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DK169747B1 - Smørefedt og fremgangsmåde til fremstilling deraf - Google Patents

Smørefedt og fremgangsmåde til fremstilling deraf Download PDF

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Publication number
DK169747B1
DK169747B1 DK621786A DK621786A DK169747B1 DK 169747 B1 DK169747 B1 DK 169747B1 DK 621786 A DK621786 A DK 621786A DK 621786 A DK621786 A DK 621786A DK 169747 B1 DK169747 B1 DK 169747B1
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DK
Denmark
Prior art keywords
lubricating grease
fatty acid
alkyl salicylate
grease according
calcium
Prior art date
Application number
DK621786A
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English (en)
Other versions
DK621786D0 (da
DK621786A (da
Inventor
Alexander Colquhoun B Macphail
Henry Rutherford
Original Assignee
Shell Int Research
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Publication date
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Publication of DK621786D0 publication Critical patent/DK621786D0/da
Publication of DK621786A publication Critical patent/DK621786A/da
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Publication of DK169747B1 publication Critical patent/DK169747B1/da

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
    • C10M159/12—Reaction products
    • C10M159/20—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products
    • C10M159/22—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products containing phenol radicals
    • C—CHEMISTRY; METALLURGY
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    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C—CHEMISTRY; METALLURGY
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    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/08—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to a carbon atom of a six-membered aromatic ring
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    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/48—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring
    • C10M129/54—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring containing hydroxy groups
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    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
    • C—CHEMISTRY; METALLURGY
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/102—Silicates
    • C10M2201/103—Clays; Mica; Zeolites
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    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/028—Overbased salts thereof
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    • C10M2207/106—Carboxylix acids; Neutral salts thereof used as thickening agents
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/06—Groups 3 or 13
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/08—Groups 4 or 14

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  • Lubricants (AREA)

Description

DK 169747 B1
Den foreliggende opfindelse arigår et smørefedt (smørrelsesmiddel; grease composition) til smøring og korrosionsbeskyttelse, som indeholder et grund-fluidum og et fortykkelsesmiddel, og som er frit for potentielt farlige 5 additiver.
Smørefedt anvendes sædvanligvis under omstændigheder hvor vand i større eller mindre mængde er til stede.
Selv om sådanne smørelsesmidler tilvejebringer smøring, beskytter de ikke nødvendigvis de metaldele som de er i 10 kontakt med mod rustdannelse. Hertil kræves smørefedt, som besidder fortrinlige smøreegenskaber og modvirker rustdannelse. Til opnåelse af disse egenskaber har det været foreslået at sætte anti-rust additiver til smørefedt. I den sammenhæng er natriumnitrit særlig 15 effektivt.- Skønt denne forbindelse medvirker til midlets oxidationsstabilitet, tilsættes også en antioxidant. Aminer og derivater heraf er velegnede og effektive antioxi-danter. Det er imidlertid kendt at nitrit, og aminer i forening kan danne nitrosaminer, af hvilke nogle anses for 20 at være kræftfremkaldende. Dette problem erkendes af de inden for området sagkyndige og der er gjort store anstrengelser for at modvirke dannelse af nitrosaminer. For eksempel fremgår det af US patentskrift nr. 4.200.542 at nitrosamindannelsen kan inhiberes ved at der til smørelses-25 midlet sættes en kombination af et askorbat eller isoas-korbat med α-tocoferol. Selv om denne sidstnævnte kombination hævdes at være effektiv, er det åbenbart at kun smørelsesmidler som ikke indeholder nitriter og/eller aminder ivater, kan løse problemet med nitrosamindannelsen til-30 strækkeligt. Ifølge nærværende opfindelse har det overraskende vist sig at kalciumalkylsalicylat udviser fortrinlige anti-rust egenskaber når det sættes til et smørefedt, således at det ikke længere er nødvendigt at tilsætte natriumnitrit. Smørefedtets dråbepunkt (dropping point), 35 dvs. den temperatur hvor smørefedtet overgår fra halvfast til flydende fase, sænkes imidlertid ved tilsætning af kalciumalkylsalicylat. Det har ligeledes overraskende vist sig, at smørefedt som indeholder en kombination af kalciumalkylsalicylat og magnesiumalkylsalicylat udviser for- DK 169747 B1 2 trinlige anti-rust egenskaber og har tilfredsstillende dråbepunkter .
I overensstemmelse hermed vedrører den foreliggende opfindelse et smørefedt eller smørelsesmiddel bestående 5 af et grund-fluidum samt et fortykkelsesmiddel, hvor smøremidlet ifølge opfindelsen er ejendommeligt ved, at det tillige indeholder kalciumalkylsalicylat og magnesiumalkylsa-licylat. Det har vist sig, at smørelsesmidler ifølge opfindelsen ikke blot besidder fortrinlige anti-rust egenskaber 10 og tilfredsstillende dråbepunkter, men også har vandudvaskningsegenskaber (water washout characteristics) som er bedre end for natriumnitrit-holdige smørelsesmidler.
Grundfluidet kan være et hvilket som helst kendt smøremiddel. Dette indbefatter mineralske kulbrinteolier, 1 s syntetiske kulbrinteolier, polymere forbindelser såsom polyolefiner og polyglykoler, estere såsom dialkylsebaci-nater, polysiloxaner, fenoxyfenylætere og andre smøremidler eller blandinger deraf. Foretrukne er mineralske og syntetiske kulbrinteolier. Disse olier kan have undergået forskellige behandlinger, især hydrobehandlmg. Smøreolier- 2 nes viskositet ligger hensigtsmæssigt mellem 2 og 60 mm /s ved 100°C, fortrinsvis mellem 3 og 50 mm^/s ved denne temperatur.
Fortykkelsesmidler kan vælges blandt et bredt ud-25 valg af forbindelser som omfatter substituerede urinstoffer, ftalocyaniner, lerarter modificeret ved behandling med et overfladeaktivt middel, hvilke lerarter fx kan vælges blandt montmorillonitter især bentonit eller attapul-git, zeolitter eller andre komplekse uorganiske silikater ^ som forekommer i naturen. Fortykkelsesmidlet vælges fortrinsvis blandt alkali- og jordalkalimetalsæber af fedtsyrer med 6 til 30 kulstofatomer. De metalsalte som anvendes i sæben er fortrinsvis litium og/eller kalciumsalte. Når alkalimetal- og jordalkalimetalsalte anvendes i 35 forening-;, er vægt forholdet alkalimetal/jordalkalimetal hensigtsmæssigt 1:2 til 20:1. Egnede fedtsyrer er stearinsyre, hydroxystearinsyre, oliesyre, palmitinsyre, myristin-syre og hydrogenerede fedtsyrer fra i naturen forekommende DK 169747 B1 3 glyceridolier, især hydrogeneret ricinusolie-fedtsyre.
Disse sæber kan anvendes i kombination med et alkalimetalsalt, fortrinsvis litiumsalt, udvalgt blandt di-alkali-metalsaltene af C4_12 alifatiske dikarboxylsyrer, alkali-5 metalsalte af aromatiske hydroxykarboxy1syrer og alkalimetalsalte af borsyrer såsom litiummetaborat, litiumtetra-borat, litiumperborat eller monolitiumsalt af ortoborsyre, eller med fosfat-, fosfit- eller tiofosfatestere.
Alkylsalicylaterne kan være neutrale kalcium- og 10 magnesiumsalte. Fortrinsvis er mindst ét af alkylsalicylaterne basisk (overbased); især foretrækkes det at begge salicylater er basiske. Det er velkendt i dette område af teknikken hvordan man fremstiller basiske metalalkyl-salicylater. En egnet metode er beskrevet i UK patent-15 skrift nr. 2.097.417. De basiske metalalkylsalicylater er sædvanligvis komplekser af metalhydroxidet og/eller -karbonat og alkylsalicylatet. Graden af basekarakter udtrykkes ved basicitetsindexen (BI) defineret som ækvivalentforholdet metalralkylsalicylsyre. Kalciumalkylsalicylatet 20 har passende en basicitetsindex på 1 til 15, fortrinsvis 2 til 10, magnesiumalkylsalicylatet har hensigtsmæssigt en basicitetsindex på 1 til 15, fortrinsvis 2 til 8. Fordelen ved at anvende basiske alkylsalicylater ligger i at de kan neutralisere syreforbindelser som kan dannes når 25 smørefedtet er i brug, således at et korrosivt angreb af disse syreforbindelser på metaldele forebygges.
Længden af alkylsalicylatets alkylkæde spiller en vigtig rolle for den ensartede fordeling af alkylsalicylatet i smørefedtet. I almindelighed kan kædelængden varie-30 re mellem 5 og 50 kulstofatomer, fortrinsvis fra 10 til 35 kulstofatomer. Kæderne kan være forgrenede, men er hensigtsmæssigt lige. Mængden af kalciumalkylsalicylat ligger fortrinsvis mellem 0,1 og 10 vægt%, især mellem 0,5 og 5 vægt%, og mængden af magnesiumalkylsalicylat er hensigts-35 mæssigt 0,05-5 vægt%, fortrinsvis 0,1-3 vægt%, idet alle procenter er regnet på vægten af den totale sammenhæng.
Smørefedtet kan yderligere inde- DK 169747 B1 4 holde andre forbindelser og additiver. Disse kan være alkoholer såsom glykol, glycerol, trimetylolpropan eller pen-taerytritol; linolie eller ricinusolie; additiver mod slid og ekstremt tryk såsom trifenylfosfortionat, zinkdialkyl-5 ditio-fosfat, blynaftenat eller sulfuriserede fedtolier; antioxidanter såsom diarylaminer, fx difenylaminer, fenyl-naftylaminer eller alkylerede derivater deraf og andre traditionelle additiver.
Smørefedtet kan fremstilles ved en hvilken som 10 helst kendt teknik, der er anvendelig til fremstilling af smørelser. Ved fremstilling af sæbeholdige smørelser indbefatter disse teknikker fremgangsmåder til inkorporering af den ønskede fedtsyre eller fedtsyrer i et passende grundfluidum, fx en mineralsk basisolie (stock oil), og 15 neutralisation af den fremkomne blanding med passende alkalimetal- eller jordalkalimetalforbindelser, ligesom fremgangsmåder til separat fremstilling af den ønskede sæbe med efterfølgende inkorporering i grundfluidet er indbefattet. Alkylsalicylaterne blandes hensigtsmæssigt med den 20 opnåede blanding, dvs. en blanding af sæben og grundfluidet. En anden måde at fremstille smørelsesmidlet ifølge opfindelsen på består i at man forsæber en ester ud fra hvilken den egnede fedtsyre vil fremkomme, under tilstedeværelse af alkali- eller jordalkalimetalforbindelser og 25 et grundfluidum ved forhøjet temperatur, dvs. fra 120 til 250°C, dehydratiserer den fremkomne blanding, sætter yderligere grundfluidum til den dehydratiserede blanding og afkøler den opnåede smørelse. Metalalkylsalicylaterne blandes passende med smørelsesmidlet under afkølingstrinnet.
30 Fremstillingen kan udføres batchvis eller på kontinuert måde.
Smørefedtet ifølge opfindelsen belyses ved hjælp af følgende eksempler.
35 DK 169747 B1 5
Eksempel 1
Et antal smørelser fremstilledes for at vise effekten af kalcium og magnesiumalkylsalicylater på dråbepunkt og anti-rust egenskaber hos et smørefedt, idet smø-5 relserne havde forskelligt indhold af kalciumalkylsalicy-lat og magnesiumalkylsalicylat.
Det afprøvede basissmørefedt bestod af 11,0 vægt% litium- og kalciumsæber af hydrogeneret fedtsyre fra ricinusolie med et Li:Ca vægtforhold på 6; 4,5 vægt% af en 10 kombination af konventionel antioxidant, anti-korrosions-additiver og additiver mod ekstremt tryk/slid; 84,5 vægt% mineralsk kulbrinteolie med en kinematisk viskositet på 100 mm^/s ved 40°C og en viskositetsindex på 90 (svarende til en kinematisk viskositet på 10,2 mm /s ved 100°C).
15 Til dette basissmørefedt sattes overbasisk kalcium- C14-18 a^ylsalicylat (Ca-AS) med BI=3,0 (BI=basicitets-index) og overbasisk magnesium-c14_lg alkylsalicylat (Mg-AS) med BI=7,5 i mængder som angivet i tabel I. Vægtprocenterne er regnet på vægten af det ovenfor nævnte 20 basissmørefedt.
Smøremidlerne blev underkastet en dråbepunktsprøve (IP 132) og en anti-rustprøve (IP 220, ved anvendelse af saltvand). Pointværdierne af den sidste prøve går fra 0 (=ingen rust) til 5 (=rustne områder som dækker mere end 25 10% af overfladen). Resultaterne fremgår af tabel I.
Tabel I
Prøve Ca-AS Mg-AS Dråbepunkt Anti-rust nr. vægt% vægt% (IP 132), C ..(IP 220) 30 1 - 198 5 2 2 - 179 2 3 3 - 177 0 4 2 1 188 2 5 3 1 187 0 35 ' ” ♦ DK 169747 B1 6
Resultaterne viser at Ca-AS forbedrer anti-rust egenskaberne betydeligt og at samtidig tilsætning af Mg-AS effektivt modvirker det fald i dråbepunkt, som er forårsaget af Ca-AS.
5 Eksempel 2 I dette eksempel sammenlignes smørefedtprøver med indhold af natriumnitrit, henholdsvis Ca-AS og Mg-AS. Smørefedtprøve 6 indeholdt: ^ q 11,0 vægt% hydrogeneret fedtsyre fra ricinusolie 1,6 vægt% litiumhydroxid, monohydrat 2.0 vægt% natriumnitrit 5.3 vægt% af en sammensætning af konventionel antioxidant, antikorrosions- og ekstremt 1^ tryk/anti-slid-additiver 80,1 vægt% kulbrinteolie som i eksempel 1. Smørefedtprøve 7 indeholdt: 12.0 vægt% hydrogeneret fedtsyre af ricinusolie 1,5 vægt% litiumhydroxid, monohydrat 20 0,2 vægt% kalciumhydroxid 4.3 vægt% af en sammensætning af konventionel antioxidant, antikorrosions og ekstremt tryk/ antislid-additiver 3.0 vægt% Ca-AS, som i eksempel 1 25 1,0 vægt% Mg-AS, som i eksempel 1 78.0 vægt% kulbrinteolie, som i eksempel 1.
Et antal data for prøverne blev bestemt. Disse frem-30 går af tabel II.
35 DK 169747 B1 7
Tabel II
Prøve nr. 67
Indtrængning ubearbejdet/bearbejdet (IP 50), dmm 239/243 238/248 5 Dråbepunkt (IP 132), °C 186 185
Vandudvaskning (ASTM D 1264), vægt% 50 1,3
Anti-rust (ASTM D 1743), points 1 1
Kobber korrosion (IP 112) En smule Ingen anløben ln Olieadskillelse (IP 121) 18 t/ 7 dage, vægt% 0,41/1,68 0,39/1,72
Rulletest (ASTM D 1831, modificeret så indtrængningsforskellen bestemmes efter 100 timer): ved oragivelsetemp., dmm 112 29 15 ved 100°C, dmm 112 94
Fra ovenstående resultater er det åbenbart at smøremidler ifølge nærværende opfindelse har samme eller bedre egenskaber end tidligere anvendte smørelser. Især er vand-20 modstandsevnen forbedret betydeligt.
25 30 35

Claims (9)

1. Smørefedt indeholdende et grundfluidum samt et for tykkelsesmiddel, kendetegnet ved, at det tillige indeholder kalciumalkylsalicylat og magnesiumalkylsalicylat. 5
2. Smørefedt ifølge krav 1, kendetegnet ved at fortykkelsesmidlet er en alkalimetalsæbe eller en jord-alkalimetalsæbe af en fedtsyre med fra 9 til 30 kulstofatomer pr. molekyle.
3. Smørefedt ifølge krav 2, kendetegnet ved 10 at det indeholder hydrogeneret ricinusoliefedtsyre som fedtsyrekomponent.
4. Smørefedt ifølge krav 2 eller 3, kendetegnet ved at metalkomponenten i fortykkelsesmidlet er litium og/eller kalcium.
5. Smørefedt ifølge et hvilket som helst af kravene 1-4, kendetegnet ved at kalciumalkylsalicyla-tet har en basicitesindex på 1 til 15 og magnesiumalkylsalicylat en basicitetsindex på 1-15.
6. Smørefedt ifølge et hvilket som helst af kravene 20 1-5, kendetegnet ved at metalalkylsalicylater- ne har en alkyldel med 5 til 50 kulstofatomer.
7. Smørefedt ifølge et hvilket som helst af kravene 1-6, kendetegnet ved at mængden af kalciumalkylsalicylat er 0,1 til 10 vægt% og mængden af magnesium- 25 alkylsalicylat 0,05 til 5 vægt%, regnet på vægten af det totale middel.
8. Fremgangsmåde til fremstilling af det i krav 1 angivne smørefedt, kendetegnet ved at man blander kalciumalkylsalicylat og magnesiumalkylsalicylat med 30 en blanding indeholdende en fedtsyresæbe og et grundfluidum.
9. Fremgangsmåde ifølge krav 8, kendetegnet ved at blandingen som indeholder en fedtsyresæbe og et grundfluidum er fremstillet ved 35 DK 169747 B1 (i) at inkorporere fedtsyren eller fedtsyrerne i grundfluidet og neutralisere den fremkomne blanding med alkalimetal- og/eller jordalkalimetalforbindelser; eller 5 (ii) at fremstille fedtsyresæben separat og inkorporere den i grundfluidet; eller (iii) at forsæbe en ester, fra hvilken fedtsyre skal opnås, under tilstedeværelse af alkali- eller jord-alkalimetalforbindelser og grundfluidum ved for-10 højet temperatur, dehydratisere den fremkomne blan ding, sætte yderligere grundfluidum til den dehy-dratiserede blanding og afkøle det fremkomne smørefedt. 15 20 25 30 35
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FI82068B (fi) 1990-09-28
US4719023A (en) 1988-01-12
ATE60793T1 (de) 1991-02-15
FI865261A (fi) 1987-06-24
EP0227182A2 (en) 1987-07-01
SG29492G (en) 1992-05-15
HK54892A (en) 1992-07-30
CA1283399C (en) 1991-04-23
AU6683886A (en) 1987-06-25
ZA869614B (en) 1987-06-22
EP0227182A3 (en) 1988-08-10
DK621786D0 (da) 1986-12-22
IE863373L (en) 1987-06-23
TR24450A (tr) 1991-10-10
AR245491A1 (es) 1994-01-31
EP0227182B1 (en) 1991-02-06
FI865261A0 (fi) 1986-12-22
IE59508B1 (en) 1994-03-09
FI82068C (fi) 1991-01-10
NO865244L (no) 1987-06-24
NO865244D0 (no) 1986-12-22
AU589478B2 (en) 1989-10-12
NZ218745A (en) 1989-01-27
DE3677479D1 (de) 1991-03-14
NO171280C (no) 1993-02-17
MY100718A (en) 1991-01-31
NO171280B (no) 1992-11-09
BR8606359A (pt) 1987-10-13
GB8531626D0 (en) 1986-02-05
DK621786A (da) 1987-06-24

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