WO2015189203A1 - Gel haute dispersibilite et son procede de preparation - Google Patents

Gel haute dispersibilite et son procede de preparation Download PDF

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Publication number
WO2015189203A1
WO2015189203A1 PCT/EP2015/062829 EP2015062829W WO2015189203A1 WO 2015189203 A1 WO2015189203 A1 WO 2015189203A1 EP 2015062829 W EP2015062829 W EP 2015062829W WO 2015189203 A1 WO2015189203 A1 WO 2015189203A1
Authority
WO
WIPO (PCT)
Prior art keywords
precipitation
aluminum
alumina
basic
acidic
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.)
Ceased
Application number
PCT/EP2015/062829
Other languages
English (en)
French (fr)
Inventor
Malika Boualleg
Céline BOUVRY
Patrick Euzen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
IFP Energies Nouvelles IFPEN
Original Assignee
IFP Energies Nouvelles IFPEN
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by IFP Energies Nouvelles IFPEN filed Critical IFP Energies Nouvelles IFPEN
Priority to US15/318,582 priority Critical patent/US20170121181A1/en
Priority to DK15727663.5T priority patent/DK3154908T3/da
Priority to BR112016028715-0A priority patent/BR112016028715B1/pt
Priority to RU2017100950A priority patent/RU2694751C2/ru
Priority to CN201580031667.0A priority patent/CN106687412B/zh
Priority to EP15727663.5A priority patent/EP3154908B1/fr
Priority to JP2016572481A priority patent/JP2017521343A/ja
Publication of WO2015189203A1 publication Critical patent/WO2015189203A1/fr
Anticipated expiration legal-status Critical
Priority to US16/045,118 priority patent/US10858262B2/en
Ceased legal-status Critical Current

Links

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
    • C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
    • 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
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0052—Preparation of gels
    • B01J13/0056—Preparation of gels containing inorganic material and water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
    • C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
    • 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
    • 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
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • 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
    • C01P2006/80—Compositional purity

Definitions

  • step a) operating at a temperature between 10 and 50 ° C, and for a duration of between 2 minutes and 30 minutes,
  • An advantage of the invention is to provide a new process for the preparation by precipitation of an alumina gel making it possible to obtain at least 40% by weight of alumina in Al 2 0 3 equivalent relative to the total amount of alumina. alumina formed at the end of the precipitation step or steps, from the first precipitation step, the amount of alumina formed at the end of the first precipitation step can even reach 100%, a second precipitation step n not being necessary in this case.
  • the dispersibility is measured by dispersing 10% of boehmite or alumina gel in a suspension of water also containing 10% of nitric acid relative to the mass of boehmite. Then, the suspension is centrifuged at 3600G rpm for 10 min. The collected sediments are dried at 100 ° C overnight and weighed.
  • X-ray diffraction on alumina or boehmite gels was performed using the conventional powder method using a diffractometer.
  • said step a) is carried out in the absence of organic additive.
  • the preparation process according to the present invention comprising at least one alumina precipitation step making it possible to obtain at least 40% by weight of alumina with respect to the total amount of alumina formed in Al 2 O 3 equivalent to Al 2 O 3. the result of the process, and at least one final heat treatment stage of the suspension obtained thus makes it possible to obtain the alumina gel according to the invention having a dispersibility index greater than 70% and a crystallite size of between 2 and 35 nm.
  • the present invention also relates to age! of alumina obtainable by the preparation process according to the invention.
  • Example 1 (comparajifl)
  • Example 2 not in accordance with the invention highlights the importance of operating during the precipitation step at low temperature and in particular during the first precipitation step.
  • a precipitation step carried out at a temperature of 70 ° C., outside the ranges claimed does not make it possible to obtain a dispersible gel.
  • Table 3 characteristics of the alumina gel obtained according to Example 3.
  • Example 4 (according to the invention): The synthesis of an alumina gel is carried out according to a preparation method according to the invention in a reactor of 71 and a final suspension of 51 in 3 steps, two precipitation steps followed a ripening stage.
  • Dispersibility index Ta 10% (%) 100

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Nanotechnology (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
PCT/EP2015/062829 2014-06-13 2015-06-09 Gel haute dispersibilite et son procede de preparation Ceased WO2015189203A1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
US15/318,582 US20170121181A1 (en) 2014-06-13 2015-06-09 Gel with high dispersibility and method for preparing same
DK15727663.5T DK3154908T3 (da) 2014-06-13 2015-06-09 Fremgangsmåde til fremstilling af gel med høj dispergerbarhed
BR112016028715-0A BR112016028715B1 (pt) 2014-06-13 2015-06-09 Processo de preparação de um gel de alumina com índice de dispersibilidade elevado
RU2017100950A RU2694751C2 (ru) 2014-06-13 2015-06-09 Гель с высокой степенью диспергируемости и способ его получения
CN201580031667.0A CN106687412B (zh) 2014-06-13 2015-06-09 具有高分散性的凝胶及其制备方法
EP15727663.5A EP3154908B1 (fr) 2014-06-13 2015-06-09 Procede de preparation de gel haute dispersibilite
JP2016572481A JP2017521343A (ja) 2014-06-13 2015-06-09 高分散性ゲルおよびその調製方法
US16/045,118 US10858262B2 (en) 2014-06-13 2018-07-25 Gel with high dispersibility and method for preparing same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1455421A FR3022235B1 (fr) 2014-06-13 2014-06-13 Gel haute dispersibilite et son procede de preparation
FR1455421 2014-06-13

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US15/318,582 A-371-Of-International US20170121181A1 (en) 2014-06-13 2015-06-09 Gel with high dispersibility and method for preparing same
US16/045,118 Division US10858262B2 (en) 2014-06-13 2018-07-25 Gel with high dispersibility and method for preparing same

Publications (1)

Publication Number Publication Date
WO2015189203A1 true WO2015189203A1 (fr) 2015-12-17

Family

ID=51688185

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2015/062829 Ceased WO2015189203A1 (fr) 2014-06-13 2015-06-09 Gel haute dispersibilite et son procede de preparation

Country Status (9)

Country Link
US (2) US20170121181A1 (https=)
EP (1) EP3154908B1 (https=)
JP (2) JP2017521343A (https=)
CN (1) CN106687412B (https=)
BR (1) BR112016028715B1 (https=)
DK (1) DK3154908T3 (https=)
FR (1) FR3022235B1 (https=)
RU (1) RU2694751C2 (https=)
WO (1) WO2015189203A1 (https=)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017129497A1 (fr) * 2016-01-29 2017-08-03 IFP Energies Nouvelles Procede de preparation d'un gel d'alumine presentant une haute dispersibilite et une taille de cristallite specifique

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111320194B (zh) * 2020-04-24 2022-08-19 山东中科天泽净水材料有限公司 一种铝胶及聚合氯化铝的制备方法
FR3112540A1 (fr) 2020-07-20 2022-01-21 IFP Energies Nouvelles Procédé de préparation d'un gel d'alumine haute dispersibilité
FR3112496A1 (fr) 2020-07-20 2022-01-21 IFP Energies Nouvelles Procédé de lavage d'une suspension d'oxydes métalliques

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2123804A (en) * 1982-06-23 1984-02-08 Grace W R & Co Dispersible alpha-aluminate monohydrate
EP0147167A2 (en) * 1983-12-22 1985-07-03 Aluminum Company Of America Continuous process for neutralization of aluminate solution to form gels and appartatus therefor
US6713428B1 (en) * 1998-07-06 2004-03-30 Instuit Francais Du Petrole Dispersible aluminium hydrate, method for preparing same and use for preparing catalysts
US7790652B2 (en) * 2003-09-17 2010-09-07 Shell Oil Company Process and catalyst for the hydroconversion of a heavy hydrocarbon feedstock

Family Cites Families (12)

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GB1603461A (en) * 1977-03-25 1981-11-25 Grace W R & Co Process for preparing crystalline allumina
SU1787941A1 (ru) * 1991-03-07 1993-01-15 Inst Chimii Tech Redkik Способ получения гидроксида алюминия
CN1120129C (zh) * 1996-03-05 2003-09-03 佐藤护郎 氧化铝溶胶的制备方法
US6312619B1 (en) * 1999-06-10 2001-11-06 Condea Vista Company Method for producing water-dispersible alpha-alumina monohydrate
JP4054183B2 (ja) * 2001-09-27 2008-02-27 触媒化成工業株式会社 アルミナ製造装置
US7422730B2 (en) * 2003-04-02 2008-09-09 Saint-Gobain Ceramics & Plastics, Inc. Nanoporous ultrafine α-alumina powders and sol-gel process of preparing same
TW200846286A (en) * 2007-05-22 2008-12-01 Grace W R & Co Alumina particles and methods of making the same
RU2409519C1 (ru) * 2009-07-08 2011-01-20 Закрытое акционерное общество "Центр инновационных керамических нанотехнологий Нанокомпозит" Способ получения нанопорошка альфа-оксида алюминия с узким распределением частиц по размерам
JP5610842B2 (ja) * 2010-05-20 2014-10-22 日揮触媒化成株式会社 アルミナ水和物微粒子、アルミナ水和物微粒子の製造方法、結合剤およびセラミック成型体
CN101928029A (zh) * 2010-09-08 2010-12-29 苏州创元投资发展(集团)有限公司 一种氧化铝溶胶的制备方法
CN102180497B (zh) * 2011-03-15 2012-09-26 宣城晶瑞新材料有限公司 高分散性纳米氧化铝的非水溶胶凝胶制备方法
CN103288114A (zh) * 2013-05-29 2013-09-11 如皋市乐恒化工有限公司 一种高纯度氧化铝的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2123804A (en) * 1982-06-23 1984-02-08 Grace W R & Co Dispersible alpha-aluminate monohydrate
EP0147167A2 (en) * 1983-12-22 1985-07-03 Aluminum Company Of America Continuous process for neutralization of aluminate solution to form gels and appartatus therefor
US6713428B1 (en) * 1998-07-06 2004-03-30 Instuit Francais Du Petrole Dispersible aluminium hydrate, method for preparing same and use for preparing catalysts
US7790652B2 (en) * 2003-09-17 2010-09-07 Shell Oil Company Process and catalyst for the hydroconversion of a heavy hydrocarbon feedstock

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017129497A1 (fr) * 2016-01-29 2017-08-03 IFP Energies Nouvelles Procede de preparation d'un gel d'alumine presentant une haute dispersibilite et une taille de cristallite specifique
FR3047238A1 (fr) * 2016-01-29 2017-08-04 Ifp Energies Now Procede de preparation d'un gel d'alumine presentant une haute dispersibilite et une taille de cristallite specifique
CN108495817A (zh) * 2016-01-29 2018-09-04 Ifp 新能源公司 生产具有高分散度和特定晶粒尺寸的氧化铝凝胶的方法
US20190055135A1 (en) * 2016-01-29 2019-02-21 IFP Energies Nouvelles Method for producing an alumina gel having a high dispersibility and a specific crystallite size
JP2019507087A (ja) * 2016-01-29 2019-03-14 イエフペ エネルジ ヌヴェルＩｆｐ Ｅｎｅｒｇｉｅｓ Ｎｏｕｖｅｌｌｅｓ 高い分散性および特定の微結晶サイズを有するアルミナゲルの製造方法
RU2731569C2 (ru) * 2016-01-29 2020-09-04 Ифп Энержи Нувелль Способ получения геля оксида алюминия, имеющего высокую диспергируемость и определенный размер кристаллитов
CN108495817B (zh) * 2016-01-29 2021-02-02 Ifp 新能源公司 生产具有高分散度和特定晶粒尺寸的氧化铝凝胶的方法
US11577964B2 (en) 2016-01-29 2023-02-14 IFP Energies Nouvelles Method for producing an alumina gel having a high dispersibility and a specific crystallite size

Also Published As

Publication number Publication date
CN106687412A (zh) 2017-05-17
DK3154908T3 (da) 2020-04-20
FR3022235A1 (fr) 2015-12-18
JP2017521343A (ja) 2017-08-03
JP2020073429A (ja) 2020-05-14
BR112016028715B1 (pt) 2022-09-06
US20180334391A1 (en) 2018-11-22
EP3154908B1 (fr) 2020-01-08
US20170121181A1 (en) 2017-05-04
CN106687412B (zh) 2018-03-13
RU2694751C2 (ru) 2019-07-16
FR3022235B1 (fr) 2021-05-07
JP6789360B2 (ja) 2020-11-25
RU2017100950A (ru) 2018-07-13
US10858262B2 (en) 2020-12-08
RU2017100950A3 (https=) 2019-02-28
EP3154908A1 (fr) 2017-04-19
BR112016028715A2 (pt) 2017-08-22

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