HK1007309B - Moulded solid products reinforced with fibres - Google Patents
Moulded solid products reinforced with fibres Download PDFInfo
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- HK1007309B HK1007309B HK98106532.5A HK98106532A HK1007309B HK 1007309 B HK1007309 B HK 1007309B HK 98106532 A HK98106532 A HK 98106532A HK 1007309 B HK1007309 B HK 1007309B
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Description
The present invention relates to a new mixture of building materials for the manufacture of solid fibrous shaped manufactured products, a manufacturing process for such shaped manufactured products and the solid shaped manufactured products manufactured using this new mixture of building materials.
It is generally known that manufactured products shaped in the most diverse ways, such as slate, flat-wall or corrugated roofing sheets, panels, tubes and other shaped products can be made from aqueous suspensions of mixtures including hydraulic binders, loads and reinforcing fibres.
Among traditional building materials, products made of fibre reinforced cement, made from asbestos and cement, have been known for decades. In the asbestos-cement industry, processes based on the winding technique of L. Hatschek (Austrian patent No. 5970) are still the most widespread techniques for the manufacture of building elements. The technology of this manufacturing process is described in detail, for example, in Harald Klosz's book Asbestos (Cement) Springerlag, 1967.
The Hatschek process for manufacturing, for example, asbestos-cement foil is based on the use of cylindrical sieve drip machines. In this process, a mat from a diluted suspension of asbestos and cement contained in a container is transferred to a felt, via a cylindrical drip, and is then rolled to the required thickness using forming cylinders. For manufacturing corrugated sheets, the asbestos sheet formed on the forming cylinder is sliced loose from this cylinder and after the desired thickness has been reached. This sheet is then oiled and cut into the shapes of the corrugated metal.
Asbestos has both strengthening properties due to its own tensile strength and implementing qualities in relation to its excellent dispersion ability in an aqueous suspension of cement. During the drip stage, due to good filtration properties and good affinity for cement, asbestos fibres can retain fine suspended particles from the composite mixture in the process of shaping. In the hydrated final product, the high tensile strength combined with the high modulus of elasticity and low elongation at rupture contribute to giving asbestos-cement manufactured products their known high bending strength.
However, in recent years asbestos has become an undesirable component for environmental and health reasons and considerable efforts have been made to replace it.
In recent years, intensive research has been devoted to the discovery of alternative fibres that can partially or totally replace asbestos in current manufacturing processes based on drainage techniques.
It is therefore desirable to use new fibres as reinforcing agents and also as implementing aids to be used with hydraulic binders, for example for cement reinforcement.
The criteria for fibres suitable for cement reinforcement and other hydraulically-sealing binders are exceptionally high.
The following properties characterize asbestos as both a reinforcing fibre and as a fibre for use in drainage technology:
1) as regards the implementation properties:
High specific surface area,good dispersion ability,excellent chemical resistance and durability,high cement holding capacity,good layer formation ability,2) with regard to strengthening qualities:
High tensile strength,high modulus of elasticity,low elongation at break.
As regards chemical criteria, resistance to alkali in high temperature saturated solutions of calcium hydroxide is particularly essential.
No natural or synthetic fibres have been discovered that exhibit the combination of all the properties of asbestos fibres. It is now known that the replacement of asbestos requires two different types of fibres corresponding to the two main functions of asbestos (see, for example, DE 3 002 484). The filtration properties of asbestos can be reproduced by the addition of natural or synthetic pulps, e.g. cellulose alone and/or synthetic fibres. Selected reinforcement fibres are used for the reinforcement of the composite manufactured product. These can be high-modulus organic or inorganic fibres which are usually cut to lengths of 1 to 15 mm.
Many synthetic fibers have been tried for cement reinforcement, but most have given poor or unsatisfactory results for a number of reasons such as insufficient chemical resistance, poor affinity for cement, insufficient mechanical properties, especially insufficient intrinsic toughness and elastic modulus, and exaggerated elongation at breakage.
In addition, the physical characteristics of the fibres must be compatible with the properties of the hydraulic binders in terms of important properties. In the case of cement, it is known that this material has a certain fragility and can, for example, break at an elongation of about 0.03%.
In addition to the above physical properties of the fibres, it is equally important that the fibres can be easily dispersed in a water suspension diluted with cement and also remain evenly dispersed when other additives are added when these fibres have to be used by drainage techniques to produce fibre-cement products.
The literature already contains countless publications about the use of various natural or synthetic organic and inorganic fibers. Fibers made of cotton, cellulose, polyamide, polyester, polyacrylonitrile, polypropylene and polyvinyl alcohol, among others, have already been investigated for cement strengthening. Similarly, work is known on fibers made of glass, steel, aramid and carbon. Of all these fibers, none has so far all the required properties, especially for cement.
For example, glass has poor chemical stability, steel is prone to corrosion and has too high a density, carbon is too brittle, adheres poorly and is expensive, cellulose has insufficient durability, and ordinary polyethylene and polypropylene have insufficient tensile strength.
To date, there are mainly two types of synthetic fibres that meet the criteria for cement reinforcement. Both are high-modulus fibres based on polyvinyl alcohol (or PVA) and polyacrylonitrile (or PAN) alone (GB 2 850 298) or in combination. The former is available, for example, under the Kuralon® brand name of the Kuraray Company, Japan (DE 2 850 337) and an example of the latter is Dolanit® manufactured by Hoechst, Germany.
These fibres are characterised by high toughness and low elongation at breakage, as shown below.
- What?
| PVA | PAN | |
| Ténacité, N/mm² | 1550 | 910 |
| Module initial N/mm² | 37000 | 17000 |
| Allongement à la rupture (%) | 7,4 | 9,0 |
In the field of fibre-cement products, it is known that the mechanical strength is lowest when composite manufactured products are in the wet state (a common situation for exposure to the environment) and therefore international standards often require that measurements be carried out under water saturation conditions.
PVA fibres with the best mechanical properties not only confer the highest wet bending strength but also a breaking energy which is much higher than in the case of PAN fibres.
The inadequacy of PVA fibres is due to their sensitivity to high temperature water and their high price.Manufactured products shaped and reinforced with PVA fibres have excellent mechanical properties in the dry state, but the high value of bending strength decreases in the wet state.
Given the correlation between the properties of the fibres and those of the resulting manufactured products, it is relatively easy to manufacture cement-fibre manufactured products with strict standards for bending strength, impact toughness and breaking energy using exclusively PVA as reinforcement fibres.
Although this solution is economically attractive, the breakdown energy is still below the value.
The purpose of the present invention is to provide solid shaped manufactured products reinforced with fibres which avoid the known disadvantages of the known state, e.g. low wet break energy and high price.
On the basis of the rule of mixtures for the strength of a composite manufactured product containing fibres in a matrix, only high modulus and high toughness fibres have so far been used for the manufacture of high bending strength cement fibres manufactured products.
A pure cement matrix has a modulus E of 15 000 N per mm2. Accordingly, according to the mixing rule for a manufactured fibre-cement mixture, the modulus E of reinforcing fibres must be greater than 15 000 N per mm2.
In this respect, it has always been argued that polypropylene fibres are generally technically poor when it comes to reinforcing cement-based materials by direct tensile or bending in the relatively brittle matrix of cement and mortar, as results comparable to those of high-modulus polyvinyl alcohol (PVA) fibres, which are to date the best substitute for asbestos, were highly unlikely.
It was unexpectedly and surprisingly found that stereo-regular polypropylene fibres with a toughness comparable to that of PAN fibres, especially with a much lower elastic modulus and a higher elongation at break, give results equal to or better than those of PVA fibres.
The object of the present invention is a solid moulded manufactured product made by means of a hydraulically-moulded composition comprising water, hydraulic binders and reinforcing fibres, and additionally, implement fibres in an amount of 0 to 10% by weight of the total dry mixture, and fillers in an amount of 0 to 50% by weight of the total dry mixture where the reinforcing fibres comprise 0,1 to 5% by weight of the total dry mixture of highly crystalline polypropylene fibres having a tensile strength in the fibre state of more than 490 N/m2 and Q < 5 and 97 HI < 100 and 94 IPF < 100,Q being the ratio of the mean molecular weight by mass to the mean molecular weight by number, HI being the content of constituents insoluble in n-heptane at boiling in % by weight and IPF being the fraction of isotactic pentades in % moles, i.e. the molar fraction of groups consisting of five monomer units (pentades) chained in the isotactic configuration.
The fibres originally contained 0,05 to 10% by weight of a hydrophilic agent which was rendered practically insoluble on the surface of the fibres by reaction with calcium ions.
If the alkali metal salt content of alkoylphosphate is less than 0.05% by weight, the dispersion of the fibres is insufficient, but if it exceeds 10% by weight, the effect is not improved.
Q is the ratio of the average molecular weight by mass to the average molecular weight by number.
In this application, Q was measured using the gel permeation chromatography (GPC) method. (a) Measuring apparatus: ALC/GPC TYPE 150C, Waters Laboratory Co. (b) Column: TSK-GER GMH6-HT (high temperature type). (c) Solvent: orthodichlorobenzene (ODCB). (d) Temperature: 115°C. (e) Detector: thermal differential refractometer. (f) Volume of solvent flowing: 1 ml per minute.
Under the above conditions, a sample of highly crystalline polypropylene gives the following results:
- What?
- What?
Where is it?
Mw: mean molecular weight by massMw = [ΣNiMi²]/[ΣNiMi]Mn: mean molecular weight in numberMn = [ΣNiMi]/[ΣNi]Q: Mw/MnMFR ratio: fluidity index.
| Polymère | Mn | Mw | Q (Mw/Mn) | MFR (g/10 min) |
| Polypropylène hautement cristallin | 40000 | 140000 | 3,5 | 15 |
As a general rule, the ratio of mean molecular weight by mass to mean molecular weight by number is used as a measure of the degree of polydispersity and when this value is greater than 1 (monodispersity), the molecular weight distribution curve becomes wider.
The concentration of HI or fraction insoluble in n-heptane is measured by completely dissolving a sample of 5 g of polypropylene in 500 ml of xylene at boiling, pouring the mixture into 5 litres of methanol to collect the precipitate, drying it and extracting it in n-heptane at boiling for 6 hours using the Soxhlet technique to obtain an extraction residue.
Err1:Expecting ',' delimiter: line 1 column 260 (char 259)
The density of polypropylene in the pastel state is approximately 0,905, which is not significantly different from that of ordinary polypropylene.
Highly crystalline polypropylene fibres have preferably a tensile strength in the fibre state of 740 N/mm2 or more and Q 4.5 and HI 98 and IPF 96.
Fibers can be cut to uneven lengths of 2-15 mm, but preferably the length of the fibers ranges from 5-10 mm. The section of the fibers can be circular or irregular in shape, for example in an X or Y shape. The fibers can be creped while being stretched or after.
Fibers may also contain charges, such as calcium carbonate, amorphous silica, natural and synthetic calcium silicates and other minerals.
The fluidity index (FMI) of polypropylene is in the range 1 < FMI < 100, preferably 5 < FMI < 30 and more preferably 10 < FMI < 20.
The melt-state spinning temperature of the fibres can be kept relatively low to reduce entanglement or bending of the molecules and this temperature is preferably in the range of 260 to 280°C.
The temperature of the tensioning is preferably 140 to 150°C to improve the tensile performance as much as possible.
Polypropylene fibres are added in an amount of 0.1 to 5% by weight and preferably 0.3 to 4% by weight, compared to the total dry mixture.
The invention is described in more detail below.
For simplicity, cement is referred to as the preferred binder in this description. However, all other hydraulically-separated binders may be used instead of cement. Appropriate hydraulically-separated binders are understood to be materials containing inorganic cement and/or an inorganic binder or adhesive that hardens by hydration. Particularly suitable binder that hardens by hydration include, for example, Portland cement, high-aluminate cement, iron Portland cement, milking cement, tracer cement, plaster, calcium silicates formed by autoclave treatment and special binding combinations.
A wide variety of fillers and additives, which, for example, can have a favourable effect on the pore structure of a cement block or which, for example, can improve the dripping behaviour of suspensions on dripping machines, are frequently added to binders.
The solid manufactured product conforming to the invention may also contain inorganic fibres or organic fibres other than polypropylene fibres.
When other synthetic organic fibres are used in combination with polypropylene fibres, the total amount of reinforcing fibres should be kept between 0.3 and 5% by weight of the total dry mixture. The ratio of the amount of other synthetic organic reinforcing fibres to the total amount of reinforcing fibres should be between 0.1 and 0.9. Examples of such fibres are polyacrylonitrile, polyvinyl alcohol, polyamide, polyester, aramide, carbon and polyfin fibres.
Alternatively, in the case of natural or synthetic inorganic fibres used in combination with polypropylene fibres, the total amount of the fibre combination may be between 2 and 20% by weight of the total dry mixture. The amount of polypropylene fibres used in such combinations should be between 0.3 and 5% by weight of the total dry mixture. Examples of inorganic fibres are glass fibres, rock wool, milk wool, wollastonite fibres, asbestos, sepillite, ceramic fibres and the like.
The manufacture of fibres used according to the invention is not the subject of this patent application. It is carried out, for example, following a known molten-state spinning process. These high-strength fibres can be produced, for example, as follows:
Polypropylene resin pellets with a melting point of 165°C with Q = 3.5, HI = 98, IPF = 97 and a fluidity index of 15 g per 10 minutes are spun at 275°C and the fibers are stretched at 150°C by a factor of 4.5 by a hot-cylinder drying process, soaked with surfactant, left to rest until the next day and air-dried. The resulting fibers have a dener of 1.9, a tensile strength of 770 N per mm2 and a breaking elongation of 25%. The fibers are cut before being used in building material mixtures.
To compare the fibers of highly crystalline polypropylene with other fibers, the following nine compositions are prepared.
Kraft pulp of refined cellulose up to 65°SR (Shopper-Riegler) is mixed with amorphous silica, inert fillers, cement and synthetic fibres at a solid concentration of 200 g per litre of complete suspension.
This suspension of fibres and cement is further diluted with water to a concentration of 30 g per litre and then transferred to a Hatschek machine.
Shortly before introducing the suspension into the basin, an additional 200 ppm of a polyacrylamide-type flocculant agent is added to improve cement retention.
The plates are produced by machine by 18 turns of the forming cylinder, and then pressed between oiled steel molds in a press under a specific pressure of 250 bar, to an average thickness of 6 mm.
The leaves are hardened under plastic cover for 28 days in a relative humidity of 100% at 20°C.
The mechanical tests shall be carried out in the wet state, i.e. under water saturation conditions according to ISO 4150
The results are given in Table II below.
The bending resistance of the samples is determined on an Instron mechanical test machine during a conventional bending test at three points.
MDR is the modulus of refraction in newtons per mm2 (N per mm2) given by the formula: Where is it?
M = (newton breakload x distance between supports) /4,W = (average sample thickness value) 2 x sample dimension measured parallel to the supports) /6.
The breakdown work under the maximum IMDR load, expressed in joules per m2 (J per m2), is the integral of the stress-strain function up to the breakdown load P.
The breakdown work (IPL20) is the integral of the stress-strain function, also expressed in J per m2, until the load (order of curve) has decreased to 20% of the maximum P value reached.
As can be inferred from the wet test table (Table II), the product manufactured in accordance with the invention is more ductile and has a strength comparable to that obtained with the best reinforcing fibres currently used in products manufactured from fibre reinforced cement.
The following compositions are prepared and cured under plastic cover for 28 days at 100% relative humidity and 20°C, and then subjected to an accelerated ageing test consisting of the following cycles:
1 - 72 hours immersion in water at 20°C.2 - 72 hours drying in the oven at 80°C.
The above treatment is repeated eight times and then the average energy of rupture in both directions relative to the orientation of the fibres in the sheet is determined under water saturation conditions.
When the fibres of the invention are used, not only is the energy of rupture much higher than with traditional fibres, but after eight cycles of water and heat treatment, this energy is fully conserved while the other fibres have lost more than 50% of their efficiency.
The results are given in Table III below. TABLEAU III
TABLEAU III
| Composition (kg) | 10 | 11 | 12 | 13 | Energie de rupture (kJ/m²) avec les fibres en question | |
| Après 28 jours | Après 8 cycles | |||||
| PVA | 2 | - | - | - | 5,0 | 2,0 |
| PAN | - | 2 | - | - | 2,5 | 1,0 |
| PVA modifié | - | - | 2 | - | 2,5 | 1,0 |
| PP (*) | - | - | - | 2 | 9,2 | 9,2 |
| Cellulose 35°SR | 4 | 4 | 4 | 4 | ||
| Charge inerte de CaCO₃ | 13 | 13 | 13 | 13 | ||
| Silice amorphe | 2 | 2 | 2 | 2 | ||
| Ciment | 79 | 79 | 79 | 79 | ||
| Total (kg) | 100 | 100 | 100 | 100 | ||
| (*) Fibre de PP conforme à l'invention. |
Claims (15)
- Shaped solid article manufactured with a hydraulically setting composition comprising water, hydraulic binders and reinforcing fibres and moreover process fibres in an amount of 0-10 wt% with respect to the total dry mix and fillers in an amount of 0-50 wt% with respect to the total dry mix, characterized in that the reinforcing fibres comprise from 0.1-5 wt% with respect to the total dry mix of highly crystalline polypropylene fibres possessing a fibre breakage strength of over 490 N/mm², and having Q < 5 and 97 < HI < 100, and 94 < IPF < 100, Q being the ratio of weight-average molecular weight to number-average molecular weight, HI being the boiling n-heptane insoluble content in wt% and IPF being the isotactic pentad fraction in mol%, the fibres having contained initially from 0.05 to 10 wt% of a hydrophilizing agent which has been made practically insoluble on the fibre surface by reacting with calcium ions.
- Article according to claim 1, characterized in that the reinforcing fibres comprise from 0.3 to 4 wt% with respect to the total dry mix of highly crystalline polypropylene fibres.
- Article according to anyone of the preceding claims, characterized in that the polypropylene fibres possess a fibre breakage strength of 740 N/mm² or more and have Q ≦ 4.5, HI ≦ 98 and IPF ≦ 96.
- Article according to anyone of the preceding claims, characterized in that the denier (d) of the polypropylene fibres is in the range of 0.5 < d < 20.
- Article according to anyone of the preceding claims, characterized in that the polypropylene fibre length ranges from 2 to 15 mm.
- Article according to anyone of the preceding claims, characterized in that the polypropylene fibre length ranges between 5 and 10 mm.
- Article according to anyone of the preceding claims, characterized in that the polypropylene fibre section is circular.
- Article according to anyone of claims 1 to 6, characterized in that the polypropylene fibres have an irregular, substantially X-shaped cross-section.
- Article according to anyone of claims 1 to 6, characterized in that the polypropylene fibres have an irregular, substantially Y-shaped cross-section.
- Article according to anyone of the preceding claims, characterized in that the polypropylene fibres are crimped.
- Article according to anyone of the preceding claims, characterized in that the polypropylene fibres comprise fillers.
- Article according to anyone of the preceding claims, characterized in that the reinforcing fibres comprise synthetic organic fibres other than polypropylene fibres.
- Article according to anyone of the preceding claims, characterized in that the reinforcing fibres further comprise inorganic fibres.
- Article according to anyone of the preceding claims, characterized in that the hydrophilizing agent is an alkyl phosphate alkali metal salt, with 8 to 18 carbon atoms.
- Article according to claim 14, characterized in that the alkali metal salt is chosen within the group comprising sodium salt and potassium salt.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP282268/91 | 1991-10-01 | ||
| JP28226891 | 1991-10-01 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| HK1007309B true HK1007309B (en) | 1999-04-09 |
| HK1007309A1 HK1007309A1 (en) | 1999-04-09 |
Family
ID=17650242
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| HK98106532A HK1007309A1 (en) | 1991-10-01 | 1998-06-24 | Moulded solid products reinforced with fibres |
Country Status (19)
| Country | Link |
|---|---|
| US (2) | US5338357A (en) |
| EP (2) | EP0537129B1 (en) |
| JP (2) | JP2633763B2 (en) |
| CN (1) | CN1050346C (en) |
| AT (1) | ATE129992T1 (en) |
| BR (1) | BR9203102A (en) |
| CA (1) | CA2077395C (en) |
| CZ (1) | CZ287155B6 (en) |
| DE (2) | DE69205942T2 (en) |
| DK (1) | DK0537129T3 (en) |
| ES (1) | ES2080476T3 (en) |
| FI (1) | FI105912B (en) |
| GR (1) | GR3018655T3 (en) |
| HK (1) | HK1007309A1 (en) |
| HU (1) | HU214790B (en) |
| MX (2) | MX9204566A (en) |
| PL (1) | PL170636B1 (en) |
| SK (1) | SK280257B6 (en) |
| ZA (1) | ZA925720B (en) |
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| US3060552A (en) * | 1953-07-09 | 1962-10-30 | Scheyer Emanuel | Heat reflective filament |
| JPS4929129B1 (en) * | 1970-04-07 | 1974-08-01 | ||
| FR2389583B1 (en) * | 1977-05-05 | 1984-11-30 | Eternit Fab Dansk As | |
| BR7807232A (en) * | 1978-11-01 | 1980-05-06 | Dansk Eternitfab As | PROCESS FOR MANUFACTURING A CONSTRUCTION PRODUCT, POLYPROPYLENE REINFORCING FIBERS, PROCESS FOR PREPARING REINFORCED POLYPROPYLENE FIBERS, AND CONSTRUCTION PRODUCT |
| FI67072C (en) * | 1979-02-09 | 1985-01-10 | Amiantus Ag | FOER FARING FOER FRAMSTAELLNING AV FIBERFOERSTAERKT HYDRAULISKT BINDANDE MATERIAL |
| US4407676A (en) * | 1981-11-25 | 1983-10-04 | Restrepo Jose M | Fiber-reinforced cement and process |
| NL8105453A (en) * | 1981-12-03 | 1983-07-01 | Stamicarbon | METHOD FOR REINFORCING WATER-CURING INORGANIC MATERIALS |
| DE3305629A1 (en) * | 1983-02-18 | 1984-08-23 | Akzo Gmbh, 5600 Wuppertal | METHOD FOR PRODUCING POLYESTER FIBERS |
| HUT48185A (en) * | 1985-10-23 | 1989-05-29 | Mta Termeszettu Domanyi Kutato | Process for producing building units, particularly prefabricated building units from after-hardening material mixture containing reinforcing fibres |
| JPH0192475A (en) * | 1987-09-30 | 1989-04-11 | Takemoto Oil & Fat Co Ltd | Oil composition for treating synthetic fiber |
| EP0343148A3 (en) * | 1988-05-17 | 1990-08-22 | Walter Basta | Specially treated plastic fibre for improved building materials |
| US5009651A (en) * | 1988-09-06 | 1991-04-23 | Kao Corporation | Surface material for sanitary articles and its preparing method |
| US5112405A (en) * | 1989-01-24 | 1992-05-12 | Sanchez Michael A | Lightweight concrete building product |
| US4969956A (en) * | 1989-12-19 | 1990-11-13 | The United States Of America As Represented By The Secretary Of Commerce | Transparent thin film thermocouple |
| JP2633763B2 (en) * | 1991-10-01 | 1997-07-23 | 大和紡績株式会社 | Polypropylene fiber for cement reinforcement |
-
1992
- 1992-05-15 JP JP4123959A patent/JP2633763B2/en not_active Expired - Fee Related
- 1992-07-13 JP JP4185525A patent/JP2633772B2/en not_active Expired - Lifetime
- 1992-07-30 ZA ZA925720A patent/ZA925720B/en unknown
- 1992-08-03 DK DK92870115.0T patent/DK0537129T3/en active
- 1992-08-03 ES ES92870115T patent/ES2080476T3/en not_active Expired - Lifetime
- 1992-08-03 AT AT92870115T patent/ATE129992T1/en not_active IP Right Cessation
- 1992-08-03 EP EP92870115A patent/EP0537129B1/en not_active Expired - Lifetime
- 1992-08-03 US US07/923,596 patent/US5338357A/en not_active Expired - Fee Related
- 1992-08-03 PL PL92295506A patent/PL170636B1/en not_active IP Right Cessation
- 1992-08-03 SK SK2410-92A patent/SK280257B6/en unknown
- 1992-08-03 CN CN92109754A patent/CN1050346C/en not_active Expired - Fee Related
- 1992-08-03 FI FI923503A patent/FI105912B/en active
- 1992-08-03 DE DE69205942T patent/DE69205942T2/en not_active Expired - Fee Related
- 1992-08-03 CZ CS19922410A patent/CZ287155B6/en not_active IP Right Cessation
- 1992-08-03 HU HU9202517A patent/HU214790B/en not_active IP Right Cessation
- 1992-08-06 MX MX9204566A patent/MX9204566A/en not_active IP Right Cessation
- 1992-08-11 BR BR929203102A patent/BR9203102A/en not_active IP Right Cessation
- 1992-08-27 DE DE69206565T patent/DE69206565T2/en not_active Expired - Lifetime
- 1992-08-27 EP EP92114661A patent/EP0535373B1/en not_active Expired - Lifetime
- 1992-09-02 CA CA002077395A patent/CA2077395C/en not_active Expired - Lifetime
- 1992-09-30 MX MX9205584A patent/MX9205584A/en unknown
-
1994
- 1994-05-27 US US08/250,658 patent/US6010786A/en not_active Expired - Lifetime
-
1996
- 1996-01-11 GR GR960400053T patent/GR3018655T3/en unknown
-
1998
- 1998-06-24 HK HK98106532A patent/HK1007309A1/en not_active IP Right Cessation
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