NO166537B - PROCEDURE FOR THE PREPARATION OF ORGANOSIL-CONTAINING ASPALT PASSES. - Google Patents
PROCEDURE FOR THE PREPARATION OF ORGANOSIL-CONTAINING ASPALT PASSES. Download PDFInfo
- Publication number
- NO166537B NO166537B NO832926A NO832926A NO166537B NO 166537 B NO166537 B NO 166537B NO 832926 A NO832926 A NO 832926A NO 832926 A NO832926 A NO 832926A NO 166537 B NO166537 B NO 166537B
- Authority
- NO
- Norway
- Prior art keywords
- organosilane
- mixture
- bitumen
- asphalt
- production
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title description 2
- 239000010426 asphalt Substances 0.000 claims abstract description 34
- 150000001282 organosilanes Chemical class 0.000 claims abstract description 34
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 239000011707 mineral Substances 0.000 claims abstract description 12
- 239000006229 carbon black Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims description 9
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims description 2
- 125000003545 alkoxy group Chemical group 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 1
- 239000000470 constituent Substances 0.000 abstract 1
- 239000004575 stone Substances 0.000 description 7
- 150000004756 silanes Chemical class 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- 229910003480 inorganic solid Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- 239000011384 asphalt concrete Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011044 quartzite Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 description 1
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Civil Engineering (AREA)
- Engineering & Computer Science (AREA)
- Structural Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Road Paving Structures (AREA)
- Working-Up Tar And Pitch (AREA)
- Special Wing (AREA)
- Window Of Vehicle (AREA)
- Fittings On The Vehicle Exterior For Carrying Loads, And Devices For Holding Or Mounting Articles (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Silicon Polymers (AREA)
- Road Paving Machines (AREA)
Abstract
Description
Oppfinnelsen angår en fremgangsmåte til fremstilling av organosilanholdige asfaltmasser som er egnet for påføring eksempelvis som gatebelegg. The invention relates to a method for the production of organosilane-containing asphalt compounds which are suitable for application, for example, as street coverings.
Organosilanholdige asfaltmasser er kjent fra forskjellige publikasjoner. Organosilane-containing asphalt compounds are known from various publications.
DE-OS 3.028.365 beskriver bituminøse bindemidler som minst inneholder et organosilan. De fremstilles ved innrøring av organosilanet i det til 120-230°C oppvarmede og således flytendegjorte bitumen. DE-OS 3,028,365 describes bituminous binders containing at least one organosilane. They are produced by stirring the organosilane into the bitumen heated to 120-230°C and thus liquefied.
I US-PS 4.036.661 omtales organosilanholdige asfaltmasser. Også i dette tilfellet foregår først tilsetningen av silanet til det smeltede bitumen som deretter blandes med mineralske bestanddeler til en som gatebelegg egnet asfalt. US-PS 4,036,661 mentions organosilane-containing asphalt compounds. In this case, too, the silane is first added to the melted bitumen, which is then mixed with mineral components to form an asphalt suitable as a road surface.
I TJS-PS 4.036.661 angis også at de mineralske bestanddeler før blandingen med bitumen kan behandles med oppløsningen av et organosilan. På grunn av økologiske belastninger og den økende brannfare som kan frembringes ved hjelp av oppløs-ningsmidlet ble det med den teoretiske omtale av disse fremgangsmåtevarianter. In TJS-PS 4,036,661 it is also stated that the mineral components can be treated with the solution of an organosilane before the mixture with bitumen. Due to ecological stress and the increasing risk of fire that can be created with the help of the solvent, there was a theoretical discussion of these method variants.
Formålet med organosilantilsetningen består i alle tilfeller i å øke klebingen mellom bitumen og asfaltens mineralske bestanddeler. The purpose of the organosilane addition is in all cases to increase the adhesion between the bitumen and the mineral components of the asphalt.
De kjente fremgangsmåter har imidlertid den ulempe at organosilanet må tilsettes til den varme bitumen. Dette fører til en lang termisk belastning av silanene som alt etter stoffegenskaper kan ha til følge stofftap og økologisk belastning ved fordamping eller spalting av silanene. However, the known methods have the disadvantage that the organosilane must be added to the hot bitumen. This leads to a long thermal load on the silanes which, depending on the material properties, can result in material loss and ecological stress through evaporation or decomposition of the silanes.
Oppfinnelsens oppgave er å tilveiebringe en fremgangsmåte til fremstilling av organosilanholdige asfaltmasser som ikke har disse ulemper. The task of the invention is to provide a method for the production of organosilane-containing asphalt compounds which do not have these disadvantages.
I henhold til dette angår foreliggende oppfinnelse en fremgangsmåte for fremstilling av organosilanholdige asfaltmasser og denne fremgangsmåte karakteriseres ved at minst ett organosilan i form av en findelt blanding som består av minst ett organosilan og sot, blandes med mineralske bestanddeler, og denne blanding sammenblandes deretter med flytende bitumen.. According to this, the present invention relates to a method for producing organosilane-containing asphalt compounds and this method is characterized by at least one organosilane in the form of a finely divided mixture consisting of at least one organosilane and carbon black, mixed with mineral components, and this mixture is then mixed with liquid bitumen..
De mineralske bestanddeler består av de materialer slik de etter kornklasser oppdeles i splitt (2-32 mm korning), bruddsand (0,09-2 mm) og fyllstoff (£ 0,09 mm) etter de tekniske forskrifter for bygningsmyndighetene for fremstilling av asfaltbelegg tilblandes til bitumen. The mineral components consist of the materials as they are divided according to grain classes into crushed stone (2-32 mm grain size), quarry sand (0.09-2 mm) and filler (£ 0.09 mm) according to the technical regulations for the building authorities for the production of asphalt pavements mixed into bitumen.
I en egnet utføre.Tsesf orm kan man som findelt uorganisk faststoff anvende fyllstoffene som for fremstilling av den organosilanholdige blanding påsprøytes eller på annen egnet måte fuktes med minst et organosilan. In a suitable embodiment, as finely divided inorganic solids, fillers can be used which, for the preparation of the organosilane-containing mixture, are sprayed on or moistened in another suitable way with at least one organosilane.
Derved kan man så vel behandle den samlede mengde eller også bare en del av det for fremstillingen av asf altbelegget nødvendige fyllstoff' med organosilan. Thereby, the total amount or even just a part of the filler required for the production of the asphalt coating can be treated with organosilane.
Sammenblandingen av en pulverformet organosilan/sotblanding som inneholder 30-60 vekt-St, fortrinnsvis 47-53 vekt-# av minst et organosilan, beregnet på den samlede mengde, er spesielt egnet for fremstilling av asfaltmasser, behandlingen av en slik blanding kan foretas analogt den i DE-PS 2.747.277 omtalte fremgangsmåte. Organosilan/sotblandingen kan etter valg først sammenblandes med en bestanddel, fortrinnsvis med fyllstoffet eller også samtidig med den samlede mineralstoff-mengde. The mixture of a powdered organosilane/soot mixture containing 30-60 wt-St, preferably 47-53 wt-# of at least one organosilane, calculated on the total amount, is particularly suitable for the production of asphalt compounds, the treatment of such a mixture can be carried out analogously the method described in DE-PS 2,747,277. The organosilane/soot mixture can, by choice, first be mixed with a component, preferably with the filler or also at the same time with the total amount of mineral matter.
Derved dimensjoneres, mengden organosilan/sotblandingen alltid således at konsentrasjonen av organosilanen, beregnet på asfaltmasse, ligger mellom 0,005 og 0,09 vekt-56. Thereby, the amount of organosilane/soot mixture is always sized so that the concentration of the organosilane, calculated on asphalt mass, is between 0.005 and 0.09 weight-56.
Spesielt egnet er pulverformige blandinger som inneholder et eller flere silaner med formel Powdery mixtures containing one or more silanes with the formula are particularly suitable
der there
der there
R<1> betyr C1_4~alkyl, R<1> means C1_4~alkyl,
R<2> betyr Cj_4-alkoksy, R<2> means C 1_4 alkoxy,
Alk betyr toverdig, mettet alifatisk C1_4-hydrokarbon, Alk means divalent saturated aliphatic C1_4 hydrocarbon,
m betyr 1 eller 2, og m means 1 or 2, and
n betyr 1-6 når m betyr 2 og n betyr 1 når m betyr 1. n means 1-6 when m means 2 and n means 1 when m means 1.
Av disse silaner anvendes fortrinnsvis forbindelsene Of these silanes, the compounds are preferably used
-sulfan . bis-(3-[trietoksisilyl]-propyl) -disulfan -sulfan. bis-(3-[triethoxysilyl]-propyl)-disulfane
-tetrasulfan. -tetrasulfan.
Spesielt egnet for oppfinnelsens formål er pulverformede konsentrater som inneholder et eller flere silaner med formel Particularly suitable for the purposes of the invention are powdered concentrates containing one or more silanes with formula
der there
R<1> betyr C1_4-alkyl R<1> means C1-4-alkyl
R<3> betyr treverdig, mettet alifatisk C^_4-hydrokarbon, R<3> means trivalent saturated aliphatic C^_4 hydrocarbon,
a betyr 1 eller 2, a means 1 or 2,
og p betyr 1 eller 2. and p means 1 or 2.
Oppfinnelsens organosilanholdige asfaltmasser kan, avhengig av typen og mengden av mineralblanding, anvendes til fremstilling av valseasfalt for gatelegging og der også til fremtilling av spesialbelegg som for eksempel for broer. The organosilane-containing asphalt compounds of the invention can, depending on the type and amount of mineral mixture, be used for the production of rolled asphalt for street laying and there also for the production of special coatings such as for bridges.
Likeledes kan de anvendes for fremstilling av støpeasfalt for gatelegging eller høybygg (for eksempel industrigulv og fugeløse gulv) eller fremstillingen av takbelegg, takbaner, underjordisk beskyttelse for kjøretøyer eller kabelmasser. Likewise, they can be used for the production of cast asphalt for street laying or high-rise buildings (for example, industrial floors and jointless floors) or the production of roof coverings, roof tracks, underground protection for vehicles or cable masses.
På grunn av innarbeidelsen av organosilanet eller organo-silanene i mineralstoffblandingen som deretter blandes med den varme bitumen fremkommer en betraktelig tidsmessig nedsettelse av den termiske belastning av de forarbeidede silaner i forhold til teknikkens stand. Videre er det knapt nok å registrere fordampningstap, da et uorganisk faststoff absorbert organosilan ikke så lett fordamper som et flytende silan som innføres i det varme bitumen. Due to the incorporation of the organosilane or organo-silanes in the mineral mixture which is then mixed with the hot bitumen, a considerable time-related reduction in the thermal load of the processed silanes occurs in relation to the state of the art. Furthermore, it is hardly enough to record evaporation losses, as an inorganic solid absorbed organosilane does not evaporate as easily as a liquid silane that is introduced into the hot bitumen.
Den mindre termiske belastning muliggjør også den økonomiske anvendelse av organosilaner som i henhold til fremgangsmåten ifølge teknikkens stand bare var å forarbeide under høye stofftap i bitumen. The lower thermal load also enables the economic use of organosilanes which, according to the method according to the state of the art, could only be processed during high substance losses in bitumen.
Overraskende viser det seg også en tydelig forbedring av virkningen av de ifølge oppfinnelsen anvendte blandinger av organosilan og uorganisk faststoff. Det kan fastslås at for eksempel for oppnåelse av omtrent like spaltestrekkfastheter .ifølge oppfinnelsen kreves bare halvparten av organosilan-mengden som må innarbeides i hehold til teknikkens stand i den varme bitumen. Surprisingly, there is also a clear improvement in the effect of the mixtures of organosilane and inorganic solid used according to the invention. It can be established that, for example, in order to achieve approximately equal split tensile strengths according to the invention, only half of the amount of organosilane that must be incorporated in accordance with the state of the art in the hot bitumen is required.
Oppfinnelsen skal forklares nærmere ved hjelp av noen eksempler. The invention will be explained in more detail with the help of some examples.
Det fremstilles en splittrik asfaltbetong 0/11, hvis bindemiddelinnhold er valgt således at det fremkommer et hulrominnhold i størrelsesorden på 7 volum-56 på Marshall-prøvelegemer. Under anvendelse av 5,4 vekt-# gatebygnings-bitumen 80 fremkommer følgende type av dosering for den splittrike asfaltbetong 0/11: Bruddsand og finsplitt inntil 5 mm kornstørrelse bestående av en kvartsitisk gråvakke fra Osnabruck. Som meget sur stentype fører den til problemer ved klebing av bindemiddelfilmen på stenoverflaten. Kvartsittsplitt A split-rich asphalt concrete 0/11 is produced, the binder content of which has been chosen so that a void content of the order of 7 volume-56 appears on Marshall specimens. Using 5.4 weight-# gatebygnings-bitumen 80, the following type of dosage appears for the fragment-rich asphalt concrete 0/11: Crushed sand and fine crushed stone up to 5 mm grain size consisting of a quartzitic gray stone from Osnabruck. As a very acidic stone type, it leads to problems when the binder film sticks to the stone surface. Quartzite split
Ifølge den karakteriserende sammensetning fremstilles Marshallprøvelegemer hvis hulrominnhold ifølge betingelsen skal ligge i en størrelsesorden på 7 volum-#. På Marshall-prøvelegemene fastslås spaltstrekkfastheten. According to the characterizing composition, Marshall specimens are produced whose void content according to the condition must be in the order of 7 volume-#. The split tensile strength is determined on the Marshall specimens.
En ugunstig affinitet mellom stenoverflate og bitumen blir ved vannlagring tydelig ved at det forskyver seg en vannfilm mellom bindemiddelhud og stenoverflate, spaltstrekkfastheten nedsettes og gjør seg delvis også merkbar ved øking av prøvelegemets volum. An unfavorable affinity between stone surface and bitumen becomes evident during water storage in that a film of water shifts between the binder skin and stone surface, the split tensile strength is reduced and is partly also noticeable when the volume of the specimen is increased.
Spaltstrekkforsøket ble gjennomført på en Universalpresse av prøveklasse I med en konstant fremmedskyvningshastighet på 50 mm/min. ved en prøvetemperatur på 25°C. Derved fremkommer spaltstrekkfastheten av tallverdiligningen: The split tensile test was carried out on a Universal press of test class I with a constant foreign displacement speed of 50 mm/min. at a test temperature of 25°C. This results in the column tensile strength of the numerical value equation:
der P betyr max. trykkraft i N, d = prøvelegemets diameter i mm, h = prøvelegemets høyde i mm. where P means max. compressive force in N, d = diameter of the specimen in mm, h = height of the specimen in mm.
Undersøkelsesresultatene er angitt nedenfor i tabell I. The survey results are set out below in Table I.
Tabellen inneholder klebemiddeltypen, doseringen henviser til bindemiddelinnhold i vekt-*, typen av tilsetningen i variasjon av en tilsetning til bitumen eller til mineralstoffblandingen. The table contains the type of adhesive, the dosage refers to binder content by weight*, the type of addition in variation of an addition to bitumen or to the mineral mixture.
Som silan finner det anvendelse bis-(3-trietoksisilylpropyl) tetrasulfan (Si 69) henholdsvis en handelsvanlig pulverformig blanding som til hver gang 50 vekt-* består av Si 69 og sot, det vil si at 0,5 vekt-* X 50S tilsvarer en Si 69-del på 0,25 vekt-*. As silane, bis-(3-triethoxysilylpropyl) tetrasulfane (Si 69) is used, respectively a commercially available powdery mixture which each time 50 wt-* consists of Si 69 and carbon black, that is, 0.5 wt-* X 50S corresponds to a Si 69 part of 0.25 wt-*.
Forsøk 1 tjener som sammenligningsforsøk uten anvendelse av et silan. Trial 1 serves as a comparison trial without the use of a silane.
Det viser seg at asfaltmassen med 0,5 vekt-* X50S i mineralstoffblandingen viser omtrent samme nedsettelse av spalt-strekkverdien som den der hvor 0,5 vekt-* Si 69 ble anbragt direkte i den varme bitumen. It turns out that the asphalt mass with 0.5 weight-* X50S in the mineral mixture shows approximately the same reduction in the split tensile value as that where 0.5 weight-* Si 69 was placed directly in the hot bitumen.
Claims (4)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3236381A DE3236381C2 (en) | 1982-10-01 | 1982-10-01 | Process for the production of organosilane-containing asphalt compounds |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| NO832926L NO832926L (en) | 1984-04-02 |
| NO166537B true NO166537B (en) | 1991-04-29 |
| NO166537C NO166537C (en) | 1991-08-07 |
Family
ID=6174680
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO832926A NO166537C (en) | 1982-10-01 | 1983-08-15 | PROCEDURE FOR THE PREPARATION OF ORGANOSIL-CONTAINING ASPALT PASSES. |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0105133B1 (en) |
| JP (1) | JPS5966456A (en) |
| AT (1) | ATE30434T1 (en) |
| CA (1) | CA1201554A (en) |
| DE (2) | DE3236381C2 (en) |
| DK (1) | DK441283A (en) |
| ES (1) | ES525075A0 (en) |
| FI (1) | FI74719C (en) |
| NO (1) | NO166537C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3516660A1 (en) * | 1985-05-09 | 1986-11-13 | Degussa Ag, 6000 Frankfurt | POWDER-BASED BINDER CONCENTRATE |
| CN102532922B (en) * | 2011-12-15 | 2013-11-06 | 四川维城磁能有限公司 | Synthetic rubber asphalt and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2609305A (en) * | 1947-07-24 | 1952-09-02 | Standard Oil Dev Co | Process for preparing asphalt coated aggregate |
| FR2102794A5 (en) * | 1970-08-21 | 1972-04-07 | France Etat | Mineral granulates - treated with a methyltrialkylsilane hydrolysate for road surfaces |
| US4036661A (en) * | 1973-02-12 | 1977-07-19 | Chevron Research Company | Asphalt mineral aggregate compositions containing silanes as adhesion promoters |
| US4173489A (en) * | 1978-04-12 | 1979-11-06 | Texaco Inc. | Asphalt mineral aggregate compositions |
-
1982
- 1982-10-01 DE DE3236381A patent/DE3236381C2/en not_active Expired
-
1983
- 1983-08-06 EP EP83107765A patent/EP0105133B1/en not_active Expired
- 1983-08-06 AT AT83107765T patent/ATE30434T1/en not_active IP Right Cessation
- 1983-08-06 DE DE8383107765T patent/DE3374205D1/en not_active Expired
- 1983-08-15 NO NO832926A patent/NO166537C/en unknown
- 1983-08-22 ES ES525075A patent/ES525075A0/en active Granted
- 1983-08-25 JP JP58154233A patent/JPS5966456A/en active Granted
- 1983-09-01 FI FI833122A patent/FI74719C/en not_active IP Right Cessation
- 1983-09-23 CA CA000437441A patent/CA1201554A/en not_active Expired
- 1983-09-27 DK DK441283A patent/DK441283A/en not_active Application Discontinuation
Also Published As
| Publication number | Publication date |
|---|---|
| DE3236381C2 (en) | 1986-11-06 |
| NO832926L (en) | 1984-04-02 |
| DK441283A (en) | 1984-04-02 |
| JPS6111975B2 (en) | 1986-04-05 |
| ES8405053A1 (en) | 1984-05-16 |
| FI833122A (en) | 1984-04-02 |
| FI74719B (en) | 1987-11-30 |
| DK441283D0 (en) | 1983-09-27 |
| JPS5966456A (en) | 1984-04-14 |
| FI833122A0 (en) | 1983-09-01 |
| EP0105133B1 (en) | 1987-10-28 |
| DE3374205D1 (en) | 1987-12-03 |
| NO166537C (en) | 1991-08-07 |
| CA1201554A (en) | 1986-03-11 |
| ES525075A0 (en) | 1984-05-16 |
| EP0105133A1 (en) | 1984-04-11 |
| FI74719C (en) | 1988-03-10 |
| ATE30434T1 (en) | 1987-11-15 |
| DE3236381A1 (en) | 1984-04-05 |
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