DE1047756B - Process for the production of amorphous, finely divided silicon dioxide - Google Patents

Process for the production of amorphous, finely divided silicon dioxide

Info

Publication number
DE1047756B
DE1047756B DEC16130A DEC0016130A DE1047756B DE 1047756 B DE1047756 B DE 1047756B DE C16130 A DEC16130 A DE C16130A DE C0016130 A DEC0016130 A DE C0016130A DE 1047756 B DE1047756 B DE 1047756B
Authority
DE
Germany
Prior art keywords
finely divided
amorphous
production
silicon dioxide
silica
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.)
Pending
Application number
DEC16130A
Other languages
German (de)
Inventor
Donald B Broughton
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.)
Godfrey L Cabot Inc
Original Assignee
Godfrey L Cabot Inc
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 Godfrey L Cabot Inc filed Critical Godfrey L Cabot Inc
Priority to DEC16130A priority Critical patent/DE1047756B/en
Publication of DE1047756B publication Critical patent/DE1047756B/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • C01B33/183—Preparation 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
    • C01B33/184—Preparation 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 by hydrolysis of tetrafluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/02—Amorphous compounds
    • 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
    • C01P2006/10—Solid density
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Description

Verfahren zur Herstellung von amorphem, feinteiligem Siliciumdioxyd Die Erfindung betrifft ein Verfahren zur Herstellung von amorpher, feinteiliger Kieselsäure, die als aktiver Füllstoff für natürlichen und künstlichen Kautschuk oder als Pigment verwendbar ist. Das Verfahren ist dadurch gekennzeichnet, daß Wasserdampf und Siliciumtetrafluorid bei Temperaturen von mehr als 700"C umgesetzt, die gebildete feinteilige Kieselsäure von dem Fluorwasserstoff bei diesen Temperaturen abgetrennt und erst danach die abgeschiedene Kieselsäure abgekühlt wird. Process for the production of amorphous, finely divided silicon dioxide The invention relates to a method for producing amorphous, finely divided Silica used as an active filler for natural and artificial rubber or can be used as a pigment. The method is characterized in that water vapor and silicon tetrafluoride reacted at temperatures of more than 700 "C, the formed finely divided silica is separated from the hydrogen fluoride at these temperatures and only then is the precipitated silica cooled.

Es ist bekannt, daß sich Siliciumtetrafluorid mit Wasserdampf umsetzen läßt entsprechend folgender Gleichung SiF4 +2H2O -SiQ +4HF Diese Reaktion ist bei Temperaturen unter 7000 C reversibel, d. h., Kieselsäure und Fluorwasserstoffsäure rekombinieren zu Siliciumtetrafluorid, wenn das bei der Hydrolyse gebildete Kieselsäureaerosol längere Zeit bei Temperaturen unter 700"C gehalten wird. Die Kieselsäure muß daher bei hohen Temperaturen aus dem Aerosol abgetrennt werden. It is known that silicon tetrafluoride react with water vapor leaves SiF4 + 2H2O -SiQ + 4HF according to the following equation. This reaction is at Reversible temperatures below 7000 C, i.e. i.e., silica and hydrofluoric acid recombine to silicon tetrafluoride when the silicic acid aerosol formed during hydrolysis is kept for a long time at temperatures below 700 ° C. The silica must therefore separated from the aerosol at high temperatures.

Die erfindungsgemäß aus trockenem Siliciumtetrafluorid mit Wasserdampf hergestellte Kieselsäure ist außerordentlich feinteilig und eignet sich insbesondere vorzüglich als Verstärkungsmittel für natürliche und synthetische Kautschukmischungen. According to the invention from dry silicon tetrafluoride with steam The silica produced is extremely finely divided and is particularly suitable Excellent as a reinforcing agent for natural and synthetic rubber compounds.

Das benötigte Siliciumtetrafiuorid läßt sich leicht aus billigen, in genügender Menge vorhandenen Rohstoffen, wie vor allem Fluorit, Sand und Schwefelsäure, herstellen. The silicon tetrafluoride required can easily be obtained from cheap, sufficient raw materials, such as fluorite, sand and sulfuric acid, produce.

Fluorit und Sand reagieren mit starker Schwefelsäure nach der Gleichung 2 CaF + SiO2 + 2 H2SO4 SiF4 + 2 CaSO4 + 2 H2O Werden die Fluorit- und Sandgemische mit etwa 700i0iger Schwefelsäure erhitzt, so entweicht SiF4 in Dampfform und läßt sich direkt für die Gewinnung von amorpher, feinteiliger Kieselsäure gemäß der Erfindung benutzen.Fluorite and sand react with strong sulfuric acid according to the equation 2 CaF + SiO2 + 2 H2SO4 SiF4 + 2 CaSO4 + 2 H2O Are the fluorite and sand mixtures When heated with about 700% sulfuric acid, SiF4 escapes in vapor form and leaves directly for the production of amorphous, finely divided silica according to the invention use.

Die Umsetzung zwischen dem Siliciumtetrafluorid und dem überhitzten Wasserdampf findet sofort bei der Berührung statt. Es treten dicke weiße Nebel von Kieselsäure auf. Aus diesen Nebeln wird die Kieselsäure bei Temperaturen von mehr als 700"C in an sich bekannter Weise abgeschieden. Sie wird als sehr feines Pulver einer Dichte von etwa 0,064 g/cm3 und einer spezifischen Oberfläche von 100 bis 200 m2/g gewonnen. The reaction between the silicon tetrafluoride and the superheated Water vapor takes place immediately upon contact. Thick white mist emerges Silica on. From these mists the silica becomes at temperatures higher than better known than 700 "C in itself Way deposited. It comes as a very fine powder a density of about 0.064 g / cm3 and a specific surface area of 100 to 200 m2 / g recovered.

Der als Nebenprodukt erhaltene Fluorwasserstoff kann zur Erzeugung von Kieselfluorwasserstoffsäure verwendet werden, aus der wiederum Siliciumtetrafluorid gewonnen wird. The hydrogen fluoride obtained as a by-product can be used for production of silicofluoric acid are used, from which in turn silicon tetrafluoride is won.

Claims (1)

PATETNSPUCH: Verfahren zur Herstellung von amorphem, feinteiligem Siliciumdioxyd, insbesondere zur Verwendung als aktiver Füllstoff für natürlichen oder synthetischen Kautschuk, durch hydrolytische Spaltung von Siliciumtetrafluorid in der Dampfphase, dadurch gekennzeichnet, daß Wasserdampf und Siliciumtetrafluorid bei Temperaturen von mehr als 700"C umgesetzt, die gebildete feinteilige Kieselsäure von dem Fluorwasserstoff bei diesen Temperaturen abgetrennt und erst danach die abgeschiedene Kieselsäure abgekühlt wird. PATETNSPUCH: Process for the production of amorphous, finely divided Silica, especially for use as an active filler for natural or synthetic rubber, by hydrolytic cleavage of silicon tetrafluoride in the vapor phase, characterized in that water vapor and silicon tetrafluoride converted at temperatures of more than 700 "C, the finely divided silica formed separated from the hydrogen fluoride at these temperatures and only then the deposited silica is cooled.
DEC16130A 1956-02-07 1956-02-07 Process for the production of amorphous, finely divided silicon dioxide Pending DE1047756B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEC16130A DE1047756B (en) 1956-02-07 1956-02-07 Process for the production of amorphous, finely divided silicon dioxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEC16130A DE1047756B (en) 1956-02-07 1956-02-07 Process for the production of amorphous, finely divided silicon dioxide

Publications (1)

Publication Number Publication Date
DE1047756B true DE1047756B (en) 1958-12-31

Family

ID=7015982

Family Applications (1)

Application Number Title Priority Date Filing Date
DEC16130A Pending DE1047756B (en) 1956-02-07 1956-02-07 Process for the production of amorphous, finely divided silicon dioxide

Country Status (1)

Country Link
DE (1) DE1047756B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1193925B (en) * 1962-08-20 1965-06-03 Hooker Chemical Corp Process for the production of amorphous, finely divided silicon dioxide and hydrogen fluoride or metal fluorides from silicon tetrafluoride, hydrofluoric acid and silicon dioxide in suspended form and exhaust gases containing water vapor
US3203759A (en) * 1960-11-03 1965-08-31 Flemmert Gosta Lennart Method of preparing silicon dioxide
DE1245342B (en) * 1961-05-29 1967-07-27 Columbian Carbon Process for the production of finely divided amorphous silicon dioxide
DE1442999B1 (en) * 1963-01-17 1970-08-27 Columbian Carbon Process for the production of finely divided amorphous silica

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3203759A (en) * 1960-11-03 1965-08-31 Flemmert Gosta Lennart Method of preparing silicon dioxide
DE1245342B (en) * 1961-05-29 1967-07-27 Columbian Carbon Process for the production of finely divided amorphous silicon dioxide
DE1193925B (en) * 1962-08-20 1965-06-03 Hooker Chemical Corp Process for the production of amorphous, finely divided silicon dioxide and hydrogen fluoride or metal fluorides from silicon tetrafluoride, hydrofluoric acid and silicon dioxide in suspended form and exhaust gases containing water vapor
DE1442999B1 (en) * 1963-01-17 1970-08-27 Columbian Carbon Process for the production of finely divided amorphous silica

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