US3297405A - Method of carbonizing animal fiber materials - Google Patents

Method of carbonizing animal fiber materials Download PDF

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Publication number
US3297405A
US3297405A US413679A US41367964A US3297405A US 3297405 A US3297405 A US 3297405A US 413679 A US413679 A US 413679A US 41367964 A US41367964 A US 41367964A US 3297405 A US3297405 A US 3297405A
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United States
Prior art keywords
air
carbonizing
animal fiber
wool
during
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
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US413679A
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English (en)
Inventor
Sperk Edgar
Vohler Otto
Jeitner Franz
Gierth Volker
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Siemens Plania Werke AG
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Siemens Plania Werke AG
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Classifications

    • 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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • 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
    • D01F9/32—Apparatus therefor
    • D01F9/326—Apparatus therefor for manufacturing filaments from proteins
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L59/00—Thermal insulation in general
    • F16L59/04—Arrangements using dry fillers, e.g. using slag wool
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/48—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances fibrous materials
    • H01B3/485—Other fibrous materials fabric
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
    • Y10S264/19—Inorganic fiber
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/30—Self-sustaining carbon mass or layer with impregnant or other layer

Definitions

  • Our invention relates to a method of carbonizing or partially carbonizing a wool-containing material
  • ⁇ vool being herein used to designate sheep wool as well as other fibrous substance of animal origin.
  • a fiber preserving substance such as formaldehyde, ammonia. carbon dioxide or mixtures thereof may be applied to the wool-containing material during the carbonizing process.
  • this graduated process is performed in air up to about 200 C. with a temperature increase of to 50 C. per hour, then up to about 300 C. with a reduced air supply at a rate of l to 10 C. per hour, and thereafter concluded up to about 1000 C. under air exclusion at a rate of 10 to 100 C. per hour.
  • Products. made according to the invention can also be employed for all other purposes of carbon and graphite materials.
  • the field of application, heretofore often limited by lack of flexibility or pliability, is considerably widened.
  • FIGS. 1, 2 and 3 are respective flow sheets relating to different embodiments of the process according to the invention.
  • FIG.'4 shows in section a vacuum furnace equipped with a heater and with insulating structure, both consisting of material produced according to the invention.
  • Example 1 A piece of a soft, 8 mm. thick wool felt of about 500 x 600 mm., spread fiat, is placed into a dryer cabinet having a venting outlet.
  • the dryer cabinet is first heated up to 240 C., the increase in temperature being about 10 C. per hour. Thereafter the cabinet is further heated up to 300 C. but at a slower rate, namely at a temperature increase of 5 C. per hour.
  • an amount of 500 g. ammonium carbonate is each time placed into the cabinet beneath the piece of wool felt.
  • the ammonium compound converts to a gas mixture of ammonia and carbon dioxide having a partial pressure varying between about 5 and 760 torr (mm/Hg).
  • the smoke gases evolving during the thermal treatment of the wool felt are continuously exhausted through the venting outlet.
  • the already partially carbonized wool felt is taken out of the dryer cabinet, embedded in carbon powder (soot or aquadag) within a graphite casing, andthcn heated in a shaft furnace up to about 1000 C. At first the temperature is increased only slowly. Commencing with 300 C. the
  • the specimen was found to have shrunk to about 470 x 360 mm. However, the originalfiber structure was clearly recognizable. The elasticity was preserved to such an extent that the specimen could be wound upon a round rod of about 20 mm. diameter.
  • the electrical resistance value measured perpendicularly to the surface of the specimen, was 8 to 11-10 ohm mm. /m.; measured in the direction of the web, the resistance was 5 to 1010, ohm mmF/m.
  • the coetficient of thermal conductance was lower than 10- kcaL/m. hour C.
  • Example 2 50 g. raw shorn (virgin) wool are kept for three hours at 85 C. in an aqueous solution of 6% formaldehyde and 2% sodium bisulfite and then well washed and dried at room temperature.
  • the wool thus treated is placed into a tubular furnace and heated at a temperature increasing 15 C. per hour up to 200 C. During heating, a current of air is sucked through the wool at a rate of about 21 liters per minute. Thereafter the increase in temperature is reduced to 3 C. per hour and the air How to 0.1 liter per minute. After reaching a temperature of 300 C., the wool is taken out of the furnace and further processed as described in Example 1.
  • the carbonized ultimate product obtained by this process exhibited the fiber structure of the original virgin wool.
  • the elasticity or pliability of the starting material was largely preserved.
  • the carbonized product could be twisted to threads of yarn.
  • Example 3 A specimen web of 100 x 500 mm. size woven from wool carded yarn and consisting of 80% of pure shorn sheep wool, was placed upon a tunnel-shaped insert into a dryer cabinet and then heated ata temperature increasing 20 C. per hour up to 200 C., then at the rate of 7 C. per hour up to 300 C. During this heat treatment. when the temperature of 240 C. was reached, ammonia gas was introduced into the dryer cabinet at a partial pressure between 50 and 200 torr. The ammonia gas atmosphere was maintained until the temperature of 300 C. was reached.
  • the further processing corresponded to the one described in Example 1.
  • the ultimate exhibited good tear strength and was elastic.
  • Its square" resistance that is the resistance value of a square of any edge length, was ohm.
  • thissquare resistance was reduced to 1 ohm.
  • Graphitized material thus produced is particularly well applicable as a heating conductor, preferably in tape form, as well as for various other purposes.
  • the sulphur content of the latter specimen was analized prior to, and after, the thermal treatment. It was found that the sulphur content of the starting material was 3.03% by weight and had declined to 2.28% after the thermal treatment. This slight reduction in sulphur content is still negligible as regards preservation of elasticity or pliability of the ultimate material.
  • the starting material for example wool felt, wool fabric or raw animal wool
  • a reduction agent such as sodium bisulfite
  • the material is heated with access of air to a temperature of 200 C. at a rate of 5 to 50 C./hour, and the evolving vapors and gases are continuously withdrawn.
  • the material is further heated with a reduced ingress of air, up to 300 C. at a rate of 1 to 10 C./hour, the evolving waste gases being likewise withdrawn continuously.
  • the further heating up to 1000". C. is applied at-a rate of 10 to 100 C./hour under exclusion of air.
  • the starting material is first heated up to 3000 4 C. in the manner described above with reference to FIG. 1.
  • a substance or mixture such as formaldehyde, ammonia and/or carbon dioxide, in gaseous constitution is supplied, resulting in a partial pressure of these gases between about 5 and 760 torr.
  • the subsequent heating up to 100 C. corresponds to the processing stage described above with reference to FIG. 1.
  • the thermal treatment is carried out in the same manner as described in the foregoing, except that an ammonia compound or a mixture of ammonium compounds is directly added during the heating period between 200 and 300 C. for the purpose of supplying ammonia and, as the case may be, also carbon dioxide.
  • the material resulting from the processes exemplified by FIGS. 1, 2 and 3 may be additionally subjected to graphitizing under exclusion of air in the known manner at temperatures up to 3000 C.
  • the vacuum furnace illustrated in FIG. 4 represents an example in which animal fiber material processed according to the invention-is employed for two different purposes.
  • the furnace comprises a vacuum-tight jacket 1 of sheet metal which surrounds a cylindrical heater body composed of a ceramic carrier tube 2 and a helical conductor tape'3 mounted on the outer cylindrical surface of the ceramic tube 2.
  • the conductor tape 3 consists of a fabric processed according to the invention and graphitized at temperatures up to about 2700 C.
  • the fiber structure and the pliability of the fibrous material are preserved in the tape so that it could be wound about the ceramic tube 2.
  • the resistance value of the tape 3 was reduced during the graphitizing process to such an extent that the graphitized material became suitable and advantageous for use as a heating resistor.
  • Shoved over the heater body 2, 3 is a cylindrical tube 4 of graphite which is heat insulated by a surrounding material 5 constituted by several concentric layers.
  • This insulating material 5 consists of carbonized wool felt made by a method according to the invention.
  • the ceramic tube is closed at both ends by respective ring-shaped cover plates 60 and 6/).
  • the end of a cy lindrical duct 7a, 7b is joined with each ring-shaped cover plate, The other end of each duct passes through the wall of the vacuum-tight jacket 1 and is heat-insulated therefrom by an insulating sealing member of annular shape.
  • the cylindrical conduits 7a and 7b thus form a connection between the interior of the ceramic tube 2 and the vicinity of the furnace and may be used for supplying and removing of the material to be heated in the furnace.
  • a free space remains between the vacuum-tight jacket 1 and the heater body of the furnace. During operation of the furnace the heat transfer through this interspace can be reduced. by evacuating it through a nipple 8 of jacket 1.
  • the process of carbonizing animal fiber material which comprises subjecting the ainmal fiber material to carbonizing heat treatment in several consecutive stages of gradually increasing temperature up to about 1000 C., permitting access of air to the material during the first stage, and reducing such access during the subsequent stages down to exclusion of air in the last stage, whereby the resulting carbonized material substantially retains mechanical fiber characteristics of the starting material.
  • the process of carbonizing animal fiber material which comprises heating the animal fiber material at a gradually increasing temperature up to about 1000" C., and applying to the material during the heating period at least one substance from the group consisting of formaldehyde, ammonia, carbon dioxide and mixtures thereof,
  • the process of'carbonizing animal fiber material which comprises subjecting the animal -fiber material to carbonizing heat treatment in several consecutive stages of gradually increasing temperature up to about 1000 C., permitting access of air to the material during the first stage, reducing such access during the subsequent stages down to exclusion of air in the last-stage, and applying to the material during the heat treatment at least one substance from the group consisting of formaldehyde, ammonia, carbon dioxide and mixtures thereof.
  • the process which comprises applying to the material during heating at a temperature above 200 C. at least one gaseous substance from the group consisting of formaldehyde, ammonia, carbon dioxide and mixtures thereof.
  • the process of carbonizing animal fiber material which comprises immersing the animal fiber material in an aqueous solution of formaldehyde, drying the material, then subjecting the dried material to carbonizing heat treatment in several consecutive stages of gradually increasing temperature up to about 1000 C., permitting access of air to the material duringthe first stage, and reducing such access during the subsequent'stages down to exclusion of air in the last stage.
  • the process of carbonizing animal fiber material which comprises heating the animal fiber material at a gradually increasing temperature up to about 1000 C., applying to the material during the heating period at least one substance from the group consisting of formaldehyde,
  • ammonia, carbon dioxide and mixtures thereof and thereafter graphitizing the material under exclusion of air at temperatures above 1000 C., up to about 3000 C.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Inorganic Fibers (AREA)
  • Carbon And Carbon Compounds (AREA)
US413679A 1963-11-21 1964-11-23 Method of carbonizing animal fiber materials Expired - Lifetime US3297405A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES88377A DE1255629B (de) 1963-11-21 1963-11-21 Verfahren zur Herstellung von Fasermaterial aus Kohlenstoff oder Graphit

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US (1) US3297405A (de)
BE (1) BE656133A (de)
CH (1) CH469643A (de)
DE (1) DE1255629B (de)
GB (1) GB1089534A (de)
SE (1) SE308908B (de)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3509400A (en) * 1966-05-17 1970-04-28 Sigri Elektrographit Gmbh Commutator carbon brush and method of its manufacture
US3619139A (en) * 1968-02-02 1971-11-09 Morganite Research & Dev Ltd Manufacture of carbon filaments
US3639140A (en) * 1968-10-12 1972-02-01 Nitto Boseki Co Ltd Process for carbonized cellulose fiber or the products thereof
US3661616A (en) * 1968-11-06 1972-05-09 Notto Boseki Co Ltd Process for carbonizing cellulose fiber or the products thereof
US3716332A (en) * 1970-07-27 1973-02-13 Ducommun Inc Carbonization of wool
US3913309A (en) * 1970-03-17 1975-10-21 Nereo Chiarotto Fibrous composition of matter
WO2006082259A1 (es) * 2005-02-21 2006-08-10 Instituto De Monocristales, S.L. Diamante sintético de distintos colores personalizado a partir de queratina humana o animal (vivo o muerto). procedimiento para su fabricación
US20100074830A1 (en) * 2006-12-15 2010-03-25 Spuehler Markus Individualized jewellery alloys and method for their production

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030017932A1 (en) * 2001-07-17 2003-01-23 Vandenbiesen Russell P. Method for making synthetic gems comprising elements recovered from complete or partial human or animal remains and the product thereof
DE102011115461A1 (de) * 2011-10-10 2013-04-11 TÜV SÜD Aktiengesellschaft Rohrleitung
DE102013101168B4 (de) * 2013-02-06 2017-01-26 Fachhochschule Schmalkalden Faser und Verfahren zu deren Herstellung
CN109913980A (zh) * 2019-02-25 2019-06-21 南开大学 一种杂原子掺杂柔性碳纤维及其制备方法和应用

Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE20028C (de) * KREUSCH & EMONDS in Dolhain bei Verviers, Belgien Verfahren und Einrichtungen zum Verkohlen von Pflanzenstoffen in Wollen, Abfällen, Lumpen u. dgl
US1895263A (en) * 1928-12-29 1933-01-24 Firm M Rudolf Jahr Method for carbonizing woolen fabrics
US2799912A (en) * 1950-12-18 1957-07-23 Greger Herbert Hans Processes for forming high temperature ceramic articles
US3011981A (en) * 1958-04-21 1961-12-05 Soltes William Timot Electrically conducting fibrous carbon
GB894458A (en) * 1958-12-18 1962-04-18 Union Carbide Corp Improvements in and relating to carbonisation
US3104159A (en) * 1958-11-21 1963-09-17 Gen Electric Co Ltd Production of graphite
US3107152A (en) * 1960-09-12 1963-10-15 Union Carbide Corp Fibrous graphite
GB942186A (en) * 1959-07-02 1963-11-20 Secr Aviation Fibrous carbon articles
US3116975A (en) * 1961-02-08 1964-01-07 Union Carbide Corp Artificial graphite process
US3125404A (en) * 1964-03-17 Tensile strength
US3174895A (en) * 1960-09-07 1965-03-23 Union Carbide Corp Graphite cloth laminates
US3179605A (en) * 1962-10-12 1965-04-20 Haveg Industries Inc Manufacture of carbon cloth
US3235323A (en) * 1960-04-14 1966-02-15 Minnesota Mining & Mfg Heat-resistant black fibers and fabrics derived from rayon

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3125404A (en) * 1964-03-17 Tensile strength
DE20028C (de) * KREUSCH & EMONDS in Dolhain bei Verviers, Belgien Verfahren und Einrichtungen zum Verkohlen von Pflanzenstoffen in Wollen, Abfällen, Lumpen u. dgl
US1895263A (en) * 1928-12-29 1933-01-24 Firm M Rudolf Jahr Method for carbonizing woolen fabrics
US2799912A (en) * 1950-12-18 1957-07-23 Greger Herbert Hans Processes for forming high temperature ceramic articles
US3011981A (en) * 1958-04-21 1961-12-05 Soltes William Timot Electrically conducting fibrous carbon
US3104159A (en) * 1958-11-21 1963-09-17 Gen Electric Co Ltd Production of graphite
GB894458A (en) * 1958-12-18 1962-04-18 Union Carbide Corp Improvements in and relating to carbonisation
GB942186A (en) * 1959-07-02 1963-11-20 Secr Aviation Fibrous carbon articles
US3235323A (en) * 1960-04-14 1966-02-15 Minnesota Mining & Mfg Heat-resistant black fibers and fabrics derived from rayon
US3174895A (en) * 1960-09-07 1965-03-23 Union Carbide Corp Graphite cloth laminates
US3107152A (en) * 1960-09-12 1963-10-15 Union Carbide Corp Fibrous graphite
US3116975A (en) * 1961-02-08 1964-01-07 Union Carbide Corp Artificial graphite process
US3179605A (en) * 1962-10-12 1965-04-20 Haveg Industries Inc Manufacture of carbon cloth

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3509400A (en) * 1966-05-17 1970-04-28 Sigri Elektrographit Gmbh Commutator carbon brush and method of its manufacture
US3619139A (en) * 1968-02-02 1971-11-09 Morganite Research & Dev Ltd Manufacture of carbon filaments
US3639140A (en) * 1968-10-12 1972-02-01 Nitto Boseki Co Ltd Process for carbonized cellulose fiber or the products thereof
US3661616A (en) * 1968-11-06 1972-05-09 Notto Boseki Co Ltd Process for carbonizing cellulose fiber or the products thereof
US3913309A (en) * 1970-03-17 1975-10-21 Nereo Chiarotto Fibrous composition of matter
US3716332A (en) * 1970-07-27 1973-02-13 Ducommun Inc Carbonization of wool
WO2006082259A1 (es) * 2005-02-21 2006-08-10 Instituto De Monocristales, S.L. Diamante sintético de distintos colores personalizado a partir de queratina humana o animal (vivo o muerto). procedimiento para su fabricación
ES2258921A1 (es) * 2005-02-21 2006-09-01 Instituto De Monocristales, S.L. Diamante sintetico de distintos colores personalizado a partir de queratina humana o animal (vivo o muerto). procedimiento para su fabricacion.
ES2258921B2 (es) * 2005-02-21 2007-04-01 Instituto De Monocristales, S.L. Diamante sintetico de distintos colores personalizado a partir de queratina humana o animal (vivo o muerto). procedimiento para su fabricacion.
US20080145299A1 (en) * 2005-02-21 2008-06-19 Instituto De Monocristales, L.S. Personalized Synthetic Diamond of Different Colours, Obtained From (Living or Dead) Human or Animal Keratin and Production Method Thereof
US20100074830A1 (en) * 2006-12-15 2010-03-25 Spuehler Markus Individualized jewellery alloys and method for their production
US8608867B2 (en) 2006-12-15 2013-12-17 Markus Spühler Individualized jewelery alloys and method for their production

Also Published As

Publication number Publication date
DE1255629B (de) 1967-12-07
CH469643A (de) 1969-03-15
BE656133A (de) 1965-05-24
SE308908B (de) 1969-03-03
GB1089534A (en) 1967-11-01

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