JP2011207744A - 多孔質チタン酸アルミニウムマグネシウムの製造方法および多孔質チタン酸アルミニウムマグネシウム - Google Patents
多孔質チタン酸アルミニウムマグネシウムの製造方法および多孔質チタン酸アルミニウムマグネシウム Download PDFInfo
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Abstract
【解決手段】 本発明の製造方法は、Al源粉末、Mg源粉末、Ti源粉末およびSi源粉末並びに細孔形成剤を含む混合物を成形して成形体を得、得られた成形体を予備焼成した後、焼成することにより多孔質チタン酸アルミニウムマグネシウムを製造する方法であり、Al源粉末、Mg源粉末、Ti源粉末およびSi源粉末の合計100質量部に対する細孔形成剤含有量が5質量部〜30質量部であり、Si源粉末は融点が600℃〜1300℃であり、混合物中のAl、Mg、TiおよびSiの元素組成比を組成式(1):
Al2(1−x)MgxTi(1+x)O5+aAl2O3+bSiO2・・・(1)
で示したときに、xは0.05≦x≦0.15を、aは0≦a≦0.1を、bは0.05≦b≦0.15をそれぞれ満足し、予備焼成後の成形体を1300℃〜1560℃で焼成することを特徴とする。
【選択図】 なし
Description
Al2(1−x)MgxTi(1+x)O5+aAl2O3+bSiO2・・・(1)
で示したときに、xが0.50、aが0.01〜0.05、bが0.02〜0.25で示される混合物を用いた例が特許文献1に、xが0.25〜0.95、aが0.1、bが0.1で示される混合物を用いた例が特許文献2に、xが0.08、aが0.07、bが0.08で示される混合物を用いた例が特許文献3にそれぞれ開示されている。かかる製造方法によれば、焼成によりアルミニウム源粉末、マグネシウム源粉末およびチタニウム源粉末が反応して、目的のチタン酸アルミニウムマグネシウムを得ることができる。
前記混合物は、アルミニウム源粉末、マグネシウム源粉末、チタニウム源粉末およびケイ素源粉末の合計含有量100質量部に対する細孔形成剤の含有量が5質量部〜30質量部であり、
前記ケイ素源粉末は、融点が600℃〜1300℃であり、
前記混合物中のAl、Mg、TiおよびSiの元素組成比を組成式(1):
Al2(1−x)MgxTi(1+x)O5+aAl2O3+bSiO2・・・(1)
で示したときに、xは0.05≦x≦0.15を、aは0≦a≦0.1を、bは0.05≦b≦0.15をそれぞれ満足し、
予備焼成後の前記成形体を1300℃〜1550℃で焼成することを特徴とする多孔質チタン酸アルミニウムマグネシウムの製造方法を提供するものである。
Al、Mg、TiおよびSiの元素組成比を組成式(1):
Al2(1−x)MgxTi(1+x)O5+aAl2O3+bSiO2・・・(1)
で示したときに、xは0.05≦x≦0.15を、aは0≦a≦0.1を、bは0.05≦b≦0.15をそれぞれ満足することを特徴とする多孔質チタン酸アルミニウムマグネシウムである。
本発明の製造方法に用いられるアルミニウム源粉末は、目的とする多孔質チタン酸アルミニウムマグネシウムを構成するアルミニウム成分となる原料粉末である。
チタニウム源粉末は、目的とする多孔質チタン酸アルミニウムマグネシウムを構成するチタニウム成分となる原料粉末である。
マグネシウム源粉末は、目的とする多孔質チタン酸アルミニウムマグネシウムを構成するマグネシウム成分となる原料粉末である。
ケイ素源粉末の融点は600℃〜1300℃である。ケイ素源粉末は、焼成時に溶融状態となり、焼成後は通常、不定形(アモルファス)のケイ素酸化物成分となって、目的のチタン酸アルミニウムマグネシウム中に含まれる原料粉末である。
細孔形成剤としては、例えばグラファイトなどの炭素材料、ポリエチレン、ポリプロピレン、ポリメタクリル酸メチルなどの樹脂類、澱粉、ナッツ殻、クルミ殻、コーンなどの植物系材料、などが挙げられる。上述した植物系材料のうち澱粉としては、例えばトウモロコシ澱粉、大麦澱粉、小麦澱粉、タピオカ澱粉、ポテト澱粉、豆澱粉、米澱粉、エンドウ澱粉、サンゴヤシ澱粉、カンナ澱粉などが挙げられる。
本発明の製造方法に適用される混合物は、上記のとおりアルミニウム源粉末、マグネシウム源粉末、チタニウム源粉末およびケイ素源粉末並びに細孔形成剤を含む混合物であるが、この混合物において、アルミニウム源粉末、マグネシウム源粉末、チタニウム源粉末およびケイ素源粉末の合計含有量100質量部に対する細孔形成剤の含有量は5質量部〜30質量部、好ましくは20質量部以下である。
バインダーとしては、例えばメチルセルロース、カルボキシルメチルセルロース、ナトリウムカルボキシルメチルセルロースなどのセルロース類、ポリビニルアルコールなどのアルコール類、リグニンスルホン酸塩などの塩、パラフィンワックス、マイクロクリスタリンワックスなどのワックス、EVA、液晶ポリマーなどの熱可塑性樹脂などが挙げられる。バインダーの使用量は、アルミニウム源粉末、チタニウム源粉末、マグネシウム源粉末およびケイ素源粉末の合計量100質量部に対して、通常1質量部〜20質量部、好ましくは15質量部以下である。
本発明の製造方法では、このような混合物を成形して成形体を得る。混合物を成形するには、例えば通常用いられるものと同様の一軸プレス機、押出成形機、打錠機、造粒機などの成形装置を用いて、目的とする多孔質チタン酸アルミニウムマグネシウムの形状に成形すればよい。
次いで、成形により得られた成形体を予備焼成する。予備焼成は通常、成形体を200℃〜900℃の温度に加熱することにより行なわれる。予備焼成中は、一定温度に維持してもよいし、上記温度範囲であれば、昇温してもよい。成形体を予備焼成することにより、成形体中の細孔形成剤が消失して、成形体中に細孔が形成される。また、通常は同時にバインダー、可塑剤、分散剤などの成形助剤や溶媒なども消失する。
本発明の製造方法では、成形体を予備焼成することにより細孔形成剤を消失させた後、焼成する。焼成は通常、予備焼成後の成形体を降温することなく、そのまま通常1300℃〜1560℃、好ましくは1450℃〜1530℃の焼成温度に昇温することにより行なわれる。
〔混合物の製造〕
以下のアルミナ源粉末、チタニウム源粉末、マグネシウム源粉末、ケイ素源粉末および細孔形成剤を以下に示す質量比で混合した。
体積基準の累積百分率50%相当粒子径(D50)が42μmの酸化アルミニウム粉末(α−アルミナ粉末)
42.3質量部
(2)チタニウム源粉末
D50が1.5μmの酸化チタン粉末(ルチル型結晶)
35.6質量部
(3)チタニウム源粉末
D50が0.4μmの酸化チタン粉末(ルチル型結晶)
4.0質量部
(4)マグネシウム源粉末
D50が4μmの酸化マグネシウム粉末
2.4質量部
(5)ケイ素源粉末
D50が9μmであり、Na、K、MgおよびAlを含み、元素組成比(酸化物換算)がNa2O:8.6質量%、K2O:5.9質量%、MgO:1.0質量%、Al2O3:11.5質量%、SiO2:72.3質量%(その他不純物元素0.7質量%)であるガラスフリット(融点:645℃)
3.6質量部
(6)細孔形成剤
D50が20μmのポリエチレン粉末
12.2質量部
メチルセルロース〔信越化学工業(株)製「SM4000」〕
5.5質量部
(8)バインダー
メチルセルロース〔信越化学工業(株)製「60SH4000」〕
2.4質量部
(9)可塑剤
ポリオキシエチレンポリオキシプロピレンブチルエーテル〔日油(株)製「50MB72」〕
4.64質量部
(10)可塑剤
グリセリン
0.4質量部
(11)イオン交換水
30.7質量部
得られた混合物を押出混練機にて混練しながら押出して成形を行い、外形が直径30mm、高さ50mmの円柱状で、高さ方向に多数の連通孔を有し、セル壁厚0.3mmのハニカム形状の成形体を得た。
この成形体を加熱炉に入れ、徐々に昇温したところ、200℃に達するまでに水分は全て揮発し、900℃に達するまでに細孔形成剤〔ポリエチレン粉末〕、バインダー〔メチルセルロース〕、可塑剤〔ポリオキシエチレンポリオキシプロピレンブチルエーテルおよびグリセリン〕は全て消失した。
予備焼成後も引き続き同じ昇温速度で加熱を続け、1450℃に加熱し、同温度に5時間保持して焼成を行い、ハニカム形状の多孔質チタン酸アルミニウムマグネシウムを得た。この多孔質チタン酸アルミニウムマグネシウムの気孔率は42.5%であった。
アルミナ源粉末、チタニウム源粉末、マグネシウム源粉末、ケイ素源粉末および細孔形成剤と成形助剤〔バインダーおよび可塑剤〕並びに水の使用量を下記表1のとおりとした以外は、実施例1と同様に操作して、多孔質チタン酸アルミニウムマグネシウムを得た。得られた多孔質チタン酸アルミニウムマグネシウムの気孔率を下記表1に示す。
Claims (2)
- アルミニウム源粉末、マグネシウム源粉末、チタニウム源粉末およびケイ素源粉末並びに細孔形成剤を含む混合物を成形して成形体を得、得られた成形体を予備焼成することにより前記細孔形成剤を消失させた後、焼成することにより前記アルミニウム源粉末、マグネシウム源粉末およびチタニウム源粉末を反応させて、多孔質チタン酸アルミニウムマグネシウムを製造する方法であり、
前記混合物は、アルミニウム源粉末、マグネシウム源粉末、チタニウム源粉末およびケイ素源粉末の合計含有量100質量部に対する細孔形成剤の含有量が5質量部〜30質量部であり、
前記ケイ素源粉末は、融点が600℃〜1300℃であり、
前記混合物中のAl、Mg、TiおよびSiの元素組成比を組成式(1):
Al2(1−x)MgxTi(1+x)O5+aAl2O3+bSiO2・・・(1)
で示したときに、xは0.05≦x≦0.15を、aは0≦a≦0.1を、bは0.05≦b≦0.15をそれぞれ満足し、
予備焼成後の前記成形体を1300℃〜1560℃で焼成することを特徴とする多孔質チタン酸アルミニウムマグネシウムの製造方法。 - Si元素を含有し、
Al、Mg、TiおよびSiの元素組成比を組成式(1):
Al2(1−x)MgxTi(1+x)O5+aAl2O3+bSiO2・・・(1)
で示したときに、xは0.05≦x≦0.15を、aは0≦a≦0.1を、bは0.05≦b≦0.15をそれぞれ満足することを特徴とする多孔質チタン酸アルミニウムマグネシウム。
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JP2008545612A (ja) * | 2005-05-31 | 2008-12-18 | コーニング インコーポレイテッド | 細孔形成剤の組合せを含有するチタン酸アルミニウムセラミック形成バッチ混合物および未焼成体、および同混合物および未焼成体の製造および焼成方法 |
JP2007105622A (ja) * | 2005-10-13 | 2007-04-26 | Ohcera Co Ltd | 排ガス浄化ハニカムフィルタ及びその製造方法 |
JP2009084064A (ja) * | 2007-09-27 | 2009-04-23 | Kyocera Corp | 耐熱性セラミック部材およびフィルタ |
WO2009093560A1 (ja) * | 2008-01-21 | 2009-07-30 | Sumitomo Chemical Company, Limited | チタン酸アルミニウムマグネシウム-アルミナ複合セラミックス |
JP2009196881A (ja) * | 2008-01-21 | 2009-09-03 | Sumitomo Chemical Co Ltd | チタン酸アルミニウムマグネシウム−アルミナ複合セラミックス |
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JP5685458B2 (ja) | 2015-03-18 |
CN102781873A (zh) | 2012-11-14 |
KR20130036194A (ko) | 2013-04-11 |
EP2546212A1 (en) | 2013-01-16 |
US20130048905A1 (en) | 2013-02-28 |
EP2546212B1 (en) | 2016-12-21 |
BR112012022551A2 (pt) | 2016-08-30 |
PL2546212T3 (pl) | 2017-06-30 |
EP2546212A4 (en) | 2014-02-19 |
US8921249B2 (en) | 2014-12-30 |
WO2011111633A1 (ja) | 2011-09-15 |
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