JP2008534416A - 高表面積を有するベーマイトおよびγ−アルミナの製造方法 - Google Patents
高表面積を有するベーマイトおよびγ−アルミナの製造方法 Download PDFInfo
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- 229910001593 boehmite Inorganic materials 0.000 title claims abstract description 108
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims abstract description 108
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 42
- -1 aluminum alkoxide Chemical class 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002904 solvent Substances 0.000 claims abstract description 26
- 238000001354 calcination Methods 0.000 claims abstract description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 48
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 16
- 150000001735 carboxylic acids Chemical class 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 11
- 239000007810 chemical reaction solvent Substances 0.000 abstract description 9
- 239000003463 adsorbent Substances 0.000 abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 6
- 238000004587 chromatography analysis Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 239000002245 particle Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 18
- 239000011148 porous material Substances 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 239000013078 crystal Substances 0.000 description 14
- 238000006460 hydrolysis reaction Methods 0.000 description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 11
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 9
- 238000005259 measurement Methods 0.000 description 7
- 230000007062 hydrolysis Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000001935 peptisation Methods 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910001679 gibbsite Inorganic materials 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003509 tertiary alcohols Chemical class 0.000 description 1
- DAOVYDBYKGXFOB-UHFFFAOYSA-N tris(2-methylpropoxy)alumane Chemical compound [Al+3].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] DAOVYDBYKGXFOB-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- A—HUMAN NECESSITIES
- A63—SPORTS; GAMES; AMUSEMENTS
- A63H—TOYS, e.g. TOPS, DOLLS, HOOPS OR BUILDING BLOCKS
- A63H3/00—Dolls
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- 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
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
- C01F7/36—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts from organic aluminium salts
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- A63—SPORTS; GAMES; AMUSEMENTS
- A63H—TOYS, e.g. TOPS, DOLLS, HOOPS OR BUILDING BLOCKS
- A63H9/00—Special methods or compositions for the manufacture of dolls, toy animals, toy figures, or parts thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/282—Porous sorbents
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- 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
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
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- B44C—PRODUCING DECORATIVE EFFECTS; MOSAICS; TARSIA WORK; PAPERHANGING
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Abstract
Description
アルコール溶媒に80〜130℃の温度でアルミニウムアルコキシドを溶解させてアルミニウムアルコキシド溶液を製造し、
前記アルミニウムアルコキシド溶液に、前記アルミニウムアルコキシド1モルに対してpKa値3.5〜5を有する有機カルボン酸0.01〜1モルと、水2〜12モルを添加した後、80〜130℃で1〜48時間加熱してベーマイトゾルを製造し、
前記ベーマイトゾルを蒸留および乾燥してアルコール溶媒を分離/回収し、粉末状のベーマイトを製造する、ことからなる高表面積を有するベーマイトの製造方法である。
。本発明は粒子サイズが3〜30nmであり、従来の方法で製造されたものに比べて比表面積が高いベーマイト、およびベーマイトをか焼して得られるγ−アルミナの製造方法である。
アルミニウムイソプロポキシド(10g)を2−プロパノール(73.5g)に添加して攪拌し、前記2−プロパノールの沸点である82.4℃まで加熱して還流させた。この時、アルミニウムイソプロポキシド混合液は澄んだスラリーとなった。前記スラリー溶液に、酢酸(0.29g)と水(5.26g)を添加して加水分解反応を行い、非晶質の水酸化アルミニウムが生成された。前記生成された水酸化アルミニウムを20時間還流することによって、解膠および結晶化させた。ここで、アルミニウムイソプロポキシド:2−プロパノール:酢酸:水のモル比は、1:25:0.1:6であった。前記ベーマイトゾルは70℃の温度で12時間真空乾燥してベーマイト粉末を得て、上記工程中に液体窒素トラップを設置して2−プロパノールを回収した。
酢酸と水を各々1.47gと5.29g使用し、アルミニウムイソプロポキシド:2−プロパノール:酢酸:水のモル比を1:25:0.5:6モルとしたこと以外は、前記実施例1と同じにして、ベーマイトとγ−アルミナを製造した。
酢酸と水を各々0.1gと5.29g使用し、アルミニウムイソプロポキシド:2−プロパノール:酢酸:水のモル比を1:25:0.035:6としたこと以外は、前記実施例1と同じにして、ベーマイトとγ−アルミナを製造した。
酢酸と水を各々0.1gと2.65g使用し、アルミニウムイソプロポキシド:2−プロパノール:酢酸:水のモル比を1:25:0.035:3としたこと以外は、前記実施例1と同じにして、ベーマイトとγ−アルミナを製造した。
2−プロパノールを2倍量使用し、アルミニウムイソプロポキシド:2−プロパノール:酢酸:水のモル比を、1:50:0.1:6としたこと以外は、前記実施例1と同じにして、ベーマイトとγ−アルミナを製造した。
2−プロパノールの代りに水44.0gを使用し、酢酸の代りに60%硝酸(0.51g)を使用し、アルミニウムイソプロポキシドを、水と硝酸が混合された溶液に添加して加熱し、還流反応を行ったこと以外は、前記実施例1と同じにして、ベーマイトとγ−アルミナを製造した。この時、アルミニウムイソプロポキシド:硝酸:水のモル比は、1:0.1:50であった。
酢酸を使用しなかったこと以外は、前記実施例1と同じにして、ベーマイトとγ−アルミナを製造した。この時、アルミニウムイソプロポキシド:2−プロパノール:水のモル比は、1:25:6であった。
Claims (5)
- (a)アルコール溶媒に80〜130℃の温度でアルミニウムアルコキシドを溶解させてアルミニウムアルコキシド溶液を製造し、
(b)前記アルミニウムアルコキシド溶液に、前記アルミニウムアルコキシド1モルに対してpKa値3.5〜5を有する有機カルボン酸0.01〜1モルと、水2〜12モルを添加し、前記混合液を80〜130℃で1〜48時間加熱してベーマイトゾルを製造し、
(c)前記ベーマイトゾルを蒸留および乾燥してアルコール溶媒を分離/回収し、粉末状のベーマイトを製造する、
高表面積を有するベーマイトの製造方法。 - (a)アルコール溶媒に80〜130℃の温度でアルミニウムアルコキシドを溶解させてアルミニウムアルコキシド溶液を製造し、
(b)前記アルミニウムアルコキシド溶液に、前記アルミニウムアルコキシド1モルに対してpKa値3.5〜5を有する有機カルボン酸0.01〜1モルと、水2〜12モルを添加した後、前記混合液を80〜130℃で1〜48時間加熱してベーマイトゾルを製造し、
(c)前記ベーマイトゾルを蒸留および乾燥してアルコール溶媒を分離/回収し、粉末状のベーマイトを製造し、
(d)前記ベーマイトを400〜700℃の温度で1〜96時間か焼する、
高表面積を有するγ−アルミナの製造方法。 - 前記アルコールは1〜4の炭素原子を有するアルコールであって、メタノール、エタノール、1−プロパノール、2−プロパノール、1−ブタノール、2−ブタノールおよび2−メチルプロパノールの中から選択されることを特徴とする、請求項1または2記載の製造方法。
- 前記アルコールはアルミニウムアルコキシド1モルに対して5〜200モルで使用することを特徴とする、請求項1または2記載の製造方法。
- 前記有機カルボン酸(organic carboxylic acid)は蟻酸、酢酸およびプリピオン酸の中から選択されることを特徴とする、請求項1または2記載の製造方法。
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KR10-2005-0024251 | 2005-03-23 | ||
PCT/KR2006/000291 WO2006101305A1 (en) | 2005-03-23 | 2006-01-25 | Method of preparing boehmite and gamma-alumina with high surface area |
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JP2010505724A (ja) * | 2006-10-06 | 2010-02-25 | ダブリュー・アール・グレイス・アンド・カンパニー−コネチカット | 硫黄に対する耐性を有するアルミナ触媒支持体 |
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JP2008031010A (ja) * | 2006-07-31 | 2008-02-14 | Kawaken Fine Chem Co Ltd | アルミナ有機溶媒分散液の製造方法 |
JP2010505725A (ja) * | 2006-10-06 | 2010-02-25 | ダブリュー・アール・グレイス・アンド・カンパニー−コネチカット | 硫黄に対する耐性を有するアルミナ触媒支持体 |
JP2010505724A (ja) * | 2006-10-06 | 2010-02-25 | ダブリュー・アール・グレイス・アンド・カンパニー−コネチカット | 硫黄に対する耐性を有するアルミナ触媒支持体 |
JP2010254553A (ja) * | 2009-03-31 | 2010-11-11 | Canon Inc | 酸化アルミニウム前駆体ゾル及び光学用部材の製造方法 |
JP2013023419A (ja) * | 2011-07-22 | 2013-02-04 | Nippon Shokubai Co Ltd | ベーマイトナノロッドおよびその製造方法、アルミナナノロッドおよびその製造方法、並びに、CuAlO2膜およびその製造方法 |
WO2021075497A1 (ja) | 2019-10-18 | 2021-04-22 | 住友化学株式会社 | ベーマイトおよびその製造方法 |
KR20220084051A (ko) | 2019-10-18 | 2022-06-21 | 스미또모 가가꾸 가부시끼가이샤 | 베마이트 및 이의 제조 방법 |
JP7393912B2 (ja) | 2019-10-18 | 2023-12-07 | 住友化学株式会社 | ベーマイトおよびその製造方法 |
Also Published As
Publication number | Publication date |
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CN101426729A (zh) | 2009-05-06 |
HK1132983A1 (en) | 2010-03-12 |
KR100579207B1 (ko) | 2006-05-12 |
CN101426729B (zh) | 2012-09-05 |
JP4814936B2 (ja) | 2011-11-16 |
EP1888463A1 (en) | 2008-02-20 |
WO2006101305A1 (en) | 2006-09-28 |
US20090104108A1 (en) | 2009-04-23 |
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