EP0000579B1 - Procédé de préparation de résines synthétiques anorganiques-organiques - Google Patents
Procédé de préparation de résines synthétiques anorganiques-organiques Download PDFInfo
- Publication number
- EP0000579B1 EP0000579B1 EP78100504A EP78100504A EP0000579B1 EP 0000579 B1 EP0000579 B1 EP 0000579B1 EP 78100504 A EP78100504 A EP 78100504A EP 78100504 A EP78100504 A EP 78100504A EP 0000579 B1 EP0000579 B1 EP 0000579B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sec
- weight
- polyisocyanate
- inorganic
- aqueous
- 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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3893—Low-molecular-weight compounds having heteroatoms other than oxygen containing silicon
- C08G18/3895—Inorganic compounds, e.g. aqueous alkalimetalsilicate solutions; Organic derivatives thereof containing no direct silicon-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/775—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur sulfur
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Definitions
- Inorganic-organic plastics based on polyisocyanates and aqueous alkali silicate solutions are known; see e.g. DT-OS 1 770 384, 2 227 147, 2 359 606, 2 359 607, 2 359 606, 2 359 609.2 359 610.2 359 611.2 359 612, DT-AS 2 325 909 and 2 310 559.
- plastics can be produced which, due to the inorganic components, have above all improved fire resistance compared to purely organic substances and which, depending on the composition and reaction conditions, can be foamed or unfoamed, hard or soft, brittle or flexible. Due to the great variability of the properties, these inorganic-organic plastics offer a wide range of possible applications.
- the plastics resulting from a W / 0 type dispersion are particularly interesting. They have high mechanical strengths, even when exposed to moisture, because the hardened, coherent organic phase envelops and thus fixes the likewise hardened aqueous, inorganic, incoherent phase.
- the perfect coherent organic phase of these plastics also depends on the improved fire resistance of such systems due to the amount of water enclosed.
- the invention is based, to avoid the disadvantages described above and to produce inorganic-organic plastics, even with high amounts of inorganic components, the task.
- the process according to the invention can be carried out continuously or preferably batchwise.
- the stable primary dispersion is first prepared from polyisocyanate, aqueous alkali silicate solution or aqueous silica sol and optionally further additives (components d) and / or e)) such as activators, emulsifiers and blowing agents and then component c) is added.
- component c component c
- the primary dispersion is generated in advance in a prechamber in accordance with the discontinuous mode of operation by means of a special mechanical arrangement, and mixing with component c) takes place continuously in a downstream mixing head.
- the individual components are mixed, for example, in the order that first spatially and temporally from components a) and b), optionally with the addition of all or part of components d) and / or e), a dispersion with the aid of a Mixing unit is produced and this dispersion in a spatially and temporally thereafter arranged mixing / aggregate component c), optionally with the addition of all or part of component d) and / or e) is added.
- Starting components (component a) to be used according to the invention are aliphatic, cycloaliphatic, araliphatic, aromatic and heterocyclic polyisocyanates, such as those e.g. by W. Siefken in Justus Liebigs Annalen der Chemie, 562, pages 75 to 136, for example those as mentioned in DE-A-2 647 482, pages 5-6.
- distillation residues obtained in the industrial production of isocyanate groups optionally dissolved in one or more of the above. called polyisocyanates to use. It is also possible to use any mixtures of the aforementioned polyisocyanates.
- polyisocyanates e.g. 2,4- and 2,6-tolylene diisocyanate as well as any mixtures of these isomers
- TDI polyisocyanates
- polyphenylpolymethylene polyisocyanates such as those produced by aniline-formaldehyde condensation and subsequent phosgenation ("crude MDI") and carbodiimide groups, urethane groups, Allophanate groups, isocyanurate groups, urea groups or biuret groups containing polyisocyanates ("modified polyisocyanates").
- polyisocyanates containing ionic groups for example sulfonated polyisocyanates (DE-A-2 227 111, 2 359 614, 2 359 615), polyisocyanates containing carboxylate groups (DE - A - 2 359 613).
- nonionic-hydrophilic polyisocyanates as described in DE-A-2 325 909, furthermore polyisocyanates containing polar groups according to DE-A-2 359 608 and phenolic OH groups containing polyisocyanates, as described in US Pat DE - A - 2 359 616.
- polyisocyanates are preferably made from polyphenyl-polymethylene polyisocyanates, such as those produced by aniline-formaldehyde condensation and subsequent phosgenation ('crude MDI'), and from the distillation residues obtainable therefrom by distillation of two-core products, which generally have a viscosity have between 5000 and 5000 000 mPa s / 25 ° C, an NCO content of 28-33 weight percent and a functionality> 2.
- aqueous alkali silicate solutions or alkaline stabilized aqueous silica sols with an inorganic solid content of 20-80% by weight are also used as starting components (component b). preferably 30-70 wt .-%, used.
- Aqueous solutions of alkali silicates are to be understood as meaning the solutions of sodium and / or potassium silicate in water which are usually referred to as “water glasses”.
- Raw technical solutions which are e.g. Calcium silicate, magnesium silicate, borates and aluminates can be used.
- the molar ratio Me 2 0 / S'0 2 (Me alkali metal, eg Na, K.) Is not critical and can fluctuate within the usual limits; preferably it is 1: 1.6 to 1: 3.3. If the water content of the plastic initially obtained by reaction with the polyisocyanate plays a minor role because water does not interfere or because it can be easily removed by drying, then only alkaline sodium silicate, of which 20-35% by weight can be used, can be safely used. Have% solutions made. Preferably, however, 32-54% by weight silicate solutions are used which only have the viscosity of less than 50,000 mPas required for problem-free processing if they are sufficiently alkaline. Ammonium silicate solutions, for example solutions of guanidinium silicate, can also be used, but these are less preferred. It can be real or colloidal solutions.
- concentration mainly depends on the desired end product.
- Compact or closed-cell materials are preferably made with concentrated silicate solutions, which are adjusted to low viscosity if necessary by adding alkali hydroxide. In this way, 40-70% by weight solutions can be produced.
- silicate solutions with a 30-35% by weight content are preferred for the production of open-pore lightweight foams in order to achieve low viscosities, sufficiently long reaction times and low densities. Even when using finely divided inorganic fillers in larger quantities, silicate solutions of 30-35% content are preferred.
- alkali silicate solutions which can be used according to the invention can be found in James G. Vail 'Soluble Silicates, their properties and uses', Reinhold Publishing Corporation, New York 1952.
- Component c) can also be identical to component b) in some cases.
- component c) are water, an aqueous alkali silicate solution or an aqueous suspension of fillers which have a solids content of between 20 and 80% by weight and at least 50% by weight of a particle size of less than 50 microns (preferably 50% by weight below 10 microns) to understand.
- Inert mineral fillers or also hydraulic mineral binders are preferably suitable as fillers. If the dry fillers already meet the particle size criteria according to the invention (at least 50% by weight less than 50 microns), they can be mixed directly with water to form a suspension. Are the particles coarser, an aqueous coarse suspension of the fillers can also be converted into a fine suspension usable according to the invention by known methods of wet grinding.
- Particularly preferred aqueous suspensions are those which are stable to sedimentation and show viscous, rapid flow behavior, as is known, for example, from paper coating slips. To produce such filler suspensions, it is therefore advantageous to use the methods known for the preparation of such coating slips.
- the filler suspension can also be prepared immediately before the addition, e.g. by metering dry fillers and water into a feed line to the mixing room in which the polyisocyanate is mixed with aqueous alkali silicate and by means of a mixing device, e.g. a screw within this feed line, the aqueous filler suspension is generated in situ.
- a mixing device e.g. a screw within this feed line
- hydraulic binders especially cement
- the use of hydraulic binders, especially cement generally requires suspension in water or aqueous alkali silicate immediately before processing with the isocyanate component, so that the setting process and any gelation process possibly caused by cement expediently take place in the finished plastic.
- the filler suspensions used preferably have a viscosity above 100 mPa s in order to ensure rheological behavior which is favorable for processing. On the other hand, they should be easy to flow and should in no way have crumbly consistency. A viscosity of 10,000 mPas is preferably not exceeded. A good and very intimate mixture with the polyisocyanate in conventional processing equipment should be ensured. On the other hand, the content of fillers in the aqueous suspension should be as high as possible in order not to introduce more water than is absolutely necessary into the plastic. Depending on the particle size and the shape of the filler particles, the filler concentration is between 20 and 80%. A content of 30-70% is preferred. Lower concentrations generally have to be selected if non-spherical fillers are also used, e.g. Asbestos, talc, clays or special iron oxides.
- isocyanate catalysts (component d) are also often used, e.g. those as described in DE-A-2 647 482, pages 13-15.
- the catalysts are generally used in an amount between about 0.001 and 10% by weight, based on the amount of polyisocyanate.
- customary additives can also be used, including the substances mentioned below: surface-active additives such as emulsifiers and foam stabilizers, reaction retarders, cell regulators of the type known per se, pigments, dyes, flame retardants of the type known per se, and further Stabilizers against aging and weather influences, plasticizers and fungistatic and bacteriostatic substances (see, for example, DE - A - 2 647 482, pages 15-16), volatile organic substances as blowing agents.
- surface-active additives such as emulsifiers and foam stabilizers, reaction retarders, cell regulators of the type known per se, pigments, dyes, flame retardants of the type known per se, and further Stabilizers against aging and weather influences, plasticizers and fungistatic and bacteriostatic substances (see, for example, DE - A - 2 647 482, pages 15-16), volatile organic substances as blowing agents.
- organic blowing agents come e.g.
- Acetone, ethyl acetate, halogen-substituted alkanes such as methylene chloride, chloroform, ethylidene chloride, vinylidene chloride, monofluorotrichloromethane, chlorodifluoromethane, dichlorodifluoromethane, butane, hexane, heptane or diethyl ether are also suitable.
- a blowing effect can also be achieved by adding compounds which decompose at temperatures above room temperature with the elimination of gases, for example nitrogen.
- Azo compounds such as azoisobutyronitrile can be achieved.
- Suspensions as component c) which are prepared with the addition of 0.05 to 20% by weight, based on filler, of one or more of the additives listed under 1), 2) and 3) are particularly preferred.
- the mixing of the reaction components is preferably carried out at room temperature.
- the choice of the mixing process largely depends on the type of component c) used.
- the batch process is preferably used when the following fillers component e) are used as aqueous suspensions with component c) (since they partially spontaneously gel aqueous alkali silicates): calcium hydroxide, magnesium hydroxide, calcium carbonate, magnesium carbonate, chalk, lime, dolomite, calcium sulfate , Gypsum and anhydride.
- fillers (component e) in a suspension as component c) which allow the use of both the batch and the continuous process (those which do not or only slowly gel aqueous alkali silicates) are e.g. Iron oxides, aluminum oxides, quartz powder, clays, asbestos, glasses in powder form, silicate minerals and water cements such as red ribbon cement, fast-setting cement or alumina cement.
- dispersions are generally obtained; which, with an increasing proportion of inorganic components and changing the W / O phase structure, undergo unstable dispersion states which, after hardening, can lead to disruptions in the structure of the inorganic-organic plastic, because inorganic substances, introduced by conventional mixing techniques, can initiate segregation processes and thus the production prevent technically usable inorganic-organic plastics.
- plastics that can be produced according to the invention including foams, open up new possibilities in building construction and civil engineering as well as in the manufacture of finished parts and elements.
- Examples of possible applications include the manufacture of convertible elements in prefabricated buildings, lost formwork, roller shutter boxes, window sills, railway and subway sleepers, curbs, stairs, the foaming of joints and the back-foaming of ceramic tiles.
- the foam concrete can also be used advantageously to bind gravel, marble pieces, etc. You can get decorative panels such as those used as facade elements.
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Polyurethanes Or Polyureas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Claims (6)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2734691 | 1977-08-02 | ||
DE19772734691 DE2734691A1 (de) | 1977-08-02 | 1977-08-02 | Verfahren zur herstellung anorganisch-organischer kunststoffe |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0000579A1 EP0000579A1 (fr) | 1979-02-07 |
EP0000579B1 true EP0000579B1 (fr) | 1980-10-29 |
Family
ID=6015397
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP78100504A Expired EP0000579B1 (fr) | 1977-08-02 | 1978-07-26 | Procédé de préparation de résines synthétiques anorganiques-organiques |
Country Status (5)
Country | Link |
---|---|
US (1) | US4276404A (fr) |
EP (1) | EP0000579B1 (fr) |
JP (1) | JPS5428398A (fr) |
DE (2) | DE2734691A1 (fr) |
IT (1) | IT1105389B (fr) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0016262A1 (fr) * | 1979-03-06 | 1980-10-01 | Bergwerksverband GmbH | Procédé de consolidation et d'étanchéification de formations géologiques et d'entassements non compacts de roches et de masses de terre |
EP0099531A2 (fr) * | 1982-07-23 | 1984-02-01 | BASF Aktiengesellschaft | Solutions de silicates alcalins stabilisées, procédé pour leur préparation, leur utilisation pour la fabrication de matériaux mousses à partir d'organosilicates et procédé pour la préparation de ces organosilicates mousses |
US4669919A (en) * | 1984-06-06 | 1987-06-02 | Kvt Kunststoffverfahrenstechnik Gmbh & Co. | Process for consolidation and sealing coal and/or rock, soil and brick formations in mining, tunnelling and construction |
DE3625278A1 (de) * | 1986-07-25 | 1988-01-28 | Kvt Kunststoff | Verfahren zur herstellung von anorganisch-organischen schaumstoffen |
US4827005A (en) * | 1984-06-06 | 1989-05-02 | Kvt Kunststoffverfahrenstechnik Gmbh & Co. | Organomineral products, a process for their manufacture and their use |
WO2001058975A1 (fr) | 2000-02-08 | 2001-08-16 | Fosroc International Limited | Compositions pour la fabrication de produits organo-mineraux, produits ainsi obtenus et leur utilisation |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
USRE31946E (en) * | 1979-03-06 | 1985-07-16 | Bergwerksverband Gmbh | Process for consolidating and sealing off geological and artificially deposited rock and earth formations |
US4518718A (en) * | 1984-05-18 | 1985-05-21 | The United States Of America As Represented By The United States Department Of Energy | Rigid zeolite containing polyurethane foams |
KR20060011868A (ko) * | 2003-05-15 | 2006-02-03 | 헌트스만 인터내셔날, 엘엘씨 | 샌드위치 패널용 폴리이소시아네이트 기재 접착제 배합물 |
US20060166834A1 (en) * | 2004-02-10 | 2006-07-27 | Halliburton Energy Services, Inc. | Subterranean treatment fluids comprising substantially hydrated cement particulates |
BE1018111A3 (nl) * | 2008-04-29 | 2010-05-04 | Maras Monique Georgette H | Werkwijze voor het bekomen van een brandwerend schuim. |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3826769A (en) * | 1969-07-14 | 1974-07-30 | Minnesota Mining & Mfg | Self-emulsified polyurethanes prepared by direct sulfonation of isocyanate |
US4097423A (en) * | 1972-06-03 | 1978-06-27 | Bayer Aktiengesellschaft | Inorganic-organic compositions |
DE2310559C3 (de) * | 1973-03-02 | 1975-09-11 | Bayer Ag, 5090 Leverkusen | Schaumbeton, ein Verfahren zu seiner Herstellung und seine Verwendung zur Herstellung von Bauelementen |
US4057519A (en) * | 1974-09-05 | 1977-11-08 | H. H. Robertson Company | Sodium silicate extended polyurethane foam |
DE2512170C3 (de) * | 1975-03-20 | 1981-06-11 | Bayer Ag, 5090 Leverkusen | Verfahren zur Herstellung von gegebenenfalls schaumförmigem, harten anorganisch-organischem Verbundmaterial |
DE2524191C3 (de) * | 1975-05-31 | 1980-04-03 | Bayer Ag, 5090 Leverkusen | Verfahren zur Herstellung bochgeffillter hydrophober Harnstoffgruppen enthaltender Leichtschaumstoffe |
DE2734690A1 (de) * | 1977-08-02 | 1979-02-08 | Bayer Ag | Verfahren zur herstellung anorganisch-organischer kunststoffe |
-
1977
- 1977-08-02 DE DE19772734691 patent/DE2734691A1/de not_active Withdrawn
-
1978
- 1978-07-26 DE DE7878100504T patent/DE2860257D1/de not_active Expired
- 1978-07-26 EP EP78100504A patent/EP0000579B1/fr not_active Expired
- 1978-07-31 IT IT50543/78A patent/IT1105389B/it active
- 1978-08-01 US US05/930,128 patent/US4276404A/en not_active Expired - Lifetime
- 1978-08-01 JP JP9324278A patent/JPS5428398A/ja active Granted
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0016262A1 (fr) * | 1979-03-06 | 1980-10-01 | Bergwerksverband GmbH | Procédé de consolidation et d'étanchéification de formations géologiques et d'entassements non compacts de roches et de masses de terre |
EP0099531A2 (fr) * | 1982-07-23 | 1984-02-01 | BASF Aktiengesellschaft | Solutions de silicates alcalins stabilisées, procédé pour leur préparation, leur utilisation pour la fabrication de matériaux mousses à partir d'organosilicates et procédé pour la préparation de ces organosilicates mousses |
EP0099531A3 (en) * | 1982-07-23 | 1986-12-10 | Basf Aktiengesellschaft | Stable water-glass solutions, process for preparing them, their use in producing organosilicate foam plastics, and process for preraring these organosilicate foams |
US4669919A (en) * | 1984-06-06 | 1987-06-02 | Kvt Kunststoffverfahrenstechnik Gmbh & Co. | Process for consolidation and sealing coal and/or rock, soil and brick formations in mining, tunnelling and construction |
US4827005A (en) * | 1984-06-06 | 1989-05-02 | Kvt Kunststoffverfahrenstechnik Gmbh & Co. | Organomineral products, a process for their manufacture and their use |
US4871829A (en) * | 1984-06-06 | 1989-10-03 | Kvt Kunststoffverfahrenstechnik Gmbh & Co. | Organomineral products, a process for their manufacture and their use |
DE3625278A1 (de) * | 1986-07-25 | 1988-01-28 | Kvt Kunststoff | Verfahren zur herstellung von anorganisch-organischen schaumstoffen |
WO2001058975A1 (fr) | 2000-02-08 | 2001-08-16 | Fosroc International Limited | Compositions pour la fabrication de produits organo-mineraux, produits ainsi obtenus et leur utilisation |
Also Published As
Publication number | Publication date |
---|---|
IT1105389B (it) | 1985-10-28 |
JPS5428398A (en) | 1979-03-02 |
EP0000579A1 (fr) | 1979-02-07 |
JPS5519929B2 (fr) | 1980-05-29 |
IT7850543A0 (it) | 1978-07-31 |
DE2860257D1 (en) | 1981-01-29 |
DE2734691A1 (de) | 1979-02-08 |
US4276404A (en) | 1981-06-30 |
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