JP2010155938A - Near-infrared absorbent and dispersion thereof - Google Patents
Near-infrared absorbent and dispersion thereof Download PDFInfo
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- 239000006185 dispersion Substances 0.000 title claims abstract description 58
- 230000002745 absorbent Effects 0.000 title claims abstract description 13
- 239000002250 absorbent Substances 0.000 title claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 37
- 150000002334 glycols Chemical group 0.000 claims abstract description 21
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 14
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical group [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000006096 absorbing agent Substances 0.000 claims description 53
- 239000012756 surface treatment agent Substances 0.000 claims description 43
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- FRQDZJMEHSJOPU-UHFFFAOYSA-N Triethylene glycol bis(2-ethylhexanoate) Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CCCC FRQDZJMEHSJOPU-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000012046 mixed solvent Substances 0.000 claims description 11
- GCDUWJFWXVRGSM-UHFFFAOYSA-N 2-[2-(2-heptanoyloxyethoxy)ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOC(=O)CCCCCC GCDUWJFWXVRGSM-UHFFFAOYSA-N 0.000 claims description 5
- SSKNCQWPZQCABD-UHFFFAOYSA-N 2-[2-[2-(2-heptanoyloxyethoxy)ethoxy]ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOCCOC(=O)CCCCCC SSKNCQWPZQCABD-UHFFFAOYSA-N 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- OJXOOFXUHZAXLO-UHFFFAOYSA-M magnesium;1-bromo-3-methanidylbenzene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C1=CC=CC(Br)=C1 OJXOOFXUHZAXLO-UHFFFAOYSA-M 0.000 claims description 5
- JEYLQCXBYFQJRO-UHFFFAOYSA-N 2-[2-[2-(2-ethylbutanoyloxy)ethoxy]ethoxy]ethyl 2-ethylbutanoate Chemical compound CCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CC JEYLQCXBYFQJRO-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 125000003827 glycol group Chemical group 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- 239000010409 thin film Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- 239000000843 powder Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000002834 transmittance Methods 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 description 1
- 229910021617 Indium monochloride Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 description 1
- 239000005340 laminated glass Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- -1 phosphate ester Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
本発明は、近赤外線の吸収効果に優れ、液中での分散性が良く、薄膜のヘーズが低い近赤外線吸収剤とその分散液に関する。 The present invention relates to a near-infrared absorber that has an excellent near-infrared absorption effect, good dispersibility in a liquid, and low haze of a thin film and a dispersion thereof.
近赤外線の吸収効果に優れた材料として、インジウム錫酸化物（ＩＴＯ）、およびアンチモン錫酸化物（ＡＴＯ）が知られており、さらに、その改良がなされている。例えば、特開平６−２４７７１６号公報（特許文献１）には、ＩＴＯ粉末を有機溶媒に含浸させ、不活性ガス定雰囲気下で熱処理することによって、インジウムと錫の合計量に対して、１〜１５モル％の錫を含有するインジウム錫酸化物（ＩＴＯ）からなる粉末が記載されている。 Indium tin oxide (ITO) and antimony tin oxide (ATO) are known as materials having an excellent near-infrared absorption effect, and further improvements have been made. For example, in JP-A-6-247716 (Patent Document 1), by impregnating an ITO powder in an organic solvent and heat-treating under a constant inert gas atmosphere, the total amount of indium and tin is 1 to 1. A powder consisting of indium tin oxide (ITO) containing 15 mol% tin is described.
この粉末はＩＴＯの一部が還元されてキャリア濃度が向上することによって抵抗が低下し、導電性を有すると共に、一定範囲量の錫を含有することによって青味を帯びた色調を有するようになる。また、このＩＴＯ粉末は高いキャリア密度に起因する近赤外線カット特性を有しているため、樹脂もしくは溶媒中に均一に分散することによって、可視光線に対して非常に高透明かつ近赤外線を効果的にカットすることが可能である。従って、このＩＴＯ粉末を用いることによって、優れた近赤外線カット特性と高い可視光線透過率、低ヘーズを兼ね備えた中間膜および合わせガラスを得ることが可能である（特開２００５−１８７２２６号公報：特許文献２）。 This powder is reduced in resistance by part of ITO being reduced and the carrier concentration is lowered, and it has conductivity, and has a bluish color tone by containing a certain amount of tin. . In addition, this ITO powder has a near-infrared cut characteristic due to a high carrier density, so it is very transparent to visible light and effective in the near-infrared by being uniformly dispersed in a resin or solvent. It is possible to cut into Therefore, by using this ITO powder, it is possible to obtain an intermediate film and a laminated glass having both excellent near-infrared cut characteristics, high visible light transmittance, and low haze (Japanese Patent Laid-Open No. 2005-187226: Patent) Reference 2).
しかし、より高い近赤外線カット特性を得るためには、膜中のＩＴＯ微粒子含有量を増加させる必要があり、ＩＴＯ微粒子含有量が増加すると、粒子による可視光線の散乱も増加するため膜ヘーズも高くなりやすいという問題があった。
本発明は、近赤外線吸収剤として用いられているＩＴＯ粉末やＡＴＯ粉末等について、従来の上記問題を解決したものであり、近赤外線の吸収効果に優れ、液中での分散性が良く、薄膜でのヘーズが低い近赤外線吸収剤とその分散液を提供する。 The present invention solves the above-mentioned problems with ITO powder and ATO powder used as near-infrared absorbers, has excellent near-infrared absorption effect, good dispersibility in liquid, and thin film A near-infrared absorber having a low haze and a dispersion thereof are provided.
本発明は上記課題を解決する手段として以下の構成を有する近赤外線吸収剤に関する。
〔１〕近赤外線吸収剤の分散液を形成する溶媒と同成分または溶媒の主成分と同成分の表面処理剤によって近赤外線吸収剤の表面が修飾されていることを特徴とする近赤外線吸収剤。
〔２〕近赤外線吸収剤がインジウム錫酸化物（ＩＴＯ）またはアンチモン錫酸化物（ＡＴＯ）である請求項１に記載する近赤外線吸収剤。
〔３〕表面処理剤がグリコール類である請求項１または請求項２に記載する近赤外線吸収剤。
〔４〕表面処理剤が、ジヘキシルアジペート、トリエチレングリコール−ジ−２−エチルヘキサノエート、テトラエチレングリコール−ジ−２−エチルヘキサノエート、トリエチレングリコール−ジ−２−エチルブチレート、テトラエチレングリコール−ジ−２−エチルブチレート、テトラエチレングリコール−ジ−ヘプタノエート、およびトリエチレングリコール−ジ−ヘプタノエートからなる群より選択される少なくとも１種である請求項１〜請求項３の何れかに記載する近赤外線吸収剤。
The present invention relates to a near-infrared absorber having the following configuration as means for solving the above problems.
[1] A near-infrared absorber, wherein the surface of the near-infrared absorber is modified with a surface treatment agent of the same component as the solvent forming the dispersion of the near-infrared absorber or the main component of the solvent. .
[2] The near infrared absorber according to claim 1, wherein the near infrared absorber is indium tin oxide (ITO) or antimony tin oxide (ATO).
[3] The near-infrared absorber according to claim 1 or 2, wherein the surface treatment agent is a glycol.
[4] Surface treatment agent is dihexyl adipate, triethylene glycol-di-2-ethylhexanoate, tetraethylene glycol-di-2-ethylhexanoate, triethylene glycol-di-2-ethylbutyrate, tetra 4. It is at least one selected from the group consisting of ethylene glycol-di-2-ethylbutyrate, tetraethylene glycol-di-heptanoate, and triethylene glycol-di-heptanoate. The near-infrared absorber to describe.
さらに本発明は、上記課題を解決する手段として以下の構成を有する近赤外線吸収剤分散液に関する。
〔５〕表面処理剤によって修飾された近赤外線吸収剤が、該表面処理剤と同成分または該表面処理剤の主成分と同成分の溶媒に分散されていることを特徴とする近赤外線吸収剤分散液。
〔６〕近赤外線吸収剤がインジウム錫酸化物（ＩＴＯ）またはアンチモン錫酸化物（ＡＴＯ）である請求項５に記載する近赤外線吸収剤分散液。
〔７〕表面処理剤がグリコール類であり、分散溶媒がグリコール類またはグリコール類を主成分としアルコールを含む混合溶媒である請求項５または請求項６に記載する近赤外線吸収剤分散液。
〔８〕表面処理剤が、ジヘキシルアジペート、トリエチレングリコール−ジ−２−エチルヘキサノエート、テトラエチレングリコール−ジ−２−エチルヘキサノエート、トリエチレングリコール−ジ−２−エチルブチレート、テトラエチレングリコール−ジ−２−エチルブチレート、テトラエチレングリコール−ジ−ヘプタノエート、およびトリエチレングリコール−ジ−ヘプタノエートからなる群より選択される少なくとも１種であり、分散溶媒が上記グリコール類とアルコールおよび水の混合溶媒である請求項５〜請求項７の何れかに記載する近赤外線吸収剤分散液。
〔９〕分散溶媒が、トリエチレングリコール−ジ−２−エチルヘキサノエート、またはトリエチレングリコール−ジ−２−エチルヘキサノエートとエタノールと水の混合溶媒である請求項８に記載する近赤外線吸収剤分散液。
Furthermore, this invention relates to the near-infrared absorber dispersion liquid which has the following structures as a means to solve the said subject.
[5] A near-infrared absorber, wherein the near-infrared absorber modified with the surface treatment agent is dispersed in the same component as the surface treatment agent or a solvent of the same component as the main component of the surface treatment agent. Dispersion.
[6] The near-infrared absorber dispersion according to claim 5, wherein the near-infrared absorber is indium tin oxide (ITO) or antimony tin oxide (ATO).
[7] The near-infrared absorber dispersion according to claim 5 or 6, wherein the surface treatment agent is glycols, and the dispersion solvent is glycols or a mixed solvent containing glycols as a main component and alcohol.
[8] Surface treatment agent is dihexyl adipate, triethylene glycol-di-2-ethylhexanoate, tetraethylene glycol-di-2-ethylhexanoate, triethylene glycol-di-2-ethylbutyrate, tetra And at least one selected from the group consisting of ethylene glycol-di-2-ethylbutyrate, tetraethylene glycol-di-heptanoate, and triethylene glycol-di-heptanoate, and the dispersion solvent is the glycols, alcohol and water. The near-infrared absorber dispersion liquid according to any one of claims 5 to 7, wherein
[9] The near infrared ray according to claim 8, wherein the dispersion solvent is triethylene glycol-di-2-ethylhexanoate, or a mixed solvent of triethylene glycol-di-2-ethylhexanoate, ethanol and water. Absorbent dispersion.
本発明の近赤外線吸収剤およびその分散液は、近赤外線吸収剤の表面が分散溶媒の主成分と同成分の表面処理剤によって修飾されているので、近赤外線吸収剤と分散溶媒の親和性がよく、アルコールによって表面処理したものよりも近赤外線吸収剤の分散性が良い。このため、従来よりも近赤外線吸収剤の分散性に優れた分散液を形成することが可能であり、近赤外線吸収特性に優れ、かつ分散液のヘーズが低い薄膜を形成することができる。また、分散時間の短縮も図れる。 The near-infrared absorber of the present invention and the dispersion liquid thereof have an affinity between the near-infrared absorber and the dispersion solvent because the surface of the near-infrared absorber is modified with the same surface treatment agent as the main component of the dispersion solvent. The dispersibility of the near-infrared absorber is better than that surface-treated with alcohol. For this reason, it is possible to form a dispersion excellent in dispersibility of near-infrared absorbers than before, and to form a thin film having excellent near-infrared absorption characteristics and low dispersion haze. Also, the dispersion time can be shortened.
以下、本発明を実施形態に基づいて具体的に説明する。
本発明の近赤外線吸収剤は、近赤外線吸収剤の分散液を形成する溶媒と同成分または溶媒の主成分と同成分の表面処理剤によって近赤外線吸収剤の表面が修飾されていることを特徴とする近赤外線吸収剤である。
Hereinafter, the present invention will be specifically described based on embodiments.
The near-infrared absorber of the present invention is characterized in that the surface of the near-infrared absorber is modified with the same component as the solvent forming the dispersion of the near-infrared absorber or the surface treatment agent of the same component as the main component of the solvent. It is a near infrared absorber.
近赤外線吸収剤としては、インジウム錫酸化物（ＩＴＯ）、またはアンチモン錫酸化物（ＡＴＯ）を用いることができる。 As the near-infrared absorber, indium tin oxide (ITO) or antimony tin oxide (ATO) can be used.
表面処理剤としては、例えば、グリコール類、またはグリコール類を主成分としアルコールを含む混合溶液を用いることができる。同様に、分散溶媒としては、グリコール類、またはグリコール類を主成分としアルコールを含む混合溶液を用いることができる。 As the surface treatment agent, for example, glycols or a mixed solution containing glycols as a main component and alcohol can be used. Similarly, as the dispersion solvent, glycols or a mixed solution containing glycols as a main component and alcohol can be used.
表面処理剤は、分散溶媒と同成分、または分散溶媒の主成分と同成分のものを用いる。分散溶媒の主成分と同成分の表面処理剤とは、例えば、分散溶媒がグリコール類、またはグリコール類を主成分としアルコールおよび水を含む混合溶媒である場合、グリコール類を表面処理剤として用い、または、グリコール類を主成分としアルコールまたは水含む混合溶液を表面処理剤として用いる。 As the surface treatment agent, the same component as the dispersion solvent or the same component as the main component of the dispersion solvent is used. The surface treatment agent having the same component as the main component of the dispersion solvent is, for example, when the dispersion solvent is a glycol or a mixed solvent containing glycols as a main component and containing alcohol and water, and using the glycols as the surface treatment agent, Alternatively, a mixed solution containing glycols as a main component and containing alcohol or water is used as the surface treatment agent.
分散溶媒のグリコール類は、具体的には、例えば、ジヘキシルアジペート、トリエチレングリコール−ジ−２−エチルヘキサノエート、テトラエチレングリコール−ジ−２−エチルヘキサノエート、トリエチレングリコール−ジ−２−エチルブチレート、テトラエチレングリコール−ジ−２−エチルブチレート、テトラエチレングリコール−ジ−ヘプタノエート、およびトリエチレングリコール−ジ−ヘプタノエートからなる群より選択される少なくとも１種を用いることができる。 Specific examples of the dispersion solvent glycol include dihexyl adipate, triethylene glycol-di-2-ethylhexanoate, tetraethylene glycol-di-2-ethylhexanoate, and triethylene glycol-di-2. -At least one selected from the group consisting of ethyl butyrate, tetraethylene glycol-di-2-ethylbutyrate, tetraethylene glycol-di-heptanoate, and triethylene glycol-di-heptanoate can be used.
表面処理剤としてグリコール類を用いた場合、分散溶媒としては、上記グリコール類を主成分とし、アルコールを含む混合溶媒、または上記グリコール類を主成分としアルコールを含み、さらに水やオクチル酸を加えた混合溶媒などが用いることができる。なお、水やオクチル酸は表面処理時に酸化剤として作用するので、単独で使用するとキャリア密度が減少するが、グリコール類と併用することによって近赤外線吸収剤と分散溶媒の親和性を高めることができる。 When glycols are used as the surface treatment agent, the dispersion solvent is the above glycols as a main component, a mixed solvent containing alcohol, or the glycols as a main component contains alcohol, and water or octylic acid is added. A mixed solvent or the like can be used. In addition, since water and octylic acid act as an oxidizing agent during the surface treatment, the carrier density decreases when used alone, but the affinity between the near-infrared absorber and the dispersion solvent can be increased by using it together with glycols. .
ＩＴＯ粉末、ＡＴＯ粉末などの近赤外線吸収剤の表面に、分散溶媒と同成分の表面処理剤または分散溶媒の主成分と同成分の表面処理剤を吸着させることにより、近赤外線吸収剤と分散溶媒との親和性が向上し、該溶媒中での近赤外線吸収剤の分散性に優れており、アルコールによって表面処理したものよりも近赤外線吸収剤の分散性が良い。このため、分散時間を短縮することができ、さらに、従来よりも近赤外線吸収剤の分散性に優れた分散液を形成することが可能であり、近赤外線吸収特性に優れ、かつ分散液のヘーズが低い薄膜を形成することができる。 By adsorbing the surface treatment agent of the same component as the dispersion solvent or the surface treatment agent of the same component as the main component of the dispersion solvent on the surface of the near infrared absorber such as ITO powder or ATO powder, the near infrared absorber and the dispersion solvent Is improved, the dispersibility of the near-infrared absorber in the solvent is excellent, and the dispersibility of the near-infrared absorber is better than that obtained by surface treatment with alcohol. For this reason, the dispersion time can be shortened, and furthermore, it is possible to form a dispersion having better dispersibility of the near-infrared absorber than before, which has excellent near-infrared absorption characteristics and has a haze of dispersion. A thin film with a low thickness can be formed.
本発明に係る近赤外線吸収剤の分散液は、具体的には、表面処理剤によって修飾された近赤外線吸収剤が、該表面処理剤と同成分または該表面処理剤の主成分と同成分の溶媒に分散されている近赤外線吸収剤分散液である。 Specifically, the near-infrared absorbent dispersion according to the present invention is such that the near-infrared absorbent modified with the surface treatment agent is the same component as the surface treatment agent or the same component as the main component of the surface treatment agent. It is a near-infrared absorber dispersion liquid dispersed in a solvent.
近赤外線吸収剤の表面に付着している表面処理剤の量は、近赤外線吸収剤の質量に対して０.００１〜５.０％が好ましい。表面処理剤の量が上記範囲より少ないと近赤外線吸収剤の分散性を十分に高めることが難しくなる。一方、上記範囲よりも多く表面処理剤を使用しても近赤外線吸収剤の分散性は上記範囲量の場合と同程度である。 The amount of the surface treatment agent adhering to the surface of the near infrared absorber is preferably 0.001 to 5.0% with respect to the mass of the near infrared absorber. When the amount of the surface treatment agent is less than the above range, it is difficult to sufficiently enhance the dispersibility of the near infrared absorber. On the other hand, even if the surface treatment agent is used more than the above range, the dispersibility of the near-infrared absorber is almost the same as that in the above range.
表面処理の方法は、ＩＴＯ粉末、ＡＴＯ粉末などの近赤外線吸収剤を表面処理剤の溶液に浸して近赤外線吸収剤の粉末表面に表面処理剤を含浸させ、これを引上げた後に窒素ガス等の不活性ガス雰囲気下で、５０〜５００℃で、１分-〜２４時間、加熱処理すると良い。上記加熱処理によってグリコール類は還元され分解される。 The surface treatment method is carried out by immersing a near-infrared absorber such as ITO powder or ATO powder in a solution of the surface treatment agent so that the surface of the near-infrared absorber powder is impregnated with the surface treatment agent. Heat treatment is preferably performed at 50 to 500 ° C. for 1 minute to 24 hours in an inert gas atmosphere. The glycols are reduced and decomposed by the heat treatment.
以下、本発明の実施例を比較例と共に示す。
〔ＩＴＯ粉末の合成〕
ＩｎＣｌ3水溶液（In金属 350g含有）９００mLと、５５％ＳｎＣｌ4水溶液１４４ｇとを混合し、この混合水溶液を、ＮＨ4ＨＣＯ3１９００ｇを含有するアルカリ水溶液６Lに加えて６０℃の液温で３０分間反応させ、反応後、イオン交換水によって繰り返し傾斜洗浄を行った。上澄み液の電気伝導度が５０００Ω・cm以上になったところで沈殿（In/Sn共沈水酸化物）を濾別し、１１０℃で一晩乾燥した後、大気中、５５０℃で３時間焼成し、粉砕して凝集体をほぐし、ＩＴＯ粉末４４０ｇを得た。
Examples of the present invention are shown below together with comparative examples.
[Synthesis of ITO powder]
900 mL of an InCl 3 aqueous solution (containing 350 g of In metal) and 144 g of a 55% SnCl 4 aqueous solution are mixed, and this mixed aqueous solution is added to 6 L of an alkaline aqueous solution containing 1900 g of NH 4 HCO 3 and added at a liquid temperature of 60 ° C. for 30 minutes. The reaction was carried out, and after the reaction, repeated washing with ion-exchanged water was performed. The precipitate (In / Sn coprecipitated hydroxide) was filtered off when the electrical conductivity of the supernatant liquid reached 5000 Ω · cm or more, dried at 110 ° C. overnight, and then baked at 550 ° C. for 3 hours in the atmosphere. The aggregate was loosened by pulverization to obtain 440 g of ITO powder.
〔表面処理〕
上記ＩＴＯ粉末４０ｇを、表面処理剤として用いた表１に示す溶媒に浸して、ＩＴＯ粉末に下記溶媒を含浸させた後、ガラスシャーレに入れ、窒素ガス雰囲気下、３３０℃にて２時間加熱処理した。
〔surface treatment〕
40 g of the above ITO powder is immersed in the solvent shown in Table 1 used as a surface treatment agent, and after impregnating the ITO powder with the following solvent, it is placed in a glass petri dish and heated at 330 ° C. for 2 hours in a nitrogen gas atmosphere. did.
〔分散液の調製〕
表面処理されたＩＴＯ粉末１０ｇを分散混合溶媒に加え、この混合溶媒をジルコニアビーズによって６０分間攪拌して分散液を調製した。分散混合溶媒は表１に示す分散溶媒３０ｇにリン酸エステル系分散剤１ｇおよびエタノール３ｇを加えたものを用いた。
(Preparation of dispersion)
10 g of the surface-treated ITO powder was added to the dispersion mixed solvent, and this mixed solvent was stirred with zirconia beads for 60 minutes to prepare a dispersion. As the dispersion mixed solvent, a dispersion solvent obtained by adding 30 g of a dispersion solvent shown in Table 1 to 1 g of a phosphate ester dispersant and 3 g of ethanol was used.
〔分散液の評価〕
上記分散液を、トリエチレングリコール−ジ−2−エチルヘキサノエートで０.７質量%まで希釈した。この希釈液を光路長１mmのガラスセルに入れ、分光透過率を日立自記分光光度計(U−4000)を用い、規格（JIS R 3216−1998）に従って測定した。さらに、ヘーズをスガ試験機製ヘーズコンピュータ(HZ-2)を用い、規格（JIS K 7136）に従って測定した。測定結果を表１に示す。
(Evaluation of dispersion)
The dispersion was diluted to 0.7% by mass with triethylene glycol-di-2-ethylhexanoate. This diluted solution was put into a glass cell having an optical path length of 1 mm, and the spectral transmittance was measured according to the standard (JIS R 3216-1998) using a Hitachi auto-spectrometer (U-4000). Furthermore, haze was measured according to the standard (JIS K 7136) using a haze computer (HZ-2) manufactured by Suga Test Instruments. The measurement results are shown in Table 1.
〔実施例１〜３〕
実施例１：表面処理剤としてトリエチレングリコール−ジ−2−エチルヘキサノエートを用いた。
実施例２：表面処理剤としてトリエチレングリコール−ジ−2−エチルヘキサノエートに無水エタノールおよび水を含む混合溶液を用いた。
実施例３：表面処理剤としてトリエチレングリコール−ジ−2−エチルヘキサノエートにオクチル酸、無水エタノール、および水を含む混合溶液を用いた。
[Examples 1-3]
Example 1: Triethylene glycol-di-2-ethylhexanoate was used as a surface treatment agent.
Example 2: A mixed solution containing triethylene glycol-di-2-ethylhexanoate and absolute ethanol and water was used as a surface treatment agent.
Example 3 A mixed solution containing triethylene glycol-di-2-ethylhexanoate, octylic acid, absolute ethanol, and water was used as a surface treatment agent.
〔比較例１〜５〕
比較例１：表面処理剤として無水エタノールを用いた。
比較例２：表面処理剤として無水エタノールに水を加えた混合溶液を用いた。
比較例３：表面処理剤としてオクチル酸を用いた。
比較例４：表面処理剤として水を用いた。
比較例５：表面処理剤を含浸させずに窒素ガス雰囲気下、３３０℃にて２時間加熱処理した。
[Comparative Examples 1-5]
Comparative Example 1: Absolute ethanol was used as a surface treatment agent.
Comparative Example 2: A mixed solution obtained by adding water to absolute ethanol was used as a surface treatment agent.
Comparative Example 3: Octylic acid was used as the surface treatment agent.
Comparative Example 4: Water was used as the surface treatment agent.
Comparative Example 5: Heat treatment was performed at 330 ° C. for 2 hours in a nitrogen gas atmosphere without impregnation with the surface treatment agent.
表１に示すように、本発明の近赤外線吸収剤を用いた分散液（実施例１〜３）は、何れも分散時間が短く、日射透過率が６０％以下であり、近赤外線吸収効果が良い。さらに、ヘーズは０.５％以下であり、可視光線の散乱が少なく可視光線透過率が高い。 As shown in Table 1, each of the dispersions (Examples 1 to 3) using the near-infrared absorber of the present invention has a short dispersion time, a solar transmittance of 60% or less, and a near-infrared absorption effect. good. Further, the haze is 0.5% or less, visible light scattering is small, and visible light transmittance is high.
一方、比較例１〜５は、何れもヘーズ０.６％以上である。また比較例１〜２は日射透過率が低く、近赤外線吸収効果は良いが、可視光線透過率が低い。比較例３〜５はヘーズが０.７以上であり、また日射透過率が高く、近赤外線吸収効果が低い。 On the other hand, all of Comparative Examples 1 to 5 have a haze of 0.6% or more. Comparative Examples 1 and 2 have low solar transmittance and good near-infrared absorption effect, but have low visible light transmittance. In Comparative Examples 3 to 5, the haze is 0.7 or more, the solar radiation transmittance is high, and the near infrared absorption effect is low.
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