JP4601977B2 - Method for curing coating film comprising photocurable coating composition, coating film formed by the method, and substrate coated with the coating film - Google Patents
Method for curing coating film comprising photocurable coating composition, coating film formed by the method, and substrate coated with the coating film Download PDFInfo
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- JP4601977B2 JP4601977B2 JP2004062271A JP2004062271A JP4601977B2 JP 4601977 B2 JP4601977 B2 JP 4601977B2 JP 2004062271 A JP2004062271 A JP 2004062271A JP 2004062271 A JP2004062271 A JP 2004062271A JP 4601977 B2 JP4601977 B2 JP 4601977B2
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- 239000003999 initiator Substances 0.000 claims description 29
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- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims description 6
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 5
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Description
本発明は、光硬化性塗料組成物からなる塗膜の硬化方法、その方法で形成された塗膜およびその塗膜で被覆された基材に関し、さらに詳しくは、用いられる光硬化性塗料組成物中の光重合開始剤の配合量をより低減しても、硬度、耐薬品性、耐汚染性、耐干割れ性に優れ、塗膜の低臭気性に優れ、低光沢の硬化塗膜が得られるような、光硬化性塗料組成物からなる塗膜の硬化方法、その方法で形成された塗膜およびその塗膜で被覆された基材に関する。 The present invention relates to a method for curing a coating film comprising a photocurable coating composition, a coating film formed by the method, and a substrate coated with the coating film, and more particularly, the photocurable coating composition used. Even if the photopolymerization initiator content is further reduced, it has excellent hardness, chemical resistance, stain resistance, and anti-cracking property, excellent low odor of the coating, and low gloss cured film. The present invention relates to a method for curing a coating film comprising a photocurable coating composition, a coating film formed by the method, and a substrate coated with the coating film.
従来では、木質基材等の表面に塗布された光硬化性塗料組成物の硬化方法としては、200〜600nm程度の波長の光を発する光源である、超高圧または高圧水銀灯、メタルハライドランプ、紫外線蛍光ランプ(ケミカルランプ)、キセノンランプ、太陽光等を使用したUV硬化法などが広く採用され、例えば、数十秒〜0.1秒程度の短時間のUV照射で硬化させている(例えば、特開2001−340799号公報、特開2003−171
459号公報、特開2003−290707号公報、特開平07−171491号公報等)。
Conventionally, as a curing method for a photocurable coating composition applied to the surface of a wooden substrate or the like, an ultrahigh pressure or high pressure mercury lamp, a metal halide lamp, or an ultraviolet fluorescent light source that emits light having a wavelength of about 200 to 600 nm. A UV curing method using a lamp (chemical lamp), a xenon lamp, sunlight or the like is widely adopted, and is cured by, for example, a short UV irradiation of about several tens of seconds to 0.1 seconds (for example, special JP 2001-340799 A, JP 2003-171 A
No. 459, JP-A No. 2003-290707, JP-A No. 07-171491, etc.).
しかしながら、これまでの通常の高圧水銀灯などを使用したUV硬化法の場合には、得られる硬化塗膜の硬度、耐薬品性、耐汚染性、耐干割れ性の点、さらには、光重合開始剤の使用量、塗膜の低臭気性の点などでさらなる改良の余地があった。 However, in the case of the conventional UV curing method using a high-pressure mercury lamp etc., the hardness, chemical resistance, stain resistance, and dry crack resistance of the resulting cured coating film, and further photopolymerization starts There was room for further improvement in terms of the amount of the agent used and the low odor of the coating film.
そこで、本発明者らは、鋭意研究を重ねたところ、特定のUVランプである無電極UVランプを使用すると、通常の高圧水銀灯を使用する場合に比べて、塗膜硬度、耐薬品性、耐汚染性、耐干割れ性等の塗膜性能が優れ、光重合開始剤の使用量を低減でき、塗膜の低臭気性に優れるなど、上記問題点を一挙に解決しうることなどを見出した。しかしながら木質基材の仕上げにおいては、低光沢の製品が需要の大半を占めているのに対して、無電極UVランプのみによる硬化では光沢が増し、低光沢化が困難である。 Therefore, the present inventors have conducted extensive research and found that when an electrodeless UV lamp, which is a specific UV lamp, is used, compared with the case of using a normal high-pressure mercury lamp, the coating film hardness, chemical resistance, It has been found that the above problems can be solved at once, such as excellent coating performance such as contamination and dry cracking resistance, reducing the amount of photopolymerization initiator used, and excellent low odor of the coating. . However, in finishing wood substrates, low gloss products occupy most of the demand, but when only electrodeless UV lamps are cured, gloss increases and low gloss is difficult.
そこで、さらに鋭意研究を重ねた結果、無電極UVランプによる完全硬化に先立ち、予め、高圧水銀ランプまたはメタルハライドランプを照射してセミキュア(半硬化)を施しておくと、その後無電極UVランプ照射による完全硬化を行った場合に、塗膜の低光沢化が可能であることなどを見出して、本発明を完成するに至った。
本発明は、上記のような従来技術に伴う問題点を解決しようとするものであって、硬度、耐薬品性、耐汚染性、耐干割れ性等の性能がより優れ、塗膜の低臭気性に優れた低光沢の硬化塗膜が得られるような、光硬化性塗料組成物からなる塗膜の硬化方法、その方法で形成された塗膜およびその塗膜で被覆された基材を提供することを目的としている。 The present invention is intended to solve the problems associated with the prior art as described above, and has better performance such as hardness, chemical resistance, stain resistance, and resistance to dry cracking, and low odor of the coating film. A coating method comprising a photocurable coating composition, a coating film formed by the method, and a substrate coated with the coating film so that a low-gloss cured coating film having excellent properties can be obtained. The purpose is to do.
本発明では、木質基材上に、(A)光硬化性樹脂と、(B)光重合開始剤と、(C)体質
顔料とを含む光硬化性塗料組成物を塗布し、高圧水銀灯またはメタルハライドランプでセミキュア(半硬化)させた後に、無電極UVランプを照射することにより完全硬化させることを特徴としている。
In the present invention, a photocurable coating composition containing (A) a photocurable resin, (B) a photopolymerization initiator, and (C) an extender pigment is applied onto a wooden substrate, and then a high pressure mercury lamp or a metal halide is applied. It is characterized by being completely cured by irradiating an electrodeless UV lamp after semi-curing (semi-curing) with a lamp.
本発明では、上記光硬化性樹脂(A)が、光重合性の(メタ)アクリロイル基を有するアクリル樹脂、ウレタンアクリレート、エポキシアクリレート、ポリエステルアクリレートからなる群から選ばれた少なくとも1種の光硬化性樹脂であることが好ましい。 In the present invention, the photocurable resin (A) is at least one photocurable resin selected from the group consisting of an acrylic resin having a photopolymerizable (meth) acryloyl group, urethane acrylate, epoxy acrylate, and polyester acrylate. A resin is preferred.
本発明では、上記光重合開始剤(B)がベンゾフェノン類、アントラキノン類、チオキサントン類、アセトフェノン類、アシルフォスフィンオキサイド類、メチルフェニルグリオキシエステル類からなる群から選ばれた光重合開始剤であることが好ましい。 In the present invention, the photopolymerization initiator (B) is a photopolymerization initiator selected from the group consisting of benzophenones, anthraquinones, thioxanthones, acetophenones, acylphosphine oxides, and methylphenylglyoxyesters. It is preferable.
本発明では、上記体質顔料(C)が、シリカ(SiO2)、タルク[Mg3(Si4O10)(OH)2]、沈降性硫酸バリウム(BaSO4)、炭酸バリウム(BaCO3)、炭酸カ
ルシウム(CaCO3)、アルミナ白(Al2(OH)3)、沈降性炭酸マグネシウム[M
gCO3・3Mg(OH)2・H2O]、ポリエチレンワックス、ビーズ顔料など、それ自
体屈折率が低く、隠蔽性(顔料、塗料などが黒白の下地を完全に覆い隠す性質をいう。)に関係ないが光沢を低下させるために用いられる白色顔料からなる群から選ばれた1種又は2種以上の体質顔料であることが好ましい。
In the present invention, the extender pigment (C) is silica (SiO 2 ), talc [Mg 3 (Si 4 O 10 ) (OH) 2 ], precipitated barium sulfate (BaSO 4 ), barium carbonate (BaCO 3 ), Calcium carbonate (CaCO 3 ), alumina white (Al 2 (OH) 3 ), precipitated magnesium carbonate [M
gCO 3 .3Mg (OH) 2 .H 2 O], polyethylene wax, bead pigments, etc., have a low refractive index per se, and have a concealing property (the property that the pigment, paint, etc. completely covers the black and white base). Although it does not matter, it is preferably one or more extender pigments selected from the group consisting of white pigments used for reducing gloss.
本発明では、上記光硬化性樹脂(A)100重量部に対して、光重合開始剤(B)を1〜15重量部の範囲で、また体質顔料(C)を1〜30重量部の範囲で使用することが好
ましい。
In the present invention, the photopolymerization initiator (B) is in the range of 1 to 15 parts by weight and the extender pigment (C) is in the range of 1 to 30 parts by weight with respect to 100 parts by weight of the photocurable resin (A). Is preferably used.
本発明では、木質基材上に、予め、シーラー塗膜、下塗り塗膜、中塗り塗膜のいずれか1種以上がその順序で形成されており、それらの塗膜のうちの最外層の塗膜上に、上記光硬化性塗料組成物を塗布し、高圧水銀灯またはメタルハライドランプでセミキュア(半硬化)させた後に、無電極UVランプを照射し完全硬化させることが好ましい。 In the present invention, one or more of a sealer coating, an undercoat coating, and an intermediate coating are formed in that order in advance on a wooden substrate, and the outermost layer of these coatings is applied. It is preferable that the photocurable coating composition is applied onto the film and semi-cured (semi-cured) with a high-pressure mercury lamp or a metal halide lamp, and then irradiated with an electrodeless UV lamp to be completely cured.
本発明では、上記完全硬化用の無電極UVランプの照射は、1本または2本以上の無電極ランプをコンベア上に所定距離離間して配設しておき、上記光硬化性塗料組成物が塗布された木質基材をコンベアに1〜150m/分の速度で搬送させることにより行うことが
好ましい。
In the present invention, the irradiation of the electrodeless UV lamp for complete curing is performed by placing one or more electrodeless lamps on a conveyor at a predetermined distance, and the photocurable coating composition is It is preferable to carry out by applying the coated wood base material to a conveyor at a speed of 1 to 150 m / min.
本発明では、光硬化性塗料組成物が塗布された木質基材に、1本当たり、24〜240W/cmの出力を有する無電極UVランプを、積算光量が100〜3000mJ/cm2
となる量で照射し、光硬化性塗料組成物からなるセミキュア(半硬化)の塗膜を完全硬化させることが好ましい。
In the present invention, an electrodeless UV lamp having an output of 24 to 240 W / cm per unit is applied to a wood base material coated with a photocurable coating composition, and the integrated light quantity is 100 to 3000 mJ / cm 2.
It is preferable to completely cure a semi-cured ( semi-cured ) coating film made of a photocurable coating composition.
本発明では、木質基材上に、予め、シーラー塗膜、下塗り塗膜、中塗り塗膜のいずれか1種以上がその順序で塗布され、かつ、高圧水銀ランプまたはメタルハライドランプの照
射が施されており、それらの塗膜のうちの最外層の塗膜上に、上記光硬化性塗料組成物を塗布し、高圧水銀ランプまたはメタルハライドランプでセミキュア(半硬化)させた後に、無電極UVランプを照射して完全硬化させることが好ましい。
In the present invention, on the wooden substrate, at least one of a sealer coating, an undercoat coating, and an intermediate coating is applied in that order in advance, and irradiation with a high-pressure mercury lamp or a metal halide lamp is performed. The above-mentioned photo-curable coating composition is applied onto the outermost coating film of these coating films, semi-cured (semi-cured) with a high-pressure mercury lamp or metal halide lamp, and then an electrodeless UV lamp is used. It is preferable to completely cure by irradiation.
本発明に係る光硬化塗膜は、上記のいずれかに記載された方法で形成された光硬化塗膜であることが好ましい。
本発明に係る塗膜付き基材は、上記のいずれかに記載された方法で形成された光硬化塗膜にて木質基材の表面が被覆されていることを特徴としている。
The photocured coating film according to the present invention is preferably a photocured coating film formed by any of the methods described above.
The base material with a coating film according to the present invention is characterized in that the surface of the wooden base material is coated with a photocured coating film formed by any of the methods described above.
本発明においては、光硬化性塗料組成物の硬化に際して、通常の高圧水銀灯、メタルハライドランプに代えて、高圧水銀ランプ、メタルハライドランプでセミキュア(半硬化)させた後に、無電極UVランプを照射して完全硬化させており、硬度、耐薬品性、耐汚染性、耐干割れ性等の性能に著しく優れ、低光沢が可能で、しかも光硬化性塗料組成物中に配合される光重合開始剤の使用量を低減でき、塗膜の低臭気性にも優れた硬化塗膜が得られる。 In the present invention, when the photocurable coating composition is cured, instead of a normal high-pressure mercury lamp or metal halide lamp, it is semi-cured (semi-cured) with a high-pressure mercury lamp or metal halide lamp and then irradiated with an electrodeless UV lamp. The photopolymerization initiator is completely cured, has excellent properties such as hardness, chemical resistance, stain resistance, and anti-cracking properties, is capable of low gloss, and is incorporated into the photocurable coating composition. A use amount can be reduced and the cured coating film excellent in the low odor property of the coating film is obtained.
また本発明によれば、上記の方法で形成された上記特性の塗膜、およびその塗膜で被覆された基材である上記特性の塗膜付き基材が提供される。 Moreover, according to this invention, the coating-material base material of the said characteristic which is a coating film of the said characteristic formed by said method and the base material coat | covered with the coating film is provided.
以下、本発明に係る光硬化性塗料組成物からなる塗膜の硬化方法、その方法で形成された塗膜およびその塗膜で被覆された基材について具体的に説明する。
<光硬化性塗料組成物からなる塗膜の硬化方法>
本発明に係る光硬化性塗料組成物からなる塗膜の硬化方法では、木質基材上に、(A)光硬化性樹脂と、(B)光重合開始剤と、(C)体質顔料とを含む光硬化性塗料組成物を塗布し、その未硬化塗膜表面に、高圧水銀ランプ、メタルハライドランプなどを照射してセミキュア(半硬化)させた後に、無電極UVランプを照射して完全硬化(本硬化)させている。
Hereinafter, a method for curing a coating film comprising the photocurable coating composition according to the present invention, a coating film formed by the method, and a substrate coated with the coating film will be specifically described.
<Curing method of coating film comprising photocurable coating composition>
In the method for curing a coating film comprising the photocurable coating composition according to the present invention, on a wooden substrate, (A) a photocurable resin, (B) a photopolymerization initiator, and (C) an extender pigment. After the photocurable coating composition is applied, the surface of the uncured coating film is irradiated with a high-pressure mercury lamp, metal halide lamp, etc., and semi-cured (semi-cured), and then irradiated with an electrodeless UV lamp to completely cure ( (Main curing).
この光硬化性塗料組成物としては、溶剤型、無溶剤の何れも使用できるが、本発明では無溶剤型塗料の方が硬化反応を迅速に進行させることができる、塗装作業性に優れ、環境汚染の恐れが少なく環境への対応の点でも優れるなどの点で望ましい。 As the photo-curable coating composition, either solvent-based or solvent-free can be used, but in the present invention, the solvent-free coating can accelerate the curing reaction, has excellent coating workability, and is environmentally friendly. It is desirable in that it has less fear of contamination and is excellent in terms of environmental response.
なお、本発明では、木質基材の表面に光硬化性塗料組成物を塗布し硬化させるに先立ち、予め、シーラー塗膜、下塗り塗膜、中塗り塗膜のいずれかを必要によりこの順序で施し、それらの塗膜の最外層上に、上記光硬化性塗料組成物を塗布し、上記のように半硬化させた後、無電極UVランプを照射し完全硬化させることが好ましい。これらシーラー塗膜、下塗り塗膜、中塗り塗膜等の硬化は、高圧水銀灯、メタルハライドランプ、無電極UVランプの何れを用いて行ってもよいが、高圧水銀灯、メタルハライドランプが好ましい。 In the present invention, prior to applying and curing the photocurable coating composition on the surface of the wooden substrate, any one of a sealer coating, an undercoat coating and an intermediate coating is applied in this order as necessary. It is preferable to apply the photo-curable coating composition on the outermost layer of these coating films, and after semi-curing as described above, irradiating with an electrodeless UV lamp and completely curing. Curing of these sealer coating, undercoat coating, intermediate coating, etc. may be carried out using any of a high pressure mercury lamp, a metal halide lamp and an electrodeless UV lamp, but a high pressure mercury lamp and a metal halide lamp are preferred.
このシーラー塗膜用塗料(シーラー)、下塗り塗膜用塗料(下塗塗料)、中塗り塗膜用塗料(中塗り塗料)としては、溶剤型、無溶剤の何れも使用できるが、本発明ではこれらは何れも無溶剤型であることが硬化反応が迅速に進行できる、塗装作業性や環境への対応に優れるなどの点で望ましい。 As the coating material for sealer coating film (sealer), coating material for undercoat coating film (undercoating coating material), and coating material for intermediate coating film (intermediate coating coating material), any of solvent type and solventless can be used. It is desirable that all of these are solvent-free in view of the fact that the curing reaction can proceed rapidly, the coating workability and the response to the environment are excellent.
本発明では、最外層となる光硬化性塗料組成物層の半硬化を行うことにより、半硬化塗膜中に含まれる体質顔料を配向させ、「JIS―K−5600の鏡面光沢度の測定法に準拠し、入射角60度にて測定した値」が30以下、好ましくは10〜30にしている。
<無電極UVランプ照射>
本発明で用いられる無電極UVランプは、マグネトロンにて発生させたマイクロ波(例:2450MHz)のエネルギーにより、ランプ内部の水銀などの発光物質を励起してプラズマ状態とし、マイクロ波を光エネルギーに転換する方式で発光し、従来の高圧水銀灯と異なりランプの内部に電極をもたない。
In the present invention, the extender pigment contained in the semi-cured coating film is oriented by semi-curing the photo-curable coating composition layer that is the outermost layer, and the method for measuring the specular gloss of JIS-K-5600 The value measured at an incident angle of 60 degrees ”is 30 or less, preferably 10-30.
<Electrodeless UV lamp irradiation>
The electrodeless UV lamp used in the present invention excites a light-emitting substance such as mercury inside the lamp into a plasma state by the energy of a microwave (eg, 2450 MHz) generated by a magnetron, and converts the microwave into light energy. Unlike conventional high-pressure mercury lamps, it does not have electrodes inside the lamp.
無電極UVランプとしては、上市されているものとしては、好適には、「Fusion
UV systems JAPAN KK」社製の「MODEL VSP/I600」
(光源部最大出力:240W/cm)、「VSP/I250」(光源部最大出力:150
W/cm)などが挙げられ、より具体的には、図1に示すように、例えば、水銀スペクト
ルと同様に、200〜280nm域及び365nm付近に強い発光ピークをもつ「Hバルブ」、「Hバルブ」に比べ短波長域(200〜280nm)の発光出力が平均15%程度アップした「Hプラスバルブ」、350〜400nm域に特に強い発光ピークをもつバルブで、UV到達深度がより大きく、UV硬化に適した「Dバルブ」、420nm域を中心に405〜425nm域に強い発光ピークをもつバルブで、酸化チタンを含んだホワイトベースコートなどの厚膜塗料やラミネート材料のUV硬化に適した「Vバルブ」、Vバルブよりもやや長波長域の400〜460nmに強い発光ピークを持つ「Qバルブ」、365〜369nm域及び406nm付近に発光ピーク出力をもち、耐候性が要求される外装コーティングなどの硬化に適した「Mバルブ」が挙げられる。
As an electrodeless UV lamp, it is preferable that "Fusion"
“MODEL VSP / I600” manufactured by “UV systems JAPAN KK”
(Light source unit maximum output: 240 W / cm), “VSP / I250” (light source unit maximum output: 150
More specifically, as shown in FIG. 1, for example, as in the case of the mercury spectrum, “H bulb”, “H bulb”, and “H” having strong emission peaks in the 200 to 280 nm region and around 365 nm. Compared to the “bulb”, the “H plus bulb” has an emission output in the short wavelength range (200 to 280 nm) that is increased by about 15% on average. The bulb has a particularly strong emission peak in the 350 to 400 nm range. "D bulb" suitable for curing, bulb with strong emission peak in the range of 405 to 425 nm centering around 420 nm, suitable for UV curing of thick film paints such as white base coat containing titanium oxide and laminate materials “Bulb”, “Q bulb” having a strong emission peak at 400 to 460 nm, which is slightly longer than the V bulb, 365 to 369 nm, and 406 n Examples thereof include “M bulb” which has an emission peak output in the vicinity of m and is suitable for curing an exterior coating or the like which requires weather resistance.
バルブ(ランプ)の選択にあたっては、用いられる光硬化性塗料組成物の種類、硬化条件、塗膜厚、素材の種類等を考慮して、好適な発光スペクトルのバルブを選択すればよい。 In selecting a bulb (lamp), a bulb having a suitable emission spectrum may be selected in consideration of the type of photocurable coating composition to be used, curing conditions, coating thickness, type of material, and the like.
本発明では、用途、光硬化性塗料組成物の種類、硬化条件、塗膜厚などを考慮すると、これらのバルブのうちでは、200〜280nm域及び365nm付近に強い発光ピークを持つ「Hバルブ」および「Hプラスバルブ」が、最外層の光硬化性塗料組成物を硬化させる上で、他のバルブに比して、使用する光重合開始剤の種類及び塗膜表面の硬化性能の点で好ましい。 In the present invention, considering the application, the type of the photocurable coating composition, the curing conditions, the coating thickness, etc., among these valves, “H bulb” having a strong emission peak in the 200 to 280 nm region and around 365 nm. And “H plus valve” are preferable in terms of the type of photopolymerization initiator used and the curing performance of the coating film surface, compared with other valves, in curing the photocurable coating composition of the outermost layer. .
なお、高圧水銀灯は、一度ランプの電源を切ってしまうと再起動に時間がかかるが、無電極UVランプは容易に再起動可能であり、作業時間のロスを低減可能である。
このような無電極UVランプを用いた未硬化光硬化性塗料組成物塗膜の硬化処理(本硬化、完全硬化)は、例えば、240W出力の上記フュージョンUVシステムズ社製のH型、D型などの無電極UVランプを1〜複数本使用する場合には、木質基材表面に塗布された未硬化光硬化性塗料組成物塗膜表面から該ランプを5〜10cm程度離間させて配置し、1〜150m/分(例:10m/分)程度の速度で木質基材をベルトコンベア等にて搬送させて行えばよい。
The high pressure mercury lamp takes a long time to restart once the lamp is turned off, but the electrodeless UV lamp can be easily restarted, and the loss of working time can be reduced.
The curing treatment (main curing, complete curing) of the uncured photocurable coating composition coating film using such an electrodeless UV lamp is, for example, H-type, D-type, etc., manufactured by Fusion UV Systems, Inc. with 240 W output. In the case of using one or more electrodeless UV lamps, the lamps are arranged at a distance of about 5 to 10 cm from the surface of the uncured photocurable coating composition applied to the surface of the wooden substrate. What is necessary is just to convey a wooden base material with a belt conveyor etc. at a speed | rate of about -150m / min (example: 10m / min).
なお、1本当たり、24〜240W/cmの出力を有する無電極UVランプでは、積算光量が100〜3000mJ/cm2となる量で光硬化性塗料組成物が塗布された木質基
材に照射し、セミキュア(半硬化)の塗膜を完全硬化させればよい。
In the case of an electrodeless UV lamp having an output of 24 to 240 W / cm per lamp, the wood substrate to which the photocurable coating composition is applied is irradiated in an amount such that the integrated light quantity is 100 to 3000 mJ / cm 2. A semi-cure ( semi-cured ) coating film may be completely cured.
本発明では、木質基材上に、光硬化性塗料組成物を塗布し、高圧水銀灯(波長254〜560nm)、メタルハライドランプ(波長:254〜560nm)、などで「セミキュア(半硬化)」させた後に、無電極UVランプを照射し「完全硬化(本硬化)」させることが、硬化塗膜の低光沢、低臭気性、硬化の程度、耐擦傷性、耐汚染性、耐薬品性、耐干割れ性の点からより好ましい。 In the present invention, a photocurable coating composition is applied onto a wooden substrate, and is “semi-cured (semi-cured)” with a high-pressure mercury lamp (wavelength: 254 to 560 nm), a metal halide lamp (wavelength: 254 to 560 nm), or the like. Later, by irradiating an electrodeless UV lamp to “completely cure (main cure)”, the cured coating has low gloss, low odor, degree of cure, scratch resistance, stain resistance, chemical resistance, drought resistance More preferable from the viewpoint of cracking property.
なお、セミキュア(半硬化)条件と、本硬化(完全硬化)条件の相違点は、下記の通り。
セミキュア(半硬化)状態とは、本願出願人が先に提案した特開2002−361173号公報の「0012」欄にも規定したように、塗料が硬化しはじめているが完全には硬化していない状態をいい、アセトン抽出ゲル分率では、10重量%以上90重量%未満であり、好ましくは、10〜60重量%、さらに好ましくは20〜50重量%の状態である。また完全硬化では、半硬化状態を脱してアセトン抽出ゲル分率が、90重量%以上である。
The difference between the semi-cure (semi-curing) condition and the main curing (complete curing) condition is as follows.
The semi-cured (semi-cured) state means that the paint has begun to harden but has not completely hardened as defined in the “0012” column of Japanese Patent Laid-Open No. 2002-361173 previously proposed by the applicant of the present application. refers to the state, the acetone extraction gel fraction is less than 1 0% by weight to 90% by weight, preferably 10 to 60 wt%, more preferably in the state of 20 to 50 wt%. In complete curing, the semi-cured state is removed and the acetone extraction gel fraction is 90% by weight or more.
ところで、本発明では、低光沢の塗膜が効率よく得られているが、これは、下記のような理由に拠ると考えられる。
すなわち、無電極UVランプは高出力であり、瞬時に未硬化塗膜は硬化する傾向が強い
ため、塗膜表面の酸素阻害の影響が少ないので得られた硬化塗膜の表面特性が優れている反面、体質顔料を増量しても、配向性が悪く塗膜の低光沢化が比較的困難である。
By the way, in the present invention, a low-gloss coating is efficiently obtained, which is considered to be due to the following reasons.
That is, the electrodeless UV lamp has a high output, and the uncured coating film has a strong tendency to be cured instantaneously. Therefore, the surface characteristics of the obtained cured coating film are excellent because the influence of oxygen inhibition on the coating film surface is small. On the other hand, even if the amount of extender pigment is increased, the orientation is poor and it is relatively difficult to reduce the gloss of the coating film.
そこで、無電極UVランプで硬化した塗膜の長所を損なわない程度に、予め、高圧水銀灯、メタルハライドランプなどでのセミキュア(半硬化)工程を取入れて実施することにより、塗膜表面の体質顔料の配向が良好になり、所望の低光沢の塗膜が得られている。
<光硬化性塗料組成物>
本発明では、上記光硬化性塗料組成物には、光硬化性樹脂(A)と光重合開始剤(B)と、体質顔料(C)とが含まれるが、これらのうち光硬化性樹脂(A)としては、電磁波中の紫外領域(200〜600nm、好ましくは200〜400nm)を利用して硬化する樹脂であり、(メタ)アクリロイル基、ビニル基、不飽和ジカルボン酸エステル等の活性二重結合を有するもののラジカル重合、エポキシ基を有するもののカチオン重合、チオール基と二重結合基の付加反応などを利用して硬化するものが挙げられる。
Therefore, by incorporating a semi-cure (semi-curing) process with a high-pressure mercury lamp, metal halide lamp, etc. in advance so as not to impair the advantages of the coating film cured with an electrodeless UV lamp, The orientation is good and a desired low gloss coating is obtained.
<Photocurable coating composition>
In the present invention, the photocurable coating composition contains a photocurable resin (A), a photopolymerization initiator (B), and an extender pigment (C). Among these, a photocurable resin ( A) is a resin that cures using an ultraviolet region (200 to 600 nm, preferably 200 to 400 nm) in an electromagnetic wave, and is an active double compound such as a (meth) acryloyl group, a vinyl group, or an unsaturated dicarboxylic acid ester. Examples include radical polymerization of those having a bond, cationic polymerization of those having an epoxy group, and curing using an addition reaction between a thiol group and a double bond group.
通常、このような樹脂(A)と光励起し易い光重合開始剤(B)とを組合わせて用い、紫外線により開始剤の開裂や水素移動でラジカルやカチオンの活性種を生成させる。この活性種が樹脂に作用して、重合または架橋反応が起こり、極短時間に硬化する。 Usually, such a resin (A) and a photopolymerization initiator (B) that is easily photoexcited are used in combination, and radical or cation active species are generated by cleavage of the initiator or hydrogen transfer with ultraviolet rays. This active species acts on the resin to cause polymerization or cross-linking reaction, and cures in an extremely short time.
本発明では上記光硬化性樹脂(A)としては、光重合性の二重結合(C=C)である(メタ)アクリロイル基を有するものが好適に用いられ、光重合性のアクリル樹脂、ウレタンアクリレート、エポキシアクリレート、ポリエステルアクリレートがより好ましく、これらの光硬化性樹脂は1種または2種以上組合わせて用いられる。 In the present invention, as the photocurable resin (A), those having a (meth) acryloyl group which is a photopolymerizable double bond (C = C) are preferably used, and a photopolymerizable acrylic resin or urethane is used. An acrylate, an epoxy acrylate, and a polyester acrylate are more preferable, and these photocurable resins are used alone or in combination.
光重合開始剤(B)としては、ベンゾフェノン類、アントラキノン類、チオキサントン類、アセトフェノン類、アシルフォスフィンオキサイド類、メチルフェニルグリオキシエステル類が挙げられる。 Examples of the photopolymerization initiator (B) include benzophenones, anthraquinones, thioxanthones, acetophenones, acylphosphine oxides, and methylphenylglyoxyesters.
体質顔料(C)としては、シリカ(SiO2)、タルク[Mg3(Si4O10)(OH)2
]、沈降性硫酸バリウム(BaSO4)、炭酸バリウム(BaCO3)、炭酸カルシウム(CaCO3)、アルミナ白(Al2(OH)3)、沈降性炭酸マグネシウム[MgCO3・3Mg(OH)2・H2O]、ポリエチレンワックス、ビーズ顔料などの白色顔料が挙げられる。
The extender pigment (C) includes silica (SiO 2 ) and talc [Mg 3 (Si 4 O 10 ) (OH) 2.
], Precipitated barium sulfate (BaSO 4 ), barium carbonate (BaCO 3 ), calcium carbonate (CaCO 3 ), alumina white (Al 2 (OH) 3 ), precipitated magnesium carbonate [MgCO 3 .3Mg (OH) 2. And white pigments such as H 2 O], polyethylene wax, and bead pigments.
なお、上記ビーズ顔料は、通常の顔料である「Fe2O3、TiO2、CaCO3、キナクリドン{7,16−dihydro−7,16−dimethylbenzo[a]benzo[5,6]quino[3,2−I]acridine−9,18−dione、H.W.SANDS CORP.製、又は長瀬産業(株)製、商品名}」等の微粉末表面
を、ポリウレタン、アクリル樹脂、エポキシ樹脂、ポリエステル、ポリアミド(ナイロン(R))、フッ素樹脂、塩化ビニル−酢酸ビニル共重合体等の弾力性のある樹脂にて、またはこれらの弾力性のある樹脂に必要に応じて可塑剤、安定剤、界面活性剤等を加えたものにて、被覆して粒状に形成したものである。
The above bead pigments are the usual pigments “Fe 2 O 3 , TiO 2 , CaCO 3 , quinacridone {7,16-dihydro-7,16-dimethylbenzo [a] benzo [5,6] quino [3,6] quino [3,6]. 2-I] acidine-9,18-dione, manufactured by HW SANDS CORP. Or manufactured by Nagase Sangyo Co., Ltd., trade name} ", and the like, polyurethane, acrylic resin, epoxy resin, polyester, In elastic resin such as polyamide (nylon (R)), fluororesin, vinyl chloride-vinyl acetate copolymer, etc., or plasticizer, stabilizer, surface activity as required for these elastic resins It is formed by coating with an agent or the like and granular.
本発明では、体質顔料(C)としては、それ自体屈折率が低く、隠蔽性(顔料、塗料などが黒白の下地を完全に覆い隠す性質をいう。)向上への寄与はなく隠蔽性に関係ないが、光沢を低下させることができる上記白色顔料が好適に用いられる。 In the present invention, the extender pigment (C) itself has a low refractive index and does not contribute to improving the concealing property (the property that the pigment, paint, etc. completely covers the black-and-white base) and relates to the concealing property. The white pigment that can reduce gloss is preferably used.
本発明の光硬化性塗料組成物には、その他、(メタ)アクリロイル基、ビニル基などの重合性二重結合を有する重合性モノマー、各種添加剤(例:消泡剤、レベリング剤、顔料分散剤)などが含まれていてもよい。 The photocurable coating composition of the present invention includes a polymerizable monomer having a polymerizable double bond such as a (meth) acryloyl group or a vinyl group, various additives (eg, antifoaming agent, leveling agent, pigment dispersion). Agent) and the like.
本発明では、上記光硬化性樹脂(A)100重量部に対して、光重合開始剤(B)を通常、1〜15重量部、好ましくは3〜6重量部の範囲で、体質顔料(C)を通常1〜30
重量部、好ましくは5〜15重量部の範囲で使用することが塗布された未硬化塗膜の硬化速度、硬化塗膜の低臭気性、硬化塗膜の色相の点から望ましい。
In the present invention, the photopolymerization initiator (B) is usually used in an amount of 1 to 15 parts by weight, preferably 3 to 6 parts by weight, based on 100 parts by weight of the photocurable resin (A). Usually 1-30
Use in an amount of parts by weight, preferably 5 to 15 parts by weight, is desirable from the viewpoint of the curing rate of the applied uncured coating film, the low odor of the cured coating film, and the hue of the cured coating film.
本発明では、木質基材上に、予め、シーラー塗膜、下塗り塗膜、中塗り塗膜のいずれかが施されていてもよい。これらシーラー塗膜、下塗り塗膜および、中塗り塗膜のすべてを塗設する場合には、その積層順序が、「木質基材/シーラー塗膜/下塗り塗膜/中塗り塗膜/光硬化性塗料組成物からなる塗膜」となるように塗設すればよい。なお、何れかの塗膜例えば、下塗塗膜を除外・省略する場合には、この順序を保持しつつ、「木質基材/シーラー塗膜/中塗り塗膜/光硬化性塗料組成物からなる塗膜」の順序で塗設すればよい。 In the present invention, any of a sealer coating, an undercoat coating, and an intermediate coating may be applied in advance on the wooden substrate. When all of these sealer coating, undercoat coating, and intermediate coating are applied, the order of lamination is “woody substrate / sealer coating / undercoating coating / intermediate coating / photocurability”. What is necessary is just to apply | coat so that it may become a "coating film consisting of a coating composition." In the case of excluding or omitting any coating film, for example, an undercoating film, while maintaining this order, “consisting of“ woody substrate / sealer coating / intermediate coating film / photocurable coating composition ”. What is necessary is just to apply in the order of "coating film".
このように木質基材上に、予め、シーラー塗膜、下塗り塗膜、中塗り塗膜のいずれか1種以上が塗布される場合には、これら各塗膜の塗布後に高圧水銀ランプまたはメタルハライドランプなどの照射を行うことができる。そして、それらの塗膜の最後の塗膜(層)上、例えば、中塗り塗膜上に、表面層(最外層、上塗層などとも言う。)となる上記光硬化性塗料組成物を塗布し、上記のように高圧水銀灯、メタルハライドランプなどでのセミキュア(半硬化)工程を実施したのち、無電極UVランプを照射し完全硬化させることが好ましい。 In this way, when any one or more of a sealer coating, an undercoat coating, and an intermediate coating are applied on the wooden substrate in advance, a high-pressure mercury lamp or a metal halide lamp is applied after each coating is applied. Irradiation can be performed. Then, the photocurable coating composition to be a surface layer (also referred to as an outermost layer or an overcoat layer) is applied on the last coating film (layer) of these coating films, for example, on the intermediate coating film. In addition, after performing the semi-cure (semi-curing) process using a high-pressure mercury lamp, a metal halide lamp, or the like as described above, it is preferable to irradiate an electrodeless UV lamp and completely cure it.
これら塗料の塗付に際しては、ロールコーター、フローコーター、ナイフコーター、エアスプレー、エアレススプレー、刷毛など、公知の何れの方法を用いてもよい。
<硬化塗膜及び該塗膜付き基材>
本発明に係る光硬化塗膜は、上記のいずれかに記載された方法で形成されている。
In applying these paints, any known method such as roll coater, flow coater, knife coater, air spray, airless spray, brush, etc. may be used.
<Hardened coating film and substrate with the coating film>
The photocured coating film according to the present invention is formed by any of the methods described above.
その塗膜厚さは、最終製品の種類、用途等により異なり、一概に決定されないが、例えば、5〜200μm(厚)程度である。
本発明に係る塗膜付き基材は、上記のいずれかに記載された方法で形成された光硬化塗膜にて木質基材の表面が被覆されていることを特徴としている。
The thickness of the coating film varies depending on the type of end product, application, etc., and is not generally determined, but is, for example, about 5 to 200 μm (thickness).
The base material with a coating film according to the present invention is characterized in that the surface of the wooden base material is coated with a photocured coating film formed by any of the methods described above.
木質基材としては、木材、合板、集成材など特に限定されない。
塗膜は、上記したように、例えば、「木質基材/シーラー塗膜/下塗り塗膜/中塗り塗膜/光硬化性塗料組成物からなる塗膜」の順序で形成されている。その場合の各層(塗膜)の厚みは、特に限定されないが、乾燥膜厚で、シーラー塗膜:3〜10μm(厚)程度、下塗り塗膜:10〜30μm(厚)程度、中塗り塗膜10〜50μm(厚)程度、光硬化性塗料組成物からなる塗膜:10〜100μm(厚)程度である。
The wood substrate is not particularly limited, such as wood, plywood, and laminated wood.
As described above, the coating film is formed in the order of, for example, “woody base material / sealer coating film / undercoat coating film / intermediate coating film / coating film made of a photocurable coating composition”. The thickness of each layer (coating film) in that case is not particularly limited, but is a dry film thickness, sealer coating film: about 3 to 10 μm (thickness), undercoat coating film: about 10 to 30 μm (thickness), intermediate coating film About 10 to 50 μm (thickness), coating film made of a photocurable coating composition: about 10 to 100 μm (thickness).
なお、必要により設けられるシーラー塗膜、下塗り塗膜、中塗り塗膜は、これらのうちの何れかの塗膜が存在しなくともよく、またこれらの全てが存在しなくともよい。
<発明の効果>
本発明においては、光硬化性塗料組成物からなる未硬化塗膜のUV硬化に際して、予め通常の高圧水銀灯やメタルハライドランプなどでセミキュア(半硬化)させた後、これら高圧水銀灯やメタルハライドランプなどに比して、所定波長域でのより高エネルギー照射が可能な無電極UVランプを用いて本硬化(完全硬化)を行っており、通常の高圧水銀灯やメタルハライドランプを使用する場合に比べて、全般的に塗膜性能が向上する傾向があり、例えば、硬度、耐薬品性、耐汚染性、耐干割れ性等の性能に優れた硬化塗膜が得られる。
In addition, the sealer coating film, the undercoat coating film, and the intermediate coating film provided as necessary may not include any of these coating films, or may not include all of them.
<Effect of the invention>
In the present invention, when UV-curing an uncured coating film made of a photocurable coating composition, it is semi-cured ( semi-cured ) with a normal high-pressure mercury lamp or metal halide lamp in advance, and then compared with these high-pressure mercury lamps and metal halide lamps. The main curing (complete curing) is performed using an electrodeless UV lamp capable of irradiating with higher energy in a predetermined wavelength range, and compared with the case of using a normal high-pressure mercury lamp or metal halide lamp. The coating film performance tends to be improved, and for example, a cured coating film having excellent performance such as hardness, chemical resistance, contamination resistance, and anti-cracking resistance can be obtained.
また、本発明においては、上記のように光硬化性塗料組成物の硬化に際して高出力の無電極UVランプを用いているので、用いられる光硬化性塗料組成物中の光重合開始剤の配合量を低減でき、得られる塗膜は低臭気性に優れる。 In the present invention, since a high-power electrodeless UV lamp is used for curing the photocurable coating composition as described above, the blending amount of the photopolymerization initiator in the photocurable coating composition to be used The resulting coating film is excellent in low odor.
また、本発明では、光硬化性塗料組成物から成る塗膜のUV硬化に際して、予め、上記波長領域に発光ピークを有する高圧水銀灯またはメタルハライドランプでセミキュア(半硬化)させた後に、上記波長領域に発光ピークを有するより高出力の無電極UVランプを照射することにより本硬化(完全硬化)させているので、高圧水銀灯またはメタルハライドランプを用いたセミキュア処理をせずに、無電極UVランプ照射のみを行う場合に比して、より一層低光沢の硬化塗膜になり、また、硬化塗膜の低臭気、硬度、耐薬品性、耐汚染性、耐干割れ性等の性能に優れた硬化塗膜が得られる。
[実施例]
以下、本発明について実施例によりさらに具体的に説明するが、本発明は係る実施例により何ら限定されるものではない。
Further, in the present invention, when UV-coating a coating film made of a photocurable coating composition, it is semi-cured (semi-cured) with a high-pressure mercury lamp or metal halide lamp having a light emission peak in the wavelength region in advance, and then in the wavelength region. Since the main curing (complete curing) is performed by irradiating a higher-power electrodeless UV lamp having an emission peak, only the electrodeless UV lamp irradiation is performed without semi-cure treatment using a high-pressure mercury lamp or a metal halide lamp. Compared to the case where it is carried out, the cured coating film has a lower gloss, and the cured coating film has excellent performance such as low odor, hardness, chemical resistance, stain resistance, and dry cracking resistance. Is obtained.
[Example]
EXAMPLES Hereinafter, although an Example demonstrates this invention further more concretely, this invention is not limited at all by the Example concerned.
次に、以下の実施例、比較例で用いた下塗用の紫外線硬化性組成物(下塗塗料)、中塗用の紫外線硬化性組成物(中塗塗料)、上塗用の紫外線硬化性組成物(上塗塗料)を示す。
[塗料組成物の調製]
<下塗り用の紫外線硬化性組成物(下塗塗料)の調製>
下塗用の紫外線硬化性組成物として、「ヒタロイド4860」(日立化成社製、ウレタンアクリレート樹脂)30重量部、
「ACMO」(興人社製、アクリルモノマー)30重量部、
「ビームセット770」(荒川化学社製、ビニルモノマー)5重量部、
「イルガキュアー184」(チバ・スペシャリティーケミカルズ社製、光重合開始剤)5重量部、
「MINEX10」(UNIMIN CANADA 社製、体質顔料)30重量部を加え攪拌して、下塗り用の紫外線硬化性組成物を調製した。
<中塗り用の紫外線硬化性組成物(中塗塗料)の調製>
中塗用の紫外線硬化性組成物として、「リポキシVR−77」(昭和高分子社製、エポキシアクリレート樹脂)45重量部、
「TRPGDA」(ダイセルUCB社製、アクリルモノマー)25重量部、
「ニューフロンテアTMP−3」(第一工業製薬社製、アクリルモノマー)15重量部、「イルガキュアー184」(チバ・スペシャリティーケミカルズ社製、光重合開始剤)3重量部、
「MINEX10」(UNIMIN CANADA 社製、体質顔料)30重量部を加え攪拌して、中塗り用の紫外線硬化性組成物を調製した。
<上塗用の紫外線硬化性組成物(i)の調製>
上塗用の紫外線硬化性組成物(塗料)(i)として、「UV−55」(大竹明新化学社製、ウレタンアクリレート樹脂)40重量部、
「GX−8301S」(第一工業製薬社製、アクリルモノマー)30重量部、
「TRPGDA」(ダイセルUCB社製、アクリルモノマー)15重量部、
「ニューフロンティアTMP−3」(第一工業製薬社製、アクリルモノマー)5重量部、「イルガキュア184」(チバ・スペシャリティーケミカルズ社製、光重合開始剤)5重量部、
「ミズカシールP−802Y」(水沢化学社製、体質顔料)5重量部を加え、攪拌して調製した。
<上塗用の紫外線硬化性組成物(ii)の調製>
上塗用の紫外線硬化性組成物(塗料)(ii)として、「UV−72」(大竹明新化学社製、ウレタンアクリレート樹脂)40重量部、
「GX−8301S」(第一工業製薬社製、アクリルモノマー)30重量部、
「TRPGDA」(ダイセルUCB社製、アクリルモノマー)15重量部、
「ニューフロンティアTMP−3」(第一工業製薬社製、アクリルモノマー)5重量部、「イルガキュア184」(チバ・スペシャリティーケミカルズ社製、光重合開始剤)5重
量部、
「ミズカシールP−802Y」(水沢化学社製、体質顔料)5重量部を加え、攪拌して調製した。
<上塗用の紫外線硬化性組成物(iii)の調製>
上塗用の紫外線硬化性組成物(塗料)(iii)として、「UV−72」(大竹明新化学社製、ウレタンアクリレート樹脂)40重量部、
「GX−8301S」(第一工業製薬社製、アクリルモノマー)24重量部、
「TRPGDA」(ダイセルUCB社製、アクリルモノマー)15重量部、
「ニューフロンティアTMP−3」(第一工業製薬社製、アクリルモノマー)5重量部、「イルガキュア184」(チバ・スペシャリティーケミカルズ社製、光重合開始剤)8重量部、
「ミズカシールP−802Y」(水沢化学社製、体質顔料)8重量部を加え、攪拌して調製した。
Next, undercoat UV curable composition (undercoat paint), intermediate coat UV curable composition (intercoat paint), top coat UV curable composition (top coat paint) used in the following Examples and Comparative Examples ).
[Preparation of coating composition]
<Preparation of UV curable composition for undercoat (undercoat)>
As UV curable composition for undercoat, “Hitaroid 4860” (Hitachi Chemical Co., Ltd., urethane acrylate resin) 30 parts by weight,
"ACMO" (manufactured by Kojinsha, acrylic monomer) 30 parts by weight,
"Beam set 770" (Arakawa Chemical Co., Ltd., vinyl monomer) 5 parts by weight,
"Irgacure 184" (Ciba Specialty Chemicals, photopolymerization initiator) 5 parts by weight,
30 parts by weight of “MINEX10” (made by UNIMIN CANADA, extender pigment) was added and stirred to prepare an ultraviolet curable composition for undercoating.
<Preparation of UV-curable composition for intermediate coating (intermediate coating)>
As an ultraviolet curable composition for intermediate coating, “Lipoxy VR-77” (manufactured by Showa Polymer Co., Ltd., epoxy acrylate resin) 45 parts by weight,
"TRPGDA" (manufactured by Daicel UCB, acrylic monomer) 25 parts by weight,
"New Frontier TMP-3" (Daiichi Kogyo Seiyaku Co., Ltd., acrylic monomer) 15 parts by weight, "Irgacure 184" (Ciba Specialty Chemicals, photopolymerization initiator) 3 parts by weight,
30 parts by weight of “MINEX10” (made by UNIMIN CANADA, extender pigment) was added and stirred to prepare an ultraviolet curable composition for intermediate coating.
<Preparation of UV curable composition (i) for top coating>
As UV curable composition (coating material) (i) for top coating, 40 parts by weight of “UV-55” (manufactured by Akira Ohtake Shin Chemical Co., Ltd., urethane acrylate resin),
"GX-8301S" (Daiichi Kogyo Seiyaku Co., Ltd., acrylic monomer) 30 parts by weight,
"TRPGDA" (manufactured by Daicel UCB, acrylic monomer) 15 parts by weight,
"New Frontier TMP-3" (Daiichi Kogyo Seiyaku Co., Ltd., acrylic monomer) 5 parts by weight, "Irgacure 184" (Ciba Specialty Chemicals, photopolymerization initiator) 5 parts by weight,
It was prepared by adding 5 parts by weight of “Mizukaseal P-802Y” (Mizusawa Chemical Co., Ltd., extender pigment) and stirring.
<Preparation of UV curable composition (ii) for top coating>
As UV curable composition (paint) (ii) for overcoating, 40 parts by weight of “UV-72” (manufactured by Akira Ohtake Shin Chemical Co., Ltd., urethane acrylate resin),
"GX-8301S" (Daiichi Kogyo Seiyaku Co., Ltd., acrylic monomer) 30 parts by weight,
"TRPGDA" (manufactured by Daicel UCB, acrylic monomer) 15 parts by weight,
"New Frontier TMP-3" (Daiichi Kogyo Seiyaku Co., Ltd., acrylic monomer) 5 parts by weight, "Irgacure 184" (Ciba Specialty Chemicals, photopolymerization initiator) 5 parts by weight,
It was prepared by adding 5 parts by weight of “Mizukaseal P-802Y” (Mizusawa Chemical Co., Ltd., extender pigment) and stirring.
<Preparation of UV curable composition (iii) for top coating>
As a UV curable composition (paint) (iii) for top coating, 40 parts by weight of “UV-72” (manufactured by Akira Otake, urethane acrylate resin),
"GX-8301S" (Daiichi Kogyo Seiyaku Co., Ltd., acrylic monomer) 24 parts by weight,
"TRPGDA" (manufactured by Daicel UCB, acrylic monomer) 15 parts by weight,
"New Frontier TMP-3" (Daiichi Kogyo Seiyaku Co., Ltd., acrylic monomer) 5 parts by weight, "Irgacure 184" (Ciba Specialty Chemicals, photopolymerization initiator) 8 parts by weight,
It was prepared by adding 8 parts by weight of “Mizukaseal P-802Y” (Mizusawa Chemical Co., Ltd., extender pigment) and stirring.
(木質床材の調製)
12mm厚なら材突き板合板上に、着色ステインをロールコーターで塗布し、80℃で1分間乾燥した後、下塗として「オーレックスNo.822F−2」(中国塗料(株)製、ウレタンアクリレート系紫外線硬化性組成物)をロールコーターで塗布し、高圧水銀灯で硬化させた。
(Preparation of wooden flooring)
If it is 12mm thick, apply colored stain on a veneer plywood with a roll coater, dry at 80 ° C for 1 minute, and then use "AULEX No. 822F-2" (made by China Paint Co., Ltd., urethane acrylate) as an undercoat UV curable composition) was applied with a roll coater and cured with a high pressure mercury lamp.
次いで、中塗り塗料として、「オーレックスNo.673B」(中国塗料(株)製、エポキシアクリレート系紫外線硬化性組成物)を塗布し、上記と同様に高圧水銀灯により硬化させ、最後に上記上塗塗料として、上記紫外線硬化性組成物(i)をフローコーターで塗布し、高圧水銀灯でセミキュアさせた後、「無電極UVランプ(Hバルブ)」(フュージョンUVシステムズ社製)で完全硬化(本硬化)させ、木質床材塗装品を得た。
(硬化条件)
(イ)高圧水銀灯:アイグラフィックス社製の高圧水銀灯を使用し、80W/cmで被塗物との距離を高さ15cmとして、10m/分の速度で搬送し積算光量が75mJ/cm2となる量で照射し硬化させた。
Next, “AUREX No. 673B” (manufactured by China Paint Co., Ltd., epoxy acrylate UV curable composition) is applied as an intermediate coating, cured with a high-pressure mercury lamp in the same manner as above, and finally the top coating The UV curable composition (i) is applied with a flow coater, semi-cured with a high-pressure mercury lamp, and then completely cured with an “electrodeless UV lamp (H bulb)” (manufactured by Fusion UV Systems) (main curing) To obtain a wooden floor coating.
(Curing conditions)
(B) High-pressure mercury lamp: Using a high-pressure mercury lamp manufactured by iGraphics, the distance from the object to be coated is 15 cm at a height of 80 W / cm, and it is conveyed at a speed of 10 m / min, and the integrated light quantity is 75 mJ / cm 2 Irradiated in an amount to cure.
なお、上記高圧水銀灯によるセミキュアの場合、搬送速度を40m/分に調整して塗膜を半硬化させた。
(ロ)無電極UVランプ:フュージョンUVシステムズ社製の「無電極UVランプ(Hバルブ)」を使用して、ランプ出力240W/cmで被塗物との距離5cmとして、10m/分の速度で搬送し、積算光量が150mJ/cm2となる量で照射し塗膜を硬化させ
た。
In the case of semi-curing with the high-pressure mercury lamp, the coating speed was semi-cured by adjusting the conveyance speed to 40 m / min.
(B) Electrodeless UV lamp: Using an “electrodeless UV lamp (H bulb)” manufactured by Fusion UV Systems, with a lamp output of 240 W / cm and a distance of 5 cm from the object to be coated, at a speed of 10 m / min. The coated film was cured by irradiating with an amount of 150 mJ / cm 2 for the integrated light quantity.
(木質床材の調製)
実施例1において、上塗用の紫外線硬化性組成物(塗料)(i)のセミキュアを行うに際して、高圧水銀灯に代えて、メタルハライドランプを使用した以外は、実施例1と同様にして木質床材塗装品を得た。
(Preparation of wooden flooring)
In Example 1, when carrying out the semi-cure of the UV curable composition (coating material) (i) for the top coating, the wooden flooring was applied in the same manner as in Example 1 except that a metal halide lamp was used instead of the high-pressure mercury lamp. I got a product.
(ハ)メタルハライドランプ:アイグラフィックス社製のメタルハライドランプを使用し、80w/cmで被塗物との距離を高さ15cmとして10m/分の速度で搬送し積算光量が50mJ/cm2となる量で照射し塗膜を硬化させた。 (C) Metal halide lamp: Uses a metal halide lamp manufactured by Eye Graphics Co., Ltd., and transports it at a speed of 10 m / min with a distance of 15 cm from the object to be coated at 80 w / cm, and the integrated light quantity becomes 50 mJ / cm 2. The coating was cured by irradiation in an amount.
(木質床材の調製)
実施例1において、無電極UVランプと被塗物との距離を5cmに代えて、10cmとした以外は、実施例1と同様にして木質床材塗装品を得た。
(Preparation of wooden flooring)
In Example 1, a wooden floor covering coated product was obtained in the same manner as in Example 1 except that the distance between the electrodeless UV lamp and the object to be coated was changed to 5 cm and changed to 10 cm.
(木質床材の調製)
実施例1において、上塗用の塗料(i)に代えて塗料(ii)を用い、また、上塗塗料の塗装に際して、フローコーターに代えて、ロールコーターを用いた以外は、実施例1と同様にして木質床材塗装品を得た。
(Preparation of wooden flooring)
In Example 1, paint (ii) was used in place of the paint (i) for top coating, and in the coating of the top paint, a roll coater was used instead of the flow coater. To obtain a wooden floor coating.
(木質床材の調製)
実施例1において、上塗用の塗料(i)に代えて塗料(iii)を用い、また、上塗塗料の塗装に際して、フローコーターに代えて、ロールコーターを用いた以外は、実施例1と同様にして木質床材塗装品を得た。
(Preparation of wooden flooring)
In Example 1, paint (iii) was used in place of paint (i) for top coating, and in the same manner as Example 1 except that a roll coater was used in place of the flow coater when applying the top paint. To obtain a wooden floor coating.
(木質床材の調製)
実施例1において、上塗の塗料の硬化を、「高圧水銀灯によるセミキュア+無電極UVランプ(Hバルブ)による本硬化」に代えて、「高圧水銀灯によるセミキュア+無電極UVランプ(Dバルブ)による本硬化」を行った以外は、実施例1と同様にして、木質床材塗装品を得た。
[比較例1]
(木質床材の調製)
実施例1において上塗の塗料の硬化を「高圧水銀灯によるセミキュア+無電極UVランプ(Hバルブ)による本硬化」に代えて、高圧水銀灯によるセミキュアを実施せず、「無電極UVランプ(Hバルブ)による本硬化のみ」を行った以外は、実施例1と同様にして、木質床材塗装品を得た。
[比較例2]
(塗料組成物の調製)
実施例1と同様にして、紫外線硬化性組成物(塗料)(i)を調製した。
(木質床材の調製)
実施例1において上塗の塗料の硬化を「高圧水銀灯によるセミキュア+無電極UVランプ(Hバルブ)による本硬化」に代えて、高圧水銀灯によるセミキュアを実施せず、「高圧水銀灯による本硬化のみ」を行った以外は、実施例1と同様にして、木質床材塗装品を得た。
[比較例3]
(木質床材の調製)
実施例5において上塗の塗料の硬化を「高圧水銀灯によるセミキュア+無電極UVランプ(Hバルブ)による本硬化」に代えて、高圧水銀灯によるセミキュアを実施せず、「高圧水銀灯による本硬化のみ」を行った以外は、実施例5と同様にして、木質床材塗装品を得た。
(Preparation of wooden flooring)
In Example 1, instead of “semi-cure using a high-pressure mercury lamp + non-cured UV lamp (H bulb)” as the curing of the top coat, “semi-curing using a high-pressure mercury lamp + non-electrode UV lamp (D bulb)” A wooden flooring coated product was obtained in the same manner as in Example 1 except that “curing” was performed.
[Comparative Example 1]
(Preparation of wooden flooring)
In Example 1, instead of “curing with a high pressure mercury lamp and semi-curing with an electrodeless UV lamp (H bulb)” instead of “high curing with a high pressure mercury lamp”, semi-curing with a high pressure mercury lamp was not performed. A wooden flooring coated product was obtained in the same manner as in Example 1 except that only the main curing was performed.
[Comparative Example 2]
(Preparation of coating composition)
In the same manner as in Example 1, an ultraviolet curable composition (paint) (i) was prepared.
(Preparation of wooden flooring)
Instead of “semi-cure with high-pressure mercury lamp + non-curing with electrodeless UV lamp (H bulb)” in Example 1, semi-cure with high-pressure mercury lamp is not performed, but “only main curing with high-pressure mercury lamp” is used. A wooden flooring coated product was obtained in the same manner as in Example 1 except that this was performed.
[Comparative Example 3]
(Preparation of wooden flooring)
Instead of “semi-cure with high-pressure mercury lamp + non-curing with electrodeless UV lamp (H bulb)” in Example 5, semi-cure with high-pressure mercury lamp is not performed, and “only main curing with high-pressure mercury lamp” is used. A wooden flooring coated product was obtained in the same manner as in Example 5 except that this was performed.
上記各実施例および各比較例で得られた木質床材塗装品について、光沢、臭気、耐擦傷性、耐汚染性、耐薬品性、耐干割れ性の評価を、下記の方法にて行った。
結果を表1に示す。
<光沢>
JIS―K−5600の鏡面光沢度の測定法に準拠し、入射角60度にて測定した。判定基準は以下の通り。
For the wooden floor coverings obtained in each of the above Examples and Comparative Examples, the gloss, odor, scratch resistance, stain resistance, chemical resistance, and dry crack resistance were evaluated by the following methods. .
The results are shown in Table 1.
<Glossy>
The measurement was performed at an incident angle of 60 degrees in accordance with the method for measuring the specular gloss of JIS-K-5600. Judgment criteria are as follows.
評価3:30以下、合格。
評価2:31〜70、不合格。
評価1:71以上、不合格。
<臭気>
上記方法で作製した木質床材の塗装品を、塗装直後(塗装後3分以内)に市販のアルミホイルで3重に巻き、その上から市販のポリ塩化ビニリデンフィルムで更に3重に梱包し、24時間室温で放置する。
Evaluation 3: 30 or less, passed.
Evaluation 2: 31-70, disqualified.
Evaluation 1: 71 or more, rejected.
<Odor>
Wrapped in 3 layers with a commercially available aluminum foil immediately after painting (within 3 minutes after painting), and then packed in 3 layers with a commercially available polyvinylidene chloride film. Leave at room temperature for 24 hours.
その後、開梱し、23℃で1時間養生した後、FLECで捕集し、ガスクロマトグラフィーにて臭気の原因となる光重合開始剤および分解物を定量測定し、3段階で評価した。
評価基準は以下の通り。
Then, after unpacking and curing at 23 ° C. for 1 hour, it was collected by FLEC, and the photopolymerization initiator and decomposition products causing odor were quantitatively measured by gas chromatography and evaluated in three stages.
The evaluation criteria are as follows.
評価3:0〜1000μg/m3、合格。
評価2:1001〜10000μg/m3、不合格。
評価1:10001μg/m3以上、不合格。
<硬化性>
木質床材塗装品の硬化性をトルエンラビング(1kg荷重で50往復)し、塗膜の状態変化により、3段階で評価した。
Evaluation 3: 0 to 1000 μg / m 3 , passed.
Evaluation 2: 1001-10000 μg / m 3 , unacceptable.
Evaluation 1: 10001 μg / m 3 or more, rejected.
<Curing property>
The curability of the wooden floor coating material was evaluated with a three-stage evaluation by toluene rubbing (50 reciprocations at 1 kg load) and the change in the state of the coating film.
評価基準は以下の通り。
評価3:塗膜に変化なし。合格。
評価2:トルエンラビングにより塗膜が若干侵される。不合格。
The evaluation criteria are as follows.
Evaluation 3: No change in coating film. Pass.
Evaluation 2: The coating film is slightly affected by toluene rubbing. failure.
評価1:塗膜はトルエンに溶解する。不合格。
<耐擦傷性>
スチールウール#0000を用いて荷重200gにてラビングを10往復し、塗膜の状態により、3段階で評価した。
Evaluation 1: The coating film dissolves in toluene. failure.
<Abrasion resistance>
The rubbing was reciprocated 10 times with a load of 200 g using steel wool # 0000, and the evaluation was made in three stages according to the state of the coating film.
評価基準は以下の通り。
評価3:塗膜に変化なし。合格。
評価2:塗膜に僅かな傷が残る。不合格。
The evaluation criteria are as follows.
Evaluation 3: No change in coating film. Pass.
Evaluation 2: Slight scratches remain on the coating film. failure.
評価1:塗膜に著しい傷が残る。不合格。
<耐汚染性(1)>
2液性の毛染め液(ビゲン(株)製、「ヘアカラー7G」)を混合し、得られた毛染め液を直径2cmの円状に滴下し、20分経過後にウエスで拭き取り、その染色の度合いで3段階評価する。
Evaluation 1: Significant scratches remain on the coating film. failure.
<Contamination resistance (1)>
A two-component hair dyeing solution (manufactured by Vigen Co., Ltd., “Hair Color 7G”) is mixed, and the obtained hair dyeing solution is dropped into a circular shape having a diameter of 2 cm. A three-level evaluation is made based on the degree of
評価基準は以下の通り。
評価3:塗膜に変化がない、または、若干の染色が認められる。合格。
評価2:塗膜にはっきりと染色が認められる。不合格。
The evaluation criteria are as follows.
Evaluation 3: There is no change in the coating film, or some staining is observed. Pass.
Evaluation 2: Dyeing is clearly observed in the coating film. failure.
評価1:塗膜に著しい染色が認められる。不合格。
<耐汚染性(2)>
青インキを時計皿に採り、スポットテストを24時間実施し、その痕跡の度合いで3段にて階評価する。
Evaluation 1: Remarkable dyeing is observed in the coating film. failure.
<Contamination resistance (2)>
A blue ink is put on a watch glass, a spot test is performed for 24 hours, and the floor is evaluated in three stages according to the degree of the trace.
評価基準は以下の通り。
評価3:塗膜に変化がない、または、若干の染色が認められる。合格。
評価2:塗膜にはっきりと染色が認められる。不合格。
The evaluation criteria are as follows.
Evaluation 3: There is no change in the coating film, or some staining is observed. Pass.
Evaluation 2: Dyeing is clearly observed in the coating film. failure.
評価1:塗膜に著しい染色が認められる。不合格。
<耐薬品性>
5%の酢酸水溶液および、1%の苛性ソーダ水溶液を時計皿にとり、スポットテストを24時間実施し、その痕跡の度合いで3段階評価する。
Evaluation 1: Remarkable dyeing is observed in the coating film. failure.
<Chemical resistance>
A 5% acetic acid aqueous solution and a 1% caustic soda aqueous solution are placed in a watch glass, and a spot test is performed for 24 hours.
評価基準は以下の通り。
評価3:塗膜に変化がない、または、若干の痕跡が認められる。合格。
評価2:塗膜にはっきりと痕跡が認められる。不合格。
The evaluation criteria are as follows.
Evaluation 3: There is no change in the coating film, or some trace is recognized. Pass.
Evaluation 2: Traces are clearly observed in the coating film. failure.
評価1:塗膜に著しい痕跡が認められる。不合格。
<耐干割れ性>
寒熱繰返し試験(塗装品を80℃で2時間保持した後、−20℃で2時間保持する。)を5回繰返し、発生した表面の割れ長さの合計を測定し、3段階で耐干割れ性を評価する。
Evaluation 1: Remarkable traces are observed in the coating film. failure.
<Dry-cracking resistance>
Repeated cold heat test (the coated product is kept at 80 ° C. for 2 hours and then kept at −20 ° C. for 2 hours) 5 times, and the total crack length of the generated surface is measured. Assess sex.
評価基準は以下の通り。
評価3:塗装品15cm×15cm当たり、割れ長さ100mm以下。合格。
評価2:塗装品15cm×15cm当たり、割れ長さ101mm〜500mm。不合格。
The evaluation criteria are as follows.
Evaluation 3: The crack length is 100 mm or less per 15 cm × 15 cm of the coated product. Pass.
Evaluation 2: Crack length of 101 mm to 500 mm per coated product 15 cm × 15 cm. failure.
評価1:塗装品15cm×15cm当たり、割れ長さ501mm以上。不合格。 Evaluation 1: The crack length is 501 mm or more per 15 cm × 15 cm of the coated product. failure.
Claims (18)
(A)光硬化性樹脂と、
(B)光重合開始剤と、
(C)体質顔料と
を含む光硬化性塗料組成物を塗布し、高圧水銀灯またはメタルハライドランプでセミキュア(半硬化)させた後に、無電極UVランプで完全硬化させることを特徴とする、光硬化性塗料組成物からなる塗膜の硬化方法。 On the wooden substrate
(A) a photocurable resin;
(B) a photopolymerization initiator;
(C) A photocurable composition comprising a photocurable coating composition containing an extender pigment, semi-cured with a high-pressure mercury lamp or metal halide lamp, and then completely cured with an electrodeless UV lamp. A method for curing a coating film comprising a coating composition.
(A)光硬化性樹脂と、
(B)光重合開始剤と、
(C)体質顔料と
を含む光硬化性塗料組成物を塗布し、高圧水銀灯またはメタルハライドランプでセミキュア(半硬化)させた後に、無電極UVランプで完全硬化させることを特徴とする、光硬化性塗料組成物からなる塗膜の製造方法。 On the wooden substrate
(A) a photocurable resin;
(B) a photopolymerization initiator;
(C) A photocurable composition comprising a photocurable coating composition containing an extender pigment, semi-cured with a high-pressure mercury lamp or metal halide lamp, and then completely cured with an electrodeless UV lamp. A method for producing a coating film comprising a coating composition.
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Citations (2)
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JPH07328534A (en) * | 1994-05-31 | 1995-12-19 | Dantani Plywood Co Ltd | Coating method for wood fiber board |
JP2003313429A (en) * | 2002-04-25 | 2003-11-06 | Toagosei Co Ltd | Active energy beam-curable aqueous emulsion composition |
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JPH07328534A (en) * | 1994-05-31 | 1995-12-19 | Dantani Plywood Co Ltd | Coating method for wood fiber board |
JP2003313429A (en) * | 2002-04-25 | 2003-11-06 | Toagosei Co Ltd | Active energy beam-curable aqueous emulsion composition |
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