DE891541C - Process for the production of highly dispersed oxides - Google Patents

Process for the production of highly dispersed oxides

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Publication number
DE891541C
DE891541C DED3517D DED0003517D DE891541C DE 891541 C DE891541 C DE 891541C DE D3517 D DED3517 D DE D3517D DE D0003517 D DED0003517 D DE D0003517D DE 891541 C DE891541 C DE 891541C
Authority
DE
Germany
Prior art keywords
production
highly dispersed
hydrogen
dispersed oxides
oxides
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
Application number
DED3517D
Other languages
German (de)
Inventor
Harry Dr Kloepfer
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.)
Evonik Operations GmbH
Original Assignee
Degussa GmbH
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 Degussa GmbH filed Critical Degussa GmbH
Priority to DED3517D priority Critical patent/DE891541C/en
Application granted granted Critical
Publication of DE891541C publication Critical patent/DE891541C/en
Expired legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14Methods for preparing oxides or hydroxides in general
    • C01B13/145After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14Methods for preparing oxides or hydroxides in general
    • C01B13/20Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state
    • C01B13/22Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state of halides or oxyhalides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14Methods for preparing oxides or hydroxides in general
    • C01B13/20Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state
    • C01B13/22Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state of halides or oxyhalides
    • C01B13/30Removal and cooling of the oxide-containing suspension
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • C01B33/183Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/07Producing by vapour phase processes, e.g. halide oxidation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/07Producing by vapour phase processes, e.g. halide oxidation
    • C01G23/075Evacuation and cooling of the gaseous suspension containing the oxide; Desacidification and elimination of gases occluded in the separated oxide
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043Drying, calcination
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Silicon Compounds (AREA)

Description

Verfahren zur Herstellung hochdisperser Oxyde Hochdisperse Oxyde, insbesondere Kieselsäure in hochdisperser Form, mit vorteilhaften und neuartigen Eigenschaften lassen sich durch thermische Zersetzung von flüchtigen Metall- oder Metalloidverbindungen herstellen. Dabei werden flüchtige Metalle und Metalloidverbindungen, insbesondere Halogenide, in dampfförmigem oder gasförmigem Zustand in Gegenwart von brennbaren Gasen, gegebenenfalls zusammen mit unbrennbaren oder stauerstoffhaltigen Gasen, mit Vorteil in einer Flamme umgesetzt und die so erhaltenen Oxydteilchen von den gasförmigen Reaktionsprodukten durch Abscheidung in einer Kammer bzw. durch Filter oder nach dem Cottrel-Verfahren getrennt. Die Abscheidung solcher hochdispersen Oxyde, die als solche nicht Gegenstand der vorliegenden Erfindung ist, kann auch an gekühlten, gegebenenfalls bewegten Flächen bei Temperaturen oberhalb des Taupunktes des Wassers bzw. der Halogenwasserstoffsäure oder anderer leicht kondensierbarer Reaktionsprodukte erfolgen, wobei in diesem Fall dafür Sorge getragen werden muß, daß die abgeschiedenen Oxydteilchen durch Abstreifen vor dem nochmaligen Hindurchführen der Zersetzungszone geschützt werden.Process for the production of highly disperse oxides Highly disperse oxides, in particular silica in highly dispersed form, with advantageous and new types Properties can be determined by thermal decomposition of volatile metal or Making metalloid compounds. Volatile metals and metalloid compounds, especially halides, in vapor or gaseous state in the presence of flammable gases, possibly together with non-flammable or oxygen-containing gases Gases, reacted with advantage in a flame and the oxide particles thus obtained of the gaseous reaction products by deposition in a chamber or by Filter or separated by the Cottrel process. The deposition of such highly dispersed Oxides, which as such are not the subject of the present invention, can also on cooled, possibly moving surfaces at temperatures above the dew point of water or hydrohalic acid or other easily condensable Reaction products take place, in which case care must be taken to ensure that that the deposited oxide particles by wiping them off before passing them through again the decomposition zone are protected.

Bei der Herstellung derartiger hochdisperser Oxyde werden zur Erzielung der Reaktionstemperatur die verdampfbaren Metall- bzw. Metalloidhalogen. ide mit Wasserstoff oder wasserstoffhaltigen Gasen umgesetzt. Es hat sich dabei ,gezeigt, daß, wenn die verwendeten wasserstoffhaltigen Gase ungesättigte Verbindungen, wie Acetylen oder dessen Homologe oder Olefine, enthalten, Verstopfungen insbesondere in den Brennern entstehen, durch die eine Verschlechterung in der Qualität der erzeugten hochdispersen Oxyde eintritt. Abgesehen von der Schädigung der Qualität wird auch die Durchsatzleistung durch derartige Abscheidungen wesentlich vermindert. Bei Verwendung von Chloriden, z. B. Siliciumtetrachlorid, als Ausgangsmaterial für die Herstellung hochwertiger feinverteilter Kieselsäure, bei der nur unter einwandfreien Versuchsbedingungen ein Siliciumdioxyd-Aerogel höchster Aktivität entsteht, sind die Produkte, die die Rohrleitungen bzw. Brenner verstopfen, sogar unter Explosionserscheinungen zersetzlich, wodurch weitere unangenehme Betriebsstörungen auftreten können.In the production of such highly disperse oxides are used to achieve the reaction temperature, the vaporizable metal or metalloid halogens. ide reacted with hydrogen or hydrogen-containing gases. It has been shown that if the hydrogen-containing gases used are unsaturated compounds, such as Acetylene or its homologues or olefins, particularly clogs arise in the burners, due to which a deterioration in the quality of the produced highly dispersed oxide occurs. Apart from the quality damage it will also the throughput is significantly reduced by such deposits. Using of chlorides, e.g. B. silicon tetrachloride, as a starting material for the production high-quality finely divided silica, which can only be used under perfect test conditions A silica airgel of the highest activity is created, the products that make up the Clog pipes or burners, even decomposable under the appearance of explosions, which can lead to further unpleasant operational disruptions.

Erfindungsgemäß werden zur Vermeidung dieser Nachteile und zur Erhöhung der Qualität der gewonnenen Produkte sowie der Betriebssicherheit der Herstellungsverfahren bei derErzeugung vonAerösolen, insbesondere von hochdispersen Siliciumdioxyd, durch Spalten der verdampften Halogenide in wasserstoffhaltigen Flammen die zugesetzten wasserstoffhaltigen Gase von ungesättigten Verbindungen, wie Acetylen, Olefinen od. dgl., befreit. Es können somit als Gase zur Erzeugung der für die Reaktion erforderlichen Temperatur neben Wasserstoff alle wasserstoffhaltigen Gase, wie Wassergas, Kokereigas, Leuchtgas und andere, herangezogen werden, die durch eine entsprechende an sich bekannte Vorbehandlung von ungesättigten Verbindungen gereinigt sind oder solche von vornherein nicht enthalten. .According to the invention to avoid these disadvantages and to increase the quality of the products obtained and the operational reliability of the manufacturing process in the production of aerosols, in particular of highly dispersed silicon dioxide Cleavage of the vaporized halides in hydrogen-containing flames the added hydrogen-containing gases from unsaturated compounds such as acetylene, olefins or the like, exempted. It can thus be used as gases to generate the gases required for the reaction Temperature in addition to hydrogen, all hydrogen-containing gases such as water gas, coke oven gas, Luminescent gas and others, are drawn upon by an appropriate per se known pretreatment of unsaturated compounds are purified or such not included from the start. .

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung hochdisperser Oxyde, vorzugsweise hochdisperser Kieselsäure, durch Zersetzen der entsprechenden Halogenide in wasserstoffhaltigen Flammen, dadurch gekennzeichnet, daß man zur Spaltung des Halogeniddampfes, vorzugsweise Siliciumhalogeniddampfes, solche wasserstoffhaltigen Gase benutzt, die frei sind von ungesättigten Verbindungen, wie Acetylen, Olefinen usw.PATENT CLAIM: Process for the production of highly dispersed oxides, preferably highly disperse silica, by decomposing the corresponding halides in hydrogen-containing Flames, characterized in that the halide vapor is split, preferably Silicon halide vapor, such hydrogen-containing gases used, which are free of unsaturated compounds such as acetylene, olefins, etc.
DED3517D 1943-07-14 1943-07-14 Process for the production of highly dispersed oxides Expired DE891541C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DED3517D DE891541C (en) 1943-07-14 1943-07-14 Process for the production of highly dispersed oxides

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DED3517D DE891541C (en) 1943-07-14 1943-07-14 Process for the production of highly dispersed oxides
DE1007493X 1948-12-31

Publications (1)

Publication Number Publication Date
DE891541C true DE891541C (en) 1953-09-28

Family

ID=25970528

Family Applications (1)

Application Number Title Priority Date Filing Date
DED3517D Expired DE891541C (en) 1943-07-14 1943-07-14 Process for the production of highly dispersed oxides

Country Status (1)

Country Link
DE (1) DE891541C (en)

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