WO2002092703A1 - Fragmentation d'oxydes et d'hydroxydes de metal enrobes - Google Patents

Fragmentation d'oxydes et d'hydroxydes de metal enrobes Download PDF

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Publication number
WO2002092703A1
WO2002092703A1 PCT/GB2002/002312 GB0202312W WO02092703A1 WO 2002092703 A1 WO2002092703 A1 WO 2002092703A1 GB 0202312 W GB0202312 W GB 0202312W WO 02092703 A1 WO02092703 A1 WO 02092703A1
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Prior art keywords
process according
particles
oxide
comminution
carried out
Prior art date
Application number
PCT/GB2002/002312
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English (en)
Inventor
Christopher Harris
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Oxonica Limited
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Publication date
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Publication of WO2002092703A1 publication Critical patent/WO2002092703A1/fr

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    • 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
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/10—Liquid carbonaceous fuels containing additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L10/00—Use of additives to fuels or fires for particular purposes
    • C10L10/06—Use of additives to fuels or fires for particular purposes for facilitating soot removal
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • 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
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • 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
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/10—Liquid carbonaceous fuels containing additives
    • C10L1/12—Inorganic compounds
    • C10L1/1233—Inorganic compounds oxygen containing compounds, e.g. oxides, hydroxides, acids and salts thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/10—Liquid carbonaceous fuels containing additives
    • C10L1/14—Organic compounds
    • C10L1/16—Hydrocarbons
    • C10L1/1608—Well defined compounds, e.g. hexane, benzene
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/10—Liquid carbonaceous fuels containing additives
    • C10L1/14—Organic compounds
    • C10L1/16—Hydrocarbons
    • C10L1/1616—Hydrocarbons fractions, e.g. lubricants, solvents, naphta, bitumen, tars, terpentine
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/10—Liquid carbonaceous fuels containing additives
    • C10L1/14—Organic compounds
    • C10L1/18—Organic compounds containing oxygen
    • C10L1/188—Carboxylic acids; metal salts thereof
    • C10L1/1881—Carboxylic acids; metal salts thereof carboxylic group attached to an aliphatic carbon atom
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/10—Liquid carbonaceous fuels containing additives
    • C10L1/14—Organic compounds
    • C10L1/18—Organic compounds containing oxygen
    • C10L1/188—Carboxylic acids; metal salts thereof
    • C10L1/1881—Carboxylic acids; metal salts thereof carboxylic group attached to an aliphatic carbon atom
    • C10L1/1883—Carboxylic acids; metal salts thereof carboxylic group attached to an aliphatic carbon atom polycarboxylic acid

Definitions

  • This invention relates to the comminution of coated metal oxides and hydroxides.
  • a process for preparing coated particles of a metal or metalloid oxide or hydroxide which comprises comminuting the oxide or hydroxide in an organic solvent in the presence of a coating agent which is an organic acid, anhydride or ester or a Lewis base. It has been found that, in this way which involves coating in situ, it is possible to significantly improve the coating of the oxide or hydroxide. Further, the resulting product can, in many instances, be used directly without any intermediate step. Thus in some coating procedures it is necessary to dry the coated particles before dispersing them in a hydrocarbon solvent. In accordance with the present invention this is not necessary although it is possible if desired.
  • a metal or metalloid oxide or hydroxide may be an individual metal or metalloid oxide or hydroxide or a mixture of two or more metal and/or metalloid oxides and/or hydroxides, and may include further metal atoms as dopant.
  • the process of the present invention is applicable to a wide range of oxides and hydroxides but it has particular application to cerium oxide.
  • Cerium oxide acts as a catalyst in automotive exhaust systems. Cerium oxide releases oxygen and is therefore capable of regulating the oxygen partial pressure in the exhaust system. With the engine working under lean conditions, cerium oxide removes excess oxygen from the exhaust gas and catalysed by, for example, platinum, NO x is reduced to nitrogen. During rich cycles, cerium oxide releases oxygen to oxidise carbon monoxide to carbon dioxide. There is, therefore, a need to make a cerium oxide readily available for catalyst systems and this can be achieved most easily by incorporating the cerium oxide into the fuel, i.e. as a fuel additive. For this purpose, the cerium oxide needs to be dispersible or soluble in the fuel. In accordance with the process of the present invention, one can obtain coated cerium oxide particles dispersed or soluble in the fuel or another hydrocarbon compatible with the fuel.
  • the present invention is applicable to other rare earth oxides and hydroxides and indeed other metal oxides and hydroxides including metals of group II of the Periodic table such as magnesium, calcium, strontium and barium, aluminium, zirconium e.g. ZrO 2 , titanium e.g. TiO 2 , nickel e.g. NiO, and iron as Fe 2 O 3 and Fe 3 Q and other transition metals as well as actinide metal oxides as well as metalloids such as silicon.
  • Particles of mixed oxides and hydroxides such as a mixture of cerium oxide and zirconium oxide can also be coated in accordance with the present invention.
  • complex materials include Zn 2 SiO 4 :Mn, YNO 4 :Dy, Y 2 O 3 :Eu, Gd 2 O 3 :Tb and ZnO:Zn.
  • the oxides and hydroxides and mixed oxides and hydroxides used in the present invention may be produced by a variety of different routes including plasma vapour synthesis, combustion synthesis, flame pyrolysis and colloid chemistry.
  • the present invention is particularly applicable to nanometre sized particles.
  • the particles which are subjected to the process should have as large a surface area as possible and preferably the particles have a surface area, before coating, of at least 10 m 2 /g and preferably a surface area of at least 50 or 75 m 2 /g, for example 80-150 m 2 /g. It is believed that the surface chemistry of the particles also has an effect on the ability to coat the particles. Thus the presence of hydroxide groups on the surface is believed to assist the coating process.
  • the resulting particles generally have a size not exceeding 1 micron and especially not exceeding 250 n , for example 100 to 150 nm, such as 120-130 nm.
  • cerium oxide particles which can be coated include those obtainable from Nanophase, typically with a primary particle size of about 180 nm (although agglomerates are also generally present such that, typically, about 75% of the particles are below 1 micron), Rhodia and Meldform.
  • the coating agent is an organic acid, anhydride or ester or a Lewis base. It will normally be soluble in the organic solvent employed. Of course the coating agent should not react chemically with the particles although there may be some binding at the interface with the particle surface.
  • the coating agent is preferably an organic carboxylic acid or an anhydride, typically one possessing at least 8 carbon atoms, for example . 10 to 25 carbon atoms, especially 12 to 18 carbon atoms such as stearic acid. It will be appreciated that the carbon chain can be saturated or unsaturated, for example ethylenically unsaturated as in oleic acid. Similar comments apply to the anhydrides which can be used.
  • a preferred anhydride is dodecylsuccinic anhydride (DDSA).
  • organic acids, anhydrides and esters which can be used in the process of the present invention include those derived from phosphoric acid and sulphonic acid.
  • the esters are typically aliphatic esters, for example alkyl esters where both the acid and ester parts have 4 to 18 carbon atoms.
  • Other coating or capping agents which can be used include Lewis bases which possess an aliphatic chain of at least 8 carbon atoms including mercapto compounds, phosphines, phosphine oxides and amines as well as long chain ethers, diols, esters and aldehydes.
  • Polymeric materials including dendrimers can also be used provided that they possess a hydrophobic chain of at least 8 carbon atoms and one or more Lewis base groups, as well as mixtures of two or more such acids and/or Lewis bases.
  • Typical polar Lewis bases include trialkylphosphine oxides P(R 3 ) 3 O, especially trioctylphosphine oxide (TOPO), trialkylphosphines, P(R 3 ) 3 , amines N(R 3 ) 2 , thiocompounds S(R 3 ) 2 and carboxylic acids or esters R 3 COOR 4 and mixtures thereof, wherein each R 3 , which may be identical or different, is selected from C 7A alkyl groups, C 2-24 alkenyl groups, alkoxy groups of formula -O(C 1-2 alkyl), aryl groups and heterocyclic groups, with the proviso that at least one group R 3 in each molecule is other than hydrogen; and wherein R 4 is selected from hydrogen and C 1-2 al
  • polar Lewis base a polymer, including dendrimers, containing an electron rich group such as a polymer containing one or more of the moieties P(R 3 ) 3 O, P(R 3 ) 3 , N(R 3 ) 2 , S(R 3 ) 2 or R 3 COOR 4 wherein R 3 and R 4 are as defined above; or a mixture of Lewis bases such as a mixture of two or more of the compounds or polymers mentioned above.
  • a C 1-4 alkyl group is an alkyl group as defined above which contains from 1 to 4 carbon atoms.
  • C 1-4 alkyl groups include methyl, ethyl, i-propyl, n-propyl, n-butyl and tert-butyl.
  • a C 2-24 alkenyl group is a linear or branched alkenyl group which may be unsubstituted or substituted at any position and which may contain heteroatoms selected from P, N, O and S. Typically, it is unsubstituted or carries one or two substituent. Suitable substituent include halogen, hydroxyl, cyano, -NR 2 , nitro, oxo, -CO 2 R, -SOR and -SO 2 R wherein each R may be identical or different and is selected from hydrogen or C 1 . 4 alkyl.
  • a C M alkenyl group is an alkenyl group as defined above which contains from 2 to 4 carbon atoms.
  • C 2-4 alkenyl groups include ethenyl, propenyl and butenyl.
  • an aryl group is typically a C 6 . 10 aryl group such as phenyl or naphthyl, preferably phenyl.
  • An aryl group may be unsubstituted or substituted at any position, with one or more substituent. Typically, it is unsubstituted or carries one or two substituent.
  • Suitable substituent include C M alkyl, C 1-4 alkenyl, each of which may be substituted by one or more halogens, halogen, hydroxyi, cyano, -NR 2 , nitro, oxo, -CO 2 R, -SOR and -SO 2 R wherein each R may be identical or different and is selected from hydrogen and C 1-4 alkyl.
  • a heterocyclic group is a 5- to 10-membered ring containing one or more heteroatoms selected from N, O and S. Typical examples include pyridyl, pyrazinyl, pyrimidinyl, pyridazinyl, furanyl, thienyl, pyrazolidinyl, pyrrolyl and pyrazolyl groups.
  • a heterocyclic group may be substituted or unsubstituted at any position, with one or more substituent. Typically, a heterocyclic group is unsubstituted or substituted by one or two substituent.
  • Suitable substituent include C M alkyl, C 1-4 alkenyl, each of which may be substituted by one or more halogens, halogen, hydroxyi, cyano, -NR 2 , nitro, oxo, -CO 2 R, -SOR and -SO 2 R wherein each R may be identical or different and is selected from hydrogen and C w alkyl.
  • halogen is fluorine, chlorine, bromine or iodine, preferably fluorine, chlorine or bromine.
  • the process of the present invention is carried out in an organic solvent.
  • the solvent is non-polar and is also preferably non-hydrophilic. It can be an aliphatic or an aromatic solvent. Typical examples include toluene, xylene, petrol, diesel fuel as well as heavier fuel oils.
  • the organic solvent used should be selected so that it is compatible with the intended end use of the coated particles. The presence of water should be avoided; the use of an anhydride as coating agent helps to eliminate any water present.
  • the particles which are subjected to comminution may desirably be at least partially coated with a coating agent e.g. an organic acid such as stearic acid to assist transfer from an aqueous phase in which they are generally produced to the organic phase in which the comminution is conducted.
  • a coating agent e.g. an organic acid such as stearic acid to assist transfer from an aqueous phase in which they are generally produced to the organic phase in which the comminution is conducted.
  • a coating agent e.g. an organic acid such as stearic acid to assist transfer from an aqueous phase in which they are generally produced to the organic phase in which the comminution is conducted.
  • a coating agent e.g. an organic acid such as stearic acid to assist transfer from an aqueous phase in which they are generally produced to the organic phase in which the comminution is conducted.
  • the particles may be at least partially dispersed before comminution.
  • a dispersant such as a
  • the process of the present invention involves comminuting the particles so as to prevent any agglomerates from forming.
  • the technique employed should be chosen so that the particles are adequately wetted by the agent and a degree of pressure or shear is desirable. Techniques which can be used for this purpose include high-speed stirring, mixing or tumbling, the use of a colloid mill, ultrasonics or ball milling. Ultrasonics, high speed mixing and ball milling are preferred.
  • ball milling can be carried out in a pot where the larger the pot the larger the balls.
  • ceramic balls of 7 to 10 mm diameter are suitable when the milling takes place in a 1.25 litre pot.
  • Ultrasonic treatment can be carried out with a conventional ultrasomcator for, say, 10 minutes to 2 hours, typically 30 minutes to 1 hour.
  • High speed mixing is typically carried out with a rotor/stator mixer at speeds typically from 1000 to 4000, generally 1500 to 2500, rpm.
  • the effectiveness of the process of the present invention can be assessed by studying the stability of the resulting suspension.
  • a turbidity procedure can be used to assess the extent to which the particles remain suspended and therefore un- agglomerated.
  • the agglomerated particles will, of course fall out of suspension and therefore reduce the turbidity of the suspension.
  • the addition of a suspension of cerium oxide particles obtained by the process of the present invention is sufficient to act as a fuel catalyst when present in a concentration of about 4 ppm. This compares with a concentration of in excess of 40 ppm for an existing coated cerium oxide product.
  • the resulting particles can be dried and re-dispersed in another organic solvent or in a polymer.
  • suitable polymers include homo- and co-polymers of ethylene, propylene or styrene, and hydrocarbon-based elastomers such as those containing propylene, butadiene or isoprene.
  • Example 1 A porcelain ball mill pot (1.25 1 capacity) with the corresponding ball charge was charged with 50 g of cerium oxide, Nanotech material from Nanophase (primary particle size about 180 nm with about 76% of the particles being below 1 micron), 200 ml of low sulphur diesel and 5 g of dodecylsuccinic anhydride. The mill was operated for 24 hours
  • a smooth stable slurry was obtained with substantially all the particles being of the primary size (about 180 nm). It is clear, therefore, that the particles have been coated by the anhydride.
  • Example 2 was repeated on a larger scale. 175.6 grams of a cerium oxide slurry
  • Example 4 (4.1%w/w) was placed in a 500ml wide-mouth bottle and a solution of 1.44 grams of DDSA in Shellsol D70 (a white spirit comprising C n hydrocarbons with paraffins and naphthenic) added. During the ultrasonic treatment the contents of the glass bottle were stirred magnetically. The suspension was treated for 60 minutes in this case.
  • DDSA a white spirit comprising C n hydrocarbons with paraffins and naphthenic

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

L'invention concerne un procédé de préparation de particules enrobées d'un oxyde ou d'un hydroxyde de métal ou métalloïde consistant à fragmenter l'oxyde ou l'hydroxyde dans un solvant organique en présence d'un agent d'enrobage lequel est un acide organique, un anhydride ou ester ou bien une base de Lewis.
PCT/GB2002/002312 2001-05-16 2002-05-16 Fragmentation d'oxydes et d'hydroxydes de metal enrobes WO2002092703A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0112000A GB0112000D0 (en) 2001-05-16 2001-05-16 Comminution of coated metal oxides and hydroxides
GB0112000.5 2001-05-16

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Publication Number Publication Date
WO2002092703A1 true WO2002092703A1 (fr) 2002-11-21

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010084318A2 (fr) 2009-01-21 2010-07-29 Oxonica Materials Limited Procédé de combustion de combustible solide
EP1512736B1 (fr) 2003-09-05 2018-05-02 Infineum International Limited Compositions d'additifs stabilisées pour carburants diesel

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19614136A1 (de) * 1996-04-10 1997-10-16 Inst Neue Mat Gemein Gmbh Verfahren zur Herstellung agglomeratfreier nanoskaliger Eisenoxidteilchen mit hydrolysebeständigem Überzug
WO1998045212A1 (fr) * 1997-04-04 1998-10-15 Rhodia Rare Earths Inc. OXYDES DE CERIUM, OXYDES DE ZIRCONIUM, OXYDES MIXTES Ce/Zr ET SOLUTIONS SOLIDES Ce/Zr PRESENTANT UNE STABILITE THERMIQUE ET UNE CAPACITE DE STOCKAGE D'OXYGENE AMELIOREES
DE19800310A1 (de) * 1998-01-07 1999-07-08 Bayer Ag Oberflächenbelegte, nichtoxidische Keramiken
WO2002034842A1 (fr) * 2000-10-27 2002-05-02 Oxonica Limited Oxydes et hydroxydes metalliques munis d'un revetement

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19614136A1 (de) * 1996-04-10 1997-10-16 Inst Neue Mat Gemein Gmbh Verfahren zur Herstellung agglomeratfreier nanoskaliger Eisenoxidteilchen mit hydrolysebeständigem Überzug
WO1998045212A1 (fr) * 1997-04-04 1998-10-15 Rhodia Rare Earths Inc. OXYDES DE CERIUM, OXYDES DE ZIRCONIUM, OXYDES MIXTES Ce/Zr ET SOLUTIONS SOLIDES Ce/Zr PRESENTANT UNE STABILITE THERMIQUE ET UNE CAPACITE DE STOCKAGE D'OXYGENE AMELIOREES
DE19800310A1 (de) * 1998-01-07 1999-07-08 Bayer Ag Oberflächenbelegte, nichtoxidische Keramiken
WO2002034842A1 (fr) * 2000-10-27 2002-05-02 Oxonica Limited Oxydes et hydroxydes metalliques munis d'un revetement

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1512736B1 (fr) 2003-09-05 2018-05-02 Infineum International Limited Compositions d'additifs stabilisées pour carburants diesel
WO2010084318A2 (fr) 2009-01-21 2010-07-29 Oxonica Materials Limited Procédé de combustion de combustible solide
WO2010084318A3 (fr) * 2009-01-21 2011-08-11 Oxonica Materials Limited Procédé de combustion de combustible solide

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