JP7258458B2 - アルミナ繊維、アルミナ繊維集合体及び排ガス浄化装置用把持材 - Google Patents
アルミナ繊維、アルミナ繊維集合体及び排ガス浄化装置用把持材 Download PDFInfo
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Description
すなわち、本発明は下記の通りである。
[2] 化学組成として、アルミナの含有量が63質量%以上97質量%未満である[1]に記載のアルミナ繊維。
[3] ムライト化率が10%以下である[1]又は[2]に記載のアルミナ繊維。
[4] [1]~[3]のいずれかに記載のアルミナ繊維からなるアルミナ繊維集合体。
[5] [4]に記載のアルミナ繊維集合体からなる排ガス浄化装置用把持材。
本実施形態のアルミナ繊維は、酸化第二鉄に換算(分析で得られたFe量をすべてFe2O3に換算)した酸化鉄の含有量(A)と酸化チタンの含有量(C)との質量比(A/C)が2~121であり、酸化カルシウムの含有量(B)と上記酸化チタンの含有量(C)との質量比(B/C)が0.4~14である。
アルミナ繊維の化学組成は、蛍光X線分析及びICP等を用いて測定することができる。
特に、酸化チタンとしてのチタン含有量及び酸化カルシウムとしてのカルシウム含有量は、後述の実施例に記載のとおりマイクロウェーブ分解後、ICP測定にて測定することができる。そして、酸化チタン及び酸化カルシウムに換算してこれらの含有量を求めることができる。
式(1):鉱物組成(ムライト化率)=h/h0×100
本実施形態のアルミナ繊維集合体は、本発明のアルミナ繊維からなる。
以下、上記の特性を有するアルミナ繊維集合体の製造方法を詳細に説明する。
すなわち、本実施形態のアルミナ繊維集合体の製造方法は、例えば、
(I)アルミナ源、シリカ源、酸化鉄源、酸化カルシウム源、酸化チタン源を含む無機繊維源と紡糸助剤とを混合し減圧濃縮することで粘調な紡糸原液を得る工程、
(II)紡糸原液を細孔より大気中に押出し、乾燥することでアルミナ繊維前駆体を得る工程、
(III)アルミナ繊維前駆体を焼成する工程、を含む。
アルミナ繊維の紡糸原液を調製する方法としては、アルミナ源と、シリカ源、酸化鉄源、酸化カルシウム源、酸化チタン源を、アルミナ繊維が最終的に所望の化学組成となるように混ぜ、さらにポリビニルアルコール、ポリエチレンオキサイド、ポリエチレングリコール等の紡糸助剤を配合して均一に混合してから減圧濃縮する。これにより、好ましくは粘度が500mPa・s以上10000mPa・s以下、より好ましくは1000mPa・s以上5000mPa・s以下の粘調な紡糸原液を調製する。
紡糸原液からアルミナ繊維前駆体を得る方法としては、例えば紡糸原液を金型ダイスの細孔から空中に糸状に噴出させながら急速乾燥する方法が挙げられる。金型ダイスの構造や形状、細孔の径や配置、また紡糸原液の吐出量や吐出圧、さらに紡糸原液を噴出させる先の空間温度、圧力、気体成分、湿度、気流の有無については特に限定はない。金型ダイスは固定された構造であっても、可動な構造であってもどちらでもよい。具体的には、周速5m/s以上100m/s以下で回転する中空円盤内に紡糸原液を供給し、円盤の円周面に設けられた直径0.1mm以上1.3mm以下の複数の細孔から紡糸原液を放射状(糸状)に噴出させ、これを乾燥風と接触させながら急速乾燥させることによりアルミナ繊維前駆体を得ることができる。
シート状またはマット状に集積成形したアルミナ繊維前駆体を焼成して、最終的にアルミナ繊維からなる集合体となす方法としては、例えばこのアルミナ繊維前駆体を、まず一段目として、集積成形後の温度、即ち通常は10℃以上150℃以下の温度から、最高温度を500℃以上1000℃以下まで大気雰囲気下で加熱する。この一段目の段階で、アルミナ繊維前駆体中に残留する水分を乾燥し、塩化水素等の揮発性の酸性成分、及び粘性付与剤の分解物であるアルデヒド類等の有機物を排出する脱脂工程を設ける。
さらに二段目として、最高温度を1000℃以上1300℃以下として大気雰囲気下でアルミナ繊維前駆体を焼成し、無機化合物の一部を結晶化させる結晶化工程を設ける。
なお、本発明の脱脂工程と結晶化工程の温度は、加熱炉内の雰囲気温度の測定値である。この場合、温度は通常加熱炉内に設置された熱電対等により計測される。
なお、(I)の工程でアルミナ繊維が最終的に所望の化学組成となるように配合した組成は、完成したアルミナ繊維の化学組成とほぼ一致することを蛍光X線分析及びICP分析により確認している。
本発明は、本発明のアルミナ繊維集合体を用いた排ガス浄化装置用把持材である。例えば、排ガス浄化装置用把持材は本発明のアルミナ質繊維集合体に無機バインダー、有機バインダーを加え、湿式成形することにより製造することが可能である。
アルミナ成分が65質量%、シリカ成分が35質量%、酸化鉄成分が0.0987質量%、酸化カルシウム成分が0.0008質量%、酸化チタン成分が0.0098質量%となるように、アルミナ固形分濃度が20.0質量%のオキシ塩化アルミニウム水溶液5000gと、シリカ濃度が20.0質量%のコロイダルシリカ3012gと、水酸化鉄(III)(米山薬品工業社製、一般試薬)0.110gと、水酸化カルシウム(和光純薬工業社製、試薬特級)0.010gと、チタンテトライソプロポキシド(和光純薬工業社製、和光一級)0.005gを混合し、さらに、アルミナ成分とシリカ成分の固形分の合計に対して8質量%となるように重合度1700の部分ケン化ポリビニルアルコール(デンカ社製)による、固形分濃度10質量%水溶液1370gを混合してから減圧脱水濃縮を行い、粘度3300mPa・sの紡糸原液を調製した。
=100(質量%)-二酸化ケイ素濃度(質量%)-酸化第二鉄濃度(質量%)-酸化カルシウム(質量%)-酸化チタン(質量%)-0.1(質量%)
なお、粉砕した繊維サンプルは、作製したアルミナ繊維集合体15gを50mmφの金型に入れ、油圧プレス機(フォーエバー社(旧マシーナ社)製、テスター25)により、28kNの荷重を2回繰り返してかけて繊維を圧縮粉砕して調製した。
・X線管球電圧、電流:40V、50mA
・測定角度2θ範囲:10~50°
・スキャンスピード:4°/分
紡糸原液の配合組成と結晶化工程における昇温速度、最高焼成温度、所要時間を下記表1~表6のように変更した他は、実施例1と同様の条件でアルミナ繊維集合体を調製し、またその物性を測定した。結果を下記表1~表6に示す。
Claims (3)
- 前記アルミナ繊維が、化学組成として、アルミナの含有量が63質量%以上97質量%未満である請求項1に記載の排ガス浄化装置用把持材。
- 前記アルミナ繊維のムライト化率が10%以下である請求項1又は2に記載の排ガス浄化装置用把持材。
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WO2014069589A1 (ja) | 2012-10-31 | 2014-05-08 | 電気化学工業株式会社 | アルミナ質繊維集合体、その製造方法および用途 |
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