US3759805A - Electrolytic treatment of filamentary carbon material - Google Patents
Electrolytic treatment of filamentary carbon material Download PDFInfo
- Publication number
- US3759805A US3759805A US00020822A US3759805DA US3759805A US 3759805 A US3759805 A US 3759805A US 00020822 A US00020822 A US 00020822A US 3759805D A US3759805D A US 3759805DA US 3759805 A US3759805 A US 3759805A
- Authority
- US
- United States
- Prior art keywords
- carbon
- electrolyte
- filamentary
- anode
- filamentary 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.)
- Expired - Lifetime
Links
- 239000003575 carbonaceous material Substances 0.000 title description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 26
- 229910052799 carbon Inorganic materials 0.000 abstract description 26
- 238000000034 method Methods 0.000 abstract description 15
- 239000003792 electrolyte Substances 0.000 abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 abstract description 10
- 239000001301 oxygen Substances 0.000 abstract description 10
- 239000007864 aqueous solution Substances 0.000 abstract description 9
- 150000008044 alkali metal hydroxides Chemical class 0.000 abstract description 7
- 238000005868 electrolysis reaction Methods 0.000 abstract description 5
- 238000010923 batch production Methods 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- -1 hydroxyl ions Chemical class 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 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
- 238000002360 preparation method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
Definitions
- a process for treating the surface of filamentary carbon which comprises making the filamentary carbon the anode of an electrolytic cell, employing as the electrolyte an aqueous solution of a solute, for example an alkali metal hydroxide, adapted to generate oxygen at the anode during electrolysis, and electrolysing the electrolyte.
- the treatment may be carried out as a batch process or a continuous process.
- This invention relates to the surface treatment of filamentary material and in particular to the preparation of the surface of filamentary carbon to improve its properties for incorporation into matrices.
- Filamentary carbon particularly that which is prepared by a process which involves heat treatment at a temperature greater than 1500 C. tends to have a smooth surface which does not bond well into a matrix. Improved bonding may be achieved by modifying the surface to some extent and this invention provides an improved process for such modification.
- a process for treating the surface of filamentary carbon comprises electrolysing an electrolyte in the form of an aqueous solution wherein the filamentary carbon is connected as the anode such that nascent oxygen is generated at the surface of the filamentary carbon.
- a suitable aqueous solution in the process of this invention contains hydroxyl ions and is of a composition such that the hydroxyl ions may be discharged at the anode during an electrolysis to produce nascent oxygen. It is known that not all aqueous solutions containing hydroxyl ions produce nascent oxygen in an electrolysis, for example solutions containing another anion which may be preferentially discharged. Such solutions are not included in the process of this invention.
- Carbon filaments suitable for use in the present invention may be produced by subjecting organic filamentary material such as polyester, polyamide, cellulosic or preferably polyacrylonitrile filaments to various conditions of temperature, time and surrounding atmosphere. Carbon filaments are commonly produced for example by heating organic filamentary material in air or other oxidising gas to a temperature within the range from about 200 to 300 C. and the product is carbonised at a temperature above 1000 C. The resulting carbonised filaments may be further heated to build up a graphitic structure within them at temperatures of from 1500 C. upwards. Filaments carbonised at a temperature lower than 1500 C. do not necessarily require surface treatment to make them suitable for incorporation in a matrix but those prepared at a temperature above 1500 C. will normally require such treatment.
- organic filamentary material such as polyester, polyamide, cellulosic or preferably polyacrylonitrile filaments
- the electrolysis in the process of this invention is carried out when the electrolyte is an aqueous solution of an alkali metal hydroxide. It is preferred to use sodium hydroxide but the other alkali metal hydroxides are also suitable.
- concentration of alkali metal hydroxide in the solution may vary within limits,
- the carbon filaments are made the anode of the electrolytic cell and the cathode is preferably a metal such as nickel which together with the carbon anode produces a cell in which nascent oxygen is produced on the surface of the filaments.
- Bundles of staple filaments may be treated in a batch process by attaching the whole bundle to a suitable electrical contact terminal and it may be desirable for them to be restrained from floating about in the cell by means of a cell separator.
- Continuous filaments may be treated by passing them continuously into the electrolytic cell and removing them therefrom and in such a case they may be connected to the source of electromotive force for example by passing them over a conducting roller which itself is connected to that source.
- a bundle of fibres of essentially graphitic structure was wrapped in a knitted polypropylene fabric.
- This polypropylene fabric acted as a cell separator in that it allowed free circulation of electrolyte solution and electric current but prevented loose fibres causing short circuits in the electrolytic cell.
- the bundle was immersed in a 15 percent aqueous solution of sodium hydroxide.
- a nickel electrode was also immersed in the sodium hydroxide solution.
- a current of 2.5 amps at a potential difference of 6 volts was applied for 5 minutes with the nickel as the cathode and the carbon fibres as the anode. The fibres were removed from the cell, allowed to drain, rinsed and dried.
- Laminates were prepared using these treated fibres and an epoxy resin and the interlaminar shear strength (a measure of resin/fibre bonding) was found to be superior to that obtained with untreated fibres.
- the interlaminar shear strength of laminates prepared with the untreated fibre was 2,700 p.s.i. kg/cm?) and that of laminates prepared with the treated fibre exceeded 7,800 p.s.i. (550 kg/cmf
- a continuous yarn of carbon fibres was passed through a bath containing 15 percent sodium hydroxide solution and was made the anode by first passing over a metal conductor roll. Nickel plates attached to the inner surface of the bath acted as cathode.
- laminates prepared with untreated yarns of carbon fibres had an interlaminar shear strength of 2,700 p.s.i. (190 kg./cm.
- a process for treating the surface of filamentary carbon to improve its bonding properties in a resin or plastic matrix which comprises making the filamentary carbon the anode of an electrolytic cell, employing an aqueous solution capable of producing nascent oxygen at the anode as the electrolyte in said cell and electrolyzing said electrolyte to generate nascent oxygen at the surface of said filamentary carbon to modify said surface.
- alkali metal hydroxide constitutes from about 10 to 20 percent by weight of the electrolyte.
- a process for treating the surface of filamentary carbon in the form of continuous filaments to improve its bonding properties in a resin or plastic matrix which comprises making the filamentary carbon the anode of an electrolytic cell, employing an aqueous solution capable of producing nascent oxygen at the anode as the electrolyte in said cell, passing the filamentary carbon continuously into said electrolyte and continuously removing the filamentary carbon from said electrolyte, and electrolyzing said electrolyte to generate nascent oxygen at References Cited UNITED STATES PATENTS 3,323,869 6/1967 Olstowski 23209.1 2,807,577 9/1957 Antonsen 204-430 2,439,442 4/1948 Amon et a1. 23209.1 3,671,411 6/1972 Ray et al 204-130 JOHN H. MACK, Primary Examiner R. L. ANDREWS, Assistant Examiner US. Cl. XJR. 204129, 294
Abstract
A PROCESS FOR TREATING THE SURFACE OF FILAMENTARY CARBON WHICH COMPRISES MAKING THE FILAMENTARY CARBON THE ANODE OF AN ELECTROLYTIC CELL, EMPLOYING AS THE ELECTROLYTE AN AQUEOUS SOLUTION OF A SOLUE, FOR EXAMPLE IN ALKALI METAL HYDROXIDE, ADAPTED TO GENERATE OXYGEN AT THE ANODE DURING ELECTROLYSIS, AND ELECTROLYSING THE ELECTROLYTE. THE TREATMENT MAY BE CARRIED OUT AS A BATCH PROCESS OR A CONTINUOUS PROCESS.
Description
United States Patent 3,759,805 ELECTROLYTIC TREATMENT OF FILAMENTARY CARBON MATERIAL Dennis R. Chapman, Dufiield, and William Crawford Paterson, Darley Abbey, England, assignors to Courtaulds Limited, London, England No Drawing. Filed Mar. 18, 1970, Ser. No. 20,822 Claims priority, application Great Britain, Mar. 19, 1969, 14,434/ 69 Int. Cl. C01d 7/34; Clllb 13/04; B011: 3/01 US. Cl. 204-130 5 Claims ABSTRACT OF THE DISCLOSURE A process for treating the surface of filamentary carbon which comprises making the filamentary carbon the anode of an electrolytic cell, employing as the electrolyte an aqueous solution of a solute, for example an alkali metal hydroxide, adapted to generate oxygen at the anode during electrolysis, and electrolysing the electrolyte. The treatment may be carried out as a batch process or a continuous process.
This invention relates to the surface treatment of filamentary material and in particular to the preparation of the surface of filamentary carbon to improve its properties for incorporation into matrices.
Filamentary carbon particularly that which is prepared by a process which involves heat treatment at a temperature greater than 1500 C. tends to have a smooth surface which does not bond well into a matrix. Improved bonding may be achieved by modifying the surface to some extent and this invention provides an improved process for such modification.
According to the invention a process for treating the surface of filamentary carbon comprises electrolysing an electrolyte in the form of an aqueous solution wherein the filamentary carbon is connected as the anode such that nascent oxygen is generated at the surface of the filamentary carbon. Thus, a suitable aqueous solution in the process of this invention contains hydroxyl ions and is of a composition such that the hydroxyl ions may be discharged at the anode during an electrolysis to produce nascent oxygen. It is known that not all aqueous solutions containing hydroxyl ions produce nascent oxygen in an electrolysis, for example solutions containing another anion which may be preferentially discharged. Such solutions are not included in the process of this invention.
Carbon filaments suitable for use in the present invention may be produced by subjecting organic filamentary material such as polyester, polyamide, cellulosic or preferably polyacrylonitrile filaments to various conditions of temperature, time and surrounding atmosphere. Carbon filaments are commonly produced for example by heating organic filamentary material in air or other oxidising gas to a temperature within the range from about 200 to 300 C. and the product is carbonised at a temperature above 1000 C. The resulting carbonised filaments may be further heated to build up a graphitic structure within them at temperatures of from 1500 C. upwards. Filaments carbonised at a temperature lower than 1500 C. do not necessarily require surface treatment to make them suitable for incorporation in a matrix but those prepared at a temperature above 1500 C. will normally require such treatment.
Preferably, the electrolysis in the process of this invention is carried out when the electrolyte is an aqueous solution of an alkali metal hydroxide. It is preferred to use sodium hydroxide but the other alkali metal hydroxides are also suitable. The concentration of alkali metal hydroxide in the solution may vary within limits,
ice
though from the point of view of speed of reaction it may be preferred to use a solution containing from about 10 to 20 percent by weight of the hydroxide.
'In the process of the invention the carbon filaments are made the anode of the electrolytic cell and the cathode is preferably a metal such as nickel which together with the carbon anode produces a cell in which nascent oxygen is produced on the surface of the filaments. Bundles of staple filaments may be treated in a batch process by attaching the whole bundle to a suitable electrical contact terminal and it may be desirable for them to be restrained from floating about in the cell by means of a cell separator. Continuous filaments may be treated by passing them continuously into the electrolytic cell and removing them therefrom and in such a case they may be connected to the source of electromotive force for example by passing them over a conducting roller which itself is connected to that source.
The process of the invention is illustrated by the following examples.
A bundle of fibres of essentially graphitic structure was wrapped in a knitted polypropylene fabric. This polypropylene fabric acted as a cell separator in that it allowed free circulation of electrolyte solution and electric current but prevented loose fibres causing short circuits in the electrolytic cell. The bundle was immersed in a 15 percent aqueous solution of sodium hydroxide. A nickel electrode was also immersed in the sodium hydroxide solution. A current of 2.5 amps at a potential difference of 6 volts was applied for 5 minutes with the nickel as the cathode and the carbon fibres as the anode. The fibres were removed from the cell, allowed to drain, rinsed and dried.
Laminates were prepared using these treated fibres and an epoxy resin and the interlaminar shear strength (a measure of resin/fibre bonding) was found to be superior to that obtained with untreated fibres. Thus, the interlaminar shear strength of laminates prepared with the untreated fibre was 2,700 p.s.i. kg/cm?) and that of laminates prepared with the treated fibre exceeded 7,800 p.s.i. (550 kg/cmf EXAMPLE 2 A continuous yarn of carbon fibres was passed through a bath containing 15 percent sodium hydroxide solution and was made the anode by first passing over a metal conductor roll. Nickel plates attached to the inner surface of the bath acted as cathode. A potential difference of 6 volts was applied between the carbon yarn anode (via the metal roll) and the nickel cathode. This potential dilference gave rise to a current of approximately 2.5 amps under the conditions used. The dwell time of the yarn in the bath was 3 minutes. The treated yarn left the bath through nip rolls to remove excess electrolyte and was then washed and dried and finally wound on to a take-up bobbin. This procedure was carried out using yarns of high tensile carbon fibres and yarns of high modulus carbon fibres. Laminates prepared from the treated yarns had superior resin/fire bonding characteristics to those of the untreated yarn. Thus, the interlaminar shear strength of laminates prepared with treated high tensile fibre was 11,700 p.s.i. (820 kg./cm. and that of laminates prepared with treated high modulus fibre was 8,100 p.s.i. (570 kg./cm. On the other hand,
laminates prepared with untreated yarns of carbon fibres had an interlaminar shear strength of 2,700 p.s.i. (190 kg./cm.
What is claimed is:
1. A process for treating the surface of filamentary carbon to improve its bonding properties in a resin or plastic matrix which comprises making the filamentary carbon the anode of an electrolytic cell, employing an aqueous solution capable of producing nascent oxygen at the anode as the electrolyte in said cell and electrolyzing said electrolyte to generate nascent oxygen at the surface of said filamentary carbon to modify said surface.
2. A process according to claim 1 wherein the solute is an alkali metal hydroxide.
3. A process according to claim 2 wherein the alkali metal hydroxide constitutes from about 10 to 20 percent by weight of the electrolyte.
4. A process for treating the surface of filamentary carbon in the form of continuous filaments to improve its bonding properties in a resin or plastic matrix which comprises making the filamentary carbon the anode of an electrolytic cell, employing an aqueous solution capable of producing nascent oxygen at the anode as the electrolyte in said cell, passing the filamentary carbon continuously into said electrolyte and continuously removing the filamentary carbon from said electrolyte, and electrolyzing said electrolyte to generate nascent oxygen at References Cited UNITED STATES PATENTS 3,323,869 6/1967 Olstowski 23209.1 2,807,577 9/1957 Antonsen 204-430 2,439,442 4/1948 Amon et a1. 23209.1 3,671,411 6/1972 Ray et al 204-130 JOHN H. MACK, Primary Examiner R. L. ANDREWS, Assistant Examiner US. Cl. XJR. 204129, 294
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB1443469 | 1969-03-19 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3759805A true US3759805A (en) | 1973-09-18 |
Family
ID=10041145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00020822A Expired - Lifetime US3759805A (en) | 1969-03-19 | 1970-03-18 | Electrolytic treatment of filamentary carbon material |
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) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3859187A (en) * | 1972-09-25 | 1975-01-07 | Celanese Corp | Electrolytic process for the surface modification of high modulus carbon fibers |
| US3865705A (en) * | 1972-04-21 | 1975-02-11 | Rhone Progil | Process for modifying the surface characteristics of carbon substrates and composite articles produced from the treated substrates |
| US4050997A (en) * | 1972-12-18 | 1977-09-27 | Maschinenfabrik Augsburg-Nurnberg Aktiengesellschaft | Method of manufacturing a fiber reinforced composite material |
| JPS54162664A (en) * | 1978-06-15 | 1979-12-24 | Usui Kokusai Sangyo Kk | Multiple layer steel pipe |
| US4234398A (en) * | 1978-04-12 | 1980-11-18 | Toray Industries, Inc. | Carbon fiber surface treatment |
| US4360417A (en) * | 1980-07-03 | 1982-11-23 | Celanese Corporation | Dimensionally stable high surface area anode comprising graphitic carbon fibers |
| US4401533A (en) * | 1980-03-05 | 1983-08-30 | Toho Belson Co., Ltd. | Surface-treatment of carbon fiber |
| US4735693A (en) * | 1984-05-18 | 1988-04-05 | Mitsubishi Rayon Co., Ltd. | Process for producing carbon fiber |
| US4814157A (en) * | 1986-02-07 | 1989-03-21 | Mitsubishi Rayon Co., Ltd. | Carbon fibers and method for producing same |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53122894A (en) * | 1977-03-30 | 1978-10-26 | Japan Exlan Co Ltd | Treating of carbon fiber |
| EP0251491B1 (en) * | 1986-05-30 | 1992-07-01 | Amoco Corporation | Multi-electrolyte treatment of carbon fibres to modify 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 US US00020822A patent/US3759805A/en not_active Expired - Lifetime
- 1970-03-18 DE DE2012981A patent/DE2012981C3/en not_active Expired
- 1970-03-19 BE BE747631D patent/BE747631A/en unknown
- 1970-03-19 FR FR7009868A patent/FR2039709A5/fr not_active Expired
- 1970-03-19 CA CA077911A patent/CA931111A/en not_active Expired
- 1970-03-19 JP JP2271370A patent/JPS5520033B1/ja active Pending
- 1970-03-19 NL NL7003914A patent/NL7003914A/xx unknown
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3865705A (en) * | 1972-04-21 | 1975-02-11 | Rhone Progil | Process for modifying the surface characteristics of carbon substrates and composite articles produced from the treated substrates |
| 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 |
| US4234398A (en) * | 1978-04-12 | 1980-11-18 | Toray Industries, Inc. | Carbon fiber surface treatment |
| JPS54162664A (en) * | 1978-06-15 | 1979-12-24 | Usui Kokusai Sangyo Kk | Multiple layer steel pipe |
| JPS5814310B2 (en) * | 1978-06-15 | 1983-03-18 | 臼井国際産業株式会社 | multilayer steel pipe |
| US4401533A (en) * | 1980-03-05 | 1983-08-30 | Toho Belson Co., Ltd. | Surface-treatment of carbon fiber |
| US4360417A (en) * | 1980-07-03 | 1982-11-23 | Celanese Corporation | Dimensionally stable high surface area anode comprising graphitic carbon fibers |
| US4735693A (en) * | 1984-05-18 | 1988-04-05 | Mitsubishi Rayon Co., Ltd. | Process for producing carbon fiber |
| US4814157A (en) * | 1986-02-07 | 1989-03-21 | Mitsubishi Rayon Co., Ltd. | Carbon fibers and method for producing same |
Also Published As
| Publication number | Publication date |
|---|---|
| DK131197C (en) | 1975-11-10 |
| GB1297946A (en) | 1972-11-29 |
| BE747631A (en) | 1970-08-31 |
| FR2039709A5 (en) | 1971-01-15 |
| DE2012981A1 (en) | 1970-11-19 |
| JPS5520033B1 (en) | 1980-05-30 |
| NL7003914A (en) | 1970-09-22 |
| DK131197B (en) | 1975-06-09 |
| CA931111A (en) | 1973-07-31 |
| DE2012981B2 (en) | 1978-11-16 |
| DE2012981C3 (en) | 1979-07-26 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| AS | Assignment |
Owner name: COURTAULDS, PLC Free format text: CHANGE OF NAME;ASSIGNOR:COURTAULDS, LIMITED;REEL/FRAME:004415/0575 Effective date: 19820520 |