JP2009215385A - Blue pigment with infrared reflectivity, coating material using the same, and resin composition - Google Patents

Blue pigment with infrared reflectivity, coating material using the same, and resin composition Download PDF

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JP2009215385A
JP2009215385A JP2008058775A JP2008058775A JP2009215385A JP 2009215385 A JP2009215385 A JP 2009215385A JP 2008058775 A JP2008058775 A JP 2008058775A JP 2008058775 A JP2008058775 A JP 2008058775A JP 2009215385 A JP2009215385 A JP 2009215385A
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blue pigment
infrared reflective
reflective blue
infrared
resin
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JP5392453B2 (en
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Kazutoshi Sanada
和俊 真田
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Toda Kogyo Corp
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Toda Kogyo Corp
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Priority to JP2008058775A priority Critical patent/JP5392453B2/en
Priority to US12/396,573 priority patent/US8961683B2/en
Priority to EP09250630A priority patent/EP2100853A3/en
Priority to CNA2009101178369A priority patent/CN101525502A/en
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Priority to US14/529,199 priority patent/US9260583B2/en
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a blue pigment with infrared reflectivity, which contains no harmful elements, is a blue pigment, and has excellent infrared reflectivity. <P>SOLUTION: The blue pigment is constituted of composite oxides containing Co, Al and Mg and is the blue pigment with infrared reflectivity, wherein a mole ratio of a Mg content of the blue pigment to all metallic elements is 11-22%; a BET specific surface area of the blue pigment is 10-100 m<SP>2</SP>/g; lightness (L<SP>*</SP>) is 35-50; and solar reflectance is 45-60%. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、有害な元素を含有せず、しかも、優れた赤外線反射性を有する熱遮蔽性塗料を得ることができる赤外線反射性青色顔料に関する。   The present invention relates to an infrared-reflective blue pigment that does not contain harmful elements and that can provide a heat-shielding paint having excellent infrared reflectivity.

屋外で用いられている道路、建築物、備蓄タンク、自動車、船舶等は、太陽の日射によって内部温度が上昇するため、建築物及び自動車等の外観塗装を白色から淡色にすることで太陽光を反射し、ある程度熱遮蔽効果を高めることが行われている。   Roads, buildings, stockpile tanks, automobiles, ships, etc. used outdoors increase the internal temperature due to solar radiation, so sunlight is reduced by changing the exterior paint of buildings and automobiles from white to light. It is reflected to increase the heat shielding effect to some extent.

しかしながら、殊に、屋外建築物の屋根などは、汚れを目立たなくするために、濃彩色から黒色を呈している場合が多く、外観塗装が濃彩色から黒色を有する建築物及び自動車等の場合には、淡色から白色の外観塗装を有する建築物及び自動車等に比べて太陽光を吸収しやすく、屋内の温度が著しく上昇する傾向にある。物品の輸送、保存に当たって、内部が高温になることは好ましいものではない。   However, in particular, the roofs of outdoor buildings are often dark to black in order to make the dirt inconspicuous, and in the case of buildings and automobiles whose exterior paint has a dark to black color. Compared to buildings and automobiles having a light-to-white appearance paint, it is easier to absorb sunlight, and the indoor temperature tends to rise remarkably. It is not preferable that the temperature of the interior becomes high during transportation and storage of the article.

そこで、地球温暖化防止のためのエネルギー節約という観点からも、濃彩色から黒色の外観を有する建築物及び自動車等の内部温度の上昇を抑制することが強く望まれている。従来の熱遮蔽性黒色塗料として、例えばＣｏＯ、Ｃｒ２Ｏ３及びＦｅ２Ｏ３からなるスピネル構造を有する黒色焼成顔料を含有する熱遮蔽性黒色塗料が開発されているけれども（例えば特許文献１参照）、顔料中にＣｒを含有するものであり、有害な元素を含有せず、しかも優れた赤外線反射性を有する赤外線反射性黒色顔料が求められていた。これに対し本出願人は、有害な元素を含有せず、しかも優れた赤外線反射性を有する赤外線反射性黒色顔料を開発し、既に特許出願を行っている（例えば特許文献２参照）。 Therefore, from the viewpoint of energy saving for preventing global warming, it is strongly desired to suppress an increase in internal temperature of buildings and automobiles having a dark to black appearance. As a conventional heat-shielding black paint, for example, a heat-shielding black paint containing a black fired pigment having a spinel structure made of CoO, Cr 2 O 3 and Fe 2 O 3 has been developed (see, for example, Patent Document 1). ), An infrared-reflective black pigment that contains Cr in the pigment, does not contain harmful elements, and has excellent infrared reflectivity. On the other hand, the present applicant has developed an infrared reflective black pigment that does not contain harmful elements and has excellent infrared reflectivity, and has already filed a patent application (see, for example, Patent Document 2).

塗料も黒色塗料以外に青、緑、赤など多くの着色塗料が使用されていることは周知のところであり、塗料等に使用する青色の無機顔料としては、従来からコバルトブルー系の顔料が広く使用されている。コバルトブルー系の顔料も種々の改良がなされた青色顔料が提案されている。例えば、赤味の微粒子型コバルトブルー系顔料の製造方法として、アルカリ剤に炭酸ソーダを利用し、アルミニウム及びコバルトの水酸化物又は炭酸塩を沈殿させる際にリン化合物を共存させる方法が提案されている（例えば特許文献３参照）。さらに出発原料の粉砕混合時にメカノケミカル効果を与えるに充分なエネルギーを加えて、コバルト及びアルミニウムが均一に存在する二次粒子とし、これを加熱焼成して透明性の高いコバルトブルー系顔料を得る方法も提案されている(例えば特許文献４参照)。
特開２０００−７２９９０号公報 特開２００７−１９７５７０号公報 特開２０００−８０３０１号公報 特開平１０−２１９１３２号公報 It is well known that many colored paints such as blue, green and red are used in addition to black paint, and cobalt blue pigments have been widely used as blue inorganic pigments for paints. Has been. Cobalt blue pigments having various improvements have been proposed. For example, as a method for producing a reddish fine particle type cobalt blue pigment, there has been proposed a method in which sodium carbonate is used as an alkaline agent and a phosphorus compound coexists when aluminum or cobalt hydroxide or carbonate is precipitated. (For example, refer to Patent Document 3). Further, a method for obtaining a cobalt blue pigment having high transparency by adding sufficient energy to give a mechanochemical effect during the pulverization and mixing of the starting materials to form secondary particles in which cobalt and aluminum are uniformly present, and then heating and firing the particles. Has also been proposed (see, for example, Patent Document 4).
JP 2000-72990 A JP 2007-197570 A JP 2000-80301 A JP-A-10-219132

今日、地球温暖化防止等の観点から青色塗料も黒色塗料と同様に、優れた赤外線反射性を有する熱遮蔽性塗料が求められている。青色塗料に使用可能な青色の顔料は、特許文献３及び特許文献４に記載の製造方法及びこれら方法により得られる青色顔料のほか多くの製造方法及び顔料が特許公開公報等に開示されているけれども、有害な元素を含有せず、しかも優れた赤外線反射性を有する赤外線反射性青色顔料は、未だ得られていない。   Today, from the viewpoint of prevention of global warming and the like, a blue paint is required to have a heat shielding paint having excellent infrared reflectivity like a black paint. As for the blue pigment that can be used for the blue paint, there are many production methods and pigments disclosed in Patent Publications and the like in addition to the production methods described in Patent Literature 3 and Patent Literature 4 and the blue pigments obtained by these methods. An infrared-reflective blue pigment that does not contain harmful elements and has excellent infrared reflectivity has not yet been obtained.

本発明の目的は、有害な元素を含有せず、しかも青色顔料であって優れた赤外線反射性を有する赤外線反射性青色顔料を提供することである。   An object of the present invention is to provide an infrared reflective blue pigment which does not contain harmful elements and which is a blue pigment and has excellent infrared reflectivity.

前記目的は、次の通りの本発明によって達成できる。   The object can be achieved by the present invention as follows.

即ち、本発明は、Ｃｏ、Ａｌ及びＭｇを含有する複合酸化物からなる青色顔料であって、該青色顔料のＭｇ含有量が全金属元素に対するモル比で１１〜２２％であり、該青色顔料のＢＥＴ比表面積が１０〜１００ｍ２／ｇであることを特徴とする赤外線反射性青色顔料である（本発明１）。 That is, the present invention is a blue pigment composed of a composite oxide containing Co, Al and Mg, wherein the blue pigment has an Mg content of 11 to 22% in terms of a molar ratio with respect to all metal elements. This is an infrared reflective blue pigment characterized by having a BET specific surface area of 10 to 100 m 2 / g (Invention 1).

また本発明は、前記赤外線反射性青色顔料の結晶構造がスピネル型である赤外線反射性青色顔料である（本発明２）。   Further, the present invention is an infrared reflective blue pigment in which the crystal structure of the infrared reflective blue pigment is a spinel type (Invention 2).

また本発明は、前記赤外線反射性青色顔料の明度（Ｌ＊）が３５〜５０である赤外線反射性青色顔料である（本発明３）。 Moreover, this invention is an infrared reflective blue pigment whose brightness (L * ) of the said infrared reflective blue pigment is 35-50 (this invention 3).

また本発明は、前記いずれか１の赤外線反射性青色顔料の日射反射率が４５〜６０％である赤外線反射性青色顔料である（本発明４）。   Moreover, this invention is an infrared reflective blue pigment whose solar reflectance of any one said infrared reflective blue pigment is 45 to 60% (this invention 4).

また本発明は、前記いずれか１の赤外線反射性青色顔料の表面がＳｉ、Ａｌ、Ｚｒ、Ｔｉから選ばれる一種以上の化合物で被覆されている赤外線反射性青色顔料である（本発明５）。   Further, the present invention is an infrared reflective blue pigment in which the surface of any one of the infrared reflective blue pigments is coated with one or more compounds selected from Si, Al, Zr, and Ti (Invention 5).

また本発明は、前記いずれか１の赤外線反射性青色顔料を塗料構成基材中に配合した塗料である（本発明６）。   Moreover, this invention is the coating material which mix | blended any one said infrared reflective blue pigment in the coating-material base material (this invention 6).

また本発明は、前記いずれか１の赤外線反射性青色顔料を用いて着色した樹脂組成物である（本発明７）。   In addition, the present invention is a resin composition colored using any one of the infrared reflective blue pigments (Invention 7).

本発明に係る赤外線反射性青色顔料は、有害な元素を含有しない青色顔料であって、しかも、赤外線反射性に優れているので赤外線反射性青色顔料として好適である。   The infrared-reflective blue pigment according to the present invention is a blue pigment that does not contain harmful elements, and is excellent in infrared reflectivity, and is therefore suitable as an infrared-reflective blue pigment.

本発明の構成をより詳しく説明すれば次の通りである。   The configuration of the present invention will be described in more detail as follows.

先ず、本発明に係る赤外線反射性青色顔料について述べる。   First, the infrared reflective blue pigment according to the present invention will be described.

本発明に係る赤外線反射性青色顔料は、Ｃｏ、Ａｌ及びＭｇを含有する複合酸化物からなる青色顔料であって、該青色顔料のＭｇ含有量が全金属元素に対するモル比で１１〜２２％であり、該青色顔料のＢＥＴ比表面積が１０〜１００ｍ２／ｇである青色顔料である。 The infrared reflective blue pigment according to the present invention is a blue pigment made of a composite oxide containing Co, Al and Mg, and the Mg content of the blue pigment is 11 to 22% in terms of a molar ratio to the total metal elements. The blue pigment has a BET specific surface area of 10 to 100 m 2 / g.

本発明に係る赤外線反性青色顔料中のＭｇの含有割合は、青色顔料中の全金属元素に対して、１１〜２２モル％であり、好ましくは１２〜２０モル％、より好ましくは１３〜２０モル％である。Ｍｇの全金属元素に対する含有割合が１１モル％未満となると、日射反射率が十分とは言い難い。一方、Ｍｇの全金属元素に対する含有割合が２２モル％を超えると、明度（Ｌ＊）が大きくなり過ぎる。本発明に係る赤外線反射性青色顔料中のＣｏの含有割合は、青色顔料中の全金属元素に対して、１２〜２２モル％が好ましい。また本発明に係る赤外線反射性青色顔料は、各種原料由来の不純物が不可避的に混入する場合もあるけれどもその量は微量であり、青色顔料中のＭｇ及びＣｏを除く金属元素は、実質的にＡｌであり、ＣｏとＭｇとの含有量とＡｌの含有量との比率がモル比で１：２が好ましい。 The content ratio of Mg in the infrared-reactive blue pigment according to the present invention is 11 to 22 mol%, preferably 12 to 20 mol%, more preferably 13 to 20 mol, based on all metal elements in the blue pigment. Mol%. If the content ratio of Mg to all metal elements is less than 11 mol%, it is difficult to say that the solar reflectance is sufficient. On the other hand, when the content ratio of Mg to all metal elements exceeds 22 mol%, the lightness (L * ) becomes too large. As for the content rate of Co in the infrared reflective blue pigment which concerns on this invention, 12-22 mol% is preferable with respect to all the metal elements in a blue pigment. In addition, the infrared reflective blue pigment according to the present invention is inevitably mixed with impurities derived from various raw materials, but the amount thereof is very small, and the metal elements other than Mg and Co in the blue pigment are substantially Al, and the ratio of the content of Co and Mg to the content of Al is preferably 1: 2 in terms of molar ratio.

本発明に係る赤外線反射性青色顔料のＢＥＴ比表面積は１０〜１００ｍ２／ｇであり、好ましくは１５〜９０ｍ２／ｇ、より好ましくは２０〜８０ｍ２／ｇ、更により好ましくは３６〜８０ｍ２／ｇである。ＢＥＴ比表面積が１０ｍ２／ｇ未満の場合には、粒子が粗大であったり、粒子及び粒子相互間で焼結が生じた粒子となっており、着色力が低下する。またＢＥＴ比表面積が１００ｍ２／ｇを超えると、粒子の微細化により凝集を起こし易く、ビヒクル中の分散が困難となり好ましくない。 The BET specific surface area of the infrared reflective blue pigment according to the present invention is 10 to 100 m 2 / g, preferably 15 to 90 m 2 / g, more preferably 20 to 80 m 2 / g, and still more preferably 36 to 80 m 2. / G. When the BET specific surface area is less than 10 m 2 / g, the particles are coarse or the particles are sintered between the particles and the coloring power is reduced. On the other hand, if the BET specific surface area exceeds 100 m 2 / g, aggregation is likely to occur due to finer particles, and dispersion in the vehicle becomes difficult.

本発明に係る赤外線反射性青色顔料の結晶構造は、スピネル型が好ましい。   The crystal structure of the infrared reflective blue pigment according to the present invention is preferably a spinel type.

本発明に係る赤外線反射性青色顔料には、不可避的に各種原料由来の不純物が混入する場合もあるけれども、この場合であっても、例えばＣｒの含有量は１ｗｔ％以下であり、殊に、Ｃｒ６＋の含有量は１０ｐｐｍ以下である。 The infrared reflective blue pigment according to the present invention may inevitably contain impurities derived from various raw materials, but even in this case, for example, the Cr content is 1 wt% or less. The content of Cr 6+ is 10 ppm or less.

本発明に係る赤外線反射性青色顔料の平均粒子径は０．０２〜１．２μｍが好ましい。赤外線反射性青色顔料の平均粒子径が１．２μｍを超える場合には、粒子サイズが大きすぎるため、着色力が低下する。平均粒子径が０．０２μｍ未満の場合には、ビヒクル中への分散が困難となる場合がある。より好ましくは０．０２〜１．１μｍ、更により好ましくは０．０２〜１．０μｍである。   The average particle diameter of the infrared reflective blue pigment according to the present invention is preferably 0.02 to 1.2 μm. When the average particle diameter of the infrared reflective blue pigment exceeds 1.2 μm, the coloring power is lowered because the particle size is too large. When the average particle size is less than 0.02 μm, dispersion in the vehicle may be difficult. More preferably, it is 0.02-1.1 micrometers, More preferably, it is 0.02-1.0 micrometers.

本発明に係る赤外線反射性青色顔料の明度（Ｌ＊）は、３５〜５０が好ましい。明度（Ｌ＊）が前記範囲外となる場合は、青色に優れるとは言い難く用途が限定されやすい。より好ましくは４０〜５０である。 The lightness (L * ) of the infrared reflective blue pigment according to the present invention is preferably 35-50. When the lightness (L * ) is outside the above range, it is difficult to say that the color is excellent in blue, and the application is likely to be limited. More preferably, it is 40-50.

本発明に係る赤外線反射性青色顔料のａ＊は１５〜３０が好ましい。ａ＊が前記範囲外の場合には、青色に優れるとは言い難く用途が限定されやすい。より好ましくは１７〜２８である。 The a * of the infrared reflective blue pigment according to the present invention is preferably 15 to 30. When a * is out of the above range, it is difficult to say that the color is excellent in blue and the application is likely to be limited. More preferably, it is 17-28.

本発明に係る赤外線反射性青色顔料のｂ＊は−４０〜−６０が好ましい。ｂ＊が前記範囲外の場合には、青色に優れるとは言い難く用途が限定されやすい。より好ましくは−４５〜−６０である。 The b * of the infrared reflective blue pigment according to the present invention is preferably -40 to -60. When b * is out of the above range, it is difficult to say that the color is excellent in blue and the application is likely to be limited. More preferably, it is −45 to −60.

本発明に係る赤外線反射性青色顔料の日射反射率は、４５〜６０％であることが好ましい。４５％未満の場合には、赤外線反射性が十分とは言い難い。より好ましくは５０〜６０％である。   The solar reflectance of the infrared reflective blue pigment according to the present invention is preferably 45 to 60%. If it is less than 45%, it is difficult to say that the infrared reflectivity is sufficient. More preferably, it is 50 to 60%.

本発明においては、粒子表面をＳｉ、Ａｌ、Ｚｒ、Ｔｉから選ばれる１種又は２種以上の化合物によって被覆しておいてもよい。被覆量は赤外線反射性青色顔料に対して０．１〜１０ｗｔ％が好ましい。より好ましくは０．２〜５ｗｔ％である。   In the present invention, the particle surface may be coated with one or more compounds selected from Si, Al, Zr, and Ti. The coating amount is preferably 0.1 to 10 wt% with respect to the infrared reflective blue pigment. More preferably, it is 0.2-5 wt%.

次に、本発明に係る赤外線反射性青色顔料の製造法について述べる。   Next, the manufacturing method of the infrared reflective blue pigment which concerns on this invention is described.

本発明に係る赤外線反射性青色顔料は、各種原料を混合、焼成して得ることができる。   The infrared reflective blue pigment according to the present invention can be obtained by mixing and firing various raw materials.

出発原料は、前記各金属元素の酸化物、炭酸塩、硝酸塩、硫酸塩などを用いることができる。   As the starting material, oxides, carbonates, nitrates, sulfates and the like of the respective metal elements can be used.

出発原料の混合は、均一に混合することができれば、特に限定されるものではなく、湿式混合でも乾式混合でもよい。また湿式合成であってもよい。   The mixing of the starting materials is not particularly limited as long as the starting materials can be uniformly mixed, and may be wet mixing or dry mixing. Also, wet synthesis may be used.

加熱焼成温度は８００〜１２００℃が好ましく、８００〜１０５０℃がより好ましい。加熱雰囲気は大気中である。   800-1200 degreeC is preferable and the heat-firing temperature has more preferable 800-1050 degreeC. The heating atmosphere is air.

加熱後の粉末は、常法に従って、水洗、粉砕を行えばよい。   The heated powder may be washed and pulverized according to a conventional method.

本発明においては、赤外線反射性青色顔料の粒子表面をＳｉ、Ａｌ、Ｚｒ、Ｔｉから選ばれる１種又は２種以上の化合物によって被覆しておいてもよい。表面処理方法は、湿式あるいは乾式方法等の常法に従って行えばよい。例えば、湿式方法は湿式分散した赤外線反射性青色顔料のスラリーに、Ｓｉ、Ａｌ、Ｚｒ、Ｔｉから選ばれる１種又は２種以上の可溶性化合物を、酸又はアルカリでｐＨ調整しながら添加・混合して被覆する方法、乾式方法はヘンシェルミキサーなどの装置中で赤外線反射性青色顔料にＳｉ、Ａｌ、Ｚｒ、Ｔｉから選ばれる１種又は２種以上のカップリング剤などにより被覆処理する方法である。   In the present invention, the particle surface of the infrared reflective blue pigment may be coated with one or more compounds selected from Si, Al, Zr, and Ti. The surface treatment method may be performed according to a conventional method such as a wet method or a dry method. For example, in the wet method, one or two or more soluble compounds selected from Si, Al, Zr, and Ti are added to and mixed with a slurry of a wet-dispersed infrared reflective blue pigment while adjusting the pH with an acid or alkali. The coating method and the dry method are methods in which an infrared reflective blue pigment is coated with one or more coupling agents selected from Si, Al, Zr, and Ti in an apparatus such as a Henschel mixer.

次に、本発明に係る赤外線反射性青色顔料を配合した塗料について述べる。   Next, a paint containing the infrared reflective blue pigment according to the present invention will be described.

本発明に係る塗料中における赤外線反射性青色顔料の配合割合は、塗料構成基材１００重量部に対して０．５〜１００重量部の範囲で使用することができ、塗料のハンドリング性を考慮すれば、好ましくは１．０〜１００重量部である。   The blending ratio of the infrared-reflective blue pigment in the paint according to the present invention can be used in the range of 0.5 to 100 parts by weight with respect to 100 parts by weight of the paint base material. For example, it is preferably 1.0 to 100 parts by weight.

塗料構成基材としては、樹脂、溶剤、必要により油脂、消泡剤、体質顔料、乾燥促進剤、界面活性剤、硬化促進剤、助剤等が配合される。   As the paint constituent base material, a resin, a solvent, and if necessary, fats and oils, an antifoaming agent, an extender pigment, a drying accelerator, a surfactant, a curing accelerator, an auxiliary agent and the like are blended.

樹脂としては、溶剤系塗料用や油性印刷インクに通常使用されているアクリル樹脂、アルキッド樹脂、ポリエステル樹脂、ポリウレタン樹脂、エポキシ樹脂、フェノール樹脂、メラミン樹脂、アミノ樹脂、塩化ビニル樹脂、シリコーン樹脂、ガムロジン、ライムロジン等のロジン系樹脂、マレイン酸樹脂、ポリアミド樹脂、ニトロセルロース、エチレン−酢酸ビニル共重合樹脂、ロジン変性フェノール樹脂、ロジン変性マレイン酸樹脂等のロジン変性樹脂、石油樹脂等を用いることができる。水系塗料用としては、水系塗料用や水性インクに通常使用されている水溶性アクリル樹脂、水溶性スチレン−マレイン酸樹脂、水溶性アルキッド樹脂、水溶性メラミン樹脂、水溶性ウレタンエマルジョン樹脂、水溶性エポキシ樹脂、水溶性ポリエステル樹脂等を用いることができる。   Resins include acrylic resin, alkyd resin, polyester resin, polyurethane resin, epoxy resin, phenol resin, melamine resin, amino resin, vinyl chloride resin, silicone resin, gum rosin that are usually used for solvent-based paints and oil-based printing inks. Rosin resins such as lime rosin, maleic acid resin, polyamide resin, nitrocellulose, ethylene-vinyl acetate copolymer resin, rosin modified phenolic resin, rosin modified maleic resin and other rosin modified resins, petroleum resins and the like can be used. . For water-based paints, water-soluble acrylic resins, water-soluble styrene-maleic acid resins, water-soluble alkyd resins, water-soluble melamine resins, water-soluble urethane emulsion resins, water-soluble epoxies commonly used for water-based paints and water-based inks Resins, water-soluble polyester resins, and the like can be used.

溶剤としては、溶剤系塗料用に通常使用されている大豆油、トルエン、キシレン、シンナー、ブチルアセテート、メチルアセテート、メチルイソブチルケトン、メチルセロソルブ、エチルセロソルブ、プロピルセロソルブ、ブチルセロソルブ、プロピレングリコールモノメチルエーテル等のグリコールエーテル系溶剤、酢酸エチル、酢酸ブチル、酢酸アミル等のエステル系溶剤、ヘキサン、ヘプタン、オクタン等の脂肪族炭化水素系溶剤、シクロヘキサン等の脂環族炭化水素系溶剤、ミネラルスピリット等の石油系溶剤、アセトン、メチルエチルケトン等のケトン系溶剤、メチルアルコール、エチルアルコール、プロピルアルコール、ブチルアルコール等のアルコール系溶剤、脂肪族炭化水素等を用いることができる。   Solvents include soybean oil, toluene, xylene, thinner, butyl acetate, methyl acetate, methyl isobutyl ketone, methyl cellosolve, ethyl cellosolve, propyl cellosolve, butyl cellosolve, propylene glycol monomethyl ether, etc. Glycol ether solvents, ester solvents such as ethyl acetate, butyl acetate, and amyl acetate, aliphatic hydrocarbon solvents such as hexane, heptane, and octane, alicyclic hydrocarbon solvents such as cyclohexane, and petroleum-based solvents such as mineral spirits Solvents, ketone solvents such as acetone and methyl ethyl ketone, alcohol solvents such as methyl alcohol, ethyl alcohol, propyl alcohol, and butyl alcohol, aliphatic hydrocarbons, and the like can be used.

水系塗料用溶剤としては、水と水系塗料用に通常使用されているエチルアルコール、プロピルアルコール、ブチルアルコール等のアルコール系溶剤、メチルセロソルブ、エチルセロソルブ、プロピルセロソルブ、ブチルセロソルブ等のグリコールエーテル系溶剤、ジエチレングリコール、トリエチレングリコール、ポリエチレングリコール、ジプロピレングリコール、トリプロピレングリコール、ポリプロピレングリコール等のオキシエチレン又はオキシプロピレン付加重合体、エチレングリコール、プロピレングリコール、１，２，６−ヘキサントリオール等のアルキレングリコール、グリセリン、２−ピロリドン等の水溶性有機溶剤とを混合して使用することができる。   Water-based paint solvents include water and alcohol-based solvents usually used for water-based paints such as ethyl alcohol, propyl alcohol and butyl alcohol, methyl cellosolve, ethyl cellosolve, propyl cellosolve, butyl cellosolve and other glycol ether solvents, diethylene glycol , Oxyethylene or oxypropylene addition polymers such as triethylene glycol, polyethylene glycol, dipropylene glycol, tripropylene glycol, polypropylene glycol, alkylene glycol such as ethylene glycol, propylene glycol, 1,2,6-hexanetriol, glycerin, It can be used by mixing with a water-soluble organic solvent such as 2-pyrrolidone.

油脂としては、あまに油、きり油、オイチシカ油、サフラワー油等の乾性油を加工したボイル油を用いることができる。   As oils and fats, boil oils obtained by processing dry oils such as linseed oil, persimmon oil, sea lion oil, safflower oil and the like can be used.

消泡剤としては、ノプコ８０３４（商品名）、ＳＮデフォーマー４７７（商品名）、ＳＮデフォーマー５０１３（商品名）、ＳＮデフォーマー２４７（商品名）、ＳＮデフォーマー３８２（商品名）（以上、いずれもサンノプコ株式会社製）、アンチホーム０８（商品名）、エマルゲン９０３（商品名）（以上、いずれも花王株式会社製）等の市販品を使用することができる。   Antifoaming agents include Nopco 8034 (product name), SN deformer 477 (product name), SN deformer 5013 (product name), SN deformer 247 (product name), SN deformer 382 (product name) (all of these are San Nopco Commercially available products such as manufactured by Co., Ltd., Antihome 08 (trade name), Emulgen 903 (trade name) (all of which are manufactured by Kao Corporation) can be used.

次に、本発明に係る赤外線反射性青色顔料を含有する樹脂組成物について述べる。   Next, the resin composition containing the infrared reflective blue pigment according to the present invention will be described.

本発明に係る樹脂組成物中における赤外線反射性青色顔料の配合割合は、樹脂１００重量部に対して０．０１〜２００重量部の範囲で使用することができ、樹脂組成物のハンドリング性を考慮すれば、好ましくは０．０５〜１５０重量部、更に好ましくは０．１〜１００重量部である。   The blending ratio of the infrared reflective blue pigment in the resin composition according to the present invention can be used in the range of 0.01 to 200 parts by weight with respect to 100 parts by weight of the resin, and the handling property of the resin composition is taken into consideration. Thus, the amount is preferably 0.05 to 150 parts by weight, more preferably 0.1 to 100 parts by weight.

本発明に係る樹脂組成物における構成基材としては、赤外線反射性青色顔料と周知の熱可塑性樹脂とともに、必要により、滑剤、可塑剤、酸化防止剤、紫外線吸収剤、各種安定剤等の添加剤が配合される。   As a constituent substrate in the resin composition according to the present invention, an infrared reflective blue pigment and a known thermoplastic resin, and additives such as a lubricant, a plasticizer, an antioxidant, an ultraviolet absorber, and various stabilizers as necessary. Is blended.

樹脂としては、ポリエチレン、ポリプロピレン、ポリブテン、ポリイソブチレン等のポリオレフィン、ポリ塩化ビニル、ポリメチルペンテン、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリスチレン、スチレン−アクリル酸エステル共重合体、スチレン−酢酸ビニル共重合体、アクリロニトリル−ブタジエン−スチレン共重合体、アクリロニトリル−ＥＰＤＭ−スチレン共重合体、アクリル系樹脂、ポリアミド、ポリカーボネート、ポリアセタール、ポリウレタン等の熱可塑性樹脂、ロジン変性マレイン酸樹脂、フェノール樹脂、エポキシ樹脂、ポリエステル樹脂、シリコーン樹脂、ロジン・エステル、ロジン、天然ゴム、合成ゴム等を用いることができる。   Examples of the resin include polyolefins such as polyethylene, polypropylene, polybutene, and polyisobutylene, polyvinyl chloride, polymethylpentene, polyethylene terephthalate, polybutylene terephthalate, polystyrene, styrene-acrylic acid ester copolymer, styrene-vinyl acetate copolymer, Acrylonitrile-butadiene-styrene copolymer, acrylonitrile-EPDM-styrene copolymer, acrylic resin, polyamide, polycarbonate, polyacetal, polyurethane and other thermoplastic resins, rosin-modified maleic acid resin, phenol resin, epoxy resin, polyester resin, Silicone resin, rosin ester, rosin, natural rubber, synthetic rubber and the like can be used.

添加剤の量は、赤外線反射性青色顔料と樹脂との総和に対して５０重量％以下であればよい。添加剤の含有量が５０重量％を超える場合には、成形性が低下する。   The amount of the additive may be 50% by weight or less based on the total of the infrared reflective blue pigment and the resin. When the content of the additive exceeds 50% by weight, the moldability is lowered.

本発明に係る樹脂組成物は、樹脂原料と赤外線反射性青色顔料をあらかじめよく混合し、次に、混練機もしくは押出機を用いて加熱下で強いせん断作用を加えて、赤外線反射性青色顔料の凝集体を破壊し、樹脂組成物中に赤外線反射性青色顔料を均一に分散させた後、目的に応じた形状に成形加工して使用する。   The resin composition according to the present invention is prepared by mixing a resin raw material and an infrared reflective blue pigment in advance, and then applying a strong shearing action under heating using a kneader or an extruder, The aggregate is broken and the infrared reflective blue pigment is uniformly dispersed in the resin composition, and then molded into a shape according to the purpose and used.

また本発明に係る樹脂組成物は、マスターバッチペレットを経由して得ることもできる。   The resin composition according to the present invention can also be obtained via a master batch pellet.

本発明におけるマスターバッチペレットは、塗料及び樹脂組成物の構成基材としての結合材樹脂と前記赤外線反射性青色顔料とを必要により、リボンブレンダー、ナウターミキサー、ヘンシェルミキサー、スーパーミキサー等の混合機で混合した後、周知の単軸混練押出機や二軸混練押出機等で混練、成形した後切断するか、又は、上記混合物をバンバリーミキサー、加圧ニーダー等で混練して得られた混練物を粉砕又は成形、切断することにより製造される。   The master batch pellet in the present invention is a blender such as a ribbon blender, a Nauter mixer, a Henschel mixer, a super mixer, etc., if necessary, a binder resin as a constituent substrate of the paint and the resin composition and the infrared reflective blue pigment. Kneaded with a well-known single-screw kneading extruder or twin-screw kneading extruder, etc., then cut or kneaded with the above mixture with a Banbury mixer, pressure kneader or the like It is manufactured by crushing, molding or cutting.

結合材樹脂と赤外線反射性青色顔料の混練機への供給は、それぞれを所定比率で定量供給してもよいし、両者の混合物を供給してもよい。   As for the supply of the binder resin and the infrared reflective blue pigment to the kneader, each of them may be supplied at a predetermined ratio, or a mixture of both may be supplied.

本発明におけるマスターバッチペレットは、平均長径１〜６ｍｍ、好ましくは２〜５ｍｍの範囲である。平均短径は２〜５ｍｍ、好ましくは２．５〜４ｍｍである。平均長径が１ｍｍ未満の場合には、ペレット製造時の作業性が悪く好ましくない。６ｍｍを超える場合には、希釈用結合材樹脂の大きさとの違いが大きく、十分に分散させるのが困難となる。また、その形状は種々のものができ、不定形及び球形等の粒状、円柱形、フレーク状等にできる。   The master batch pellet in the present invention has an average major axis of 1 to 6 mm, preferably 2 to 5 mm. The average minor axis is 2 to 5 mm, preferably 2.5 to 4 mm. When the average major axis is less than 1 mm, the workability at the time of producing the pellet is poor, which is not preferable. When the thickness exceeds 6 mm, the difference from the size of the binder resin for dilution is large, and it becomes difficult to sufficiently disperse. Moreover, the shape can be various, and can be indefinite and spherical, cylindrical, flakes, and the like.

本発明におけるマスターバッチペレットに使用する結合材樹脂としては、前記樹脂組成物用樹脂と同一の樹脂が使用できる。   As the binder resin used for the master batch pellet in the present invention, the same resin as the resin for resin composition can be used.

なお、マスターバッチペレット中の結合材樹脂の組成は、希釈用結合材樹脂と同一の樹脂を用いても、また、異なる樹脂を用いてもよいが、異なる樹脂を使用する場合には、樹脂同士の相溶性により決まる諸特性を考慮して決めればよい。   The composition of the binder resin in the masterbatch pellet may be the same resin as the diluent binder resin or a different resin, but if different resins are used, What is necessary is just to determine in consideration of the various characteristics determined by the compatibility.

マスターバッチペレット中に配合される赤外線反射性青色顔料の量は、結合材樹脂１００重量部に対して１〜２００重量部、好ましくは１〜１５０重量部、より好ましくは１〜１００重量部である。１重量部未満の場合には、混練時の溶融粘度が不足し、赤外線反射性青色顔料の良好な分散混合が困難である。２００重量部を超える場合には、赤外線反射性青色顔料に対する結合材樹脂が少ないため、赤外線反射性青色顔料の良好な分散混合が難しく、また、マスターバッチペレットの添加量のわずかな変化によって樹脂組成物中に配合される赤外線反射性青色顔料の含有量が大きく変化するため所望の含有量に調製することが困難となり好ましくない。また、機械摩耗が激しく適当ではない。   The amount of the infrared reflective blue pigment blended in the master batch pellet is 1 to 200 parts by weight, preferably 1 to 150 parts by weight, more preferably 1 to 100 parts by weight with respect to 100 parts by weight of the binder resin. . When the amount is less than 1 part by weight, the melt viscosity at the time of kneading is insufficient, and it is difficult to disperse and mix the infrared reflective blue pigment. When the amount exceeds 200 parts by weight, the amount of the binder resin for the infrared reflective blue pigment is small, so that it is difficult to disperse and mix the infrared reflective blue pigment. Since the content of the infrared-reflective blue pigment blended in the product greatly changes, it is difficult to prepare the desired content, which is not preferable. Also, mechanical wear is severe and not suitable.

＜作用＞
本発明において最も重要な点は、本発明に係る赤外線反射性青色顔料は、有害元素を含有することなく、高い赤外線反射性を有するという事実である。 <Action>
The most important point in the present invention is the fact that the infrared-reflective blue pigment according to the present invention has high infrared reflectivity without containing harmful elements.

本発明に係る赤外線反射性青色顔料が青色でかつ高い赤外線反射性を有する理由は、未だ明らかではないが、後出する実施例及び比較例から明らかなとおり、Ｃｏ、ＡｌとともにＭｇを含有させ、Ｍｇの含有量を該青色顔料の全金属元素に対するモル比で１１〜２２％とし、かつ該青色顔料のＢＥＴ比表面積を１０〜１００ｍ２／ｇとすることで、青色でかつ日射反射率を向上させることができたものである。 The reason why the infrared-reflective blue pigment according to the present invention is blue and has high infrared reflectivity is not yet clear, but as will be apparent from Examples and Comparative Examples described later, Co and Al are included together with Mg, By making the Mg content a molar ratio of the blue pigment to all metal elements of 11 to 22% and the BET specific surface area of the blue pigment of 10 to 100 m 2 / g, it is blue and the solar reflectance is improved. It was possible to make it.

また、本発明に係る赤外線反射性青色顔料は、Ｃｒ６＋などの有害金属元素を含有しておらず、安全な顔料である。 Further, the infrared reflective blue pigment according to the present invention does not contain a harmful metal element such as Cr 6+ and is a safe pigment.

本発明の代表的な実施例は、次の通りである。   A typical embodiment of the present invention is as follows.

粒子の平均粒子径は電子顕微鏡写真に示される粒子３５０個の粒子径をそれぞれ測定し、その平均値で示した。   The average particle size of the particles was measured by measuring the particle size of 350 particles shown in the electron micrograph, and the average value was shown.

比表面積は、ＢＥＴ法により測定した値で示した。   The specific surface area was shown by the value measured by BET method.

赤外線反射性青色顔料の金属元素の含有量は、「蛍光Ｘ線分析装置３０６３Ｍ型」（理学電機工業株式会社製）を使用し、ＪＩＳ Ｋ０１１９の「けい光Ｘ線分析通則」に従って測定した。   The content of the metal element of the infrared reflective blue pigment was measured using a “fluorescence X-ray analyzer 3063M type” (manufactured by Rigaku Denki Kogyo Co., Ltd.) in accordance with “General X-ray fluorescence analysis rules” of JIS K0119.

Ｃｒ６＋の測定方法は、「ＩＣＰ発光分光分析装置」（エスエスアイ・ナノテクノロジー（株）社製）を使用し、ＪＩＳ Ｋ０１０２ ６５．２．４の「ＩＣＰ 発光分光分析法」に従って測定した。 The measuring method of Cr 6+ was measured according to “ICP emission spectroscopic method” of JIS K0102 652.4 using “ICP emission spectroscopic analyzer” (manufactured by SSI Nanotechnology Co., Ltd.).

赤外線反射性青色顔料の色相（Ｌ＊値、ａ＊値、ｂ＊値）は、試料０．５ｇとヒマシ油０．５ｍｌとをフーバー式マーラーで練ってペースト状とし、このペーストにクリアラッカー４．５ｇを加え、混練、塗料化してキャストコート紙上に１５０μｍ（６ｍｉｌ）のアプリケーターを用いて塗布した塗布片（塗膜厚み：約３０μｍ）を作製した塗膜片について、「多光源分光測色計ＭＳＣ−ＩＳ−２Ｄ」（スガ試験機株式会社製）を用いて測定を行い、ＪＩＳ Ｚ ８７２９に定めるところに従って表色指数（Ｌ＊値、ａ＊値、ｂ＊値）で示した。 The hue (L * value, a * value, b * value) of the infrared reflective blue pigment was prepared by mixing 0.5 g of a sample and 0.5 ml of castor oil with a Hoover-type Mahler to form a paste. .5 g, kneaded and coated to form a coating piece (coating thickness: about 30 μm) coated on cast-coated paper using a 150 μm (6 mil) applicator. Measurement was performed using “MSC-IS-2D” (manufactured by Suga Test Instruments Co., Ltd.), and the color index (L * value, a * value, b * value) was indicated according to JIS Z 8729.

赤外線反射性青色顔料の日射特性は、上記の色相を測定するために作製した塗膜片について、「分光光度計 Ｕ−４１００」（株式会社日立ハイテクノロジーズ）を用いて測定を行い、ＪＩＳ Ｒ３１０６−１９９８に定めるところに従って波長３００〜２１００ｎｍにおける日射反射率（％）で示した。   The solar radiation characteristics of the infrared reflective blue pigment were measured using “spectrophotometer U-4100” (Hitachi High-Technologies Corporation) for the coating film piece prepared for measuring the above hue, and JIS R3106. The solar reflectance (%) at a wavelength of 300 to 2100 nm is shown in accordance with 1998.

実施例１
ＣｏＯとＭｇＯ、Ａｌ２Ｏ３をＣｏＯｘ・ＭｇＯ１−ｘ・ｎＡｌ２Ｏ３（ｘ＝０．５，ｎ＝１）となるように計量、混合し電気炉で１０５０℃で２時間焼成した。焼成品を粉砕し平均粒子径０．２μｍ、ＢＥＴ比表面積３６ｍ２／ｇの青色顔料を得た。得られた青色顔料の結晶構造はスピネル型であった。 Example 1
CoO, MgO, and Al 2 O 3 were weighed and mixed so as to be CoO x · MgO 1-x · nAl 2 O 3 (x = 0.5, n = 1) and baked in an electric furnace at 1050 ° C. for 2 hours. . The fired product was pulverized to obtain a blue pigment having an average particle size of 0.2 μm and a BET specific surface area of 36 m 2 / g. The crystal structure of the obtained blue pigment was a spinel type.

この顔料をラッカー色塗りし色見本試料を作製し、Ｕ−４１００日立分光光度計を用いて波長２５０ｎｍ〜２５００ｎｍ範囲で反射率を評価した。結果は、波長３００〜２１００ｎｍにおける反射率が５０％であった。   A swatch sample was prepared by coating this pigment with a lacquer color, and the reflectance was evaluated in the wavelength range of 250 nm to 2500 nm using a U-4100 Hitachi spectrophotometer. As a result, the reflectance at a wavelength of 300 to 2100 nm was 50%.

実施例２〜３、比較例１〜４
組成割合及び焼成温度を変化させた以外は前記実施例１と同様にして青色顔料を得た。 Examples 2-3 and Comparative Examples 1-4
A blue pigment was obtained in the same manner as in Example 1 except that the composition ratio and the firing temperature were changed.

このときの製造条件を表１に、得られた赤外線反射性青色顔料の諸特性を表２に示す。   The production conditions at this time are shown in Table 1, and the properties of the obtained infrared reflective blue pigment are shown in Table 2.

実施例４
前記実施例１と同様にして青色顔料を得た。次いで、得られた青色顔料を水中に湿式分散させ、７０℃に保温した青色顔料のスラリーに対し水ガラス０．５ｗｔ％を滴下しながら塩酸及び水酸化ナトリウムでｐＨ７に調整し１時間維持した。その後、水洗・乾燥・粉砕処理した。 Example 4
A blue pigment was obtained in the same manner as in Example 1. Next, the obtained blue pigment was wet-dispersed in water, adjusted to pH 7 with hydrochloric acid and sodium hydroxide while dropping 0.5 wt% of water glass to the blue pigment slurry kept at 70 ° C., and maintained for 1 hour. Then, it washed with water, dried and pulverized.

実施例５及び実施例６
表面処理条件を変化させた以外は前記実施例４と同様にして青色顔料を得た。 Example 5 and Example 6
A blue pigment was obtained in the same manner as in Example 4 except that the surface treatment conditions were changed.

表２における結晶構造のうち、「ｓｐｉｎｅｌ」はスピネル型を示すものである。なお、Ｃｒ６＋の含有量が「５ｐｐｍ未満」とは、前記測定装置の検出限界以下であることを示す。 Of the crystal structures in Table 2, “spinel” indicates a spinel type. The Cr 6+ content “less than 5 ppm” indicates that the content is below the detection limit of the measuring device.

Figure 2009215385
Figure 2009215385

Figure 2009215385
Figure 2009215385

本発明に係る赤外線反射性青色顔料は、赤外線反射性に優れているので赤外線反射性青色顔料として好適である。   Since the infrared reflective blue pigment according to the present invention is excellent in infrared reflectivity, it is suitable as an infrared reflective blue pigment.

Claims (7)

Ｃｏ、Ａｌ及びＭｇを含有する複合酸化物からなる青色顔料であって、該青色顔料のＭｇ含有量が全金属元素に対するモル比で１１〜２２％であり、該青色顔料のＢＥＴ比表面積が１０〜１００ｍ２／ｇであることを特徴とする赤外線反射性青色顔料。 A blue pigment comprising a composite oxide containing Co, Al and Mg, wherein the blue pigment has a Mg content of 11 to 22% in terms of a molar ratio to all metal elements, and the BET specific surface area of the blue pigment is 10 Infrared reflective blue pigment characterized in that it is ˜100 m 2 / g. 請求項１記載の赤外線反射性青色顔料の結晶構造がスピネル型である赤外線反射性青色顔料。   An infrared reflective blue pigment, wherein the crystal structure of the infrared reflective blue pigment according to claim 1 is a spinel type. 請求項１又は２記載の赤外線反射性青色顔料の明度（Ｌ＊）が３５〜５０である赤外線反射性青色顔料。 The infrared reflective blue pigment whose brightness (L * ) of the infrared reflective blue pigment of Claim 1 or 2 is 35-50. 請求項１乃至３のいずれか１項に記載の赤外線反射性青色顔料の日射反射率が４５〜６０％である赤外線反射性青色顔料。   The infrared reflective blue pigment whose solar reflectance of the infrared reflective blue pigment of any one of Claims 1 thru | or 3 is 45 to 60%. 請求項１乃至４のいずれか１項に記載の赤外線反射性青色顔料の表面がＳｉ、Ａｌ、Ｚｒ、Ｔｉから選ばれる一種以上の化合物で被覆されている赤外線反射性青色顔料。   The infrared reflective blue pigment in which the surface of the infrared reflective blue pigment of any one of Claims 1 thru | or 4 is coat | covered with the 1 or more types of compound chosen from Si, Al, Zr, Ti. 請求項１乃至５のいずれか１項に記載の赤外線反射性青色顔料を塗料構成基材中に配合した塗料。   The coating material which mix | blended the infrared reflective blue pigment of any one of Claims 1 thru | or 5 in the coating-material base material. 請求項１乃至５のいずれか１項に記載の赤外線反射性青色顔料を用いて着色した樹脂組成物。   A resin composition colored using the infrared reflective blue pigment according to claim 1.
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