JP5037471B2 - ベーマイト型結晶アルミナの製造方法とベーマイト型結晶アルミナ - Google Patents
ベーマイト型結晶アルミナの製造方法とベーマイト型結晶アルミナ Download PDFInfo
- Publication number
- JP5037471B2 JP5037471B2 JP2008261743A JP2008261743A JP5037471B2 JP 5037471 B2 JP5037471 B2 JP 5037471B2 JP 2008261743 A JP2008261743 A JP 2008261743A JP 2008261743 A JP2008261743 A JP 2008261743A JP 5037471 B2 JP5037471 B2 JP 5037471B2
- Authority
- JP
- Japan
- Prior art keywords
- aluminum
- aluminum oxide
- oxide
- boehmite
- alumina
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 52
- 229910001593 boehmite Inorganic materials 0.000 title claims description 31
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000013078 crystal Substances 0.000 title claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229910001868 water Inorganic materials 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 239000011148 porous material Substances 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 238000010335 hydrothermal treatment Methods 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- -1 aluminum alkoxide compound Chemical class 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 5
- 229910052753 mercury Inorganic materials 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035515 penetration Effects 0.000 claims 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- WMWXXXSCZVGQAR-UHFFFAOYSA-N dialuminum;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3] WMWXXXSCZVGQAR-UHFFFAOYSA-N 0.000 description 12
- 239000002002 slurry Substances 0.000 description 11
- 239000003054 catalyst Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 5
- 238000000634 powder X-ray diffraction Methods 0.000 description 5
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 5
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000004438 BET method Methods 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- QFCVQKSWGFVMTB-UHFFFAOYSA-N trihexoxyalumane Chemical compound [Al+3].CCCCCC[O-].CCCCCC[O-].CCCCCC[O-] QFCVQKSWGFVMTB-UHFFFAOYSA-N 0.000 description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- GKQPCPXONLDCMU-CCEZHUSRSA-N lacidipine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C1=CC=CC=C1\C=C\C(=O)OC(C)(C)C GKQPCPXONLDCMU-CCEZHUSRSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 150000005671 trienes Chemical class 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/447—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/447—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes
- C01F7/448—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes using superatmospheric pressure, e.g. hydrothermal conversion of gibbsite into boehmite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
- Compositions Of Oxide Ceramics (AREA)
Description
ベーマイト→γ一Al2 O3 →δ−Al2 O3 →θ−Al2 O3→α−Al2 O3
また、アルミニウムと酸素の化合物を、水と、ジルコニウム、チタン、ランタンおよび/またはホウ素の酸化物又は酸化物水和物との存在下に、ただし前記酸化物は酸化アルミニウムに対して0.1〜5重量%の量とし、40ないし240℃で少なくとも8時間にわたって水熱処理することにより熟成させ、020反射面でnm単位で決定される結晶子の大きさを、120反射面で決定される結晶子の大きさから1.5nmだけ減じた値より大きくすることを特徴とする。
本発明に係るベーマイト型結晶アルミナは、020反射面でnm単位で決定される結晶子の大きさが、120反射面で決定される結晶子の大きさから1.5nmだけ減じた値より大きく、ジルコニウム、チタン、ランタンおよび/またはホウ素の酸化物または酸化物水和物が含まれており、前記酸化物が酸化アルミニウムに対して0.1〜5重量%の量で含まれていることを特徴とする。
製造に当たっては、酸化アルミニウム水和物のスラリーにわずかなせん断効果を加えることが好ましい。本発明で言うわずかなせん断効果とは、回転速度0.5ないし3m/sで運転される撹拌機(たとえばプロペラ撹拌機)によって作られるせん断を意味する。スラリーに使用される酸化アルミニウム水和物の粒子径は1ないし12μmが好ましく、特に6ないし12μmが好ましい。
結晶子の大きさ=(K×λ×57.3)/(β×cosθ)
K(形状係数): 0.992
入(X線の波長): 0.154nm
β(装置に固有の線幅の広がり補正): 反射に依存
θ: 反射に依存
以下に述べるようにしてアルミニウムアルコラートを中性加水分解し、出発原料のアルミナスラリーを調製した。
た。
反射面 β θ 結晶子の大きさ
120 0.919 14゜ 9.8n m
020 0 919 7゜ 6.7n m
120反射面の方が、020反射面より3.1nmだけ大きい。
比較例で述べた、Al2 O3を10ないし11重量%含有するpH9のアルミナスラリー500gを回分式反応装置に仕込んだ。反応装置の圧力を98℃の常圧とした。反応条件を調整した後、通常の摸拝機を使用し、摸拝速度1.6m/s、回転数500回転/分で16時間熟成した。比較例で説明した方法によって得られた結晶子の大きさは、120面で13.5nm、020面で12.1nmであった。
比較例で述べた、Al2 O3を10ないし11重量%含有するpH9のアルミナスラリー500gを回分式反応装置に仕込んだ。反応装置の圧力を3bar、110℃とした。反応条件を調整した後、通常の撹拌機を使用し、撹拌速度1.6m/s、回転数500回転/分で40時間熟成した。
比較例で述べた、Al2 O3を10ないし11重量%含有するpH9のアルミナスラリー500gを回分式反応装置に仕込んだ。反応装置の圧力を3bar、110℃とした。反応条件を調整した後、通常の撹拌機を使用して撹拌速度1.6m/s、回転数500回転/分で60時間熟成した。
比較例で述べた、Al2 O3を10ないし11重量%含有するpH9のアルミナスラリー600gにテトレンの20%水溶液50gを加え、68時間煮沸還流させた。その間、その時々に応じて1時間後に水300gを添加した。混合物に水200gを加えて希釈し、噴霧乾燥させた。
アルミニウム・トリーn−ヘキサノラートの6.02%n−ヘキサノール溶液300gに90℃で5%テトレン水溶液360gを加えて混合し、90℃で30分撹拌した。反応混合物から共沸蒸留によってヘキサノールを除去した。つづいて残留物を90℃で24時間撹拌した。その間、場合に応じて1時間後、2時間後および3時間後に水100gを添加した。反応混合物を噴霧乾燥した。
アルミニウム・トリーn−ヘキサノラートの6.02%n−ヘキサノール溶液300gに90℃で5%テトレン水溶液360gを加えて混合し、90℃で30分撹拌した。反応混合物から共沸蒸留によってヘキサノールを除去した。つづいて、残留物を90℃で68時間撹拌した。その間、場合に応じて1時間後、2時間後および3時間後に水100gを添加した。反応混合物を噴霧乾燥した。
Claims (10)
- アルミニウムと酸素の化合物を水および少なくとも二座塩基の存在下に、30ないし240℃で0.5ないし170時間にわたって水熱処理することにより熟成させることを特徴とするベーマイト型結晶アルミナの製造方法。
- アルミニウムと酸素の化合物を、水と、ジルコニウム、チタン、ランタンおよび/またはホウ素の酸化物又は酸化物水和物との存在下に、ただし前記酸化物は酸化アルミニウムに対して0.1〜5重量%の量とし、
40ないし240℃で少なくとも8時間にわたって水熱処理することにより熟成させ、
020反射面でnm単位で決定される結晶子の大きさを、120反射面で決定される結晶子の大きさから1.5nmだけ減じた値より大きくすることを特徴とするベーマイト型結晶アルミナの製造方法。 - 前記ベーマイト型結晶アルミナをか焼により熱処理し、60m2/gより大きな表面積を有する酸化アルミニウムを得ることを特徴とする請求項1または2記載の方法。
- 前記ベーマイト型結晶アルミナをか焼により熱処理し、水銀浸透法で決定される細孔容積が、1.8ないし100nmの細孔半径に対して、0.6cm3/gより大きい細孔容積を有する酸化アルミニウムを得ることを特徴とする請求項1または2記載の方法。
- 前記ベーマイト型結晶アルミナが800ないし1500℃で少なくとも0.5時間のか焼処理が行われることを特徴とする請求項1または2記載の方法。
- 前記ベーマイト型結晶アルミナの熱処理により、純θ相または純δ相酸化アルミニウムを得ることを特徴とする請求項1または2記載の方法。
- 前記アルミニウムと酸素の化合物が、少なくとも1つのアルミニウムアルコキシド化合物の加水分解によって得られたものであることを特徴とする請求項1または2記載の方法。
- 020反射面でnm単位で決定される結晶子の大きさが、120反射面で決定される結晶子の大きさから1.5nmだけ減じた値より大きく、
ジルコニウム、チタン、ランタンおよび/またはホウ素の酸化物または酸化物水和物が含まれており、前記酸化物が酸化アルミニウムに対して0.1〜5重量%の量で含まれていることを特徴とするベーマイト型結晶アルミナ。 - 請求項8に記載のベーマイト型結晶アルミナを、800〜1500℃で少なくとも0.5時間か焼して得られたことを特徴とする酸化アルミニウム。
- θ相またはδ相で存在することを特徴とする請求項9記載の酸化アルミニウム。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19836821.6 | 1998-08-14 | ||
DE19836821A DE19836821A1 (de) | 1998-08-14 | 1998-08-14 | Böhmitische Tonerden und aus diesen erhältliche phasenreine, hochtemperaturstabile und hochporöse Aluminiumoxide |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2000564900A Division JP4238963B2 (ja) | 1998-08-14 | 1999-08-05 | ベーマイト型結晶アルミナとそれから得られる純単一相から成る高温安定性高多孔性酸化アルミニウム |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2009001492A JP2009001492A (ja) | 2009-01-08 |
JP5037471B2 true JP5037471B2 (ja) | 2012-09-26 |
Family
ID=7877491
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2000564900A Expired - Lifetime JP4238963B2 (ja) | 1998-08-14 | 1999-08-05 | ベーマイト型結晶アルミナとそれから得られる純単一相から成る高温安定性高多孔性酸化アルミニウム |
JP2008261743A Expired - Fee Related JP5037471B2 (ja) | 1998-08-14 | 2008-10-08 | ベーマイト型結晶アルミナの製造方法とベーマイト型結晶アルミナ |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2000564900A Expired - Lifetime JP4238963B2 (ja) | 1998-08-14 | 1999-08-05 | ベーマイト型結晶アルミナとそれから得られる純単一相から成る高温安定性高多孔性酸化アルミニウム |
Country Status (6)
Country | Link |
---|---|
US (3) | US6773690B1 (ja) |
EP (2) | EP2258659B1 (ja) |
JP (2) | JP4238963B2 (ja) |
DE (1) | DE19836821A1 (ja) |
WO (1) | WO2000009445A2 (ja) |
ZA (1) | ZA200001778B (ja) |
Families Citing this family (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19836821A1 (de) * | 1998-08-14 | 2000-02-24 | Rwe Dea Ag | Böhmitische Tonerden und aus diesen erhältliche phasenreine, hochtemperaturstabile und hochporöse Aluminiumoxide |
JP5117657B2 (ja) * | 1999-08-11 | 2013-01-16 | アルベマーレ ネザーランズ ビー.ブイ. | 安価な前駆体から擬結晶性ベーマイトを製造する方法 |
FR2823193B1 (fr) | 2001-04-04 | 2004-02-13 | Pro Catalyse | Agglomeres d'alumine, leur procede de preparation, et leurs utilisations comme support de catalyseur, catalyseur ou absorbant |
FR2823194B1 (fr) * | 2001-04-10 | 2004-02-13 | Pro Catalyse | Agglomeres d'alumine utilisables, notamment, comme supports de catalyseur, catalyseurs ou adsorbants, et leurs procedes de preparation |
US7341976B2 (en) * | 2002-10-16 | 2008-03-11 | Conocophillips Company | Stabilized boehmite-derived catalyst supports, catalysts, methods of making and using |
WO2004035196A2 (en) * | 2002-10-16 | 2004-04-29 | Conocophillips Company | A stabilized transition alumina catalyst support from boehmite and catalysts made therefrom |
DE10332775A1 (de) * | 2003-07-17 | 2005-02-17 | Sasol Germany Gmbh | Verfahren zur Herstellung böhmitischer Tonerden mit hoher a-Umwandlungstemperatur |
CN1942242B (zh) * | 2004-03-12 | 2011-07-27 | 圣戈本陶瓷及塑料股份有限公司 | 用于催化剂载体的喷雾干燥的氧化铝 |
TWI297673B (en) * | 2004-11-11 | 2008-06-11 | Univ Nat Cheng Kung | High specific surface area composite alumina powder with thermal resistance and method for producing the same |
JP4782445B2 (ja) * | 2005-03-09 | 2011-09-28 | 富士フイルム株式会社 | Bi12MO20粉体の製造方法および放射線撮像パネルを構成する光導電層 |
CN101175567B (zh) * | 2005-05-12 | 2011-06-08 | 索维公司 | 氧氯化催化剂和使用这种催化剂的方法 |
MX2008002612A (es) * | 2005-08-25 | 2009-02-25 | Sasol North America Inc | Proceso para producir aluminas de boehmita de alta porosidad. |
TWI432381B (zh) * | 2005-12-12 | 2014-04-01 | Grace W R & Co | 氧化鋁粒子 |
TW200846286A (en) * | 2007-05-22 | 2008-12-01 | Grace W R & Co | Alumina particles and methods of making the same |
CN101827651B (zh) | 2007-08-29 | 2015-06-10 | 太平洋工业发展公司 | 稀土氧化铝颗粒生产方法和应用 |
FR2927267B1 (fr) * | 2008-02-07 | 2010-04-16 | Inst Francais Du Petrole | Catalyseur d'hydrogenation selective et son procede de preparation |
DE102008058393A1 (de) | 2008-11-21 | 2010-05-27 | Süd-Chemie AG | Aluminiumoxidhaltige Adsorbentien zur Aufreinigung von Biodiesel |
US8329607B2 (en) | 2009-01-16 | 2012-12-11 | Basf Corporation | Layered diesel oxidation catalyst composites |
DE102009032080A1 (de) | 2009-07-07 | 2011-01-13 | Süd-Chemie AG | Verfahren zur Auftrennung von Alkohol-Keton-Gemischen |
TWI666310B (zh) | 2013-03-15 | 2019-07-21 | Advanced Refining Technologies Llc | 觸媒組成物、加氫處理重烴類部分之方法及製備沉澱氧化鋁組成物的方法 |
CN104148096B (zh) * | 2013-05-15 | 2016-05-25 | 中国石油化工股份有限公司 | 一种双金属重整催化剂及其制备方法 |
EP3059012A1 (en) * | 2015-02-17 | 2016-08-24 | SASOL Germany GmbH | Coated composites of al2o3-ceo2/zro2 and a method for their production |
JP6652410B2 (ja) * | 2016-03-07 | 2020-02-19 | 曙ブレーキ工業株式会社 | 摩擦材 |
WO2018021192A1 (ja) | 2016-07-29 | 2018-02-01 | 住友化学株式会社 | アルミナおよびそれを用いた自動車触媒の製造方法 |
EP3599221A1 (en) * | 2018-07-27 | 2020-01-29 | SASOL Germany GmbH | Alpha alumina with high purity and high relative density, a method for its production and its use |
CN115996791A (zh) | 2020-06-26 | 2023-04-21 | 巴斯夫欧洲公司 | 生产多孔α-氧化铝催化剂载体的方法 |
US20230256420A1 (en) | 2020-06-26 | 2023-08-17 | Basf Se | Shaped catalyst body for the production of ethylene oxide |
US20230256415A1 (en) | 2020-06-26 | 2023-08-17 | Basf Se | Production of porous alpha-alumina supports from boehmitic derived aluminas |
CN117545552A (zh) | 2021-06-25 | 2024-02-09 | 巴斯夫欧洲公司 | 高纯度压片阿尔法氧化铝催化剂载体 |
Family Cites Families (37)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3714343A (en) * | 1967-06-26 | 1973-01-30 | Mitsubishi Chem Ind | Alumina hydrate,theta-alumina and a method for the manufacture thereof |
US4055509A (en) * | 1972-09-22 | 1977-10-25 | Continental Oil Company | Method for increasing the water dispersibility of alpha alumina monohydrate |
US3898322A (en) | 1972-12-15 | 1975-08-05 | Continental Oil Co | Alumina having a binodal pore volume distribution |
US4061594A (en) * | 1974-01-10 | 1977-12-06 | Rhone-Poulenc Industries | Alumina-based bodies obtained by agglomeration which are resistant to elevated temperatures |
US4081353A (en) * | 1976-10-15 | 1978-03-28 | Gulf Research & Development Company | Hydrodesulfurization with a specific alumina-supported catalyst |
US4179408A (en) * | 1977-03-25 | 1979-12-18 | W. R. Grace & Co. | Process for preparing spheroidal alumina particles |
US4117106A (en) * | 1977-08-01 | 1978-09-26 | Continental Oil Company | Method for producing bayerite |
JPS5527830A (en) * | 1978-08-15 | 1980-02-28 | Chiyoda Chem Eng & Constr Co Ltd | Production of alumina carrier |
US4360449A (en) * | 1979-09-04 | 1982-11-23 | Conoco Inc. | Alumina dispersion behavior |
US5244648A (en) * | 1980-12-23 | 1993-09-14 | Rhone-Poulenc Industries | Process for the preparation of alumina agglomerates |
JPS6046923A (ja) * | 1983-08-23 | 1985-03-14 | Mitsubishi Chem Ind Ltd | ベ−マイト |
IT1184114B (it) * | 1985-01-18 | 1987-10-22 | Montedison Spa | Alfa allumina sotto forma di particelle sferiche,non aggregate,a distribuzione granulometrica ristretta e di dimensioni inferiori a 2 micron,e processo per la sua preparazione |
US4676928A (en) * | 1986-01-30 | 1987-06-30 | Vista Chemical Company | Process for producing water dispersible alumina |
US4744974A (en) * | 1986-09-23 | 1988-05-17 | Vista Chemical Company | Process for production of alumina |
US4797139A (en) * | 1987-08-11 | 1989-01-10 | Norton Company | Boehmite produced by a seeded hydyothermal process and ceramic bodies produced therefrom |
DE3823895C1 (ja) * | 1988-07-14 | 1989-12-21 | Condea Chemie Gmbh, 2212 Brunsbuettel, De | |
FR2663245B1 (fr) * | 1990-06-13 | 1992-09-18 | Rhone Poulenc Chimie | Composition a base d'alumine pour catalyseur et procede de fabrication. |
US5569325A (en) * | 1991-04-22 | 1996-10-29 | Condea Vista Company | Process for growing crystals |
DE69211641T2 (de) * | 1991-04-26 | 1996-10-10 | Condea Vista Comp | Verfahren zur herstellung von submikronischen aluminateilchen |
FR2676437B1 (fr) * | 1991-05-14 | 1993-09-17 | Rhone Poulenc Chimie | Alumine stabilisee par la silice et son procede de preparation. |
JP3377799B2 (ja) * | 1991-07-26 | 2003-02-17 | 旭硝子株式会社 | 記録用シート |
CA2131796C (en) * | 1992-03-12 | 2004-01-27 | Lewis Bernard Decker Jr. | Preparation of alumina having increased porosity |
US5593654A (en) * | 1992-03-12 | 1997-01-14 | Condea Vista Company | Preparation of stabilized alumina having enhanced resistance to loss of surface area at high temperatures |
JP2887023B2 (ja) * | 1992-03-30 | 1999-04-26 | ワイケイケイ株式会社 | 微細板状ベーマイト粒子及びその製造方法 |
US5237949A (en) * | 1992-05-29 | 1993-08-24 | Shell Offshore Inc. | Floating platform shallow draft hull/deck mating |
FR2697832B1 (fr) * | 1992-11-12 | 1994-12-30 | Rhone Poulenc Chimie | Alumine stabilisée par du lanthane et son procédé de préparation. |
US5837634A (en) * | 1992-11-12 | 1998-11-17 | Condea Vista Company | Process for producing stabilized alumina having enhanced resistance to loss of surface area at high temperatures |
DE4337643C1 (de) * | 1993-11-04 | 1995-08-03 | Rwe Dea Ag | Verfahren zur Herstellung von in Wasser dispergierbaren Tonerdehydraten böhmitischer Struktur und Verwendung derselben |
JP2883299B2 (ja) * | 1994-09-16 | 1999-04-19 | キヤノン株式会社 | 被記録媒体、その製造方法、被記録媒体を用いたインクジェット記録方法 |
JP2887098B2 (ja) * | 1994-10-26 | 1999-04-26 | キヤノン株式会社 | 被記録媒体、その製造方法及び画像形成方法 |
US5759213A (en) * | 1995-04-24 | 1998-06-02 | University Of Florida | Method for controlling the size and morphology of alpha-alumina particles |
JPH0976371A (ja) * | 1995-09-12 | 1997-03-25 | Mitsubishi Electric Corp | 多孔質プラスチック軸受およびその製造方法 |
JPH11246218A (ja) * | 1998-03-04 | 1999-09-14 | Asahi Glass Co Ltd | アルミナゾル、アルミナゾルの製造方法および記録シート |
DE19836821A1 (de) * | 1998-08-14 | 2000-02-24 | Rwe Dea Ag | Böhmitische Tonerden und aus diesen erhältliche phasenreine, hochtemperaturstabile und hochporöse Aluminiumoxide |
JP2000256011A (ja) * | 1999-03-10 | 2000-09-19 | Taimei Chemicals Co Ltd | ベーマイト及びその製造方法 |
US6262132B1 (en) * | 1999-05-21 | 2001-07-17 | Energy International Corporation | Reducing fischer-tropsch catalyst attrition losses in high agitation reaction systems |
EP1491500A2 (en) * | 1999-08-11 | 2004-12-29 | Albemarle Netherlands B.V. | Quasi-crystalline boehmites containing additives |
-
1998
- 1998-08-14 DE DE19836821A patent/DE19836821A1/de not_active Withdrawn
-
1999
- 1999-08-05 JP JP2000564900A patent/JP4238963B2/ja not_active Expired - Lifetime
- 1999-08-05 EP EP10012099.7A patent/EP2258659B1/de not_active Expired - Lifetime
- 1999-08-05 US US09/529,484 patent/US6773690B1/en not_active Expired - Lifetime
- 1999-08-05 WO PCT/DE1999/002464 patent/WO2000009445A2/de active Application Filing
- 1999-08-05 EP EP99952321A patent/EP1025045B1/de not_active Expired - Lifetime
-
2000
- 2000-04-07 ZA ZA200001778A patent/ZA200001778B/xx unknown
-
2004
- 2004-08-06 US US10/913,802 patent/US20050019249A1/en not_active Abandoned
-
2008
- 2008-08-13 US US12/190,799 patent/US8414854B2/en not_active Expired - Fee Related
- 2008-10-08 JP JP2008261743A patent/JP5037471B2/ja not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
ZA200001778B (en) | 2001-01-09 |
JP4238963B2 (ja) | 2009-03-18 |
EP2258659A3 (de) | 2012-09-12 |
JP2009001492A (ja) | 2009-01-08 |
EP1025045A2 (de) | 2000-08-09 |
EP1025045B1 (de) | 2013-02-27 |
US6773690B1 (en) | 2004-08-10 |
US8414854B2 (en) | 2013-04-09 |
WO2000009445A3 (de) | 2000-05-18 |
DE19836821A1 (de) | 2000-02-24 |
WO2000009445A2 (de) | 2000-02-24 |
JP2002522343A (ja) | 2002-07-23 |
US20050019249A1 (en) | 2005-01-27 |
US20080305333A1 (en) | 2008-12-11 |
EP2258659B1 (de) | 2015-10-07 |
EP2258659A2 (de) | 2010-12-08 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5037471B2 (ja) | ベーマイト型結晶アルミナの製造方法とベーマイト型結晶アルミナ | |
JP3016865B2 (ja) | 混合セリウムないしジルコニウム酸化物,並びにこれらの製造方法及び使用方法 | |
Sarkar et al. | Synthesis and characterization of sol–gel derived ZrO2 doped Al2O3 nanopowder | |
Jung et al. | The effects of synthesis and pretreatment conditions on the bulk structure and surface properties of zirconia | |
US5064628A (en) | Novel ceric oxides and preparation thereof | |
JP2655138B2 (ja) | 新規な形態的特徴を有する酸化第二セリウム | |
US6214306B1 (en) | Composition based on zirconium oxide and cerium oxide, preparation method therefor and use thereof | |
DK1719737T3 (en) | PROCEDURE FOR PREPARING A TEMPERATURE-STABLE TiO2 / SiO2 MIXTURE OXIDE AND ITS USE AS A CATALYST CARRIER | |
EP1618069B1 (en) | Nanoporous ultrafine alpha-alumina powders and sol-gel process of preparing the same | |
US6555496B1 (en) | Micro-crystalline boehmites containing additives | |
JP4406359B2 (ja) | 酸化ジルコニウムと、セリウム、ランタン及び他の希土類元素の酸化物とを用いた組成物、その調製方法、並びに触媒としての使用 | |
Dell’Agli et al. | The effect of mineralizers on the crystallization of zirconia gel under hydrothermal conditions | |
Wang et al. | Phase transformation and nanocrystallite growth behavior of 2 mol% yttria-partially stabilized zirconia (2Y-PSZ) powders | |
Mondal et al. | Monolithic t‐ZrO2 Nanopowder through a ZrO (OH) 2· xH2O Polymer Precursor | |
JP4191044B2 (ja) | ジルコニウム及びチタンをベースとする酸化物を調製する方法、この方法により得られる酸化物、及びこの酸化物の触媒としての使用 | |
JPH0664918A (ja) | アルミナ水和物およびアルミナゾルの製造方法 | |
CN102924092A (zh) | 一种高分散片状氧化铝的低成本、无污染制备方法 | |
Manriquez et al. | X-ray diffraction, and Raman scattering study of nanostructured ZrO2-TiO2 oxides prepared by sol–gel | |
US20160236176A1 (en) | Method of making highly porous, stable aluminum oxides doped with silicon | |
Hernandez et al. | The role of the synthesis route to obtain densified TiO2-doped alumina ceramics | |
Caracoche et al. | Nanostructural study of sol-gel-derived zirconium oxides | |
TW200932669A (en) | Purified powder of nanometric particles | |
JP2000256011A (ja) | ベーマイト及びその製造方法 | |
JP2009067666A (ja) | セリア−ジルコニア固溶体ゾルおよびその製造方法 | |
EP0808800A2 (en) | Praseodymium-zirconium-oxides for catalyst and washcoat |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20081104 |
|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20081104 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20111122 |
|
A601 | Written request for extension of time |
Free format text: JAPANESE INTERMEDIATE CODE: A601 Effective date: 20120220 |
|
A602 | Written permission of extension of time |
Free format text: JAPANESE INTERMEDIATE CODE: A602 Effective date: 20120227 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20120521 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20120612 |
|
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20120704 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20150713 Year of fee payment: 3 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 5037471 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
LAPS | Cancellation because of no payment of annual fees |