WO2013034632A3 - Process for the continuous synthesis of metal oxide nanoparticles by hydrothermal reaction in a supercritical medium - Google Patents

Process for the continuous synthesis of metal oxide nanoparticles by hydrothermal reaction in a supercritical medium Download PDF

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Publication number
WO2013034632A3
WO2013034632A3 PCT/EP2012/067391 EP2012067391W WO2013034632A3 WO 2013034632 A3 WO2013034632 A3 WO 2013034632A3 EP 2012067391 W EP2012067391 W EP 2012067391W WO 2013034632 A3 WO2013034632 A3 WO 2013034632A3
Authority
WO
WIPO (PCT)
Prior art keywords
internal tube
water
hydrothermal reaction
reactor
aqueous
Prior art date
Application number
PCT/EP2012/067391
Other languages
French (fr)
Other versions
WO2013034632A2 (en
Inventor
Jean-Christophe Ruiz
Christophe Joussot-Dubien
Hubert-Alexandre Turc
Frédéric CHARTON
Anne ROUBAUD
Original Assignee
Commissariat à l'énergie atomique et aux énergies alternatives
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 Commissariat à l'énergie atomique et aux énergies alternatives filed Critical Commissariat à l'énergie atomique et aux énergies alternatives
Publication of WO2013034632A2 publication Critical patent/WO2013034632A2/en
Publication of WO2013034632A3 publication Critical patent/WO2013034632A3/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/06—Ferric oxide (Fe2O3)
    • 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
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/008—Processes carried out under supercritical conditions
    • 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
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
    • C01B13/366—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions by hydrothermal processing
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/006—Alkaline earth titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0036—Mixed oxides or hydroxides containing one alkaline earth metal, magnesium or lead
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/04—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Cobaltates
    • C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/04—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Abstract

The invention relates to a process for the continuous synthesis of nanometre-sized inorganic particles of metal oxides by hydrothermal reaction in a supercritical medium. It comprises: a) introduction of pressurized water into an annular zone and through a first end of a reactor of essentially tubular shape comprising an external wall and an internal tube; b) heating of the water in the annular zone; c) introduction of the heated and pressurized water into the internal tube and simultaneous introduction of an aqueous and/or alcoholic solution of metallic or organometallic precursors into said internal tube at the second end of the reactor; d) mixing of the water and of the aqueous and/or alcoholic solution in a first part of the internal tube, followed by a cooling of the mixture obtained in a second part of the internal tube; and e) isobaric discharge of the cooled mixture from the reactor using the internal tube. The water and the aqueous and/or alcoholic solution travels continuously or almost continuously through the internal tube.
PCT/EP2012/067391 2011-09-09 2012-09-06 Process for the continuous synthesis of metal oxide nanoparticles by hydrothermal reaction in a supercritical medium WO2013034632A2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1158037A FR2979842B1 (en) 2011-09-09 2011-09-09 PROCESS FOR THE CONTINUOUS SYNTHESIS OF METAL OXIDE NANOPARTICLES BY HYDROTHERMAL REACTION IN A SUPERCRITICAL ENVIRONMENT
FR1158037 2011-09-09

Publications (2)

Publication Number Publication Date
WO2013034632A2 WO2013034632A2 (en) 2013-03-14
WO2013034632A3 true WO2013034632A3 (en) 2013-08-01

Family

ID=46799257

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2012/067391 WO2013034632A2 (en) 2011-09-09 2012-09-06 Process for the continuous synthesis of metal oxide nanoparticles by hydrothermal reaction in a supercritical medium

Country Status (2)

Country Link
FR (1) FR2979842B1 (en)
WO (1) WO2013034632A2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7013040B2 (en) 2013-11-19 2022-01-31 プロメシアン パーティクルズ リミテッド Mixing reactor and method

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3082439B1 (en) * 2018-06-14 2021-04-23 Commissariat Energie Atomique REACTOR FOR TREATMENT BY HYDROTHERMAL OXIDATION OF AN ORGANIC MATERIAL IN A REACTIONAL MEDIUM
EP4114559A1 (en) * 2020-03-05 2023-01-11 Kraczek, John Troy Conversion of supercritical water energy into electrical power
CN114797725B (en) * 2022-04-29 2023-06-13 西安交通大学 Internal heating type supercritical water oxidation reactor
FR3137381A1 (en) * 2022-07-04 2024-01-05 Commissariat A L'energie Atomique Et Aux Energies Alternatives Injection device for a salt separator, of the type with a surface scraped by at least one rotor rotating in a heating envelope, Salt separator and associated biomass gasification installation.

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10005681A1 (en) * 2000-02-07 2001-08-16 Atc Dr Mann Process and device for the decontamination of water containing metals and / or radioactive substances
US20070206435A1 (en) * 2004-02-11 2007-09-06 Lester Edward H Counter Current Mixing Reactor
US20080135496A1 (en) * 2000-10-10 2008-06-12 Christophe Joussot-Dubien Device for supercritical water oxidation of materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10005681A1 (en) * 2000-02-07 2001-08-16 Atc Dr Mann Process and device for the decontamination of water containing metals and / or radioactive substances
US20080135496A1 (en) * 2000-10-10 2008-06-12 Christophe Joussot-Dubien Device for supercritical water oxidation of materials
US20070206435A1 (en) * 2004-02-11 2007-09-06 Lester Edward H Counter Current Mixing Reactor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7013040B2 (en) 2013-11-19 2022-01-31 プロメシアン パーティクルズ リミテッド Mixing reactor and method

Also Published As

Publication number Publication date
FR2979842B1 (en) 2013-10-04
FR2979842A1 (en) 2013-03-15
WO2013034632A2 (en) 2013-03-14

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