JP6436495B2 - 多孔質材料上に堆積させた寸法の小さい分子篩結晶を含む触媒組成物 - Google Patents
多孔質材料上に堆積させた寸法の小さい分子篩結晶を含む触媒組成物 Download PDFInfo
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- JP6436495B2 JP6436495B2 JP2016522613A JP2016522613A JP6436495B2 JP 6436495 B2 JP6436495 B2 JP 6436495B2 JP 2016522613 A JP2016522613 A JP 2016522613A JP 2016522613 A JP2016522613 A JP 2016522613A JP 6436495 B2 JP6436495 B2 JP 6436495B2
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Images
Classifications
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- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
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- B01J29/405—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
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- B01J29/42—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing iron group metals, noble metals or copper
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Description
あるいは、上記の従来技術は、担体上にゼオライトのシード(種)またはゼオライト前駆体元素を堆積し、その後に気相転移等の結晶成長工程を行うことを記載している。形成されたゼオライト結晶はXRDで証明されている。
本発明の特定の目的は、表面積が改善された触媒組成物を提供することにある。
本発明のさらに特定の目的は、改善された活性と選択性とを有する触媒組成物を提供することにある。
本発明の別の目的は、上記触媒組成物の製造方法を提供することにある。
さらに、触媒反応の実行中の小さいサイズの分子篩結晶粒子を安定化させるというニーズもある。
(1)リン
(2)B、Cr、Co、Ga、Fe、Li、Mg、Ca、Mn、La、Ti、Mo、W、Ni、Ag、Sn、Zn、Pt、Pd、Ru、Re、Os、Auの群の中から選択される少なくとも一つの金属またはこれらの任意の組み合わせ、
(3)シリカ、シリカアルミナ、金属シリケート、金属酸化物、例えば、ZrO2および/または金属、アモルファスアルモホスフェート(alumophosphate)またはシリカアルモホスフェート、シリカと金属酸化物の混合物を含むゲル、非晶質アルモホスフェートまたはこれらの任意の組合せの中から選択される少なくとも一つの結合剤。
a)無機多孔質材料を用意し、
b)必要に応じて上記無機多孔性材料を400℃〜1200℃の温度でか焼し、
c)少なくとも1種の電荷表面改質剤を含む溶液を用意し、
d)工程b)で得られた材料と工程c)の溶液を接触させて、電荷表面改質剤で変性された非晶質無機多孔質体を作り、
e)分子篩の前駆体を含む溶液を用意し、
f)下記のi)および/またはii)で反応させて分子篩にし、
ii)工程d)で得られた上記の改質された多孔質材料を工程e)の溶液と接触させ、得られた混合物を0〜50時間の間、触媒組成物のTPDアンモニアにより測定した酸度が無機多孔質材料の酸度と比較して少なくとも10%増加するまで熟成し、この熟成は触媒組成物のX線回折パターンに分子篩の結晶が現れる前に停止し、
上記熟成時間は無機多孔質体のX線回折パターンに変化がなくなるまで、すなわち、熟成時間は触媒組成物の所望の酸度になるまで行い、はX線回折パターンに分子篩が表われる前に熟成を停止し、
h)工程g)で得られた固体をか焼する。
(1)触媒組成物をリンを含む溶液で含浸してリンを導入し、必要に応じて、この工程の後にか焼および/またはスチーム処理を行う、
(2)B、Cr、Co、Ga、Fe、Li、Mg、Ca、Mn、La、Ti、Mo、W、Ni、Ag、Sn、Zn、Pt、Pd、Ru、Re、Os、Auの群の中から選択される少なくとも一つの金属またはこれらの任意の組み合わせの中から選択される金属の塩を含む溶液で触媒組成物を含浸することによって金属を添加し、
(3)噴霧、乾燥、押出または当業者に公知の任意の適切な方法によって、シリカ、シリカアルミナ、金属シリケート、金属酸化物、例えばZrO2および/または金属、アモルファスアルモホスフェートまたはシリカアルモホスフェート、シリカと金属酸化物との混合物を含むゲル、非晶質アルモホスフェートまたはこれらの任意の組合せの中から選択される少なくとも一つの結合剤を加え、
(4)押出成形で触媒組成物を成形する。
本発明触媒組成物では、触媒組成物の総重量に対して分子篩の結晶を0.1〜50重量%、好ましくは1〜40重量%、より好ましくは1〜30重量%の範囲で含む。本発明触媒組成物は分子篩結晶が小さいサイズであることに特徴がある。「小さい」という用語は平均粒径が50nm以下、好ましくは40nm以下、好ましくは30nm以下、好ましくは15nm以下であることを意味する。分子篩結晶の直径は走査型電子顕微鏡(SEM)で測定される。
以下に記載の調製方法は上記触媒組成物を調製するのに使用される。上記の全ての触媒組成物の実施形態は互いにリンクされ、全ての製造方法の実施形態および以下に記載する全ての関連実施形態と組み合わせて考慮する必要がある。
a)無機多孔質材料を用意する工程
無機多孔質材料は分子篩結晶の担体として使用される。これは、少なくともメソポーラス、すなわち、少なくとも2nmの気孔を有する。無機多孔質材料はマクロ多孔性、すなわち、少なくとも50nmの気孔を有するのが有利である。担体の細孔直径は少なくとも100nm、好ましくは少なくとも200nmであるのが好ましい。細孔を大径にすると、担体自体の内部に分子篩結晶を受ける追加のアクセス可能な表面積を与えることができる。
好ましい実施形態では、多孔性材料の前駆体をアルコキシド経路で得るか、アルコキシド経路で得られたアルミナ前駆体から得る。
好ましい実施形態では、多孔質材料のASTM D4365を用いて測定した細孔容積は少なくとも0.25cm3/gである。
このか焼では固体を少なくとも400℃でガス循環無し、または、空気流下、酸素流下またはN2流下で炉内で高温処理する。この触媒組成物の調製での最初のオプションのか焼は多孔性材料を安定化するために使用される。安定化とは、か焼によって工程f)で分子篩の前駆体を含む溶液と接触した時の表面安定性を向上させることを意味する。か焼成の効果は物質を構成する各元素の溶解を制限することにもあるということは当業者には理解できよう。最初の工程でのか焼は、例えば多孔質材料を表面改質剤または分子篩の前駆体を含む溶液と接触させる工程時にアルミニウムの溶解を制限するのに使用する。
表面電荷改質剤は多孔質材料の表面電荷を改質可能な任意タイプの成分で構成できる。特定の理論に拘束されるものではないが、分子篩の結晶化時に非常に小さな結晶が形成され、これらの小さなサイズの結晶が電気的に帯電し、その電荷が溶液中に存在する対イオンによって補償されると考えられる。小さなサイズの結晶はこの電荷のために無機多孔質支持体上に直接堆積することができない。本発明者は、小さなサイズの結晶を多孔質表面上に堆積させる前に、表面電荷改質剤を無機多孔質体に含浸させることで、小さい結晶を多孔質表面上に良好に分散させることができるということを発見した。これは無機多孔質体表面上に堆積させた表面電荷改質剤が熟成段階時の小さな結晶と多孔質材料表面との間の静電反発力を制限して無機多孔質体表面上への小さい結晶の堆積を容易にするためと考えられる。
上記の材料と溶液との接触は触媒組成物の調製で使用される通常の任意の含浸方法法で実施できる。例えば、多孔性を完全に充填することができる正確な量の溶液と固体とを接触させる湿潤含浸技術で行うことができる。また、固体を大過剰の溶液と接触させる平衡含浸技術で行い、次いで過剰の液体を濾過または蒸発で固体から分離することもできる。一つの実施形態では、含浸を室温で行う。別の実施形態では、含浸を室温〜150℃の範囲の温度で行うことができる。含浸工程の最適化法は当技術分野で知られている。表面電荷改質剤を含浸で行う場合の多孔質支持体表面上の表面電荷改質剤薬剤の分散が良好か否かは多孔質材料の表面電荷を測定することで確認できる。具体的には、多孔質材料のゼータ電位をモニターする。ゼータ電位の詳細はUllmann's Encyclopaedia of Industrial Chemistry, 6th edition, volume 11, p.702-703に記載されている。この文献の内容は本明細書に組み込まれる。
分子篩のシード(種)または分子篩の前駆体を含む溶液は、溶液に可溶性で且つ対応する分子篩の調製に用いることができる限り、任意の形態の元素で構成できる。分子篩の前駆体を含む溶液の調製に好ましい実施形態は、適切な量のケイ酸ナトリウム、アルミン酸ナトリウム、水酸化ナトリウムと、必要に応じて用いる有機テンプレートとを混合する工程を含む。最も好ましい実施形態では、上記の混合を、得られた混合物を種が熟成するのに十分な時間かつ曇りが発生しない時間の間、制御された方法で加熱して実行する。
i)工程e)の溶液を0〜50時間、熟成してDLSによって測定される最大寸法が50nm、好ましくは最大寸法が10nmの分子篩結晶を作り、工程d)で得られた多孔質材料の表面上に分子篩の結晶を形成するのに適した条件下で、熟成した溶液を改質された多孔質材料と接触させる、および/または
ii)工程d)で得られた改質された多孔質材料を工程e)の溶液と接触させ、得られた混合物を、X線回折パターンを変えずに触媒組成物の酸度を増加させ、および/または分子篩の結晶を形成することができる条件下で0〜50時間、熟成する。
g)工程f)後に得られた混合物に液体が存在する場合に液体から固体を分離する工程
液体からの固体の分離は当技術分野で公知の任意の手段で行うことができ、例えば、濾過、少なくとも100℃での乾燥、ナノ濾過等を挙げることができる。
工程h)で行うか焼は固体中に存在する有機化合物をO2または空気または任意の酸化性雰囲気下で燃焼除去するために行う。さらに、表面上に存在する不純物(有機成分以外の成分、例えば対イオン)を除去することができる。このか焼は少なくとも400℃の温度で行われる。か焼は400℃〜1200℃の温度範囲で行うのが好ましい。
本発明方法を用いることで表面上に分子篩の小さい結晶が分散した触媒組成物を製造することができる。
(1)触媒組成物をリンを含む溶液で含浸してリンを導入する(この工程の後に必要に応じてか焼および/またはスチロム処理工程を続けることができる)。
(2)選択された金属塩を含む溶液を触媒組成物に含浸することによってB、Cr、Co、Ga、Fe、Li、Mg、Ca、Mn、La、Ti、Mo、W、Ni、Ag、Sn、Zn、Pt、Pd、Ru、Re、Os、Auの群の中から選択される少なくとも1種の金属またはこれらの任意の組み合わせを添加する。
(3)噴霧乾燥、押出または当業者に公知の任意の適切な方法を用いて、シリカ、シリカアルミナ、金属シリケート、金属酸化物、例えばZrO2および/または金属、アモルファスアルモホスフェートまたはシリカアルモホスフェート、シリカ及び金属酸化物の混合物を含むゲル、非晶質アルモホスフェートまたはこれらの任意の組合せの中から選択される少なくとも一つの結合剤を加える。
(4)押出成形して触媒組成物を成形する。
本発明触媒は酸性活性サイトを必要とする任意の反応で触媒として使用することができ、さらに、担体として酸の特性が要求される場合に支持体として使用することもできる。本発明触媒組成物は例えば機械的混合物または配合物の成分として他の触媒と一緒に助触媒として使用することもできる。本発明触媒組成物は配合(formulaqtion)の前または配合操作の一部として添加することができる。例えば、本発明触媒組成物はFCC反応の触媒またはFCC反応の触媒添加物として使用することができる。
表面積および細孔容積の測定は通常の表面積測定法を用いたN2吸着で測定する。特に「BET」測定法のような表面積測定法を使用することができる(表面積はASTM D3663、細孔容積はD4365)。当技術分野で周知の他の技術、例えば水銀吸着法(ASTM D4284)も使用できる。本明細書に記載の全ての測定とデータプロットはMicromeritics(登録商標)トリスター3000アナライザを用いて作製した。
酸度はピリジン吸着量で測定し、このピリジン吸着量は赤外線測定で定量化する。IRスペクトルを4cm-1の光学分解能でNicolet Magna 550 FT-IR分光計で記録し、フーリエ変換のゼロフィリングのレベルは1にする。測定前に触媒を自己支持ディスクでプレスしてディスク(直径:1.6cm、10mg/cm2)にし、106Torr(14132.17Pa)まで723°Kで4時間、IRセル(真空ラインに接続されている)中で活性化した。IRセルはKBr窓を備えて、それによって400cm-1までのスペクトル領域のスペクトルを記録した。吸着されたガスの圧力は2つBarocelゲージで測定した。その1つはセルのサンプル収容区画に直接結合した。その他方を用いて吸着前にセルに入れた容積が既知のガスの量を測定することができる。操作中およびスペクトルの記録時のサンプル温度はヒータ中またはセルの冷媒室中に挿入したクロメル−アルメル熱電対でモニターした。ピリジン吸着:ピリジン(Py)は423°Kで行った。さらに423°Kで過剰なプローブ分子を排気した。吸着−排出をスペクトルに変化が観察されなくなるまで数回繰り返した。吸着されたピリジン量Pyは吸光係数ε1545(B−ピリジン)=1.8cmμmol-1とε1455(L−ピリジン)=1.5cmμmol-1とを用いて測定した。このピリジン吸着量からブレンステッド酸サイトおよびルイス酸サイトを定量化することができる。
活性化:この手順は50cm3/分の流速のHe下で行う。温度を20℃/分の温度上昇率で室温から600℃まで上げ、次いで、温度を600℃に1時間維持する。次に温度を10℃/分の冷却速度で100℃へ下げる。
飽和:この工程は100℃で行う。最初の1時間、Heに希釈した10重量%NH3混合物の30cm3/分の流れに固形物を接触させ、次の2時間は50cm3/分の流量で固体と接触させる。
分析:この工程は50cm3/分の流量下で行う。10℃/分の温度上昇率で温度を600℃に上げ、600℃の温度に達した後、この温度を1時間維持する。その後、セルを冷却し、秤量する。固体上に堆積したNH3の量を100℃から600℃の温度範囲でサンプルから脱着したηmolNH3として、測定後に取り出したサンプルの重量で規格化して求める。
変性多孔質材料上に含浸前に熟成した前駆体溶液を用いて調製した触媒組成物
この触媒組成物は以下の手順に従って調製した。多孔質材料はSiralox TH30(Sasol社、Al2O3/SiO2−70/30重量%)で、この上に分子篩ZSM−5結晶を分散させた。
分子篩の前駆体を含む溶液(ZSM−5前駆体溶液−4.5(TPA)2O:25SiO2:0.25Al2O3:430H2O:Si/Al=50)は、TPAOH(テトラプロピルアザニウムヒドロキサイド、CAS[66082−78−8])、H2O、硫酸アルミニウム[10043−01−3]およびTEOS(テトラエトキシシラン;CAS[9044−80−8]を混合して調製した。各成分は上記順番で徐々に添加し、激しく撹拌しながら1時間、室温(RT)で加水分解した。次に、容器を閉じ、さらに3時間撹拌した。得られた溶液を多孔質材料上で使用する前に、種々時間:12時間、36時間、48時間、72時間、96時間、120時間、144時間、168時間、192時間、100℃で熟成した。
実施例1で調製した材料の触媒テスト
調製した触媒組成物のTiPBz分解の触媒試験を実施した([図4]参照)。長い結晶化時間(36時間以上)を掛けて調製した触媒組成物は、初期Siralox TH30(600゜C)の活性より高い活性を有することは明らかである。いかなる理論に拘束されるものではないが、結晶化時間をより長くした触媒がより多くの酸サイトを有し、表面積を発達させると解釈される([表3][表4])。この高い酸度はSiralox TH30の表面上に堆積した分子篩の小さな結晶に由来する。Siralox TH30上に分子結晶の結晶を析出させた触媒組成物は、Siralox TH30よりも高い変換率を与える。
熟成した前駆体溶液を使用し、乾燥およびか焼して調製した触媒組成物、多孔質材料との接触はしない
分子篩の前駆体溶液はTPAOH(テトラプロピルアザニウムハイドロオキサイド;CAS[66082−78−8])、H2O、硫酸アルミニウムおよびTEOS(テトラエトキシシラン;CAS[9044−80−8])を混合して調製した。各成分を上記の順序で順次加え、室温で3時間激しく撹拌しながら加水分解した。得られた溶液を使用前に100℃で12時間、熟成した。動的光散乱(DLS)の結果は、100℃で12時間熟成させたシード溶液中に狭い粒度分布を有する10nm以下の粒子が存在することを示している。溶液を蒸発させ、100℃で乾燥し、550℃で4時間か焼して触媒組成物を調製した。以下、このサンプルを「乾燥シード」とよぶ。
1回または複数回の含浸で改質された多孔質材料上に含浸する前に熟成した前駆体溶液を用いて調製した触媒組成物
多孔質材料はSiralox TH30(Sasol社)である。この多孔質材料上に堆積工程を繰り返して分子篩結晶を分散させて一連の触媒組成物を作った。
ZSM−5前駆体溶液は、TPAOH(テトラプロピルアザニウムハイドロオキサイド;CAS[66082−78−8])、H2O、硫酸アルミニウムおよびTEOS(テトラエトキシシラン;CAS[9044−80−8])を混合することによって調製した。各成分を上記の順序で順次加え、室温で3時間激しく撹拌しながら加水分解した。得られた溶液を使用前に100℃で12時間熟成した。動的光散乱(DLS)の結果は、100℃で12時間熟成させたシード溶液中に狭い粒度分布を有する10nm以下の粒子が存在することを示している。
使用した多孔質材料はAl2O3:SiO2比が70:30の噴霧乾燥形(〜40〜60μm)のSasol社から商業的に入手可能なシリカアルミナ酸化物のSiralox TH30である。使用前に600℃で2時間か焼した。この焼成でSiralox 30のアモルファスDRX信号は変化しなかった(図5参照)。
その後、同じ手順を使用してZSM−5前駆体溶液の含浸を3回繰り返した。特性評価前に固体を550℃で空気中で4時間か焼した。
得られた固形物はDRX([図5]参照)で特徴付けた。DRXパターンは固体がモルファスパターンを保存することを示している。同様に、「乾燥シード」もアモルファスDRXパターンを有する。
以下、上記サンプルを「1回含浸」または「3回含浸」とよぶ
実施例3で調製した材料の触媒試験
上記で調製した触媒組成物を用いてTiPBzクラッキング(分解)の触媒試験を実施した([図8]参照)。Siralox TH30を1回含浸して調製した材料の場合でも、「乾燥シード」(比較例)および含浸なしのSiralox TH30よりも高い活性を示す。実施例1で調製した材料も「乾燥シード」(比較例)よりも高い活性を示す。従って、多孔質材料上に上記シードを分散させる技術的利点は活性が高くなることと、シード含有物質のハンドリングが容易になる点にある。さらに、マトリックス上に活性サイトが分散していることで材料の配合(formulation)がより容易になる。
押出し成形物での処理
改質された多孔質材料を含浸する前に前駆体溶液を熟成する触媒組成物の調製
多孔質材料は1.5mmの押出し成形した円筒形のSiralox TH30(Sasol,Al2O3/SiO2−70/30重量%)で、この上にZSM−5分子篩の結晶を分散させた。触媒組成物は実施例1に記載の手順に従って144時間の熟成時間で調製した。ZSM−5が含浸されたサンプルに「C144」のサフィックスを付ける。合成には5gのサンプル用い、試薬の量は担体の量に比例して調整した。得られた触媒組成物で測定した表面積および酸サイトは[表5]に要約した。
27 Al MAS NMRによる各種触媒のキャラクタリゼーション
触媒組成物を27Al MAS NMRを用いてさらに特徴付けた。すなわち、各27Alサイトは互いに明確に異なる化学シフト(δ)を基にして容易に解析できるので、27Al MAS NMRを用いることによってゼオライトでの配位とアルミニウム種の局所構造とを決定することができる。[図13]は複合材料およびその前駆体の27Al MAS NMRスペクトルを示している。出発溶液の27Al NMRスペクトルは、アルミニウム原子が4配位でシリカ四面体格子内に組み込まれている四面体配位アルミニウム(AlIV)の51.3ppmの特性ピーク信号を示す。100℃で12時間熟成した後には、化学シフト約0.7ppmのピークで示されるように、熟成した前駆体中にもいくつかの八面体配位アルミニウム(AlVI)が存在する。
Claims (23)
- 少なくとも2ナノメートルの細孔径を有する無機多孔質材料と、分子篩結晶とを含む触媒組成物であって、
(1)走査型電子顕微鏡を用いて測定した上記分子篩結晶の平均直径が50nmを越えず、
(2)アンモニア昇温脱離法TPD NH3で測定した上記触媒組成物の酸サイトの濃度が50〜1200μmol/gの範囲内にあり、
(3)上記触媒組成物のX線回折パターンが上記無機多孔材料のX線回折パターンと同じである、
ことを特徴とする触媒組成物。 - 150℃でのピリジン脱着によって測定したブレンステッド酸サイト濃度が少なくとも10μmol/gである請求項1に記載の触媒組成物。
- 上記無機多孔質材料が非晶質である請求項1または2に記載の触媒組成物。
- 分子篩結晶を触媒組成物の全重量に対して30重量%以下含有する請求項1〜3のいずれか一項に記載の触媒組成物。
- 以下の一つまたは複数の特徴を有する請求項1〜4のいずれか一項に記載の触媒組成物:
(1)ASTM D3663を用いて測定した表面積が少なくとも250m2/gである、
(2)触媒組成物の全細孔容積をVtotal、触媒組成物の微孔容積をVmicroとしたときに、Vtotal/Vmicroの比が少なくとも5である(VtotalおよびVmicroはASTM D4365を用いて測定する) - 以下の一つまたは複数の特徴を有する請求項5に記載の触媒組成物:
(1)ASTM D3663を用いて測定した表面積が少なくとも350m 2 /gである、
(2)Vtotal/Vmicroの比が10以上である。 - 無機多孔質材料がメソポーラス容積および/またはマクロポーラス容積を有する細孔を有し、分子篩結晶がミクロポーラス容積を有する細孔を有し、メソポーラス容積および/またはマクロポーラス容積に対するミクロポーラス容積の比が0.2〜0.005である(上記容積はASTM D4365を用いて測定する)請求項1〜6のいずれか一項に記載の触媒組成物。
- 下記の一つまたは複数をさらに含む請求項1〜7のいずれか一項に記載の触媒組成物:
(1)リン
(2)B、Cr、Co、Ga、Fe、Li、Mg、Ca、Mn、La、Ti、Mo、W、Ni、Ag、Sn、Zn、Pt、Pd、Ru、Re、Os、Auの群の中から選択される少なくとも一つの金属またはこれらの任意の組み合わせ、
(3)シリカ、シリカアルミナ、金属シリケート、金属酸化物および/または金属、アモルファスアルモホスフェート(alumophosphate)またはシリカアルモホスフェート、シリカと金属酸化物の混合物を含むゲル、非晶質アルモホスフェートまたはこれらの任意の組合せの中から選択される少なくとも一つの結合剤。 - 分子篩結晶の孔径が2nm以下である請求項1〜8のいずれか一項に記載の触媒組成物。
- 分子篩結晶の孔径が0.5〜0.12nmの範囲である請求項9に記載の触媒組成物。
- 分子篩結晶がMFI型である請求項1〜10のいずれか一項に記載の触媒組成物。
- 分子篩結晶がZMS−5型である請求項11に記載の触媒組成物。
- 無機多孔質材料が下記の(1)または(2)である請求項1〜12のいずれか一項に記載の触媒組成物:
(1)シリカアルミナ、SiO2、Al2O3またはこれらの混合物、または
(2)Al/Siの原子比が>1であるAl2O3とSiO2とを含む非晶質無機材料。 - 無機多孔質材料がSi、O、Alとは異なる他の元素を500重量ppm以下の濃度で含む請求項13に記載の触媒組成物。
- 以下のa)、c)〜f)の工程を含む、請求項1〜14のいずれか一項に記載の触媒組成物の製造方法。
a)無機多孔質材料を用意し、
c)無機表面改質剤、イオン性または非イオン性界面活性剤、水溶性アニオンポリマー、水溶性カチオンポリマーの中から選択される少なくとも1種の電荷表面改質剤を含む溶液を用意し、
d)工程c)の溶液と工程b)で得られた材料とを接触させて、電荷表面改質剤で変性された非晶質無機多孔質体を作り、
e)分子篩の前駆体を含む溶液を用意し、
f)上記分子篩を下記i)および/またはii)と反応させる:
i)工程e)の溶液を0〜50時間の間、熟成(maturating)し、この熟成工程の後に動的光散乱(DLS)測定を行い、分子篩結晶が50nmの最大寸法になった時に熟成を停止し、変性された非晶質無機多孔質材料を熟成した溶液と接触させて分子篩結晶を工程d)で得られた変性された非晶質無機多孔質材料の表面上に堆積させる、および/または、
ii)工程d)で得られた変性された非晶質無機多孔質材料を工程e)の溶液と接触させ、得られた混合物を0〜50時間の間熟成してTPDアンモニアで測定した触媒組成物の酸度が無機多孔質材料の酸度と比較して少なくとも10%増加させ、
g)工程f)で得られた混合物の液体(存在する場合)から固体を分離し、
h)工程g)で得られた固体をか焼する。 - 工程a)と工程c)の間に、非晶質な上記無機多孔質材料を400℃〜1200℃の温度でか焼する工程b)をさらに有する請求項15に記載の触媒組成物の製造方法。
- 工程h)を実施する前に工程e)〜g)を少なくとも2回繰り返す請求項15または16に記載の方法。
- 工程h)を実施する前に溶液の熟成を各回で少なくとも30分間かつ最大で100時間行う請求項17に記載の方法。
- 工程e)〜g)を少なくとも1回実行し、溶液の熟成を最大で10時間行う請求項15〜18のいずれか一項に記載の方法。
- 溶液の熟成を最大で50時間行う請求項19に記載の方法。
- 工程h)の後に下記の工程の一つまたは複数を行う請求項15〜20ずれか一項に記載の方法:
(1)触媒組成物にリンを含む溶液を含浸させてリンを導入する、
(2)B、Cr、Co、Ga、Fe、Li、Mg、Ca、Mn、La、Ti、Mo、W、Ni、Ag、Sn、Zn、Pt、Pd、Ru、Re、Os、Auの群の中から選択される少なくとも1種の金属またはこれらの任意の組み合わせを添加して、触媒組成物を選択された金属塩を含む溶液で含浸する、
(3)噴霧乾燥、押出または当業者に公知の任意の適切な方法を用いて、シリカ、シリカアルミナ、金属シリケート、金属酸化物および/または金属、アモルファスアルモホスフェートまたはシリカアルモホスフェート、シリカ及び金属酸化物の混合物を含むゲル、非晶質アルモホスフェートまたはこれらの任意の組合せの中から選択される少なくとも一つの結合剤を加える、
(4)押出成形して触媒組成物を成形する。 - (1)の工程の後に焼成および/または蒸気処理の工程を行う請求項21に記載の方法。
- 請求項1〜13のいずれか一項に記載の触媒組成物の下記での使用:
1)流動接触分解反応、
2)バイオマス、ごみ、プラスチック誘導体の触媒熱分解またはその従来の化石原料との共同処理、
3)重質炭化水素および超重質原料の水素化分解、
4)オレフィンのオリゴマー化反応、
5)酸素化分子のオレフィン、ガソリン、芳香族化合物または蒸留物への変換、
6)オレフィンの軽質オレフィンへのクラッキング、
7)C4−C12パラフィンの接触分解、
8)異性化反応、
9)ガソリンの改質、
10)アルキル化反応、
11)アルコールの対応オレフィンへの脱水反応、
12)脱水素反応。
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CN114669287A (zh) * | 2022-04-26 | 2022-06-28 | 西安科技大学 | 一种有序介孔钛铝复合氧化物包覆ts-1分子筛材料及其制备方法 |
KR20240063619A (ko) * | 2022-11-03 | 2024-05-10 | 한국에너지기술연구원 | 양기능성 촉매, 양기능성 촉매의 브뢴스테드 산점 농도 측정 방법, 및 양기능성 촉매에서 피셔-트롭쉬 합성반응용 촉매 및 분해반응용 촉매의 배합 비율을 결정하는 방법 |
KR20240081806A (ko) * | 2022-12-01 | 2024-06-10 | 한국화학연구원 | 유기화합물로부터 산소를 선택적으로 제거하여 올레핀 및 파라핀 중 하나 이상의 탄화수소 화합물을 제조하는 RuSn/SiAl 촉매 |
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US20190168194A1 (en) | 2019-06-06 |
BR112016000038B1 (pt) | 2021-03-16 |
US20160136625A1 (en) | 2016-05-19 |
US10239051B2 (en) | 2019-03-26 |
EP3016738A1 (en) | 2016-05-11 |
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