CA1197335A - Stretch wrap cling polyethylene film - Google Patents
Stretch wrap cling polyethylene filmInfo
- Publication number
- CA1197335A CA1197335A CA000410431A CA410431A CA1197335A CA 1197335 A CA1197335 A CA 1197335A CA 000410431 A CA000410431 A CA 000410431A CA 410431 A CA410431 A CA 410431A CA 1197335 A CA1197335 A CA 1197335A
- Authority
- CA
- Canada
- Prior art keywords
- film
- composition
- resin
- sorbitan monooleate
- linear low
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
Abstract
ABSTRACT
Films especially useful for the stretch wrapping of pal-let loads are prepared from compositions consisting essential-ly of a linear low density polyethylene resin free of any polymerized vinyl acetate groups and from about 0.3 to about 3.0 wt % sorbitan monooleate based on the weight of the resin.
Films especially useful for the stretch wrapping of pal-let loads are prepared from compositions consisting essential-ly of a linear low density polyethylene resin free of any polymerized vinyl acetate groups and from about 0.3 to about 3.0 wt % sorbitan monooleate based on the weight of the resin.
Description
BACKGROUND OF TME INVENTION
The use of compositions based on et~71ene homopolymer or copolymers in the manufacture of stretch wrap films having good cling and optical properties is known, e.g., as shown in U.S. Patent Nos. 4,073,782 and 4,222,913.
U.S. Patent No. 4,073,782 discloses stretch wrap films made from a ternary composition wherein the resin component is a polyethylene of any suitable density, a copolymer of ethylene and vinyl acetate, or a mixture of the above mentioned polyethylene and copolymer. The remaining essential components of the ternary composition are sorbitan monooleate, which is mainly used as an antihazing agent, and a liquid paraffin, as an adhesive-ness modifier. ~hen polyethylene is chosen as the resin component, the sorbitan ~onooleate concentration should range between about 0.5 to 2.0% based on the polyethlene weight. The liquid paraffin concentration should fall in the ranye of 0.5 to 6% of the polymer. If no liquid paraffin is used, a film produced from the resulting binary composition is exceedingly sticky and cannot be used ~s wrapping material. Although the films produced in accordance with the teachings of the aforementioned patent perf~rm very well i~ most applications, their strength and toughness properties are somewhat inferior for ., 733~
use in stretch wrapping of pallet loads. U.S. Patent No.
4,222,913 discloses improvement in these properties by the use of a resin which is a blend of ethylen~-vinyl acetate copoly-I mer with a copolymer of propylene and small amounts of ethy-1 lene.
The recently developed linear low density polyethylenes I have the desired strength and toughness properties required for stretch wrap applications, but do not possess the re-quired cling, which in the case of conventional polyethylene, can at least be partially obtained by incorporation of vinyl acetate as a comonomer.
It is, therefore, an object of the present invention to provide a composition from which films can be prepared having improved strength, toughness and cling properties.
It is another object to provide a composition suitable for manufacture of pallet wrap stretch films of superior cling quality which will function at both ambient and winter warehouse temperatures.
A further object is to provide stretch wrap films of improved properties. Other objects will become apparent fr~m a reading of the specification and appended claims.
THE INVENTION
In accordance with the present invention there is pro-vided a composition suitable for a stretch wrap film manu-facture essentially consisting of:
(a) a linear low density polyethylene resin free of any polymerized vinyl acetate groups, and (b) ~rom about 0.3 to about 3.0 weight percent o~ sorbitan monooleate based on the weight of the resin. Preferably the sorbitan mono-oleate concentration is maintained in the range from about 0.7 to about 1.7 weight ~.
Contrary to the findings of the prior art, the polyethy-lene composition of this invention does not require the pres-ence of a liquid paraffin in order to prevent excessive stick-ine~s or adherence of the resulting film to itself or to film processing equipment, e.g., during roll wind-off.
The linear low density polyethylene (LLDPE) component of the composition of the invention is a copolymer of ethylene with one or more comonomers selected from C4 to C10 alpha ole-fins such as butene-l, hexene-l, etc. It has a density usu-ally in the range of from about 0.900 to about 0.940 g/cc and j preferably the density should be maintained between 0.916 to 0.928 g/cc for film making purposes. The melt index should range between about 0.1 and 10 g/10 min. and preferably be-tween about 0.5 and about 3.0 g/10 min. Such polymer resins are commercially available and are manufactured in low pres~
sure vapor phase and liquid phase processes using transition metal catalysts.
The sorbitan monooleate which is a commercially avail-able viscous liquid, can be incorporated into the composition by any convenient method, e.g./ by pumping it at a desired rate to the hopper of an extruder and coextruding the blend of LLDPE and sorbitan monooleate to form strands which upon cooling are chopped into pellets. Alternatively, the LLDPE
resin in granular pellet form can be blended in the same man-ner with the sorbitan monooleate in the extruder used in the film forming process.
Various methods may be used for producing the film, e.g., by any of the known tubular blowing methods or by the so called chilled roll casting methods. The thickness of the film can be between about 0.2 and about 2 mil and should preferably be in the range of from about 0.3 to about 1.5 mil. Since the films of these invention have greater tear and puncture reslstance, tensile strength and elongation compared to films prepared from conventional low density polyethylene or ethylene-vinyl acetate copolymers, the ilm thickness can be considerably reduced at equivalen-t stretch wrap per-_~_ ~37~3S
formance. Because of the aforementioned desired properties, the films perform extremely well as stretch pallet wrap material. In addition, the films have generally good opti-cal qualities such as low haze levels and high gloss, and are resistant to fogging and can, therefore, also be used with advantage for wrapping of food to be displayed or stored in refrigerated cases.
The following examples further illustrate the advan-tages of the invention:
1.2 parts sorbitan monooleate and 98.8 parts of LLDPE
powder (7-8 wt % polymerized l-butene, 0.916 density, 0.6 melt index) were thoroughly mixed in a ribbon blender and extruded into pellets, and, subsequently, blown into film using a 2-1/2" Davis Screw Extruder having the fluted head screw connected to a 4" die having a die gap of 0.086".
The die temperature was maintained at about 450F, whi;e the average barrel temperature was about 430 F. The line speed was 42 feet per minute. The film produced had a thickness of 1 mil. Table 1 shows the results of physical testing of the film.
Testing of this film at both room temperature and 37 F
showed excellent cling.
Using the materials and procedure described in Example 1 36" wide films were produced having thicknesses of 1.19 mil, 0.66 mil and 0.30 mil. 44" square pallets supporting four 21" diameter rolls of film set on end (36" high) were wrapped with each of the ilms. The test procedure entailed wrapping the pallets at ever increasing tension until the film tore of and then backing off the tension to the point where good pallet wraps could be obtained. Resistance to tear propaga-33~
tion was measured by initiating a cut and timing tear propa-gation. Maximum tension settings, operating tension settings and resistance to tear propagation are presented in Table 2, which also shows the results of testing (Example 5) a conven-tional commercial ethylene-vinyl acetate copolymer stretch wrap film (12~ VA).
The major difference between the films of Examples 2-4 vs. that of Example 5 was their resistance to tear propaga tion. The films of the present invention (Example 2-4) tore very slowly for a few seconds and stopped leaving a tight pallet, while the film of Example 5 zippered upon testing leaving a loose pallet.
Various modification and alterations can of course be made to the composition and films without departing from the scope of the invention, which is defined by the specifica-tion and appended claims.
,, \
1~ ' ! TABL~ 1 (1) I Haze , Total 13.7 i,Internal 3.4
The use of compositions based on et~71ene homopolymer or copolymers in the manufacture of stretch wrap films having good cling and optical properties is known, e.g., as shown in U.S. Patent Nos. 4,073,782 and 4,222,913.
U.S. Patent No. 4,073,782 discloses stretch wrap films made from a ternary composition wherein the resin component is a polyethylene of any suitable density, a copolymer of ethylene and vinyl acetate, or a mixture of the above mentioned polyethylene and copolymer. The remaining essential components of the ternary composition are sorbitan monooleate, which is mainly used as an antihazing agent, and a liquid paraffin, as an adhesive-ness modifier. ~hen polyethylene is chosen as the resin component, the sorbitan ~onooleate concentration should range between about 0.5 to 2.0% based on the polyethlene weight. The liquid paraffin concentration should fall in the ranye of 0.5 to 6% of the polymer. If no liquid paraffin is used, a film produced from the resulting binary composition is exceedingly sticky and cannot be used ~s wrapping material. Although the films produced in accordance with the teachings of the aforementioned patent perf~rm very well i~ most applications, their strength and toughness properties are somewhat inferior for ., 733~
use in stretch wrapping of pallet loads. U.S. Patent No.
4,222,913 discloses improvement in these properties by the use of a resin which is a blend of ethylen~-vinyl acetate copoly-I mer with a copolymer of propylene and small amounts of ethy-1 lene.
The recently developed linear low density polyethylenes I have the desired strength and toughness properties required for stretch wrap applications, but do not possess the re-quired cling, which in the case of conventional polyethylene, can at least be partially obtained by incorporation of vinyl acetate as a comonomer.
It is, therefore, an object of the present invention to provide a composition from which films can be prepared having improved strength, toughness and cling properties.
It is another object to provide a composition suitable for manufacture of pallet wrap stretch films of superior cling quality which will function at both ambient and winter warehouse temperatures.
A further object is to provide stretch wrap films of improved properties. Other objects will become apparent fr~m a reading of the specification and appended claims.
THE INVENTION
In accordance with the present invention there is pro-vided a composition suitable for a stretch wrap film manu-facture essentially consisting of:
(a) a linear low density polyethylene resin free of any polymerized vinyl acetate groups, and (b) ~rom about 0.3 to about 3.0 weight percent o~ sorbitan monooleate based on the weight of the resin. Preferably the sorbitan mono-oleate concentration is maintained in the range from about 0.7 to about 1.7 weight ~.
Contrary to the findings of the prior art, the polyethy-lene composition of this invention does not require the pres-ence of a liquid paraffin in order to prevent excessive stick-ine~s or adherence of the resulting film to itself or to film processing equipment, e.g., during roll wind-off.
The linear low density polyethylene (LLDPE) component of the composition of the invention is a copolymer of ethylene with one or more comonomers selected from C4 to C10 alpha ole-fins such as butene-l, hexene-l, etc. It has a density usu-ally in the range of from about 0.900 to about 0.940 g/cc and j preferably the density should be maintained between 0.916 to 0.928 g/cc for film making purposes. The melt index should range between about 0.1 and 10 g/10 min. and preferably be-tween about 0.5 and about 3.0 g/10 min. Such polymer resins are commercially available and are manufactured in low pres~
sure vapor phase and liquid phase processes using transition metal catalysts.
The sorbitan monooleate which is a commercially avail-able viscous liquid, can be incorporated into the composition by any convenient method, e.g./ by pumping it at a desired rate to the hopper of an extruder and coextruding the blend of LLDPE and sorbitan monooleate to form strands which upon cooling are chopped into pellets. Alternatively, the LLDPE
resin in granular pellet form can be blended in the same man-ner with the sorbitan monooleate in the extruder used in the film forming process.
Various methods may be used for producing the film, e.g., by any of the known tubular blowing methods or by the so called chilled roll casting methods. The thickness of the film can be between about 0.2 and about 2 mil and should preferably be in the range of from about 0.3 to about 1.5 mil. Since the films of these invention have greater tear and puncture reslstance, tensile strength and elongation compared to films prepared from conventional low density polyethylene or ethylene-vinyl acetate copolymers, the ilm thickness can be considerably reduced at equivalen-t stretch wrap per-_~_ ~37~3S
formance. Because of the aforementioned desired properties, the films perform extremely well as stretch pallet wrap material. In addition, the films have generally good opti-cal qualities such as low haze levels and high gloss, and are resistant to fogging and can, therefore, also be used with advantage for wrapping of food to be displayed or stored in refrigerated cases.
The following examples further illustrate the advan-tages of the invention:
1.2 parts sorbitan monooleate and 98.8 parts of LLDPE
powder (7-8 wt % polymerized l-butene, 0.916 density, 0.6 melt index) were thoroughly mixed in a ribbon blender and extruded into pellets, and, subsequently, blown into film using a 2-1/2" Davis Screw Extruder having the fluted head screw connected to a 4" die having a die gap of 0.086".
The die temperature was maintained at about 450F, whi;e the average barrel temperature was about 430 F. The line speed was 42 feet per minute. The film produced had a thickness of 1 mil. Table 1 shows the results of physical testing of the film.
Testing of this film at both room temperature and 37 F
showed excellent cling.
Using the materials and procedure described in Example 1 36" wide films were produced having thicknesses of 1.19 mil, 0.66 mil and 0.30 mil. 44" square pallets supporting four 21" diameter rolls of film set on end (36" high) were wrapped with each of the ilms. The test procedure entailed wrapping the pallets at ever increasing tension until the film tore of and then backing off the tension to the point where good pallet wraps could be obtained. Resistance to tear propaga-33~
tion was measured by initiating a cut and timing tear propa-gation. Maximum tension settings, operating tension settings and resistance to tear propagation are presented in Table 2, which also shows the results of testing (Example 5) a conven-tional commercial ethylene-vinyl acetate copolymer stretch wrap film (12~ VA).
The major difference between the films of Examples 2-4 vs. that of Example 5 was their resistance to tear propaga tion. The films of the present invention (Example 2-4) tore very slowly for a few seconds and stopped leaving a tight pallet, while the film of Example 5 zippered upon testing leaving a loose pallet.
Various modification and alterations can of course be made to the composition and films without departing from the scope of the invention, which is defined by the specifica-tion and appended claims.
,, \
1~ ' ! TABL~ 1 (1) I Haze , Total 13.7 i,Internal 3.4
(2) Gloss , 45 4 ~
60~ 6.5
60~ 6.5
(3) Dart Impact , g/mil 121
(4) Elmendoxf Tear, g/mil MD 131
(5)
(6) Tensile Strength @ Yield ,psi MD
(6) Tensile Strength @ Break MD 4580 (6) Elongation @ Break, MD 357 (6) 4 1% SecaIlt Modulus psi MD 2.72 x 10 TD 3.36 x 10 (1) ASTM D-1003 (2) ASTM D-2457 (3) ASTM D-1709 (4) MD - Machine Direotion (5) TD - Transverse Direction (6) ASTM D-882 ,~
TAB,,E 2 Ex. No.Gauge Max~ Ten. Run Ten. T.D. Tear Time Notes 2 1.19 mil 23% 16% 5-10 sec. Excellent Tear.Very tight pallet.
3 .56 mil 20% 17% 5-10 sec. Excellent Tear.Very tight pallet.
4 .30 mil 14% 12% 5-10 sec. Excellent Teari but looser than Ex. 3.
1.05 mil 23% 20% 1-3 sec. Poor tear (Zipper erfect).
Normal pallet.
(6) Tensile Strength @ Break MD 4580 (6) Elongation @ Break, MD 357 (6) 4 1% SecaIlt Modulus psi MD 2.72 x 10 TD 3.36 x 10 (1) ASTM D-1003 (2) ASTM D-2457 (3) ASTM D-1709 (4) MD - Machine Direotion (5) TD - Transverse Direction (6) ASTM D-882 ,~
TAB,,E 2 Ex. No.Gauge Max~ Ten. Run Ten. T.D. Tear Time Notes 2 1.19 mil 23% 16% 5-10 sec. Excellent Tear.Very tight pallet.
3 .56 mil 20% 17% 5-10 sec. Excellent Tear.Very tight pallet.
4 .30 mil 14% 12% 5-10 sec. Excellent Teari but looser than Ex. 3.
1.05 mil 23% 20% 1-3 sec. Poor tear (Zipper erfect).
Normal pallet.
Claims (10)
1. A stretch wrap film composition consisting essentially of (a) a linear low density polyethylene resin free of any polymerized vinyl acetate groups said resin being a copolymer of ethylene with one or more comonomers selected from C4 to C10 alpha-olefins and having a density in the range of from about 0.900 to about 0.940g/cc and a melt index between about 0.1 and 10g/10 min. and (b) from about 0.3 to about 3.0 weight percent sorbitan monooleate based on the weight of the resin, said composition in film form having excellent cling properties without exhibiting excessive adherence to film processing equipment.
2. The composition of claim 1 wherein the concentration of sorbitan monooleate is maintained in the range from about 0.7 to about 1.7 weight percent.
3. The composition of claim 1 wherein said density is between about 0.916 and about 0.928g/cc.
4. The composition of claim 1 wherein the melt index of the linear low density polyethylene ranges between about 0.5 and about 3.0 g/10 min.
5. A stretch wrap film having excellent cling properties without exhibiting excessive adherence to film processing equipment and having been prepared from a composition consisting essentially of (a) a linear low density polyethylene resin free of any polymerized vinyl acetate groups said resin being a copolymer of ethylene with one or more comonomers selected from C4 to C10 alpha-olefins and having a density in the range of from about 0.9.00 to about 0.940g/cc and a melt index between about 0.1 and 10g/10 min. and (b) from about 0.3 to about 3.0 weight percent sorbitan monooleate based on the weight of the resin.
6. The film of claim 5 wherein the concentration of sorbitan monooleate is maintained in the range from about 0.7 to about 1.7 weight percent.
7. The film of claim 5 wherein said density is between about 0.916 and about 0.928g/cc.
8. The film of claim 5 wherein the melt index of the linear low density polyethylene ranges between about 0.5 and about 3.0g/10 min.
9. The film of claim 5 having a thickness of from about 0.2 to about 2 mil.
10. The film of claim 9 wherein the thickness is from about 0.3 to about 1.5 mil.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/326,716 US4379197A (en) | 1981-12-02 | 1981-12-02 | Stretch wrap film composition |
| US326,716 | 1989-03-21 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1197335A true CA1197335A (en) | 1985-11-26 |
Family
ID=23273376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000410431A Expired CA1197335A (en) | 1981-12-02 | 1982-08-30 | Stretch wrap cling polyethylene film |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US4379197A (en) |
| JP (1) | JPS5898346A (en) |
| CA (1) | CA1197335A (en) |
| DE (1) | DE3244294A1 (en) |
| FR (1) | FR2517316B1 (en) |
| GB (1) | GB2111508B (en) |
| IT (1) | IT1154381B (en) |
Families Citing this family (60)
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|---|---|---|---|---|
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| US10780669B2 (en) | 2009-11-16 | 2020-09-22 | The Glad Products Company | Films and bags with visually distinct regions and methods of making the same |
| US9114596B2 (en) | 2009-11-16 | 2015-08-25 | The Glad Products Company | Incrementally-stretched adhesively-laminated films and methods for making the same |
| US9186862B2 (en) | 2009-11-16 | 2015-11-17 | The Glad Products Company | Multi-layered lightly-laminated films and methods of making the same |
| CN102762680A (en) * | 2009-11-16 | 2012-10-31 | 格拉德产品公司 | Discontinuously laminated film |
| US11345118B2 (en) | 2009-11-16 | 2022-05-31 | The Glad Products Company | Films and bags with visually distinct regions and methods of making the same |
| US8940377B2 (en) | 2009-11-16 | 2015-01-27 | The Glad Products Company | Multi-layered bags with discrete non-continuous lamination |
| CN204222116U (en) | 2011-04-25 | 2015-03-25 | 格拉德产品公司 | Multilayer film |
| CA2832649C (en) | 2011-04-25 | 2018-11-20 | The Glad Products Company | Thermoplastic films with visually-distinct stretched regions and methods for making the same |
| FR3087936B1 (en) | 2018-10-24 | 2022-07-15 | Aledia | ELECTRONIC DEVICE |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5758290B2 (en) * | 1974-05-02 | 1982-12-09 | Mitsubishi Plastics Ind | |
| GB1491872A (en) * | 1974-07-05 | 1977-11-16 | Exxon Research Engineering Co | Olefin polymer compositions suitable for fabricating into self-sealing films |
| GB1494332A (en) * | 1974-07-09 | 1977-12-07 | Exxon Research Engineering Co | Self-sealing films |
| JPS5423378B2 (en) * | 1975-01-31 | 1979-08-13 | ||
| GB1532780A (en) | 1975-03-07 | 1978-11-22 | Ici Ltd | Polyolefine film |
| JPS5243880A (en) * | 1975-10-03 | 1977-04-06 | Asahi Dow Ltd | Lapping films and its method of manufacturing |
| JPS5914060B2 (en) * | 1976-09-10 | 1984-04-03 | 昭和電工株式会社 | adhesive polyethylene film |
| JPS5436359A (en) * | 1977-08-04 | 1979-03-17 | Mitsubishi Chem Ind Ltd | Preparation of polyolefin film |
| JPS5481354A (en) * | 1977-12-12 | 1979-06-28 | Toppan Printing Co Ltd | Polyolefin film with excellent anti-fogging properties |
| DE2801541A1 (en) * | 1978-01-14 | 1979-07-19 | Hoechst Ag | AETHYLENE COPOLYMERS AND THEIR USE FOR THE PRODUCTION OF FILMS |
| GB2038845B (en) * | 1978-12-18 | 1982-12-08 | Du Pont Canada | Polyolefin composition for manufacture of film having cling properties |
| US4359561A (en) * | 1979-06-18 | 1982-11-16 | Union Carbide Corporation | High tear strength polymers |
| US4327009A (en) * | 1980-09-29 | 1982-04-27 | The Dow Chemical Company | Anti-block additives for olefin polymers |
| US4367256A (en) * | 1981-05-15 | 1983-01-04 | Union Carbide Corporation | Cling-wrap polyethylene film |
-
1981
- 1981-12-02 US US06/326,716 patent/US4379197A/en not_active Expired - Lifetime
-
1982
- 1982-08-30 CA CA000410431A patent/CA1197335A/en not_active Expired
- 1982-10-01 FR FR8216531A patent/FR2517316B1/en not_active Expired
- 1982-10-27 JP JP57187632A patent/JPS5898346A/en active Granted
- 1982-11-09 GB GB08231939A patent/GB2111508B/en not_active Expired
- 1982-11-30 DE DE19823244294 patent/DE3244294A1/en not_active Withdrawn
- 1982-12-01 IT IT24539/82A patent/IT1154381B/en active
Also Published As
| Publication number | Publication date |
|---|---|
| US4379197A (en) | 1983-04-05 |
| IT8224539A0 (en) | 1982-12-01 |
| GB2111508A (en) | 1983-07-06 |
| IT1154381B (en) | 1987-01-21 |
| DE3244294A1 (en) | 1983-06-09 |
| FR2517316A1 (en) | 1983-06-03 |
| JPH03421B2 (en) | 1991-01-08 |
| JPS5898346A (en) | 1983-06-11 |
| GB2111508B (en) | 1985-01-09 |
| FR2517316B1 (en) | 1986-09-12 |
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Legal Events
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| MKEX | Expiry |