JP6441366B2 - 単結晶MgTiO3フレークの製造方法 - Google Patents
単結晶MgTiO3フレークの製造方法 Download PDFInfo
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Description
1.発明の分野
本発明は、単結晶MgTiO3フレークの製造方法、この方法により製造される単結晶MgTiO3フレークならびにそれらの使用、特に顔料としての使用、に関する。
例えば雲母、タルク、ガラスフレーク、MIO(雲母状酸化鉄)などの無機顔料は、長年、被覆されまたは未被覆のいずれかで、複数の目的のために塗料、フィルム、コーティング組成物および化粧品などの形成において用いられている。
例えば、特許文献1に記載されている方法により得られるヘキサチタン酸カリウム(K2Ti6O13)は多結晶である。そのため、それらの屈折率は同じ組成の単結晶チタン酸の屈折率より低い。さらに、高温加熱溶解工程および高温加熱焼成工程の条件は、時間がかかり、費用がかかり、および製造方法においてより複雑さをもたらす。
本発明者らは、上述の問題が解決され得ること、および顔料としての使用に適している単結晶MgTiO3フレークが、MgTiO3前駆体を形成するためにリン化合物とチタン化合物をマグネシウム化合物の存在下で混合することにより、およびその後得られた前駆体を焼成することにより効率的に製造され得ることを見出し、本発明を完成した。
(1)以下の工程:
1.少なくとも1つのチタン化合物、少なくとも1つのマグネシウム化合物および少なくとも1つのリン化合物を混合することにより、MgTiO3前駆体を形成すること、および
2.単一の焼成工程として800℃〜1400℃の範囲における温度でMgTiO3前駆体を焼成すること、
により単結晶MgTiO3フレークを製造する方法。
(3)混合工程において融剤が存在する、(1)または(2)のいずれか一に記載の方法。
(4)融剤がNa2SO4、K2SO4、NaClおよびKClの1または2以上から選択される化合物である、(3)に記載の方法。
(5)方法が焼成工程の前にMgTiO3前駆体の乾燥を含む、(2)〜(4)のいずれか一に記載の方法。
(7)(3)に記載の焼成工程において得られた生成物が熱い水で処理される、(3)〜(6)のいずれか一に記載の方法。
(8)チタン化合物が四塩化チタン、硫酸チタニル、硫酸チタンおよび三塩化チタンの1以上から選択される化合物である、(1)〜(7)のいずれか一に記載の方法。
(10)リン化合物がリン酸三ナトリウム、五酸化リン、リン酸、亜リン酸およびリン酸三カリウムの1以上から選択される化合物である、(1)〜(9)のいずれか一に記載の方法。
(11)(1)〜(10)のいずれか一に記載の方法により得られた単結晶MgTiO3フレーク。
(13)相当する円の直径と同等のものによると、10〜100μmの範囲の粒径を有する、(11)または(12)に記載の単結晶MgTiO3フレーク。
(14)塗料、インク、コーティング組成物、プラスチックまたは化粧品における、(11)〜(13)のいずれか一に記載の単結晶MgTiO3フレークの使用。
本発明によると、顔料としての使用に適している単結晶MgTiO3フレークを効率的に製造する方法を提供することができる。
以下、本発明による単結晶MgTiO3フレークの製造方法およびこの方法により得られた単結晶MgTiO3フレークが詳細に記載される。しかしながら、本発明の意図が続く限り、これらの特別な態様に限定されない。
以下、本発明の製造方法を詳細に説明する。
その上、急なpH変化を抑制するためにチタン化合物の添加はより時間をかけて徐々に行うことが望ましい。
− MgTiO3フレークを乾燥するために、MgTiO3フレークを乾燥するための工程(以下、「乾燥工程2」と略す)。本工程はこれに限定されないが、この乾燥工程は好ましくは20℃〜180℃の温度範囲で実施される。
無機チタン化合物は、好ましくは無機チタン塩である。チタン塩の例は:四塩化チタン、硫酸チタニル、硫酸チタンおよびトリクロロチタンである。しかしながら、費用や入手しやすさの観点から、四塩化チタンおよび硫酸チタンが好ましい。ここで、使用されるチタン化合物の種類は1つの種類に限られず、少なくとも2つの種類が共に用いられ得る。
脱イオン水1600gに、5.6gのリン酸ナトリウムを加え95℃に加熱しながら撹拌する。この溶液に水酸化ナトリウム水溶液(32.0%濃度)でpHを調整しながら2時間にわたって総量210gの四塩化チタン溶液(四塩化チタン64gおよびに塩化マグネシウム10gを含む、水中における32.0%濃度)を加える。全ての四塩化チタン溶液を加えた後、pHを7まで上げる。さらに、130gの硫酸ナトリウムを撹拌下で加える。その後、得られる溶液を乾燥し、最後に1000℃で2時間焼成する。冷却後、得られた生成物を塩化物および硫酸ナトリウムを除くために撹拌下温水で洗浄し、MgTiO3フレークを得る。
Claims (11)
- 以下の工程:
1.少なくとも1つのチタン化合物、少なくとも1つのマグネシウム化合物および少なくとも1つのリン化合物を混合することにより、MgTiO3前駆体を形成すること、ここで該混合工程において融剤が存在する、および
2.単一の焼成工程として800℃〜1400℃の範囲における温度でMgTiO3前駆体を焼成すること、
により単結晶MgTiO3フレークを製造する方法。 - 混合が水媒体中で行われる、請求項1に記載の方法。
- 融剤がNa2SO4、K2SO4、NaClおよびKClの1または2以上から選択される化合物である、請求項1または2に記載の方法。
- 方法が焼成工程の前にMgTiO3前駆体の乾燥を含む、請求項1〜3のいずれか一項に記載の方法。
- 焼成が酸素含有雰囲気において行われる、請求項1〜4のいずれか一項に記載の方法。
- 請求項1に記載の焼成工程において得られた生成物が水で処理される、請求項1〜5のいずれか一項に記載の方法。
- チタン化合物が四塩化チタン、硫酸チタニル、硫酸チタンおよび三塩化チタンの1または2以上から選択される化合物である、請求項1〜6のいずれか一項に記載の方法。
- マグネシウム化合物が塩化マグネシウム、硫酸マグネシウムおよび炭酸マグネシウムの1以上から選択される化合物である、請求項1〜7のいずれか一項に記載の方法。
- リン化合物がリン酸三ナトリウム、五酸化リン、リン酸、亜リン酸およびリン酸三カリウムの1以上から選択される、請求項1〜8のいずれか一項に記載の方法。
- 塗料、インク、コーティング組成物、プラスチックまたは化粧品における、請求項1〜9のいずれか一項に記載された方法により得られた単結晶MgTiO3フレークの使用。
- 白色顔料、光触媒、色素増感太陽電池のためのホスト材料、UV吸収剤または撥水剤としての、請求項10に記載の使用。
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| EP13005968.6 | 2013-12-20 | ||
| EP13005968 | 2013-12-20 | ||
| PCT/EP2014/003099 WO2015090500A2 (en) | 2013-12-20 | 2014-11-20 | Method for the production of single crystalline mgtio3 flakes |
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| CN112295585A (zh) * | 2020-10-27 | 2021-02-02 | 南昌航空大学 | 一种钛酸镁/石墨相氮化碳复合可见光催化剂的制备方法及应用 |
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| WO2000035811A1 (en) * | 1998-12-11 | 2000-06-22 | Showa Denko K.K. | Perovskite type composite oxide containing titanium |
| JP4572439B2 (ja) * | 1999-06-30 | 2010-11-04 | 住友化学株式会社 | チタン酸マグネシウム粉末の製造方法 |
| TWI291936B (ja) * | 2001-05-31 | 2008-01-01 | Tdk Corp | |
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| JP4493260B2 (ja) * | 2002-06-11 | 2010-06-30 | 株式会社クボタ | チタン酸化合物粉末及び化粧料 |
| JP4356552B2 (ja) * | 2003-08-13 | 2009-11-04 | 堺化学工業株式会社 | ペロブスカイト化合物粉体の製造方法 |
| JP2010002367A (ja) | 2008-06-23 | 2010-01-07 | National Institute Of Advanced Industrial & Technology | 信号計測システム |
| FR2936513B1 (fr) * | 2008-09-30 | 2011-08-05 | Saint Gobain Ct Recherches | Procede de fabrication d'un derive, d'un hydrate ou d'un oxyde de zirconium |
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| JP2017501103A (ja) | 2017-01-12 |
| EP3084050A2 (en) | 2016-10-26 |
| WO2015090500A3 (en) | 2015-08-27 |
| US10316427B2 (en) | 2019-06-11 |
| US20160312378A1 (en) | 2016-10-27 |
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