JP7149109B2 - 少なくとも2種のマラカイト粉体の混合物から固体を調製する方法 - Google Patents
少なくとも2種のマラカイト粉体の混合物から固体を調製する方法 Download PDFInfo
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- JP7149109B2 JP7149109B2 JP2018109898A JP2018109898A JP7149109B2 JP 7149109 B2 JP7149109 B2 JP 7149109B2 JP 2018109898 A JP2018109898 A JP 2018109898A JP 2018109898 A JP2018109898 A JP 2018109898A JP 7149109 B2 JP7149109 B2 JP 7149109B2
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Description
本発明は、固体の調製方法であって、以下の工程:
a) 異なる粒子サイズを有する少なくとも2種のCu2(OH)2CO3粉体および少なくとも1種のバインダを含む一式の化合物を混合する工程;
b) 工程a)の混合物を水溶液と接触させ、これにより得られたペースト状物を混錬する工程;
c) 工程b)において混錬されたペースト状物を、3~25MPaの圧力で押し出す工程;
d) 酸素を含むガス流下に10分~6時間の継続期間にわたって140℃~500℃の温度で押出物を焼成する工程
を含む、方法に関する。
以降の説明において、用語「本発明により調製された固体」は、限定なしで、前記固体の用途に応じて吸着剤並びに触媒または捕捉塊を意味する。
本発明によると、本調製方法は、異なる粒子サイズを有する少なくとも2種のCu2(OH)2CO3粉体および少なくとも1種のバインダを含む一式の化合物を混合する工程a)を含む。
xn(Pn)は、前記一式の化合物中のマラカイト粉体Pnの質量割合であり、
D50(Pn)は、前記一式の化合物のマラカイト粉体PnのD50である。
Cu2(OH)2CO3粉体は、当業者に知られているあらゆる供給源に由来する。
工程a)において混合される一式の化合物は、少なくとも1種のバインダを含む。前記バインダにより、良好な機械的強度を提供しながら前記吸着剤を形成することが可能となる。前記バインダは、有利には、粉体の形態である。
本発明によると、吸着剤の調製方法は、工程a)の混合物を水溶液と接触させ、得られたベースト状物を混錬する工程b)を含む。
本発明によると、吸着剤の調製方法は、工程b)において混錬されたペースト状物を、3~25MPaの圧力で押し出す工程c)を含む。
本発明によると、吸着剤の調製方法は、140℃~500℃の温度で、10分~6時間の継続期間にわたって、酸素を含むガス流下に押出物を焼成する工程d)を含む。
・ 50~99重量%、好ましくは60~95重量%、より好ましくは75~85重量%の質量相当のCuO;550℃での2時間にわたる強熱減量の後に測定され、含有率は、前述の式により決定される;
・ 1~50重量%、好ましくは5~40重量%、より好ましくは15~25重量%のバインダ;質量百分率は、強熱減量の後に測定される。
機械的特性は、ASTM D 6175-3法によって記載されている粒子ごとの破砕試験(EGG)によって決定される。これは、少なくとも50個の粒子を含む代表的サンプルの各粒子の破壊強度を測定することからなる。結果は、押出物の長さによって荷重される。EGG値は、サンプル粒子の全てについての測定されかつ押出物の単位長さに縮小された破壊強度(daN・mm-1で表される)の平均である。
本発明は、本発明による方法によって調製された固体の使用にも関する。
図1は、下記の固体による不純物捕捉容量を測定する手順により得られ得る破過曲線の略図である。図1において、tpは、破過時間であり、tfは、破過時間の終わりである。
(調製された固体による不純物捕捉容量を測定する手順)
本発明による方法によって調製された固体の不純物捕捉容量は、破過試験を用いて測定される。
qi:固体によって捕捉された種iの質量(g)である;
Di E:種iの流入量(mol・紛-1)である;
Mi:種iのモル質量(g・mol-1)である;
Ci E:流入ガスの種iの含有率である;
Ci S:反応器出口における種iの含有率である;
tp:図1に示されるような種iの破過に必要とされる時間(分)である。
実施例1において、参照固体A1、A2、A3、A4およびA5は、以下の手順:
a) Cu2(OH)2CO3粉体およびバインダを含む一式の化合物を混合する工程;
b) 工程a)の混合物を水溶液と接触させ(解膠)、それにより得られたペースト状物を、Z-アーム混合器において30分にわたり25回転・分-1のアーム回転スピードで混錬する工程;
c) 工程b)において混錬されたペースト状物を、3mmの径および5~10mmの長さに、ピストン押出機によって、固体に応じた可変圧力で押し出す工程;
d) 押出物を固体に応じた可変温度で焼成する工程であって、1時間にわたって、空気流下に行われる、工程
により調製される。
実施例2において、本発明に合致するB1~B4として参照される固体は、以下の手順:
a) 2種のCu2(OH)2CO3粉体およびバインダを含む一式の化合物を混合する工程;
b) 工程a)の混合物を水溶液と接触させ(解膠)、こうして得られたペースト状物を、Z-アーム混合器において30分にわたり、25回転・分-1のアーム回転スピードで混錬する工程;
c) 工程b)において混錬されたペースト状物を、ピストン押出機により、3mmの径および5~10mmの長さに、固体に応じた可変圧力で押し出す工程;
d) 実施例に応じた可変温度で押出物を焼成する工程であって、1時間にわたって空気流下に行われる、工程
による混錬および押出によって調製される。
実施例3では、固体C1およびC2が、実施例2の操作方法に従って混錬しかつ押し出すことによって調製される。
Claims (14)
- 固体の調製方法であって、以下の工程:
a) 異なる粒子サイズを有する少なくとも2種のCu2(OH)2CO3粉体および少なくとも1種のバインダを含む一式の化合物を混合する工程;
b) 工程a)の混合物を水溶液と接触させ、これにより得られたペースト状物を混錬する工程;
c) 工程b)において混錬されたペースト状物を、3~25MPaの圧力で押し出す工程;
d) 酸素を含むガス流下に10分~6時間の継続期間にわたって140℃~500℃の温度で押出物を焼成する工程
を含み、
前記一式の化合物の荷重された中位径は、10~45μmであり、前記一式の化合物の荷重された中位径Dmは、式:
x n (Pn)は、前記一式の化合物中のマラカイト粉体Pnの質量割合であり、
D 50 (Pn)は、前記一式の化合物のマラカイト粉体PnのD 50 である
方法。 - 前記一式の化合物は、0.1~99.9重量%の、そのD50が1~15μmである第1のマラカイト粉体と、99.9~0.1重量%の、そのD50が25~100μmである第2のマラカイト粉体とを含み、重量百分率は、マラカイト粉体の全重量に対して表される、請求項1に記載の方法。
- 前記一式の化合物は、工程a)において乾式混合される、すなわち、液体を加えずに混合される、請求項1または2に記載の方法。
- 前記バインダは、粘土から選択されるか、または、アルミナ、アルミナの前駆体、シリカおよびそれらの混合物からなる群から選択される、請求項1~3のいずれか1つに記載の方法。
- 調製方法において用いられるバインダの量は、前記バインダが、調製される固体の50重量%未満を示すようにされる、請求項1~4のいずれか1つに記載の方法。
- 前記工程b)の前記水溶液は、酸性または塩基性の解膠剤を含有する、請求項1~5のいずれか1つに記載の方法。
- 前記工程b)の前記水溶液は、硝酸を含有し、HNO3の質量/金属酸化物の質量の比は、0.5~10重量%である、請求項6に記載の方法。
- 前記塩基性解膠剤は、水酸化ナトリウム、水酸化カリウム、アンモニア、テトラエチルアンモニウムヒドロキシド(TEAOH)、炭酸アンモニウムおよびそれらの混合物からなる群から選択され、塩基性解膠剤の質量/金属酸化物の質量の比は、1~10重量%である、請求項6に記載の方法。
- 前記工程b)の水溶液は、酸も塩基も加えられていない水溶液である、請求項1~5のいずれか1つに記載の方法。
- 工程c)から得られた押出物を、工程d)において焼成する前に、70~160℃の温度で1~24時間の継続期間にわたって乾燥させる、請求項1~9のいずれか1つに記載の方法。
- 焼成の工程d)を、200℃~500℃の温度で行う、請求項1~10のいずれか1つに記載の方法。
- 気体または液体の供給原料を精製するための、請求項1~11のいずれか1つに記載の方法によって調製された固体の使用。
- デュサン反応のための触媒としての、請求項1~11のいずれか1つに記載の方法によって調製された固体の使用。
- メタノール合成反応のための触媒としての、請求項1~11のいずれか1つに記載の方法によって調製された固体の使用。
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