DE2027132A1 - - Google Patents

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Publication number
DE2027132A1
DE2027132A1 DE19702027132 DE2027132A DE2027132A1 DE 2027132 A1 DE2027132 A1 DE 2027132A1 DE 19702027132 DE19702027132 DE 19702027132 DE 2027132 A DE2027132 A DE 2027132A DE 2027132 A1 DE2027132 A1 DE 2027132A1
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Germany
Prior art keywords
felts
exposed
compressive stresses
density
thickness
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
DE19702027132
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German (de)
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.)
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Publication date
Application filed filed Critical
Priority to DE19702027132 priority Critical patent/DE2027132A1/de
Priority to FR7117580A priority patent/FR2095578A5/en
Publication of DE2027132A1 publication Critical patent/DE2027132A1/de
Pending legal-status Critical Current

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Classifications

    • 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
    • D01F9/26—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 polyesters
    • 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
    • D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
    • 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
    • D01F9/18—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from proteins, e.g. from wool
    • 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
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles

Description

Verfahren zur Herstellung von Kohlenstoff- und GraphitfilzProcess for the production of carbon and graphite felt

Die Erfindung betrifft ein Verfahren zur"Herstellung von dünnen Kohlenstoff- und Graphitfilzen durch kontinuierliches oder stufenweises Erhitzen von Filzen aus polymeren Kunststoffen oder natürlichen Fasern in inerter oder reduzierender Atmosphäre.The invention relates to a method of "manufacturing of thin carbon and graphite felts by continuously or stepwise heating of Felts made of polymer plastics or natural fibers in an inert or reducing atmosphere.

Als Ausgangsmaterialien für die Herstellung von Kohlenstoff- und Graphitfilzen sind zahlreiche natürliche und künstliche Faserstoffe, wie z.B. Wolle, Zellwolle, Polyacrylnitril und Polyester, bekanntgeworden. Die in Form von gewalkten oder genadelten Filzen vorliegenden Ausgangsmaterialien werden einer Pyrolyse unterworfen, wobei zunächst durch Zyklisierungs- und Dehydrierungsreaktionen vernetzte Molekülanordnungen entstehen. Der ersten Pyrolysestufe im Temperaturbereich zwischen etwa 80 bis 3000C folgt eine Karbonisierungsstufe, die bis etwa 1000 bis 12000C reicht, und durch weiteres Erhitzen bis auf etwa 30000C kann der karbonisierte Filz in Graphit umgewandelt werden. Die Temperaturbehandlung erfolgt kontinuierlich oder stufenweise.Numerous natural and synthetic fiber materials, such as wool, rayon, polyacrylonitrile and polyester, have become known as starting materials for the production of carbon and graphite felts. The starting materials in the form of felted or needled felts are subjected to pyrolysis, whereby initially crosslinked molecular arrangements result from cyclization and dehydrogenation reactions. The first pyrolysis stage in the temperature range between approximately 80 to 300 ° C. is followed by a carbonization stage that extends up to approximately 1000 to 1200 ° C., and the carbonized felt can be converted into graphite by further heating up to approximately 3000 ° C. The temperature treatment takes place continuously or in stages.

Kohlenstoff-und Graphitfilze werden u.a. als Elektroden oder Katalysatorträger in Akkumulatoren oder Brennstoffzellen und im Verbund mit Kunstharzen zur Auskleidung von chemischen Apparaten und Armaturen verwendet. Wegen des geringen Volumenbedarfs sindCarbon and graphite felts are used, among other things, as electrodes or catalyst carriers in accumulators or fuel cells and in combination with synthetic resins used for lining chemical apparatus and fittings. Because of the low volume requirements

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— 2 —- 2 -

BAD ORIGINALBATH ORIGINAL

für diese Anwendungen dünne Filze besonders geeignet. Filze, besonders genadelte Filze, mit einer Dicke kleiner als 3 mm sind nicht in gleichförmiger Qualität herstellbar. Im allgemeinen sind die in einer Filzbahn vorhandenen Dichteunterschiede um so größer, je dünner der Filz ist. Die Dichteunterschiede bleiben auch nach der Karbonisierung und Graphitierung von Filzen erhalten, so daß diese Produkte wegen der daraus folgenden unterschiedlichen Wärmeleitfähigkeiten nur sehr begrenzt verwendbar sind.thin felts are particularly suitable for these applications. Felts, especially needled felts, with a thickness less than 3 mm cannot be produced in a uniform quality. Generally they are in a felt sheet The thinner the felt, the greater the differences in density. The density differences also remain obtained after carbonization and graphitization of felts, so that these products because of it The following different thermal conductivities can only be used to a very limited extent.

Der Erfindung liegt die Aufgabe zugrunde, dünne Kohlenstoff- und Graphitfilze herzustellen, die diese Nachteile nicht aufweisen und deren Dichte konstant ist.The invention has for its object to produce thin carbon and graphite felts that do not have these disadvantages and their density is constant.

Die Aufgabe nach der Erfindung wird dadurch gelöst, daß dicke Ausgangsfilze während der Temperaturbehandlung unter Druckspannungen gehalten werden. Nach der Erfindung beträgt die angelegte Druck—The object according to the invention is achieved in that thick starting felts during the temperature treatment be held under compressive stresses. According to the invention, the applied pressure is

spannung mindestens 10 kp/cm .tension at least 10 kp / cm.

Nach einer Ausgestaltung der Erfindung werden Filze mindestens in einem Abschnitt der Temperaturbehandlung Druckspannungen ausgesetzt. Gemäß der Erfindung ist es vorteilhaft, Filze in einem Abschnitt der Temperaturbehandlung, also im Bereich der Zyklisierungs- und Dehydrierüngsreaktionen oder im Karbo— nisierungs- oder Graphiterungsbereich Druckspannungen auszusetzen. Nach der Erfindung sind TemperaturenAccording to one embodiment of the invention, felts are exposed to compressive stresses at least in one section of the temperature treatment. According to the invention, it is advantageous to subject felts to compressive stresses in a section of the temperature treatment, that is to say in the area of the cyclization and dehydrogenation reactions or in the carbonization or graphitization area. According to the invention are temperatures

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BAD ORIGINALBATH ORIGINAL

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zwischen 200 und 3000C, zwischen 300 und 10000C
und zwischen 1000 und 3000°C vorteilhaft.between 200 and 300 0 C, between 300 and 1000 0 C
and between 1000 and 3000 ° C advantageous.

Die Erfindung beruht auf der Erkenntnis, daß bei der Anlegung einer Druckspannung während der
thermischen Behandlung von Filzen die Schrumpfung der Filze senkrecht zur Spannungsrichtung vermindert wird. Da die Volumenschrumpfung praktisch
unverändert bleibt, nimmt entsprechend die Dicke der Filze ab.The invention is based on the knowledge that when applying a compressive stress during the
thermal treatment of felts reduces the shrinkage of the felts perpendicular to the direction of tension. Because the volume shrinkage practical
remains unchanged, the thickness of the felts decreases accordingly.

Die Vorteile des erfindungsgemäßen Verfahrens bestehen insbesondere in der Herstellung von Kohlenstoff- und Graphitfilzen geringer Dicke und gleichmäßiger Dichte. Ein weiterer Vorteil des erfindungsgemäßen Verfahrens ist die Verdichtung des Filzes, wodurch die V7ärmeleitfähigkeit, die besonders für als Auskleidungen von chemischen Apparaten verwendete Filze vorteilhaft ist, erhöht wird.The advantages of the method according to the invention consist in particular in the production of carbon and graphite felts of small thickness and uniform density. Another advantage of the invention The process is the compression of the felt, whereby the thermal conductivity, which is particularly useful for as Felts used in linings of chemical apparatus is advantageous.

Die Erfindung wird in den folgenden Ausführungsbeispielen näher erläutert.The invention is embodied in the following working examples explained in more detail.

Beispiel 1example 1

Filze aus Zellulose, Polyacrylnitril und Wolle wurden auf 3000C erhitzt, wobei die Aufheizgeschwindigkeit bis 2000C 50°C/h und zwischen 200 und 3000C 12°C/h betrug. Die Filze wurden dann in einem elektrisch beheizten Ofen unter Luftabschluß auf 1000°C erhitzt. Die Aufheizgeschwindigkeit betrug 5 C/h bis 650 und 15°C/h von 650 bis 10000C. Die Filzbahnen, deren Dickei etwa 5 mm betrucpn,wurden während der Karbonisierungsphase mit Graphitplatten verschiedenen Ge-Felts of cellulose, polyacrylonitrile and wool were heated to 300 0 C, the heating rate was up to 200 0 C 50 ° C / h between 200 and 300 0 C 12 ° C / h. The felts were then heated to 1000 ° C. in an electrically heated oven with the exclusion of air. The heating rate was 5 C / h to 650 and 15 ° C / h from 650 to 1000 0 C. The felts whose Dickei betrucpn about 5 mm, were different during the overall Karbonisierungsphase with graphite plates

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BAD ORIGINALBATH ORIGINAL

1 098B0/07951 098B0 / 0795

wichtes belastet. Die erzielten Änderungen der Dicke sind der' Tabelle I zu entnehmen.weight burdened. The changes in thickness achieved are shown in Table I.

Tabelle ITable I.

Beispiel 2Example 2 Zellu
loseZellu
loose Polyacryl
nitrilPolyacrylic
nitrile WolleWool AusgangsmaterialSource material 5,05.0 5,25.2 5,55.5 Dicke (mm)Thickness (mm) 0,130.13 0,0 70.0 7 0,180.18 Dichte (g/cm )Density (g / cm) Kohlenstoff-FilzCarbon felt 2,82.8 4,34.3 3,53.5 2
Dicke (mm) P=O p/cm2
Thickness (mm) P = O p / cm 1,61.6 3,33.3 2,52.5 10 "10 " 1,11.1 2,52.5 1,81.8 50· »50 · » 1,01.0 1,81.8 1,31.3 200 ··200 ·· 0,090.09 0,070.07 0,160.16 Dichte (g/cm3) P=O p/cm2 Density (g / cm 3 ) P = O p / cm 2 0,110.11 0,090.09 0,180.18 10 "10 " 0,140.14 0,110.11 0,220.22 50 "50 " 0,160.16 0,160.16 0,280.28 200 "200 "

20 cm breite Filzstreifen wurden wie in Beispiel 1 auf 3000C erhitzt und dann mit einer Geschwindigkeit von 4 m/h durch einen Ofen gezogen, wobei die Aufheizgeschwindigkeit zwischen 300 und 500°C ca. 3000°C/h und zwischen 500 und 10QO0C ca. 6000°C/h betrug. Der Ofen wies in Temperaturbereichen um 350 bzw. < 6000C zwei Rollenpaare auf, die eine Kraft von etwa 20 kp auf den Filz ausübten. Die Eigenschaften der erhaltenen Filze sind in der Tabelle II zusammengestellt. 20 cm wide strip of felt were heated as in Example 1 at 300 0 C and then drawn at a speed of 4 m / h through an oven wherein the heating rate between 300 and 500 ° C 3000 ° C / h between 500 and 10QO 0 C was approx. 6000 ° C / h. The oven had two pairs of rollers in temperature ranges around 350 and < 600 ° C., which exerted a force of about 20 kp on the felt. The properties of the felts obtained are summarized in Table II.

• ■ BAU ORIGINAL'• ■ BAU ORIGINAL '

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Tabelle IITable II

Zellu
loseZellu
loose Polyacryl
nitrilPolyacrylic
nitrile WolleWool AusgangsmaterialSource material ohne Pressungwithout pressing 2,72.7 4,14.1 3,33.3 Dicke (mm)Thickness (mm) 0,080.08 0,070.07 0,160.16 Dichte (g/cm )Density (g / cm) mit Pressungwith pressing 1,11.1 ■ 1,6■ 1.6 1,11.1 Dicke (mm)Thickness (mm) 0,150.15 0,170.17 0,300.30 Dichte (g/cm )Density (g / cm) Beispiel 3Example 3

Ein Zellulosefilz mit einer Dicke von 5,2 mm und einer Dichte von 0,14 g/cm wurde wie in Beispiel 1 auf 300 erhitzt und dabei durch Graphitplatten mit einem DruckA cellulose felt with a thickness of 5.2 mm and one Density of 0.14 g / cm was heated to 300 as in Example 1 and thereby through graphite plates with a pressure

2
von 100 p/cm belastet. Die Dicke des ohne weitere Belastung karbonisierten Kohlenstoff-Filzes betrug nur 0,9 mm gegenüber 2,9 mm eines ohne Druckspannungen erhitzten Filzes, die Dichte war 0,19 bzw. 0,09 g/cm- .2
loaded by 100 p / cm. The thickness of the carbon felt carbonized without further loading was only 0.9 mm compared to 2.9 mm of a felt heated without compressive stresses, the density was 0.19 or 0.09 g / cm-.

Beispiel 4Example 4

Ohne mechanische Belastung hergestellte Kohlenstoff-Filze wurden in einem Graphitierungsöfen bis auf 28000C erhitzt und dabei durch Graphitplatten mitCarbon felts produced without mechanical stress were heated in a graphitizing furnace up to 2800 ° C. and in the process by means of graphite plates

einem Druck von 100 p/cm belastet. Die Ergebnisse gibt die Tabelle III wieder.loaded with a pressure of 100 p / cm. The results are shown in Table III.

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Tabelle IIITable III Zellu
loseZellu
loose Polyacryl
nitrilPolyacrylic
nitrile WolleWool AusgangsmaterialSource material 2,62.6 4,04.0 3,53.5 drucklos graphitiertgraphitized without pressure 0,090.09 0,080.08 0,14 .0.14. Dicke (mm)Thickness (mm) Dichte (g/cm )Density (g / cm) unter Druck graphiunder pressure graphi 0,60.6 1,51.5 1,41.4 tiertanimals 0,350.35 0,210.21 0,320.32 Dicke (mm)Thickness (mm) Dichte (g/cm )Density (g / cm)

6 Patentansprüche PA 9/12/70 Dr. We/ost6 patent claims PA 9/12/70 Dr. We / ost

109850/0795109850/0795

Claims (6)

PatentansprücheClaims Verfahren zur Herstellung von dünnen Kohienstoff- und Graphitriizer. durch stufenweises oder kontinuierliches Erhitzen von Filzen aus polymeren Kunststoffen oder natürlichen Fasern in inerter oder reduzierender Atmosphäre,dadurch ge- ■ ■ kennzeichnet ,"daß die Filze während der Temperaturbehandlung unter Druckspannung gehalten werden.Process for the production of thin carbon and graphitriizer. by gradual or continuous Heating of felts made of polymeric plastics or natural fibers in an inert or reducing atmosphere, thereby reducing ■ ■ indicates "that the felts during the temperature treatment are kept under compressive stress. 2. Verfahren nach Anspruch 1, dadurch g e k e η η zeichnet , daß die angelegten Druckspannun-2. The method according to claim 1, characterized in that g e k e η η that the applied compressive stress gen mindestens 10 p/cm betragen.at least 10 p / cm. 3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet , daß Filze in einem Abschnitt der Temperaturbehandlung Druckspannungen ausgesetzt sind.3. The method according to claim 1 and 2, characterized in that felts in one Section of the temperature treatment are exposed to compressive stresses. 4. Verfahren nach Anspruch 1 bis 3, dadurch g e kennzeichnet , daß Filze zwischen 200 und 300° Druckspannungen ausgesetzt werden.■4. The method according to claim 1 to 3, characterized g e indicates that felts are exposed to compressive stresses between 200 and 300 ° 5. Verfahren nach Anspruch 1 bis 3, dadurch g e k ennzeichnet , daß Filze zwischen 300 und 10000C Druckspannungen ausgesetzt werden.5. The method according to claim 1 to 3, characterized in that felts between 300 and 1000 0 C are exposed to compressive stresses. 6. Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß Filze zwischen 1000 und 30000C Druckspannungen ausgesetzt werden6. The method according to claim 1 to 3, characterized in that felts between 1000 and 3000 0 C are exposed to compressive stresses BAD ORiGiNALBAD ORiGiNAL PA 9/12/70 Dr. We/ostPA 9/12/70 Dr. We / ost 109850/0795109850/0795
DE19702027132 1970-06-03 1970-06-03 Pending DE2027132A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE19702027132 DE2027132A1 (en) 1970-06-03 1970-06-03
FR7117580A FR2095578A5 (en) 1970-06-03 1971-05-14 Graphitc carbon felt prodn - esp needle felt prodn - by heating natural or synthetic fibres in carbonizing atmosphere

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19702027132 DE2027132A1 (en) 1970-06-03 1970-06-03

Publications (1)

Publication Number Publication Date
DE2027132A1 true DE2027132A1 (en) 1971-12-09

Family

ID=5772853

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19702027132 Pending DE2027132A1 (en) 1970-06-03 1970-06-03

Country Status (2)

Country Link
DE (1) DE2027132A1 (en)
FR (1) FR2095578A5 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2749061A1 (en) * 1976-11-03 1978-05-18 Courtaulds Ltd COMPOSITE MATERIAL
DE2900938A1 (en) * 1978-01-12 1979-07-19 Dunlop Ltd PROCESS FOR PRODUCING NON-WOVEN FABRIC SUBSTRATES FOR COMPOSITE STRUCTURES REINFORCED WITH CARBON FIBERS
DE19543795A1 (en) * 1995-11-24 1997-05-28 Temic Bayern Chem Airbag Gmbh Gas generator for vehicular airbag system

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2749061A1 (en) * 1976-11-03 1978-05-18 Courtaulds Ltd COMPOSITE MATERIAL
DE2900938A1 (en) * 1978-01-12 1979-07-19 Dunlop Ltd PROCESS FOR PRODUCING NON-WOVEN FABRIC SUBSTRATES FOR COMPOSITE STRUCTURES REINFORCED WITH CARBON FIBERS
DE19543795A1 (en) * 1995-11-24 1997-05-28 Temic Bayern Chem Airbag Gmbh Gas generator for vehicular airbag system
DE19543795B4 (en) * 1995-11-24 2005-03-24 Temic Bayern-Chemie Airbag Gmbh Pyrotechnic gas generator

Also Published As

Publication number Publication date
FR2095578A5 (en) 1972-02-11

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