JP2014501219A - 金属ナノ粒子をメソ構造化酸化物マトリクス中に捕捉されて含む球状材料、および精製方法における触媒としてのその使用 - Google Patents
金属ナノ粒子をメソ構造化酸化物マトリクス中に捕捉されて含む球状材料、および精製方法における触媒としてのその使用 Download PDFInfo
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- JP2014501219A JP2014501219A JP2013545452A JP2013545452A JP2014501219A JP 2014501219 A JP2014501219 A JP 2014501219A JP 2013545452 A JP2013545452 A JP 2013545452A JP 2013545452 A JP2013545452 A JP 2013545452A JP 2014501219 A JP2014501219 A JP 2014501219A
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- metal
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- metal nanoparticles
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- 239000011159 matrix material Substances 0.000 title claims abstract description 78
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 61
- 239000000463 material Substances 0.000 title claims description 134
- 239000003054 catalyst Substances 0.000 title description 27
- 238000000746 purification Methods 0.000 title 1
- 229910052751 metal Inorganic materials 0.000 claims abstract description 76
- 239000002184 metal Substances 0.000 claims abstract description 76
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 49
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 43
- 239000012798 spherical particle Substances 0.000 claims abstract description 42
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000010937 tungsten Substances 0.000 claims abstract description 40
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 39
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011733 molybdenum Substances 0.000 claims abstract description 34
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- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 31
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 31
- 239000011147 inorganic material Substances 0.000 claims abstract description 31
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- 239000010955 niobium Substances 0.000 claims abstract description 31
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 28
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 25
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 25
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 15
- 239000010936 titanium Substances 0.000 claims abstract description 15
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 14
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 14
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- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 11
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 9
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 8
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- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 8
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052718 tin Inorganic materials 0.000 claims abstract description 8
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- 239000010457 zeolite Substances 0.000 claims description 92
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 85
- 239000002243 precursor Substances 0.000 claims description 83
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- 239000000203 mixture Substances 0.000 claims description 70
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- 238000000034 method Methods 0.000 claims description 58
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 238000002360 preparation method Methods 0.000 claims description 43
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 31
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 24
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- 229910052717 sulfur Inorganic materials 0.000 claims description 14
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- 229910052698 phosphorus Inorganic materials 0.000 claims description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 229910052731 fluorine Inorganic materials 0.000 claims description 12
- 239000011574 phosphorus Substances 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 11
- 229910017052 cobalt Inorganic materials 0.000 claims description 11
- 239000010941 cobalt Substances 0.000 claims description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 11
- 239000011737 fluorine Substances 0.000 claims description 11
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 150000002739 metals Chemical class 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 230000000737 periodic effect Effects 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
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- 239000001301 oxygen Substances 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
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- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 238000010924 continuous production Methods 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract 2
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 13
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 3
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- 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
- B01J29/48—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 arsenic, antimony, bismuth, vanadium, niobium tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
Description
1)水素化脱水素相の良好な分散を、特に高い金属含有率のために確実なものにする(例えば、遷移金属をベースとする粒子のサイズを制御する、熱処理後にこれらの粒子の特性を維持する、等によって);
2)硫化に対して抵抗性である種の形成を制限する(例えば、活性相を形成する遷移金属間のより良好な相乗効果を得る、水素化脱水素活性相(および/またはその前駆体)と採用された多孔性担体との間の相互作用を制御する、等によって);
3)開発された活性な表面積を高く維持しながら、反応物質および反応生成物の良好な分散を確実なものとする(多孔性担体の化学的、表面組織的および構造的な特性の最適化);
ために用いられ得るだろうこれらの触媒の調製のための新規な方法を開発することによって向上させられ得るだろう。
本発明は、少なくとも2つの基本球状粒子によって構成された無機材料であって、前記球状粒子のそれぞれは、金属ナノ粒子を含み、この金属ナノ粒子は、ラマン分光法において750〜1050cm−1の範囲の波数を有する少なくとも1つのバンドを有し、かつ、バナジウム、ニオブ、タンタル、モリブデンおよびタングステンから選択される少なくとも1種の金属を含有し、前記金属ナノ粒子は、メソ構造化マトリクス内に存在し、このメソ構造化マトリクスは、ケイ素、アルミニウム、チタン、タングステン、ジルコニウム、ガリウム、ゲルマニウム、スズ、アンチモン、鉛、バナジウム、鉄、マンガン、ハフニウム、ニオブ、タンタル、イットリウム、セリウム、ガドリニウム、ユーロピウムおよびネオジムおよびこれらの元素の少なくとも2種の混合によって構成される群から選択される少なくとも1種の元素Yの酸化物をベースとし、前記マトリクスは、1.5〜50nmの範囲の径を有する細孔を有し、かつ、1〜30nmの範囲の厚さを有する無定形壁を有し、前記基本球状粒子は、200ミクロンの最大径を有し、前記金属ナノ粒子は、厳密に1nm未満の最大寸法を有する、無機材料に関する。
本発明の材料であって、金属ナノ粒子を、前記材料を構成する基本球状粒子のそれぞれのメソ構造化マトリクス中に捕捉されて含む、材料は、有利な触媒前駆体である。それは、同時に、金属ナノ粒子の存在に密接に関連する特性、特に、活性相のより良好な分散、水素化脱水素部位と任意の酸性部位との間のより良好な相乗効果、硫化に対して抵抗性の相の低減、並びに、少なくとも1種の元素Yの酸化物をベースとするメソ構造化材料に特有の、構造的、表面組織的、かつ場合による酸塩基の特性および酸化還元特性、特に、試薬および反応生成物の非制限的物質移動および高い活性表面積の値を有する。金属ナノ粒子は、硫化後に、本発明の材料から得られる触媒中に存在する活性硫化相の前駆体種である。
本発明は、少なくとも2つの基本球状粒子によって構成された無機材料であって、前記球状粒子のそれぞれは、金属ナノ粒子を含み、この金属ナノ粒子はラマン分光法において750〜1050cm−1の範囲の波数を有する少なくとも1つのバンドを有し、かつ、バナジウム、ニオブ、タンタル、モリブデンおよびタングステンから選択される少なくとも1種の金属を含有し、前記金属ナノ粒子は、メソ構造化マトリクス内に存在し、このメソ構造化マトリクスは、ケイ素、アルミニウム、チタン、タングステン、ジルコニウム、ガリウム、ゲルマニウム、スズ、アンチモン、鉛、バナジウム、鉄、マンガン、ハフニウム、ニオブ、タンタル、イットリウム、セリウム、ガドリニウム、ユーロピウムおよびネオジム、並びに、それらの元素の少なくとも2種の混合によって構成された群から選択される少なくとも1種の元素Yの酸化物をベースとし、前記マトリクスは、1.5〜50nmの範囲の径を有する細孔を有し、かつ、厚さが1〜30nmの範囲の無定形壁を有し、前記基本球状粒子の最大径は200ミクロンであり、前記金属ナノ粒子の最大寸法は厳密に1nm未満である、無機材料に関する。
される少なくとも1種のゼオライトを含む。種々のゼオライト、特に異なる構造型のゼオライトのナノ結晶は、本発明による材料を構成する球状粒子のそれぞれの中に存在してよい。特に、本発明による材料を構成する球状粒子のそれぞれは、有利には、少なくとも第1のゼオライトナノ結晶と、少なくとも第2のゼオライトナノ結晶とを含んでよく、第1のゼオライトナノ結晶は、ゼオライトIZM−2、ZSM−5、ZSM−12、ZSM−48、ZSM−22、ZSM−23、ZBM−30、EU−2、EU−11、シリカライト、ベータ、ゼオライトA、フォージャサイト、Y、USY、VUSY、SDUSY、モルデナイト、NU−10、NU−87、NU−88、NU−86、NU−85、IM−5、IM−12、IM−16、フェリエライトおよびEU−1から、好ましくは、MFI、BEA、FAUおよびLTAの構造型のゼオライトから選択され、第2のゼオライトナノ結晶は、第1のゼオライトナノ結晶のものとは異なっており、かつ、ゼオライトIZM−2、ZSM−5、ZSM−12、ZSM−48、ZSM−22、ZSM−23、ZBM−30、EU−2、EU−11、シリカライト、ベータ、ゼオライトA、フォージャサイト、Y、USY、VUSY、SDUSY、モルデナイト、NU−10、NU−87、NU−88、NU−86、NU−85、IM−5、IM−12、IM−16、フェリエライトおよびEU−1から、好ましくはMFI、BEA、FAUおよびLTAの構造型を有するゼオライトから選択される。ゼオライトナノ結晶は、有利には、全体的にシリカであるか、または、ケイ素に加えて、アルミニウム、鉄、ホウ素、インジウム、ガリウムおよびゲルマニウムから選択される少なくとも1種の元素T、好ましくはアルミニウムを含有する、少なくとも1種のゼオライトを含む。
a)溶液中:
− 少なくとも1種の界面活性剤と;
− ケイ素、アルミニウム、チタン、タングステン、ジルコニウム、ガリウム、ゲルマニウム、スズ、アンチモン、鉛、バナジウム、鉄、マンガン、ハフニウム、ニオブ、タンタル、イットリウム、セリウム、ガドリニウム、ユーロピウムおよびネオジム、並びに、それらの元素の少なくとも2種の混合によって構成される群から選択される少なくとも1種の元素Yの少なくとも1種の前駆体と;
− ラマン分光法において750〜1050cm−1の範囲の波数を有する少なくとも1つのバンドを有する金属ナノ粒子中に存在する、バナジウム、ニオブ、タンタル、モリブデンおよびタングステンから選択される少なくとも1種の金属を含有する少なくとも1種の第1の金属前駆体と;
− 場合による、最大ナノメートル寸法が300nmに等しいゼオライト結晶が分散している、少なくとも1種のコロイド溶液と;
を混合する工程と:
b)工程a)で得られた前記溶液のエアロゾル噴霧により、球状液体小滴が形成されるに至る工程と;
c)前記小滴を乾燥させる工程と;
d)少なくとも前記界面活性剤を除去して、前記金属ナノ粒子が捕捉された前記メソ構造化無機材料を得る工程と;
を含む。
以下の実施例において、用いられたエアロゾル技術は、本発明の開示において上記に記載されたものであった。用いられた分散ラマン分光計は、Horiba Jobin-Yvonによって供給された市販のLabRAM Aramisの装置であった。用いられたレーザの励起波長は532nmであった。以下の実施例1〜5の実施におけるこのスペクトログラフの操作は、上記に記載された。
0.29gのMoCl5と、0.04gのCo(OH)2と、15.0gの置換水(permutated water)を含有する水溶液を、撹拌しながら、周囲温度で調製した。
0.17gのWCl4と、0.02gのNi(OH)2と、15.0gの置換水とを含有する水溶液を、撹拌しながら、周囲温度で調製した。
0.35gのWCl4と、0.04gのNi(OH)2と、15.0gの置換水とを含有する水溶液を、撹拌しながら、周囲温度で調製した。
0.14gのアルミニウム トリ−sec−ブトキシドを、3.50mLの水酸化物TPAOH、0.01gの水酸化ナトリウムNaOH、および4.30mLの水を含有する溶液中に添加した。アルミニウムアルコキシドを溶解させた後、5.90gのオルトケイ酸テトラエチル(TEOS)を添加した。溶液を、周囲温度で5時間にわたり撹拌し、次いで、T=95℃で12時間にわたりオートクレーブ処理した。得られた白色溶液は、動的光散乱(dynamic light scattering:DLS)によって測定される、135nmの寸法を有するZSM−5のナノ結晶を含有していた。この溶液を、20000rpmで30分間にわたり遠心分離にかけた。固体を水中に再分散させて、次いで、再度20000rpmで30分間にわたり遠心分離にかけた。この洗浄を2回行った。ナノ結晶はゲルを形成し、これを、終夜60℃でオーブン乾燥させた。
0.14gのアルミニウム トリ−sec−ブトキシドを、3.50mLの水酸化物TPAOH、0.01gの水酸化ナトリウムNaOH、および4.30mLの水を含有する溶液中に添加した。アルミニウムアルコキシドを溶解させた後、5.90gのオルトケイ酸テトラエチル(TEOS)を添加した。溶液を、周囲温度で5時間にわたり撹拌し、次いで、T=95℃で12時間にわたりオートクレーブ処理した。得られた白色溶液は、DLSによって測定される、135nmに等しい寸法を有するZSM−5のナノ結晶を含有していた。この溶液を、20000rpmで30分間にわたり遠心分離にかけた。固体を水中で再分散させて、次いで、再度20000rpmで30分間にわたり遠心分離にかけた。この洗浄を2回行った。ナノ結晶はゲルを形成し、これを、終夜60℃でオーブン乾燥させた。
Claims (15)
- 少なくとも2つの基本球状粒子によって構成された無機材料であって、前記球状粒子のそれぞれは、金属ナノ粒子を含み、該金属ナノ粒子は、ラマン分光法において750〜1050cm−1の範囲の波数を有する少なくとも1つのバンドを有し、かつ、バナジウム、ニオブ、タンタル、モリブデンおよびタングステンから選択される少なくとも1種の金属を含有し、前記金属ナノ粒子は、メソ構造化マトリクス内に存在し、該メソ構造化マトリクスは、ケイ素、アルミニウム、チタン、タングステン、ジルコニウム、ガリウム、ゲルマニウム、スズ、アンチモン、鉛、バナジウム、鉄、マンガン、ハフニウム、ニオブ、タンタル、イットリウム、セリウム、ガドリニウム、ユーロピウムおよびネオジム、並びに、それらの元素の少なくとも2種の混合によって構成された群から選択される少なくとも1種の元素Yの酸化物をベースとし、前記マトリクスは、1.5〜50nmの範囲の径を有する細孔を有し、かつ、厚さが1〜30nmの範囲の無定形壁を有し、前記基本球状粒子の最大径は200ミクロンであり、前記金属ナノ粒子の最大寸法は厳密に1nm未満である、無機材料。
- 前記メソ構造化マトリクスは、酸化アルミニウム、酸化ケイ素、酸化ケイ素および酸化アルミニウムの混合物または酸化ケイ素および酸化ジルコニウムの混合物によって構成される、請求項1に記載の材料。
- 前記マトリクスは、4〜20nmの範囲の径を有する細孔を有する、請求項1または2に記載の材料。
- 前記マトリクスは、1〜10nmの範囲の厚さの無定形壁を有する、請求項1〜3のいずれか1つに記載の材料。
- 前記金属ナノ粒子は、モリブデンおよび/またはタングステンを含有する、請求項1〜4のいずれか1つに記載の材料。
- 前記金属ナノ粒子は、ラマン分光法において750〜950cm−1の範囲または950〜1050cm−1の範囲の波数を有する少なくとも1つのバンドを有する、請求項1〜5のいずれか1つに記載の材料。
- 球状粒子のそれぞれは、前記材料の0.1〜30重量%を表すゼオライトナノ結晶を含む、請求項1〜6のいずれか1つに記載の材料。
- 前記ゼオライトナノ結晶は、MFI、BEA、FAUおよびLTAの構造型のゼオライトから選択される少なくとも1種のゼオライトを含む、請求項7に記載の材料。
- 球状粒子のそれぞれは、有機剤と、元素周期律分類の第VIII族金属と、リン、フッ素、ケイ素およびホウ素、並びにそれらの混合物によって構成されるドーピング元素のリストに属するドーピング種とから選択される1種以上の追加要素を含む、請求項1〜8のいずれか1つに記載の材料。
- 追加要素としての前記第VIII族金属は、コバルト、ニッケルおよびこれら2種の金属の混合物から選択される、請求項9に記載の材料。
- 50〜1100m2/gの範囲の比表面積を有する、請求項1〜10のいずれか1つに記載の材料。
- 請求項1〜11のいずれか1つに記載の無機材料の調製方法であって、少なくとも以下の連続する工程:
a)溶液中:
− 少なくとも1種の界面活性剤と;
− ケイ素、アルミニウム、チタン、タングステン、ジルコニウム、ガリウム、ゲルマニウム、スズ、アンチモン、鉛、バナジウム、鉄、マンガン、ハフニウム、ニオブ、タンタル、イットリウム、セリウム、ガドリニウム、ユーロピウムおよびネオジム、並びに、それらの元素の少なくとも2種の混合によって構成される群から選択される少なくとも1種の元素Yの少なくとも1種の前駆体と;
− ラマン分光法において750〜1050cm−1の範囲の波数を有する少なくとも1つのバンドを有する金属ナノ粒子中に存在する、バナジウム、ニオブ、タンタル、モリブデンおよびタングステンから選択される少なくとも1種の金属を含有する少なくとも1種の第1の金属前駆体と;
− 場合による、最大ナノメートル寸法が300nmに等しいゼオライト結晶が分散している、少なくとも1種のコロイド溶液と;
を混合する工程と:
b)工程a)で得られた前記溶液のエアロゾル噴霧により、球状液体小滴が形成されるに至る工程と;
c)前記小滴を乾燥させる工程と;
d)少なくとも前記界面活性剤を除去する工程と;
を含む、方法。 - バナジウム、ニオブ、タンタル、モリブデンおよびタングステンから選択される金属をベースとする少なくとも前記第1の金属前駆体と、第VIII族金属をベースとする少なくとも1種の第2の単金属前駆体とを、前記工程a)を行う前に溶解させ、次いで、前記溶液を、前記工程a)による混合物中に導入する、請求項12に記載の調製方法。
- 炭化水素供給原料の転換方法であって、
1)請求項1〜11のいずれか1つに記載のメソ構造化無機材料を、少なくとも1種の硫黄含有化合物を含む供給原料と接触させること、次いで、2)前記工程1)から得られた前記材料を、前記炭化水素供給原料と接触させることを含む、炭化水素供給原料の転換方法。 - 前記供給原料は、窒素、酸素および/または硫黄から選択されるヘテロ元素を含有する分子を含む、請求項14に記載の転換方法。
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Also Published As
Publication number | Publication date |
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US20140027346A1 (en) | 2014-01-30 |
WO2012085354A1 (fr) | 2012-06-28 |
FR2969511B1 (fr) | 2012-12-28 |
CN103547363A (zh) | 2014-01-29 |
EP2654945A1 (fr) | 2013-10-30 |
ZA201304070B (en) | 2014-02-26 |
FR2969511A1 (fr) | 2012-06-29 |
EP2654945B1 (fr) | 2019-08-21 |
JP5907992B2 (ja) | 2016-04-26 |
CN103547363B (zh) | 2017-05-03 |
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