CA2271818C - Process for the preparation of pulverulent heterogeneous substances - Google Patents

Process for the preparation of pulverulent heterogeneous substances Download PDF

Info

Publication number
CA2271818C
CA2271818C CA002271818A CA2271818A CA2271818C CA 2271818 C CA2271818 C CA 2271818C CA 002271818 A CA002271818 A CA 002271818A CA 2271818 A CA2271818 A CA 2271818A CA 2271818 C CA2271818 C CA 2271818C
Authority
CA
Canada
Prior art keywords
process according
suspension
dispersion
emulsion
flow
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 - Lifetime
Application number
CA002271818A
Other languages
French (fr)
Other versions
CA2271818A1 (en
Inventor
Martin Foerster
Andreas Gutsch
Rainer Domesle
Ralph Kiessling
Oliver Stohr
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.)
Umicore AG and Co KG
Original Assignee
Umicore AG and Co KG
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 Umicore AG and Co KG filed Critical Umicore AG and Co KG
Publication of CA2271818A1 publication Critical patent/CA2271818A1/en
Application granted granted Critical
Publication of CA2271818C publication Critical patent/CA2271818C/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/06Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
    • B01J2/08Gelation of a colloidal solution
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027Powdering

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Glanulating (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Steroid Compounds (AREA)

Abstract

A suspension, dispersion or emulsion is introduced into a burner. An optionally two-stage after-treatment is then carried out. The resulting powder can be employed as a catalyst.

Description

Process for the preparation of pulverulent heterogeneous substances The invention relates to a process for the preparation of pulverulent heterogeneous substances.
It is known to prepare pulverulent heterogeneous substances from oxides and salts starting from a suspension, dispersion or emulsion.
Spray driers (or similar) are usually employed for drying for suspensions, dispersions or emulsions. This is followed by a rotary tube for calcining (or similar). The losses of powder by cleaning and handling, and also during operation of the plant are or can be considerable, and/or the expenditure on personnel is high.
Drying and calcining in batches (for example in vessels in a muffle furnace) is used as an alternative. However, there is the risk here of a very wide range of product quality due to diffusion processes and temperature gradients in the powder.
There is thus the object of developing a process for the preparation of pulverulent heterogeneous substances which does not have these disadvantages.
The invention provides a process for the preparation of pulverulent heterogeneous substances, characterized in that a dispersion, suspension or emulsion is introduced into a turbulent or laminar burner, this dispersion, suspension or emulsion is treated there under the conditions established there, the resulting reaction mixture is introduced into a downstream flow-through tube, the powder is treated further there, the powder is subsequently fed, optionally, to a washer, a separator or a filter, subjected, optionally, to a further treatment there, and subsequently transported further via an appropriate device.
In the high temperature flow reactor, the dispersion, suspension or emulsion can be present as a gas-borne group of particles.
The high temperature flow reactor can be heated by feeding in non-combustible hot gases.
The high temperature flow reactor can be heated indirectly by heating up the walls adjacent to the reaction space.
Heating can be achieved here by electrical plasma and/or inductive plasma.
A high-energy laser light beam and/or microwave energy can additionally be fed to the high temperature flow reactor.
In addition to the dispersion, suspension or emulsion, non-combustible reactive gases or vapours can be fed to the high temperature flow reactor, it being possible for the reaction product to be a highly disperse nanostructured solid which adds on to the surface of the particles of the dispersion, emulsion or suspension.
The reaction product can form homogeneous molecular layers on the particles of the dispersion, emulsion or suspension, the particles of the dispersion, emulsion or suspension being coated with a mono- or multimolecular layer.
The non-combustible reactive gases or vapours can be metal chlorides and/or organometallic compounds, as well as mixtures of these compounds.
The temperature in the reaction space can be above 1000 °C.
The suspension, dispersion or emulsion can be fed to the reaction space axially in co- or countercurrent or radially.
The dispersion, emulsion or suspension can be fed to the reaction space radially.
The dispersion, emulsion or suspension can be a solids suspension, a solution, powder, pastes, melts or granules with or without dissolved "salts". The dispersion, emulsion or suspension is metered into the space in finely divided form by atomizing, wave-breaking, as a mist or jet.
The secondary gas mentioned in the figure can be air, ambient air with oxygen contents of between 0 and 100 0, dry or humid, water vapour, other vapours or gases, IS nitrogen and the like.
The burner can be of a known design with pulsatory combustion. Such a burner is described in the document DD
114 454.
A burner of high turbulence can preferably be employed to improve the transportation of material. In particular, a spinning burner, possibly with an overlaid pulsation, can be employed.
The liquid phase of the suspension, dispersion or emulsion can be water, alcohol, liquid organic hydrocarbons or organic solvents.
The components present as the solid in the suspension, dispersion or emulsion can be, individually or as a mixture: oxides, nitrides or carbides of aluminium, silicon, cerium, zirconium, titanium, crystallized-out salts of aluminium, silicon, cerium, zirconium, lanthanum, barium, metals such as, for example, nickel, silver, palladium, gold, rhodium, platinum, carbon black, organic compounds.
The dissolved or non-dissolved salts can be nitrates, acetates, carbonates, chlorides of aluminium, cerium, silicon, zirconium, titanium, lanthanum, barium, platinum, rhodium, palladium, iridium, potassium, calcium and ammonium and mixtures of these components.
A combustible gas, such as, for example, hydrogen and/or methane, can be used as the fuel.
The temperature in the burner can be 500 to 2000 °C.
The temperature after the burner and the reducing or oxidizing atmosphere in the flow-through tube can be established via the ratio of oxygen (from the combustion air) to hydrogen and the flow rates. Moreover, further reactive or inert gases and vapours can be fed into the tube.
The dispersion, emulsion or suspension of the solid can be sprayed or dripped into the flame of the burner.
The water or the solvent evaporates and the powder formed is calcined, oxidized or reduced and sintered at high temperatures in the gas atmosphere present. The residence time of the powder in the hot gas phase can be varied in the range from 0.01 second up to minutes by the separating device (cyclone, high temperature filter). The mass and heat transfer is significantly better than in a rotary tube or in a muffle furnace.

With spray calcining, the surfaces to be cleaned are considerably smaller compared with a spray drier with subsequent calcining in a rotary tube and the losses of substance are low. Due to the use of a continuous process, 5 the range of product quality is narrow. Compared with the rotary tube, the losses during start-up and shut-down are very low.
The powder in the waste air filters/cyclone of a rotary tube has a wide range of product quality and often cannot be used, while in the process according to the invention the range of product quality in the waste air filter/
cyclone is a very narrow range.
The in situ treatment of the waste air can have an effect as a further advantage. The salts are often nitrates, acetates and ammonium compounds, the decomposition products of which, NO, NH3 and CHNO, can be reduced in amount by adjusting the composition of the hot waste gases or can be treated in a downstream catalyst without additional heating up.
The products which can be prepared are heterogeneous powders/granules:
1. Mixed agglomerates and/or mixed aggregates of different oxides/metals/nitrides/carbides/carbon black.
2. Base substances (support material) (possibly in shell form) impregnated/covered/coated with oxides/metals/
nitrides/carbides.
3. Combination of 1. and 2.
The substances prepared according to the invention can be employed as a catalyst, for the production of ductile ceramic components, for the production of components with a quantum mechanics activity, in particular sensors and photoelectrically active emitters, and as oxygen stores, NOX stores, CnHm stores for catalysis and adsorbents.
The process according to the invention is shown and explained in more detail in the drawing:
Figure 1 shows a burner 1, to which the flow-through tube 2 is connected. The washer 3, the separator 4, the filter 5 and the fan 6 are connected to the flow-through tube 2.
In the process according to the invention, a dispersion, suspension or emulsion, a secondary gas, combustion air and fuel are introduced into the burner 1. The reaction mixture reacted in the burner 1 is introduced into the flow-through tube 2. A reducing or oxidizing gas atmosphere can be established in the flow-through tube 2. The reacted reaction mixture can be treated in the flow-through tube 2 such that a) the dispersion, suspension or emulsion is dried, b) the water of crystallization is driven off, c) the powder is calcined, substances such as nitrates, acetates, carbonates being decomposed to gases, d) the powder is oxidized or reduced, e) the powder is sintered, f) the specific surface area of the powder is decreased.
After passage through the flow-through tube 2, the powder can be treated in the washer 3 if a dispersion is to be prepared or contact with air is to be avoided.
Alternatively, after leaving the flow-through tube 2, the powder can be separated off via the separating device 4, for example for brief treatment at high temperatures.
In another alternative, the powder can be separated off by means of the filter 5 for a longer treatment at high temperatures.
The waste gas can be discharged by means of the fan 6.
Example 1 A aluminium oxide/water suspension with dissolved platinum l0 nitrate is introduced into the burner 1. The suspension comprises 400 g/1 aluminium oxide g/1 platinum nitrate 800 g/1 water.

Hydrogen is employed as the fuel.
The burner temperature is 1,200 °C, and the residence time is approx. 1 sec.
The powder separated off in the cyclone is dry and no longer contains nitrate ions. The platinum is deposited in a finely disperse form on the surface of the aluminium oxide.
Example 2 An aqueous suspension which comprises 400 g/1 aluminium oxide, 100 g/1 cerium acetate, 100 g/1 zirconium nitrate and 800 g/1 water is introduced into the burner 1. Natural gas is employed as the fuel. The burner temperature is 1,000 °C. The powder separated off in the cyclone is dry and contains neither acetate ions nor nitrate ions. The cerium oxide and the zirconium oxide are deposited in a finely divided form on the surface of the aluminium oxide.
Example 3 A moist powder comprising 78 wt.o aluminium oxide 20 wt.o water 2 wt.o platinum nitrate is treated with natural gas at a burner temperature of 900 °C
The powder separated off in the cyclone is dry and contains no nitrate ions. The platinum is deposited in a finely divided form on the surface of the aluminium oxide.

Claims (15)

1. A process for the preparation of a pulverulent heterogeneous substance, comprising introducing a dispersion, suspension or emulsion into a turbulent or laminar burner, heating the dispersion, suspension or emulsion under reaction conditions established in said burner to obtain a reaction mixture powder, introducing said reaction mixture powder into a downstream high temperature flow through tube reactor, treating said powder with a gas, optionally feeding said powder to a washer, a separator or a filter.
2. The process according to claim 1, wherein said dispersion, suspension or emulsion is present in said high temperature flow through tube reactor as a gas-borne group of particles.
3. The process according to claim 1 or 2, further comprising heating said flow through tube reactor by an exothermic combustion reaction which takes place in the tube.
4. The process according to claim 1 or 2, further comprising heating said high temperature flow through tube reactor by feeding in non-combustible hot gases.
5. The process according to any one of claims 1 to 4, further comprising heating said high temperature flow through tube reactor indirectly by heating up the walls of the flow through tube reactor.
6. The process according to any one of claims 1 to 4, further comprising heating said flow through tube reactor by electrical plasma and/or inductive plasma.
7. The process according to any one of claims 1 to 6, further comprising subjecting the flow through tube reactor to a high-energy laser light beam and/or microwave energy.
8. The process according to claim 7, further comprising, in addition to the dispersion, suspension or emulsion in the form of particles, feeding a non-combustible reactive gas or vapor to the flow through tube reactor to produce a reaction product which is a highly dispersed nano-structured solid which adds on to the surface of the particles of the dispersion, suspension or emulsion.
9. The process according to claim 8, wherein the reaction product formed thereby is a homogeneous molecular layer on the particles of the dispersion, suspension, or emulsion, the particles of the dispersion, suspension or emulsion being thereby coated with a mono- or multimolecular layer.
10. The process according to claim 8 or 9, wherein the non-combustible reactive gas or vapor is at least one of a metal chloride or organometallic compound.
11. The process according to any one of claims 1 to 10, wherein the temperature of the reaction is above 1000°C.
12. The process according to any one of claims 1 to 10, wherein the reaction temperature is 500 to 2000°C.
13. The process according to any one of claims 1 to 12, wherein the dispersion, suspension or emulsion is fed to the burner axially in co- or countercurrent or radially.
14. The process according to claim 13, wherein the dispersion, suspension or emulsion is fed to the flow through tube reactor radially.
15. The process according to any one of claims 1 to 14, wherein the powder is in a hot gas phase for at least 0.01 seconds.
CA002271818A 1998-05-12 1999-05-11 Process for the preparation of pulverulent heterogeneous substances Expired - Lifetime CA2271818C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19821144.9 1998-05-12
DE19821144A DE19821144A1 (en) 1998-05-12 1998-05-12 Process for the production of powdery heterogeneous substances

Publications (2)

Publication Number Publication Date
CA2271818A1 CA2271818A1 (en) 1999-11-12
CA2271818C true CA2271818C (en) 2006-12-05

Family

ID=7867464

Family Applications (1)

Application Number Title Priority Date Filing Date
CA002271818A Expired - Lifetime CA2271818C (en) 1998-05-12 1999-05-11 Process for the preparation of pulverulent heterogeneous substances

Country Status (13)

Country Link
EP (1) EP0957064B1 (en)
JP (1) JP4828674B2 (en)
KR (1) KR100624991B1 (en)
CN (1) CN1170626C (en)
AT (1) ATE251087T1 (en)
BR (1) BR9901526A (en)
CA (1) CA2271818C (en)
DE (2) DE19821144A1 (en)
DK (1) DK0957064T3 (en)
ES (1) ES2207047T3 (en)
MX (1) MXPA99004399A (en)
PT (1) PT957064E (en)
ZA (1) ZA993249B (en)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1129764B1 (en) 2000-03-01 2005-10-26 Umicore AG & Co. KG Catalyst for purifying diesel engines exhaust gases and process for its preparation
EP1190768A1 (en) * 2000-09-26 2002-03-27 Degussa AG Noble metal catalyst
DE10342826B3 (en) 2003-09-17 2005-05-12 Degussa Ag Dispersion of pyrogenic ceria
JP2007083113A (en) * 2005-09-20 2007-04-05 Chugai Ro Co Ltd Powder production apparatus
WO2008004407A1 (en) * 2006-06-08 2008-01-10 Pultech Corporation Method of pulverization drying and pulverization drying apparatus
CN101479023A (en) 2006-06-29 2009-07-08 乌米科雷股份两合公司 Three-way catalyst
DE102006039462B4 (en) * 2006-08-23 2010-02-18 Ibu-Tec Advanced Materials Ag Process for the production of particles
EP1974809B1 (en) 2007-03-19 2010-09-29 Umicore AG & Co. KG Double layer three-way catalytic converter
DE102007046158B4 (en) 2007-09-27 2014-02-13 Umicore Ag & Co. Kg Use of a catalytically active particulate filter for the removal of particles from the exhaust gas of combustion engines operated with predominantly stoichiometric air / fuel mixture
ATE457813T1 (en) 2007-09-28 2010-03-15 Umicore Ag & Co Kg REMOVAL OF PARTICLES FROM THE EXHAUST GAS OF COMBUSTION ENGINES OPERATED WITH A PREMIUM STOICHIOMETRIC AIR/FUEL MIXTURE
DE102009023877A1 (en) 2009-06-04 2010-12-16 Süd-Chemie AG New catalyst carrier comprising a porous, micropore carrier, and a catalytically active component, where the micropores are free of the catalytically active component, useful for treating exhaust fumes from fossil, synthetic or biofuels
DE102010007499A1 (en) 2010-02-09 2011-08-11 Umicore AG & Co. KG, 63457 Volumetric coating arrangement
CN104334272B (en) 2012-06-06 2018-07-06 优美科股份公司及两合公司 For the startup catalyst of diesel particulate filter device upstream
JP6246192B2 (en) 2012-06-06 2017-12-13 ユミコア アクチェンゲゼルシャフト ウント コンパニー コマンディートゲゼルシャフト Three-way catalyst system

Family Cites Families (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2560357A (en) * 1946-08-15 1951-07-10 Standard Oil Dev Co Production of solid fuel agglomerates
DD114454A1 (en) * 1974-04-02 1975-08-05
DE2640520A1 (en) * 1976-09-09 1978-03-16 Cordes Wilh Maschf Overflow pipe for washing machine tub - has a weighted or spring-loaded cover or valve , to prevent unnecessary escape of steam
JPS59206042A (en) * 1983-05-07 1984-11-21 Sumitomo Electric Ind Ltd Process and apparatus for producing fine powder
DE3345983C2 (en) * 1983-12-20 1986-09-04 Wolfgang 4600 Dortmund Seidler Method and device for the production of spherical metallic particles
DE3602647A1 (en) * 1985-02-02 1986-08-07 Toyota Jidosha K.K., Toyota, Aichi PRODUCTION OF SILICONE CERAMIC POWDERS
JPH068170B2 (en) * 1985-10-29 1994-02-02 宇部興産株式会社 Method for producing high-purity magnesium oxide fine powder
DE3719825A1 (en) * 1987-06-13 1988-12-29 Kernforschungsz Karlsruhe METHOD FOR PRODUCING CERAMIC POWDERS AND DEVICE FOR IMPLEMENTING THE SAME
JP2566805B2 (en) * 1988-01-28 1996-12-25 日鉄化工機株式会社 Method for producing complex oxide powder
US4937062A (en) * 1988-03-07 1990-06-26 Cabot Corporation High surface area metal oxide foams and method of producing the same
FR2629487B1 (en) * 1988-03-29 1991-12-20 Philips Ind Commerciale LAUNDRY WASHING MACHINE WITH OVERFLOW
DE4222944C2 (en) * 1992-07-11 1998-06-18 Aeg Hausgeraete Gmbh Program-controlled drum washing and spinning machine with a swinging suspended washing unit
DE4222945A1 (en) * 1992-07-11 1994-01-13 Licentia Gmbh Program-controlled drum washing machine and spinner - has washing aggregate with washing soln. container having mass equalisation device in form of receptacle connected to fresh water supply
US5618580A (en) * 1992-12-28 1997-04-08 Kao Corporation Method for producing ceramic fine particles and apparatus used therefor
JP3032098B2 (en) * 1993-02-09 2000-04-10 新日本製鐵株式会社 Soft ferrite raw material powder and method and apparatus for producing the same
JP2704485B2 (en) * 1993-09-09 1998-01-26 株式会社豊田中央研究所 Method for producing oxide powder
JP2769290B2 (en) * 1994-03-31 1998-06-25 科学技術振興事業団 Manufacturing method of ceramic fine powder by mist pyrolysis method
GB9409660D0 (en) * 1994-05-13 1994-07-06 Merck Patent Gmbh Process for the preparation of multi-element metaloxide powders
US5498446A (en) * 1994-05-25 1996-03-12 Washington University Method and apparatus for producing high purity and unagglomerated submicron particles
DE4443156A1 (en) * 1994-12-05 1996-06-13 Aeg Hausgeraete Ag Washing machine has ventilation device

Also Published As

Publication number Publication date
JP2000061288A (en) 2000-02-29
ZA993249B (en) 1999-11-11
ATE251087T1 (en) 2003-10-15
KR100624991B1 (en) 2006-09-20
ES2207047T3 (en) 2004-05-16
EP0957064B1 (en) 2003-10-01
JP4828674B2 (en) 2011-11-30
DE19821144A1 (en) 1999-11-18
CN1240674A (en) 2000-01-12
CN1170626C (en) 2004-10-13
MXPA99004399A (en) 2004-09-27
KR19990088176A (en) 1999-12-27
PT957064E (en) 2004-03-31
BR9901526A (en) 2000-01-25
DE59907148D1 (en) 2003-11-06
EP0957064A1 (en) 1999-11-17
DK0957064T3 (en) 2003-12-22
CA2271818A1 (en) 1999-11-12

Similar Documents

Publication Publication Date Title
CA2271818C (en) Process for the preparation of pulverulent heterogeneous substances
KR100239294B1 (en) Catalytic method and device for controlling voc, co and halogenated organic emissions
JP3626754B2 (en) Catalytic incineration of organic compounds
KR950007317B1 (en) Catalytic destruction of organohalogen compounds
US7288501B2 (en) Process and apparatus for the thermal treatment of pulverulent substances
JP2009091238A (en) Ceric oxide washcoat
CA2375250A1 (en) Spray pyrolysis or spray-drying process, and plant for carrying it out
JP2001017857A (en) Spray pyrolytic apparatus
US6228292B1 (en) Process for the preparation of pulverulent heterogeneous substances
US20170173567A1 (en) Method of preparing selective catalytic reduction composite catalyst
WO2021029410A1 (en) Method for manufacturing catalyst for voc treatment
JPH09202607A (en) Production of oxide powder
JP4923027B2 (en) Method for preparing vanadia-titania catalyst for chlorinated organic compound decomposition using solvothermal synthesis process
US9321033B2 (en) Process for thermal fixation of catalytically active component onto alumina support
Quincoces et al. Preparation and characterization of supported vanadia catalyst for the selective catalytic reduction of NO with NH3
JPH07155599A (en) Catalyst for removal of nox in water gas and its production
JP2948578B1 (en) Exhaust gas treatment catalyst, method for producing the same, exhaust gas treatment method and treatment apparatus
JP2003210983A (en) Organohalogen decomposition catalyst and method for manufacturing the same
Goldstein et al. NO x control in catalyst manufacture
JP2001079394A (en) Catalyst, method and device for treating exhaust gas
JPH0893455A (en) Device and method for controlling exhaust emission using infrared ray

Legal Events

Date Code Title Description
EEER Examination request
MKEX Expiry

Effective date: 20190513