DE1216174B - Process for the production of macroporous glassy carbon - Google Patents

Process for the production of macroporous glassy carbon

Info

Publication number
DE1216174B
DE1216174B DES94543A DES0094543A DE1216174B DE 1216174 B DE1216174 B DE 1216174B DE S94543 A DES94543 A DE S94543A DE S0094543 A DES0094543 A DE S0094543A DE 1216174 B DE1216174 B DE 1216174B
Authority
DE
Germany
Prior art keywords
macroporous
carrier
production
glassy carbon
impregnated
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
DES94543A
Other languages
German (de)
Inventor
Gilberte Moutard
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.)
Mersen SA
Original Assignee
Carbone Lorraine SA
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 Carbone Lorraine SA filed Critical Carbone Lorraine SA
Publication of DE1216174B publication Critical patent/DE1216174B/en
Pending legal-status Critical Current

Links

Classifications

    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04C—STRUCTURAL ELEMENTS; BUILDING MATERIALS
    • E04C2/00—Building elements of relatively thin form for the construction of parts of buildings, e.g. sheet materials, slabs, or panels
    • E04C2/02—Building elements of relatively thin form for the construction of parts of buildings, e.g. sheet materials, slabs, or panels characterised by specified materials
    • E04C2/10—Building elements of relatively thin form for the construction of parts of buildings, e.g. sheet materials, slabs, or panels characterised by specified materials of wood, fibres, chips, vegetable stems, or the like; of plastics; of foamed products
    • E04C2/20—Building elements of relatively thin form for the construction of parts of buildings, e.g. sheet materials, slabs, or panels characterised by specified materials of wood, fibres, chips, vegetable stems, or the like; of plastics; of foamed products of plastics
    • E04C2/205—Building elements of relatively thin form for the construction of parts of buildings, e.g. sheet materials, slabs, or panels characterised by specified materials of wood, fibres, chips, vegetable stems, or the like; of plastics; of foamed products of plastics of foamed plastics, or of plastics and foamed plastics, optionally reinforced
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/354—After-treatment
    • C01B32/384—Granulation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/245—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds from polyurethanes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Architecture (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Civil Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Ceramic Products (AREA)

Description

BUNDESREPUBLIK DEUTSCHLANDFEDERAL REPUBLIC OF GERMANY

DEUTSCHESGERMAN

PATENTAMTPATENT OFFICE

AUSLEGESCHRIFTEDITORIAL

Int. α.:Int. α .:

Nummer: Aktenzeichen:
Anmeldetag:
Auslegetag: Number: Case number:
Registration date:
Display day:

C04bC04b

Deutsche KL: 80 b-8/12 German KL: 80 b -8/12

1216174
S94543VIb/80b
9. Dezember 1964
5. Mai 1966 1 216174
S94543VIb / 80b
December 9, 1964
May 5th 1966

Glasiger Kohlenstoff mit schneckenlinienförmigem Gefüge ist zur Herstellung von Stücken aus hartem und dichtem Kohlenstoff sehr geschätzt. Eines der Verfahren zur Herstellung von glasigem Kohlenstoff besteht darm, bestimmte durch Wärme härtbare Harze langsam in reduzierender Atmosphäre zu karbonisieren, wodurch feste kompakte und dichte Produkte erzielt werden.Vitreous carbon with a helical structure is used to make pieces of hard and dense carbon. One of the methods of making glassy carbon insists on slowly carbonizing certain thermosetting resins in a reducing atmosphere, whereby strong, compact and dense products are obtained.

Der Erfindung liegt die Aufgabe zugrunde, einen amorphen, harten, starkporigen Kohlenstoff sowie ein Verfahren zu seiner Herstellung zu schaffen. Zur Lösung dieser Aufgabe wird gemäß der Erfindung ein makroporiger Träger wie eine Schaummasse aus Polyurethan oder Polyolefin mit einem Harz imprägniert, das durch Wärme verfestigbar und verkokbar ist und sich während der Karbonisation in glasigen amorphen Kohlenstoff umwandelt, während sich der Träger langsam zersetzt und seine Struktur am Endprodukt hinterläßt.The invention is based on the object of an amorphous, hard, highly pored carbon as well to create a process for its manufacture. To solve this problem, according to the invention a macroporous carrier such as a foam mass made of polyurethane or polyolefin impregnated with a resin, which can be solidified and coked by heat and becomes glassy during carbonization converts amorphous carbon while the carrier slowly decomposes and its structure on the end product leaves behind.

Für den Träger wählt man z. B. einen Polyurethanschaum, der eine Dichte von 0,25 hat. Das Imprägniermittel ist vorzugsweise ein durch Wärme härtbares Phenol- oder Furanharz. Die Imprägnierung kann durch jegliche bekannte Mittel vorgenommen werden. Sie erfolgt z. B. durch einfaches Eintauchen in ein Harzbad mit einem 2%igen Zusatz eines entsprechenden Katalysators. Gegebenenfalls wird die Imprägnierung in einem Autoklav vorgenommen, in dem man abwechselnd Unter- und Überdruck herstellt. Nach der Imprägnierung kann das überschüssige Imprägnierharz durch Trocknen bzw. Absaugen ausgetrieben werden. Das Gewicht des imprägnierten und getrockneten Schaumes ist etwa zehnmal größer als sein Ursprungsgewicht. Das Imprägniermittel kann gegebenenfalls in einem geeigneten Lösungsmittel, wie z. B. Benzol, verdünnt werden. Der imprägnierte Schaum bleibt während 4 bis 8 Tagen in ruhendem Zustand, damit die Polymerisation des Harzes erfolgt und die Verfestigung vollständig wird. Anschließend an die Polymerisation findet nach herkömmlichen Verfahren in einer reduzierenden Atmosphäre bei 1200° C die Karbonisation statt, wobei eine mittlere Heizgeschwindigkeit von 5 bis 10° C pro Stunde eingehalten wird und gegebenenfalls eine Graphitbehandlung oder Reinigung bei höherer Temperatur erfolgt.For the carrier you choose z. B. a polyurethane foam, which has a density of 0.25. The impregnating agent is preferably a thermosetting phenolic or furan resin. The impregnation can be done by any known means. It takes place z. B. by simple Immersion in a resin bath with a 2% addition of an appropriate catalyst. Possibly the impregnation is carried out in an autoclave, in which one alternates negative and positive pressure manufactures. After impregnation, the excess impregnation resin can be dried or removed. Aspiration to be expelled. The weight of the impregnated and dried foam is approx ten times greater than its original weight. The impregnating agent can optionally be in a suitable one Solvents such as B. benzene, are diluted. The impregnated foam remains for 4 to 8 days at rest so that the resin polymerizes and solidifies completely will. Subsequent to the polymerization takes place according to conventional processes in a reducing Atmosphere at 1200 ° C the carbonization takes place, with a medium heating rate of 5 to 10 ° C per hour and optionally a graphite treatment or cleaning takes place at a higher temperature.

Man erhält einen glasigen, glänzenden harten Kohlenstoff, dessen Dichte in der Größenordnung von 0,1 bis 0,4 liegt und der eine Druckfestigkeit von 5 bis 20 kg/cm2 aufweist. Dieses makroporige Material gemäß der Erfindung findet Anwendung im Bereich der Wärmeisolierung und beim Aufbau von Verfahren zur Herstellung makroporigen glasigen KohlenstoffsA glassy, shiny hard carbon is obtained, the density of which is in the order of 0.1 to 0.4 and a compressive strength of 5 to 20 kg / cm 2 . This macroporous material according to the invention finds application in the field of thermal insulation and in the construction of processes for the production of macroporous glassy carbon

Anmelder:Applicant:

Societe Le Carbone-Lorraine, ParisSociete Le Carbone-Lorraine, Paris

Vertreter:Representative:

Dipl.-Ing. Dipl. eoc. publ. D. Lewinsky,Dipl.-Ing. Dipl. Eoc. publ. D. Lewinsky,

Patentanwalt,Patent attorney,

München-Pasing, Agnes-Bernauer-Str. 202Munich-Pasing, Agnes-Bernauer-Str. 202

Als Erfinder benannt:Named as inventor:

Gilberte Moutard, Neuilly-sur-Seine (Frankreich)Gilberte Moutard, Neuilly-sur-Seine (France)

Beanspruchte Priorität:Claimed priority:

Frankreich vom 13. Dezember 1963 (957 094)France of December 13, 1963 (957 094)

Filtern. Permeabilitätsmessungen wurden bei scheibenförmigen Mustern mit 50 mm Durchmesser und mm Stärke durchgeführt. Die Gasdurchlässigkeit des Materials wurde ermittelt, indem man die Durchflußmenge pro Stunde in Litern gemessen hat, wobei das Gas durch einen Querschnitt von 1 cm2 und 1 cm Dicke des Musters unter einem bestimmten Druck hindurchdiffundierte:Filter. Permeability measurements were carried out on disk-shaped samples with a diameter of 50 mm and a thickness of 50 mm. The gas permeability of the material was determined by measuring the flow rate per hour in liters, the gas diffusing through a cross-section of 1 cm 2 and 1 cm thickness of the sample under a certain pressure:

GasdurchlässigkeitGas permeability DrückePress 5 mm 5 mm 10 mm 10 mm 20 mm 20 mm Durchflußmenge in Liter je StundeFlow rate in liters per hour 32,8
49,6
76,532.8
49.6
76.5

WasserdurchlässigkeitWater permeability

DrückePress Durchflußmenge in Liter je StundeFlow rate in liters per hour 20 g
40 g 20 g
40 g 6,4
10,76.4
10.7

Claims (3)

Patentansprüche:Patent claims: 1. Verfahren zur Herstellung makroporigen glasigen Kohlenstoffs, dadurch gekennzeichnet, daß zunächst ein makroporiger1. A process for the production of macroporous vitreous carbon, characterized in that that initially a macroporous 609 567/484609 567/484 Träger mittels eines durch Wärme härtbaren Harzes imprägniert wird, sodann der imprägnierte Träger in inerter Atmosphäre bei 1200° C karbonisiert und hierbei der Träger zersetzt und gleichzeitig das die Struktur des Trägers besitzende Imprägniermittel verkohlt wird und daß schließlich eine Graphitbehandlung und/oder Reinigung erfolgt.Carrier is impregnated by means of a thermosetting resin, then the impregnated Carrier is carbonized in an inert atmosphere at 1200 ° C and the carrier is decomposed and at the same time the impregnating agent having the structure of the support is carbonized and that finally a graphite treatment and / or cleaning takes place. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Träger eine Schaummasse aus Polyurethan verwendet wird.2. The method according to claim 1, characterized in that a foam mass is used as the carrier made of polyurethane is used. 3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß das durch Wärme härtbare Harz, das der Imprägnierung dient und in glasigen Kohlenstoff umwandelbar ist, aus der Gruppe der Furan- und Phenolharze gewählt wird.3. The method according to claim 1 and 2, characterized in that the curable by heat Resin, which is used for impregnation and can be converted into glassy carbon, from the group furan and phenolic resins are chosen.
DES94543A 1963-12-13 1964-12-09 Process for the production of macroporous glassy carbon Pending DE1216174B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR957094A FR1388818A (en) 1963-12-13 1963-12-13 Macroporous glassy carbon

Publications (1)

Publication Number Publication Date
DE1216174B true DE1216174B (en) 1966-05-05

Family

ID=8818793

Family Applications (1)

Application Number Title Priority Date Filing Date
DES94543A Pending DE1216174B (en) 1963-12-13 1964-12-09 Process for the production of macroporous glassy carbon

Country Status (3)

Country Link
DE (1) DE1216174B (en)
FR (1) FR1388818A (en)
GB (1) GB1031126A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0204013A1 (en) * 1985-06-01 1986-12-10 SIGRI GmbH Process for producing vitreons carbon articles with a foam-type structure

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4067956A (en) * 1976-10-08 1978-01-10 Chemotronics International, Inc. Reticulated anisotropic porous vitreous carbon
US4417872A (en) 1982-02-01 1983-11-29 Energy Research Corporation Heat treating
DE3323801A1 (en) * 1983-07-01 1985-01-03 C. Conradty Nürnberg GmbH & Co KG, 8505 Röthenbach METHOD FOR PRODUCING A SHOOTABLE CARBON MATERIAL
DE8413711U1 (en) * 1984-05-05 1985-08-29 Philips Patentverwaltung Gmbh, 2000 Hamburg Sample carrier for flameless atomic absorption and emission spectroscopy
CA1291110C (en) * 1985-11-18 1991-10-22 Christopher John Carruthers Edwards Porous carbon structures and methods for their preparation
JP2003128475A (en) * 2001-10-18 2003-05-08 Mitsubishi Pencil Co Ltd Carbonaceous, porous body and its manufacturing method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0204013A1 (en) * 1985-06-01 1986-12-10 SIGRI GmbH Process for producing vitreons carbon articles with a foam-type structure

Also Published As

Publication number Publication date
FR1388818A (en) 1965-02-12
GB1031126A (en) 1966-05-25

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