of applications such as hospitals, nursing homes, health facilities, food processing factories, schools, public facilities, and home appliances, and contribute to the development of Japanese industries.

1 容器体部
2 撹拌分散用プロペラ
3 高速回転軸
4 低速回転軸
5 真空ポンプ
6 操作盤
DESCRIPTION OF SYMBOLS 1 Container body part 2 Propeller for stirring dispersion 3 High-speed rotating shaft 4 Low-speed rotating shaft 5 Vacuum pump 6 Operation panel

Claims (32)

抗菌塗料に於いて、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とするナノオーダー分散型抗菌塗料。   A nano-order dispersion type antibacterial paint characterized in that the emulsion diameter is adjusted to 10 μm or less by stirring and dispersing while performing degassing under reduced pressure. 抗菌塗料に於いて、該抗菌塗料は抗菌剤として金属或いは金属化合物の微粒子を含み、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項1記載のナノオーダー分散型抗菌塗料。   In the antibacterial paint, the antibacterial paint contains fine particles of a metal or a metal compound as an antibacterial agent, and the emulsion diameter is adjusted to 10 μm or less by stirring and dispersing while performing degassing under reduced pressure. The nano-order dispersion type antibacterial paint according to 1. 抗菌塗料に於いて、該抗菌剤はプラチナ、銀、チタン、酸化銀或いは酸化チタンの微粒子のうち1種又は複数を含み、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項1記載のナノオーダー分散型抗菌塗料。   In the antibacterial paint, the antibacterial agent contains one or more of platinum, silver, titanium, silver oxide or titanium oxide fine particles, and the emulsion diameter is reduced to 10 μm or less by stirring and dispersing while performing degassing under reduced pressure. The nano-order dispersion type antibacterial paint according to claim 1, which is prepared. 抗菌塗料に於いて、該抗菌剤は平均粒径が1〜10nmのプラチナ微粒子であり、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項1記載のナノオーダー分散型抗菌塗料。   In the antibacterial paint, the antibacterial agent is platinum fine particles having an average particle diameter of 1 to 10 nm, and the emulsion diameter is adjusted to 10 μm or less by stirring and dispersing while degassing under reduced pressure. Item 2. The nano-order dispersed antibacterial paint according to item 1. 抗菌塗料に於いて、該抗菌塗料はさらに顔料を含み、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項1記載のナノオーダー分散型抗菌塗料。   2. The nano-order dispersion type according to claim 1, wherein the antibacterial paint further contains a pigment, and the emulsion diameter is adjusted to 10 [mu] m or less by stirring and dispersing while performing degassing under reduced pressure. Antibacterial paint. 該エマルジョン径を5μm以下に調製したことを特徴とする、請求項1乃至5記載のナノオーダー分散型抗菌塗料。   6. The nano-order dispersed antibacterial paint according to claim 1, wherein the emulsion diameter is adjusted to 5 μm or less. 該エマルジョン径を1μm以下に調製したことを特徴とする、請求項1乃至6記載のナノオーダー分散型抗菌塗料。   7. The nano-order dispersed antibacterial paint according to claim 1, wherein the emulsion diameter is adjusted to 1 μm or less. 該エマルジョン径を0.5μm以下に調製したことを特徴とする、請求項1乃至7記載のナノオーダー分散型抗菌塗料。   8. The nano-order dispersed antibacterial paint according to claim 1, wherein the emulsion diameter is adjusted to 0.5 μm or less. 該減圧脱気の圧力が1Pa乃至50000Paであることを特徴とする、請求項1乃至8記載のナノオーダー分散型抗菌塗料。   9. The nano-order dispersed antibacterial paint according to claim 1, wherein the pressure of the vacuum degassing is 1 Pa to 50000 Pa. 該減圧脱気の圧力が1Pa乃至5000Paであることを特徴とする、請求項9記載のナノオーダー分散型抗菌塗料。   The nano-order dispersed antibacterial paint according to claim 9, wherein the pressure of the vacuum degassing is 1 Pa to 5000 Pa. 該減圧脱気の圧力が1Pa乃至500Paであることを特徴とする、請求項10記載のナノオーダー分散型抗菌塗料。   The nano-order dispersed antibacterial paint according to claim 10, wherein the pressure of the vacuum degassing is 1 Pa to 500 Pa. ナノオーダー分散型抗菌塗料であって、塗料組成物原料として合成樹脂エマルジョンおよび/または樹脂を100重量部、抗菌剤を0.1重量部乃至50重量部、水を50重量部乃至200重量部の範囲で混合した塗料組成物原料エマルジョンを用いることを特徴とする、請求項1乃至11記載のナノオーダー分散型抗菌塗料。   A nano-order dispersion type antibacterial paint comprising 100 parts by weight of a synthetic resin emulsion and / or resin as a raw material for a paint composition, 0.1 to 50 parts by weight of an antibacterial agent, and 50 to 200 parts by weight of water The nano-order dispersed antibacterial paint according to any one of claims 1 to 11, wherein a coating composition raw material emulsion mixed in a range is used. 塗料組成物にはさらに増粘剤、分散剤、湿潤剤、消泡剤、抑泡剤、成膜助剤、凍結防止剤、凍結安定剤、防腐剤、沈降防止剤、付着防止剤、乾燥調製剤、或いは熱変換剤・断熱材・遮熱剤などの温度抑制剤、からなる群より選ばれた1種または2種以上の補助剤を含んでなることを特徴とする、請求項1乃至12記載のナノオーダー分散型抗菌塗料。   The coating composition further includes thickeners, dispersants, wetting agents, antifoaming agents, antifoaming agents, film forming aids, antifreezing agents, freezing stabilizers, preservatives, antisettling agents, antiadhesives, and dry-control agents. The composition comprises one or more auxiliary agents selected from the group consisting of a preparation or a temperature inhibitor such as a heat conversion agent, a heat insulating material and a heat shielding agent. The nano-order dispersed antibacterial paint as described. 該撹拌分散は、容器体中で減圧し、プロペラを用いて撹拌することにより行われたことを特徴とする、請求項1乃至15記載のナノオーダー分散型抗菌塗料。   16. The nano-order dispersion type antibacterial paint according to claim 1, wherein the stirring dispersion is performed by reducing the pressure in the container body and stirring with a propeller. 該撹拌分散工程中のプロペラの回転数は200rpm乃至5000rpmの範囲で行われたことを特徴とする、請求項14記載のナノオーダー分散型抗菌塗料。   The nano-order dispersive antibacterial coating material according to claim 14, wherein the rotation speed of the propeller during the stirring and dispersing step is in a range of 200 rpm to 5000 rpm. 該エマルジョンに用いる樹脂をワックスエステルに変更することにより、ワックスとして使用可能であることを特徴とする、請求項1乃至15記載のナノオーダー分散型抗菌塗料。   16. The nano-order dispersed antibacterial paint according to claim 1, which can be used as a wax by changing the resin used in the emulsion to a wax ester. 抗菌塗料の製造方法に於いて、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とするナノオーダー分散型抗菌塗料の製造方法。   In the method for producing an antibacterial paint, a method for producing a nano-order dispersive antibacterial paint characterized in that the emulsion diameter is adjusted to 10 μm or less by stirring and dispersing while performing degassing under reduced pressure. 抗菌塗料の製造方法に於いて、該抗菌塗料は抗菌剤として金属或いは金属化合物の微粒子を含み、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項17記載のナノオーダー分散型抗菌塗料の製造方法。   In the method for producing an antibacterial paint, the antibacterial paint contains fine particles of a metal or a metal compound as an antibacterial agent, and the emulsion diameter is adjusted to 10 μm or less by stirring and dispersing while performing degassing under reduced pressure. A method for producing a nano-order dispersed antibacterial paint according to claim 17. 抗菌塗料の製造方法に於いて、該抗菌剤はプラチナ、銀、チタン、酸化銀或いは酸化チタンの微粒子のうち1種又は複数を含み、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項17記載のナノオーダー分散型抗菌塗料の製造方法。   In the method for producing an antibacterial paint, the antibacterial agent contains one or more fine particles of platinum, silver, titanium, silver oxide or titanium oxide, and the emulsion diameter is reduced by stirring and dispersing while performing vacuum degassing. The method for producing a nano-order dispersed antibacterial paint according to claim 17, wherein the nano-order dispersed antibacterial paint is prepared to have a thickness of 10 µm or less. 抗菌塗料の製造方法に於いて、該抗菌剤は平均粒径が1〜10nmのプラチナ微粒子であり、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項17記載のナノオーダー分散型抗菌塗料の製造方法。   In the method for producing an antibacterial paint, the antibacterial agent is platinum fine particles having an average particle diameter of 1 to 10 nm, and the emulsion diameter is adjusted to 10 μm or less by stirring and dispersing while performing vacuum degassing. The method for producing a nano-order dispersed antibacterial paint according to claim 17. 抗菌塗料の製造方法に於いて、該抗菌塗料はさらに顔料を含み、減圧脱気を行いながら撹拌分散を行うことによりエマルジョン径を10μm以下に調製したことを特徴とする、請求項17記載のナノオーダー分散型抗菌塗料の製造方法。   18. The method according to claim 17, wherein the antibacterial paint further contains a pigment, and the emulsion diameter is adjusted to 10 μm or less by stirring and dispersing while performing degassing under reduced pressure. Manufacturing method of order-dispersed antibacterial paint. 該エマルジョン径を5μm以下に調製したことを特徴とする、請求項17乃至21記載のナノオーダー分散型抗菌塗料の製造方法。   The method for producing a nano-order dispersed antibacterial paint according to any one of claims 17 to 21, wherein the emulsion diameter is adjusted to 5 µm or less. 該エマルジョン径を1μm以下に調製したことを特徴とする、請求項17乃至22記載のナノオーダー分散型抗菌塗料の製造方法。   23. The method for producing a nano-order dispersed antibacterial paint according to claim 17, wherein the emulsion diameter is adjusted to 1 μm or less. 該エマルジョン径を0.5μm以下に調製したことを特徴とする、請求項17乃至23記載のナノオーダー分散型抗菌塗料の製造方法。   24. The method for producing a nano-order dispersed antibacterial paint according to claim 17, wherein the emulsion diameter is adjusted to 0.5 [mu] m or less. 該減圧脱気の圧力が1Pa乃至50000Paであることを特徴とする、請求項17乃至24記載のナノオーダー分散型抗菌塗料の製造方法。   25. The method for producing a nano-order dispersed antibacterial paint according to claim 17, wherein the pressure of the vacuum degassing is 1 Pa to 50000 Pa. 該減圧脱気の圧力が1Pa乃至5000Paであることを特徴とする、請求項25記載のナノオーダー分散型抗菌塗料の製造方法。   The method for producing a nano-order dispersed antibacterial paint according to claim 25, wherein the pressure of the vacuum degassing is 1 Pa to 5000 Pa. 該減圧脱気の圧力が1Pa乃至500Paであることを特徴とする、請求項26記載のナノオーダー分散型抗菌塗料の製造方法。   27. The method for producing a nano-order dispersed antibacterial paint according to claim 26, wherein the pressure of the vacuum degassing is 1 Pa to 500 Pa. ナノオーダー分散型抗菌塗料の製造方法であって、塗料組成物原料として合成樹脂エマルジョンおよび/または樹脂を100重量部、抗菌剤を0.1重量部乃至50重量部、水および/または溶媒を50重量部乃至200重量部の範囲で混合した塗料組成物原料エマルジョンを用いることを特徴とする、請求項17乃至27記載のナノオーダー分散型抗菌塗料の製造方法。   A method for producing a nano-order dispersion type antibacterial paint, comprising 100 parts by weight of a synthetic resin emulsion and / or resin as a raw material for a paint composition, 0.1 to 50 parts by weight of an antibacterial agent, and 50 of water and / or solvent. 28. The method for producing a nano-order dispersed antibacterial coating material according to claim 17 or 27, wherein the coating composition raw material emulsion mixed in the range of parts by weight to 200 parts by weight is used. 塗料組成物にはさらに増粘剤、分散剤、湿潤剤、消泡剤、抑泡剤、成膜助剤、凍結防止剤、凍結安定剤、防腐剤、沈降防止剤、付着防止剤、乾燥調製剤、或いは熱変換剤・断熱材・遮熱剤などの温度抑制剤、からなる群より選ばれた1種または2種以上の補助剤を含んでなることを特徴とする、請求項17乃至28記載のナノオーダー分散型抗菌塗料の製造方法。   The coating composition further includes thickeners, dispersants, wetting agents, antifoaming agents, antifoaming agents, film forming aids, antifreezing agents, freezing stabilizers, preservatives, antisettling agents, antiadhesives, and dry-control agents. 29. The composition according to claim 17, comprising one or more adjuvants selected from the group consisting of a preparation, or a temperature inhibitor such as a heat conversion agent, a heat insulating material, and a heat shielding agent. A method for producing the nano-order dispersed antibacterial paint as described. 該撹拌分散は、容器体中で減圧し、プロペラを用いて撹拌することにより行われたことを特徴とする、請求項17乃至29記載のナノオーダー分散型抗菌塗料の製造方法。   30. The method for producing a nano-order dispersion type antibacterial paint according to claim 17, wherein the stirring and dispersing is performed by reducing the pressure in the container body and stirring with a propeller. 該撹拌分散工程中のプロペラの回転数は200rpm乃至5000rpmの範囲で行われたことを特徴とする、請求項30記載のナノオーダー分散型抗菌塗料の製造方法。   The method for producing a nano-order dispersive antibacterial paint according to claim 30, wherein the rotation speed of the propeller during the stirring and dispersing step is in the range of 200 rpm to 5000 rpm. 該エマルジョンに用いる樹脂をワックスエステルに変更することにより、ワックスとして使用可能であることを特徴とする、請求項17乃至31記載のナノオーダー分散型抗菌塗料の製造方法。   32. The method for producing a nano-order dispersed antibacterial paint according to claim 17, wherein the resin used for the emulsion can be used as a wax by changing to a wax ester.
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