DE2012981A1 - Process for the surface treatment of thread-like material - Google Patents
Process for the surface treatment of thread-like materialInfo
- Publication number
- DE2012981A1 DE2012981A1 DE19702012981 DE2012981A DE2012981A1 DE 2012981 A1 DE2012981 A1 DE 2012981A1 DE 19702012981 DE19702012981 DE 19702012981 DE 2012981 A DE2012981 A DE 2012981A DE 2012981 A1 DE2012981 A1 DE 2012981A1
- Authority
- DE
- Germany
- Prior art keywords
- electrolyte
- fibers
- anode
- thread
- carbon
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims description 12
- 239000000463 material Substances 0.000 title description 5
- 238000004381 surface treatment Methods 0.000 title description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000003792 electrolyte Substances 0.000 claims description 7
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims description 3
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 2
- 239000000835 fiber Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000000243 solution Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- -1 hydroxyl ions Chemical class 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- 235000010716 Vigna mungo Nutrition 0.000 description 1
- 244000042295 Vigna mungo Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000002101 lytic effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/16—Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Reinforced Plastic Materials (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Description
P.Λ..?..6.^. r sib "P.Λ ..? .. 6. ^. r si b "
zu der Patentanmeldungto the patent application
der Firmaof the company
COtTRTAUIDS LIMITED
18, Hanover Square, London V. 1., EnglandCOtTRTAUIDS LIMITED
18, Hanover Square, London V. 1., England
betreffendconcerning
Materialmaterial
Die Erfindung bezieht eich auf die Oberfläohenbehandlung von fadenförmigem Material und insbesondere auf die Bearbeitung der Oberflache von fadenförmigem Kohlenetoff, um dessen Eigenschaften sam Einarbeiten in Matrizen eu verbessern. The invention relates to surface treatment of thread-like material and in particular on machining the surface of filiform carbon to improve its properties sam incorporation in matrices eu.
Fadenförmiger Kohlenstoff, insbesondere derjenige, der oaoh einem Verfahren hergestellt wird« bei dem eine Wärmebehandlung bei einer Temperatur höher als 1.50O0O angewendet wird, neigt dazu, eine glatte Oberfläche zu besitzen, die sich nicht so leicht mit einer Matrix verbindet. Sine bessere Bindefähigkeit kann erreicht werden, wenn man die Oberfläche in einem gewissen Umfang modifiziert» Die vorliegendeFilamentous carbon, especially the one that is prepared by a process oaoh "is higher in the heat treatment at a temperature applied as 1.50O 0 O, tends to have a smooth surface which does not bond easily with a matrix. Its better binding capacity can be achieved by modifying the surface to a certain extent »The present
009847/1714009847/1714
. BAD ORIGINAL. BATH ORIGINAL
fizierungsverfahren.fication procedure.
OβmaΒ der Erfindung besteht ein Verfahren sum Behandeln der Oberfläche von faden- bzw. faserförmlgem Kohlenstoff darin, daß man einen Elektrolyt in Form einer wäaerigen Lösung elekfcrolyaiert, wobei der fadenförmige Kohlenstoff an die Anode geschaltet 1st, fl0 dag natsierender Sauerstoff *n der Oborfläche dos faden -bzw. faserftSrmigen Materials erzeugt wird. Eine für das erfindungegemäße Verfahren geeignete wKsarlse Lösung enthält Hydroxylionen und besitzt eine solche Zusammensetzung, daß während der Elektrolyse, die trassierenden Sauerstoff erseugt, Hydroxylionen an der Anode entstehen. Su ist bekannt, da0 nioht «lit wässrigen Lösungen, die Hydroxylioaen enthalten, bei einer Elektrolyse naszlerenden Sauerstoff erzeugen, z.B. Lösungen, die ein anderes Anion enthalten, das vorzugsweise in Freiheit gesetzt wird· Sοlohe Löfungeo eignen sich fUr das exflndungsgemäde Verfahren nicht.OβmaΒ of the invention consists of a method to treat the surface of filamentary or fibrous carbon in that an electrolyte in the form of an aqueous solution is elekfcrolyaiert, the filamentary carbon is connected to the anode, while the nating oxygen flows into the surface of the surface -respectively. fibrous material is generated. A wKsarlse solution suitable for the process according to the invention contains hydroxyl ions and has a composition such that hydroxyl ions are formed at the anode during the electrolysis, which sucks in the passing oxygen. It is known that aqueous solutions which contain hydroxyl ions produce nascent oxygen during electrolysis, for example solutions which contain another anion, which is preferably released. Solvents such as these are not suitable for the method according to the invention.
PUr die Zwecke der Erfindung geeignete Eohlenstoffäden bzw. - fasern können hergestellt werden, indem man organisches fadenförmiges Material, wie Polyester, Polyamid, Cellulose oder vorzugsweise Polyaorylnitrilfädon bzw.-fasern verschiedenen Bedingungen hinsichtlich temperatur,Carbon filaments suitable for the purposes of the invention or fibers can be produced by using organic thread-like material, such as polyester, polyamide, cellulose or preferably polyaorylnitrilfädon or fibers different conditions in terms of temperature,
BAD ORIGiMALBATH ORIGiMAL
009847/17S4009847 / 17S4
Behandlungedauer und Umgebungsatmosphäre auasetzt. Im allgemeinen werden Rohlenstoffasern z.B. dadurch berge» stellt, daß man ein organieoheo faden- bzw. fassrfBrmiges Material In Luft oder einem anderen oxydierenden Qa· auf etwa 200 bio 3000C erhitzt und das Produkt bei einer Temperatur oberhalb von 10000C karbonisiert. Die resultierenden karbonisierten Fäden können weiter auf 150O0C und höher erhitzt werden« um «ine Graphitetruktur zu ersielen. Fäden, die bei niedrigeren Temperaturen ale 150O0C karbonisiert »orden sind, benötigen uioht ootwendlgerweiee «ine Oberflächenbehandlung, damit eie zum Einarbeiten in eine Matrix geeignet werden. Diejenigen jedoch, die bei einer Temperatur oberhalb von 15000C hergestellt worden sind, bedürfen in der Regel einer solchen Behandlung.Duration of treatment and ambient atmosphere. In general, for example, be characterized Rohlenstoffasern provides mountains "that a thread or organieoheo fassrfBrmiges material in air or another oxidizing · Qa is heated to about 200 0 C and 300 bio carbonized product at a temperature above 1000 0 C. The resulting carbonized filaments can be further heated to 150o 0 C and higher "to ersielen to" ine Graphitetruktur. Are carbonized threads ale at lower temperatures 150o C 0 "orden need uioht ootwendlgerweiee" ine surface treatment so e'e for incorporation into a matrix suitable to be. However, those which have been produced at a temperature above 1500 ° C. generally require such a treatment.
Torzugoweise wird die erfindungegemäß durchzuführende Elektrolyse ir.it einem Elektrolyt durchgeführt, dar eine wässrige Lösung eines Alkalihydroxyds enthält« Ee ist forsaaieben, Natriumhydroxid zu verwenden, dooh ist jedes andere Alkali« ' hydroxyd ebenfalls ceeigoet. Dia Konzentration des Alkallhydroxyds in der Lösung kann innerhalb bestimmter Grenzen sohwanken, dooh wird vom Standpunkt einer schnellen Reaktion eine Lusung bevorzugt, die etwa 10 bis 20 Gewichtsprozent Hydroxyd enthält·Torzugoweise the electrolysis to be carried out according to the invention ir. carried out with an electrolyte, is an aqueous one Solution of an alkali hydroxide contains «Ee is forsaaieben, To use sodium hydroxide, dooh is any other alkali «' hydroxyd also ceeigoet. The concentration of the alkali hydroxide in the solution can vary within certain limits, dooh becomes from the standpoint of a quick reaction a solution preferably that is about 10 to 20 percent by weight Hydroxide contains
009847/175* ΒΑ0 009847/175 * ΒΑ0
20129312012931
ale Anode der Elektrolytzelle geschaltet» während die Kathode vorzugsweise ein Metall, wie okel 1st, das zusammen mit der Konlenstoffanode eine Zelle bildet, in der naazieren« der Sauerstoff an der Oberfläche der Fäden erzeugt wird. Bündel von Stapelfasern können in einem absatzweise arbeitenden Yerfanren behandelt warden, indem das gesamte Bündel an einem geeigneten elektriaohen Xontakt befestigt wird. Dabei kann es erwünscht sein, daβ ihre Bewegungsfreiheit in der Zelle mit Hilfe eines ZeΙΐβαββparatore eingeengt wird· Kontinuierliche Fäden werden behandelt, indem sie kontinuierlich durch die £lektrolytselle geleitet und dann daraua entfernt werden. In einem aolchen Fall können sie mit dar Stromquelle s.B. dadurch verbunden sein, daa sie über eine leitende Waise laufen, die Ihreraeita mit der Stromquelle in Verbindung steht.All the anode of the electrolytic cell is switched while the cathode preferably a metal, like okel 1st, that together forms a cell with the Konlenstoffanode in which naazieren « the oxygen is generated on the surface of the threads. Bundles of staple fibers can be handled in an intermittent way by removing the whole Bundle attached to a suitable electrical contact will. It may be desirable that their freedom of movement constricted in the cell with the help of a ZeΙΐβαββparatore is · Continuous filaments are treated by being passed continuously through the electrolyte cell and then be removed. In such a case you can use the power source s.B. be connected by daa they run across a senior orphan who is youraeita with connected to the power source.
Bas erfindungsfeaäte Terfahren wird duroh die folgenden Beispiele nlfaer erläutert.The inventive method is based on the following Examples are explained below.
Sin Bündel aaa la wesentlichen Orasbitfaeern words In ein gewirktes Polypropylentuch eingewlokelt. masse Polypropylentuch wirkte als Zellen·«parator, weil es frais Zirkulation dar SlektrolytlOsang and dee Slektrolytetreues tulleβ, aber verhinderte, tot lose Fasern einen Knrseehlal in der Slektro·Sin bunch aaa la essential Orasbitfaeern words In a knitted polypropylene cloth. bulk polypropylene cloth acted as a cell parator because there was frais circulation The slectrolyte loosang and the slectrolyte faithful tulleβ, but prevented dead loose fibers from creating a Knrseehlal in the slektro
BAD ORiGfNALBAD ORiGfNAL
009847/17*4009847/17 * 4
lytzelle hervorriefen« Das Bündel wurde in eine 15proaeotige wäserige Lusung von Natriumhydroxyd eingetaucht. Eben« falls wurde in die Natrlumhydroxydiesung eine Hlokelelek~ trode eingetaucht. Ein Strom von 2,5 A mit einer Potential«, diffesens. von 6 Volt wurde 5 Minuten lang hindurobgeachiokt, wobei das Nickel als Kathode und die Kohlenatoffasern als Anode geschaltet waren. Die Fasern wurden von der Zeile entfernt, man Heß aia abtropfen, spülte ale ab und trocknete* lytic cell elicited. The bundle was transformed into a proaeotige watery solution of sodium hydroxide immersed. Just" If so, a Hlokelelek was added to the sodium hydroxide solution trode immersed. A current of 2.5 A with a potential «, diffesens. of 6 volts was hindurobgeachiokt for 5 minutes, with the nickel as the cathode and the carbon fibers as Were connected to the anode. The fibers were removed from the line, the hess aia drained, ale rinsed and dried *
Mit Hilfe dieser so behandelten Pasern und einem Epoxyharz wurden Laminate hergestellt. Die interlaminare Scherfestigkeit (ein MaQ für die Bindung zwischen Harz urid Fasern) erwies eich als Überragend gegenüber den Laminaten mit anhebende!» ten Fasern,* Unbehandelte Fasern ergaben in einem Laminat eine interlaminare Scherfestigkeit von 190 kg/cm . Bln. Wert* dem ein solcher von 550 kg/cm bei einem Laminat gegenübersteht, das mit erfindungsgemäS behandelten Fasern hergestellt wordenWith the help of these treated fibers and an epoxy resin laminates were made. The interlaminar shear strength (a measure of the bond between resin urid fibers) was proven eich as outstanding compared to the laminates with lifting! " th fibers, * Untreated fibers gave a interlaminar shear strength of 190 kg / cm. Bln. Value * dem a laminate of 550 kg / cm, the fibers treated according to the invention have been produced
ist. ■ · ■ " '-■■'/",;is. ■ · ■ "'- ■■' /" ,;
B s i a p-l e 1_ g .i B sia pl e 1_ g .i
Ein kontinuierliches darn aus Kohlenatoffasern wurde durch ein Bad geschickt, das 15 gawlohtsprozentige Natriurahydroxyd lösung enthielt. Bs wprde als Anode geeonaltet, lodern es iunäohst liber eine metallische leitungswalze lief οA continuous darn made of carbon fibers was made through sent a bath containing 15% sodium hydroxide solution contained. If it were used as an anode, it would blaze ο ran over a metal guide roller
/BAD / BA D
009847/V764"009847 / V764 "
Nickelplatten waren an der inneren Oberfläche des Bede als Kathoden befestigt. Es wurde zwischen der Kohlenstoffgarn-Anode (Über die Netallwalze) und der Nickelkathode eine Potentialdifferenz von 6 Volt angewandt. Diese Potentialdifferenz ergab eine Stromstärke von ungefähr 2,5 A unter den angewendeten Bedingungen. Die Verweildauer des ea?ns in dem Bad betrug 3 Minuten. Das behandelte Garn verlies das Bad durch Quetschwalzen, um tiber schlissige η Elektrolyt zu entfernen. Ea wurde dann gewaschen und getrocknet und schließlich auf β inn Aufnahmespule gewickelt. Dieses Verfahren aurde mit Garnen aus hoch zugfesten Kohlenstoffasern und mit Garnen aus Kohlenetoffasern mit hohem Modul durchgeführt. Laminate, welche aus den behandelten Garnen hergestellt worden sind, hatten Überragende Hars/Faser-Bindungaeigenschaften Im Vergleich zu dem unbehandelten Garn. So betrug die interlatainam Scherfestigkeit von Laminaten mit erfindungsgemäÖ behandelten Fasern mit hoher Festigkeit 820 kg/cm und die von Laminaten mit erfindungsgemJ»3 be-Nickel plates were on the inner surface of the bede attached as cathodes. It was between the carbon yarn anode A potential difference of 6 volts is applied (via the Netall roller) and the nickel cathode. This potential difference resulted in a current of approximately 2.5 A below the conditions applied. The length of stay of the ea? Ns in the bath was 3 minutes. The treated yarn left the bath through nip rollers in order to remove the electrolyte to remove. Ea was then washed and dried and finally wound onto β in the take-up spool. This process is carried out with yarns made from high tensile strength carbon fibers and performed with high modulus carbon fiber yarns. Laminates made from the treated yarns had superior fiber / fiber bonding properties Compared to the untreated yarn. So was the interlatainam shear strength of laminates with fibers treated according to the invention with high strength 820 kg / cm and that of laminates with 3 loads according to the invention
J,J,
handelten Fasern mit hohem Modul 570 kg/cm . Andererseits hatten Laminate, die mit unbehandelten Garnen von £ohlen~ stoffasern hergestellt worden waren, ein« interlaminare Scherfestigkeit von 190 kg/cm .traded high modulus fibers 570 kg / cm. on the other hand had laminates made with untreated yarn from £ ohlen ~ fabric fibers had been produced, an “interlaminar shear strength of 190 kg / cm.
BAD ORIGINALBATH ORIGINAL
0.9847/175;0.9847 / 175;
Claims (2)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB1443469 | 1969-03-19 |
Publications (3)
Publication Number | Publication Date |
---|---|
DE2012981A1 true DE2012981A1 (en) | 1970-11-19 |
DE2012981B2 DE2012981B2 (en) | 1978-11-16 |
DE2012981C3 DE2012981C3 (en) | 1979-07-26 |
Family
ID=10041145
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE2012981A Expired DE2012981C3 (en) | 1969-03-19 | 1970-03-18 | Process for modifying the surface of carbon fibers |
Country Status (9)
Country | Link |
---|---|
US (1) | US3759805A (en) |
JP (1) | JPS5520033B1 (en) |
BE (1) | BE747631A (en) |
CA (1) | CA931111A (en) |
DE (1) | DE2012981C3 (en) |
DK (1) | DK131197B (en) |
FR (1) | FR2039709A5 (en) |
GB (1) | GB1297946A (en) |
NL (1) | NL7003914A (en) |
Families Citing this family (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2180617B1 (en) * | 1972-04-21 | 1974-09-13 | Rhone Progil | |
US3859187A (en) * | 1972-09-25 | 1975-01-07 | Celanese Corp | Electrolytic process for the surface modification of high modulus carbon fibers |
US4050997A (en) * | 1972-12-18 | 1977-09-27 | Maschinenfabrik Augsburg-Nurnberg Aktiengesellschaft | Method of manufacturing a fiber reinforced composite material |
JPS53122894A (en) * | 1977-03-30 | 1978-10-26 | Japan Exlan Co Ltd | Treating of carbon fiber |
JPS585288B2 (en) * | 1978-04-12 | 1983-01-29 | 東レ株式会社 | Carbon fiber surface electrolytic treatment method and its electrolytic cell |
JPS5814310B2 (en) * | 1978-06-15 | 1983-03-18 | 臼井国際産業株式会社 | multilayer steel pipe |
JPS56128362A (en) * | 1980-03-05 | 1981-10-07 | Toho Beslon Co | Production of carbon fiber |
US4360417A (en) * | 1980-07-03 | 1982-11-23 | Celanese Corporation | Dimensionally stable high surface area anode comprising graphitic carbon fibers |
GB2161273B (en) * | 1984-05-18 | 1988-04-13 | Mitsubishi Rayon Co | Testing carbon fibre |
JPS62276075A (en) * | 1986-02-07 | 1987-11-30 | 三菱レイヨン株式会社 | Carbon fiber and its production |
DE3780092T2 (en) * | 1986-05-30 | 1993-02-18 | Amoco Corp | MULTIPLE ELECTROLYTIC TREATMENT OF CARBON FIBERS TO IMPROVE SHEAR RESISTANCE. |
-
1969
- 1969-03-19 GB GB1443469A patent/GB1297946A/en not_active Expired
-
1970
- 1970-03-18 DK DK135670AA patent/DK131197B/en unknown
- 1970-03-18 DE DE2012981A patent/DE2012981C3/en not_active Expired
- 1970-03-18 US US00020822A patent/US3759805A/en not_active Expired - Lifetime
- 1970-03-19 JP JP2271370A patent/JPS5520033B1/ja active Pending
- 1970-03-19 NL NL7003914A patent/NL7003914A/xx unknown
- 1970-03-19 CA CA077911A patent/CA931111A/en not_active Expired
- 1970-03-19 BE BE747631D patent/BE747631A/en unknown
- 1970-03-19 FR FR7009868A patent/FR2039709A5/fr not_active Expired
Also Published As
Publication number | Publication date |
---|---|
CA931111A (en) | 1973-07-31 |
NL7003914A (en) | 1970-09-22 |
US3759805A (en) | 1973-09-18 |
BE747631A (en) | 1970-08-31 |
DK131197B (en) | 1975-06-09 |
FR2039709A5 (en) | 1971-01-15 |
DK131197C (en) | 1975-11-10 |
DE2012981B2 (en) | 1978-11-16 |
GB1297946A (en) | 1972-11-29 |
JPS5520033B1 (en) | 1980-05-30 |
DE2012981C3 (en) | 1979-07-26 |
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Legal Events
Date | Code | Title | Description |
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C3 | Grant after two publication steps (3rd publication) | ||
EHJ | Ceased/non-payment of the annual fee |