SE177064C1 - - Google Patents
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- SE177064C1 SE177064C1 SE177064DA SE177064C1 SE 177064 C1 SE177064 C1 SE 177064C1 SE 177064D A SE177064D A SE 177064DA SE 177064 C1 SE177064 C1 SE 177064C1
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Uppfinnare: J Hughes och J M Socsan Prioritet begeird fran den 22 september 1958 (Storbritannien) Uppfinningen hanfor sig till smOrjoljor innehallande viskositetsindex forhattrande me-del. Inventors: J Hughes and J M Socsan Priority requested from 22 September 1958 (Great Britain) The invention relates to lubricating oils containing viscosity index hating agents.
Smorjoljor med formaga att astadkomma effektiv smorjning Mom cit brett temperaturonirade framstallas i allmanhet genom att blanda ett polymert viskositetsindex f5rbattrande medel med en olja av lag viskositet. Det polymera media fortjockar oljan forutom att det forbattrar dess viskositetsindex, men graden av fortjockning vid lag temperatur avviler vanligtvis foga Iran den som erballes vid hog temperatur. Andra polymera viskositetsindex fOrbattrande medel sasom Plexol 966 (en sampolymer av laurylmetakrylat och N-vinylpyrrolidon) ha storre fortjockningskraft vid 116ga an vid laga temperaturer, men Okningen av f5rtj ockningsfonnagan med temp eraturen upphor vid c:a 100° C. Ett idealiskt viskositetsindex forbattrande medel for framstallning ay smOrjoli or for anvandande mom alt brett temperaturomrade bör vara verksarnt detta avseende liven vid temperaturer avsevart ovanfor 100° C, samtidigt som fortjockningsformagau vid raga temperatures bor vara mycket lkgre eller noll. Med ett sadant viskositetsindex forbattrande medel skulle en utgangsolja med hogre viskositet kunna anvandas, vilket skulle resultera i en lagre oljekonsumtion och hattre smorjning vid hoga motorhastigheter och temperaturer. Lubricating oils capable of providing effective lubrication with a wide range of temperatures are generally prepared by mixing a polymeric viscosity index improver with a low viscosity oil. The polymeric media thickens the oil in addition to improving its viscosity index, but the degree of thickening at low temperature usually does not adhere to the one obtained at high temperature. Other polymeric viscosity index improvers such as Plexol 966 (a copolymer of lauryl methacrylate and N-vinylpyrrolidone) have greater thickening power at 116 degrees Celsius at low temperatures, but the increase in temperature increase with temperature ceases at about 100 ° C. for production of lubricants or for use with a wide temperature range, this should be effective with respect to life at temperatures well above 100 ° C, while thickening forms at low temperatures should be much lower or zero. With such a viscosity index improver, a starting oil of higher viscosity could be used, which would result in lower oil consumption and less lubrication at high engine speeds and temperatures.
Foreliggande uppfinning avser en smorjolj a innehallande ett sadant viskositetsindex forbattrande medel. The present invention relates to a lubricating oil a containing such a viscosity index improving agent.
Smorjoljekompositionen enligt uppfinningen kannetecknas vasentligen darav, att den be-star av en smorjolja och 0,1-20 vikt- % av ett salt av en oljeloslig polymer amin och en organof osforsyra. The lubricating oil composition according to the invention is essentially characterized in that it consists of a lubricating oil and 0.1-20% by weight of a salt of an oil-soluble polymeric amine and an organophosphoric acid.
Forutom att de verka sasom viskositetsindex forbattrande medel bibringa namnda salter olj an Oven hogtrycksegenskaper till foljd av den fosforhaltiga sura delens av molekylen inverkan. In addition to acting as viscosity index improvers, said salts impart oil to the above high pressure properties due to the effect of the phosphorus-containing acidic moiety of the molecule.
I det foljande avses med uttrycket »polymer amin» en godtycklig polymer eller sampolymer innehallande grupper med basisk kvave. Dessa grupper kunna salunda utgoras av amino-, imino-, amido- eller imido-grutpper eller av kvaveatomer i en heterocyklisk ring. Med uttrycket »salt» avses icke enbart ett verkligt salt utan Oven ett delvis eller helt dissocierat salt. Salunda skola dâ det Or tal om ett salt av en oljeloslig polymer amin och en organofosfors3Ta och da. texten sa medgiver inkluderas rena blandningar av aminen och syran. Det torde inses, att ett material, som bildar ett verkligt salt vid en temperatur, kan utgora endast en blandning vid en hogre temperatur. Vidare avses med uttrycket »organofosforsyra» en godtycklig sur organisk forening harledd fah en av fosfors syror. SO t. ex inkluderar uttrycket partiella estrar av fosfors oxisyror och tiosyror saint ay fosfon- och fosfinsyror. In the following, the term "polymeric amine" means any polymer or copolymer containing basic nitrogen groups. These groups can thus consist of amino, imino, amido or imido large groups or of nitrogen atoms in a heterocyclic ring. The term "salt" means not only a real salt but also a partially or completely dissociated salt. Salunda should then there Or talk of a salt of an oil-soluble polymer amine and an organophosphorus3Ta and da. the text said admits included pure mixtures of amine and acid. It will be appreciated that a material which forms an actual salt at a temperature may be only a mixture at a higher temperature. Furthermore, the term "organophosphoric acid" refers to any acidic organic compound derived from one of the phosphoric acids. SO, for example, the term partial esters of phosphorus oxyacids and thioacids include saint ay phosphonic and phosphinic acids.
De polymera aminerna, vilkas fOrutnamnda salter anvandas enligt uppfinningen, a.ro vOlkAndn material. De kunna utgoras av enkla polymerer, I. ex..sadan som erhallits genom att polymerisera vinylpyridin, vinylkinolin eller aminostyren, polyaminer framstallda genom att, 1 naryaro ay ammonia.k eller primara eller sekundara aminer reducera sampolymerer av en monoolefin och koloxid, hydrerade sampolymerer av 1,3-butadien och akrylnitril, polymerer och sampolymerer av akrylater och metakrylater av hydroxialkyl-tert.-aminer, &Isom dietylaminoetylmetakrylat, samt polymera aminer erhallna genom att la'ta polymerer innehallande epoxigrupper reagera med ammoniak eller primara eller .sekundara aminer. Emellertid Oro de foredragna polymera aminerna sadana corn erhallas genom sampolymerisering av en polymeriserbar heterocyklisk kvavebasfarening, sasom en vinylpyridin eller vinylpyrrolidon, och polymeriserbara omattade material, som aro fria Iran heterocykliska kvavehaltiga radikaler, exempelvis sadana 2— — -som beskrivas i brittiska patentet 760 551. A-v denna klass av polymera aminer aro de lampligast, som ha en molekylarvikt mellan 75000 och 1000000 °eh aro harledda fran en vinylpyridin och akrylsyra, en alfa-substituerad akrylsyra eller en ester, nitril eller amid av en sadan syra. Foretradesvis uppgar i denna sampolymer molara forhallandet mellan poly-. meriserbar kvavebasforening och polymeriserbart omattat material fritt fran. heteroeykliska kvavehaltiga radikaler till mellan 1 : 1 och : 4. Speciellt lampliga aro de sampolymerer, som beskrivas i franska patentet 1 178 735 och belgiska patentet 563 612 och som innefatta sampolymerer av stearylmetakrylat, laurylmetakrylat och 2-mety1-5-vinyl-pyridin samt sampolymerer av stearylmetakrylat, laurylmetakrylat, metylmetakrylat och 2-mety1-5-vinyl-pyridin och liknande sampolymerer, i v11- ka metylmetakrylatet ãr ersatt med butylmetakrylat och 2-mety1-5-vinyl-pyridinen ãr ersatt med 5-ety1-2-vinyl-pyridin. Andra lampliga polymera aminer aro de som i handeln ga under benamningen »Acryloid», t. ex. Acryloid 966 och 917, samt de som saljas av E. I. du Pont de Nemours & Co. under beteckningen LOA 564 och 565. The polymeric amines, the aforementioned salts of which are used in accordance with the invention, a.ro volcanic materials. They may consist of simple polymers, e.g., those obtained by polymerizing vinylpyridine, vinylquinoline or aminostyrene, polyamines prepared by reducing, in naryaro ay ammonia.k or primary or secondary amines copolymers of a monoolefin and carbon monoxide, hydrogenated copolymers of 1,3-butadiene and acrylonitrile, polymers and copolymers of acrylates and methacrylates of hydroxyalkyl tert-amines, & Isom diethylaminoethyl methacrylate, and polymeric amines obtained by reacting polymers containing epoxy groups with ammonia or primary or secondary amines. However, the preferred polymeric amines such corn are obtained by copolymerizing a polymerizable heterocyclic nitrogen base compound, such as a vinylpyridine or vinylpyrrolidone, and polymerizable unsaturated materials which are free of Iran heterocyclic nitrogen-containing radicals, such as those described in the patent. Of this class of polymeric amines, the most suitable are those having a molecular weight between 75,000 and 1000000 ° C and are derived from a vinylpyridine and acrylic acid, an alpha-substituted acrylic acid or an ester, nitrile or amide of such an acid. Preferably, in this copolymer, the molar ratio of poly-. merisable nitrogen base compound and polymerizable unsaturated material free from. heterocyclic nitrogen-containing radicals of between 1: 1 and: 4. Particularly suitable are the copolymers described in French patent 1,178,735 and Belgian patent 563,612 which comprise copolymers of stearyl methacrylate, lauryl methacrylate and 2-methyl-5-vinyl-pyridine and copolymers of stearyl methacrylate, lauryl methacrylate, methyl methacrylate and 2-methyl-5-vinyl-pyridine and similar copolymers, in which the methyl methacrylate is replaced by butyl methacrylate and the 2-methyl-5-vinyl-pyridine is replaced by 5-ethyl-2-ethyl -pyridine. Other suitable polymeric amines are those commercially available under the name "Acryloid", e.g. Acryloid 966 and 917, as well as those sold by E. I. du Pont de Nemours & Co. under the designation LOA 564 and 565.
De organo-fosforsyror, som anvandas for bildande av salterna enligt uppfinningen, utgoras foretradesvis av partiella estrar av ox!syror av fosfor siirskilt av fosforsyra. De kunna utgiiras av alkyl-, eykloalkyl- eller aryl-estrar, °eh foretradesvis ha de upp till 30 kolatomer i molekylen. Typiska sadana estrar aro mono- ()eh-hexyl-,-nonyl-, -decyl-, -dodecyl- och -oktadecyl-estrarna av fosforsyra och fosforsyrlighet, mono- eller dieyklohexylfosfat eller -fosfit samt mono- eller di-fenyl-, -kresyl- eller -xylenylfosfat eller -fosfit. Av dessa aro di-estrarna av fosforsyra att foredraga. The organophosphoric acids used to form the salts of the invention are preferably constituted by partial esters of oxalic acids of phosphorus, especially phosphoric acid. They may be formed from alkyl, cycloalkyl or aryl esters, or preferably have up to 30 carbon atoms in the molecule. Typical such esters are the mono- () eh-hexyl-, - nonyl-, -decyl-, -dodecyl- and -octadecyl esters of phosphoric acid and phosphoric acid, mono- or dieyklohexyl phosphate or phosphite and mono- or di-phenyl-, -cresyl or xylenyl phosphate or phosphite. Of these, the diesters of phosphoric acid are preferred.
De partiella estrarna av fosfors tiosyror kunna avenledes anvandas, exempelvis de ovan angivna estrarna, van i en eller flera syreatomer ersatts med en svavelatom, sasom dinonyl- eller dicyklohexyl-ditiofosforsyra och monodecyl-monotiof osforsyra. The partial esters of phosphorous thioacids can also be used, for example the esters mentioned above, used in one or more oxygen atoms replaced by a sulfur atom, such as dinonyl or dicyclohexyl dithiophosphoric acid and monodecyl monothiophosphoric acid.
De alkoholer och fenoler, fran vilka de oi4an angivna partiella estrarna aro harledda, kunna vara substituerade exempelvis med halogenatomer eller hydroxi-, eter-, karbalkoxi-, nitro- eller eyano-grupper. Salunda kan man anvanda sadana partiella estrar som di-klorfenylfosfat. The alcohols and phenols from which the above-mentioned partial esters are derived may be substituted, for example, by halogen atoms or hydroxy, ether, carbalkoxy, nitro or eyano groups. Thus, such partial esters as dichlorophenyl phosphate can be used.
Organo-fosforsyran kan utgOras av en fosfinsyra, sasom di-oktan- eller di-tetradekan-1- fosfinsyra, di-bensylfosfinsyra, difenylfosfinsyra, fenylmetylfosfinsyra, fenyletylfosfinsyra och isobutylfenylfosfinsyra eller av en fosfonsyra, sasom bensen-, p-toluen-, hexan-, oktan-, dekan- eller dodekan-1-fosfonsyra och cyklohexanfosfonsyra. Rolvategruppen i fosfin- eller fosfonsyran kan vara substituerad, exempelvis sasom i di(alfa-hydroxilsopropyl)fos finsyra, 2-kloretanfosfonsyra, 1-karboetoxipropan-1- eller -2-fosfonsyra, 3-hydroxipropan-1-fosfonsyra. &Liana syror kan framstallas pa salt som framgar av brittiska patentet 660 918. The organophosphoric acid may be a phosphinic acid, such as di-octane or di-tetradecan-1-phosphinic acid, di-benzylphosphinic acid, diphenylphosphinic acid, phenylmethylphosphinic acid, phenylethylphosphinic acid and isobutylphenylphosphinic acid, , octane, decane or dodecane-1-phosphonic acid and cyclohexane phosphonic acid. The rolvate group in the phosphinic or phosphonic acid may be substituted, for example as in di (alpha-hydroxylsopropyl) phosphinic acid, 2-chloroethanephosphonic acid, 1-carboethoxypropane-1- or -2-phosphonic acid, 3-hydroxypropane-1-phosphonic acid. & Liana acids can be prepared on salt as shown in British Patent 660,918.
De motsvarande tiofasfon- och tiofosfinsyrorna kunna avenledes anvandas. The corresponding thiophosphonic and thiophosphinic acids can also be used.
De enligt uppfinningen anvanda salterna kunna framstallas genom en godtycklig bruklig metod for beredning av salter av organiska airliner och organiska syror. Salunda kan den polymera aminen 16m i ett organiskt 15sningsmedel, exempelvis bensen eller xylen, och syran tillsattas till losningen under omroring. Syran sjalv kart givetvis Visas i ett lampligt losningsmedel. Alternativt kan den polymera aminen suspenderas i ett lampligt vatskeformigt medium och syran inroras i suspensionen. Da. man anvander dessa m.etoder kan det vara nodvandigt att isolera saltet genom att avlagsna losnings- eller suspensionsmedlet innan saltet tillsattes till smorjoljan. Enklare metoder, sasom att helt enkelt tillsatta syran till den smalta polymera aminen, are ibland avenledes lampliga. Vidare kunna syran och den polymera aminen tillsattas smorjoljan fOr att Mika salthildning in situ. The salts used according to the invention can be prepared by any conventional method for preparing salts of organic airlines and organic acids. Thus, the polymeric amine 16m in an organic solvent, for example benzene or xylene, and the acid can be added to the solution with stirring. The acid itself map of course Appears in a suitable solvent. Alternatively, the polymeric amine can be suspended in a suitable liquid medium and the acid stirred in the suspension. Yes. When using these methods, it may be necessary to isolate the salt by removing the release or suspending agent before adding the salt to the lubricating oil. Simpler methods, such as simply adding the acid to the narrow polymeric amine, are sometimes equally suitable. Furthermore, the acid and the polymeric amine can be added to the lubricating oil to increase salinity in situ.
Det är icke vasentligt att samtliga basiska kva.vegrupper i polymeren neutraliseras genom syran. I sjalva verket kunna battre resultat ernas, omit slutprodukten innehaller nagra oneutraliserade basiska kvaveatomer. Att kvarlamna nagra oneutraliserade basiska kvaveatomer kan vara onskvart, am saltet skall tjana sasom en detergent-tillsats forutom sasom viskositetsindex forbattrande medal. It is not essential that all basic nitrogen groups in the polymer be neutralized by the acid. In fact, better results can be obtained, because the end product contains some unneutralized basic nitrogen atoms. Leaving some unneutralized basic nitrogen atoms can be unfortunate, but the salt should serve as a detergent additive in addition to the viscosity index improving medal.
Smorjoljan i smorjoljekompositionerna enligt uppfinningen kan utgoras av en godtycklig naturlig eller syntetisk olja med smorjande egenskaper. Salunda kan oljan utgoras air en kolvatesmorjolja harledd fran en paraffinisk eller naftenisk raolja eller fran blandningar av sadana. Viskositeten hos dessa oljor kan variera inom ett brett omrade, exempelvis fran 100 SUS vid 38° G till 100 SUS vid 100° C. Kolvatesmorjoljorna kunna vara blandade med feta oljor, sasom rieinolja eller spackolja, och/eller med syntetiska jor, sasom polymeriserade (definer, sampolymerer av elkylenglykoler och alkylenoxider, organiska estrar, sasom di(2-etylhexyl)sebacat, dioktylftalat och trioktylfosfat, polymer tetrahydrofuran och polyalkylsilikonpolymerer, sasom dimetylsilikonpolymerer. Om onskvart kunna syntetiska smorjoljor anvandas sasom enda utga.ngsolja eller oeksa kunna de vara blandade med feta oljor eller derivat av sadana. The lubricating oil in the lubricating oil compositions of the invention may be any natural or synthetic oil having lubricating properties. Thus, the oil may be composed of a carbonate lubricating oil derived from a paraffinic or naphthenic crude oil or from mixtures thereof. The viscosity of these oils can vary within a wide range, for example from 100 SUS at 38 ° G to 100 SUS at 100 ° C. The carbonate lubricating oils may be mixed with fatty oils, such as castor oil or fuel oil, and / or with synthetic ions, as polymerized ( defines, copolymers of alkylene glycols and alkylene oxides, organic esters, such as di (2-ethylhexyl) sebacate, dioctyl phthalate and trioctyl phosphate, polymer tetrahydrofuran and polyalkylsilicone polymers, as well as dimethylsilicone polymers. fatty oils or derivatives thereof.
Salterna tillsattas till smorjoljan i en proportion av 0,1-20 vikt-% och vanligtvis 1-5 vat-%. The salts are added to the lubricating oil in a proportion of 0.1-20% by weight and usually 1-5% by water.
Smorjoljekompositioner enligt uppfinningen kunna modifieras genom infiirande av mindre mangder, sasom 0,01-2 %, av andra — — tillsatser, sasom flytpunktsnedsattande medel, antioxidanter, fluorescensmedel, korrosionsinhibitorer, oljighetsmedel och losningsframjande medel. Bland dylika material kunna namnas polymerer med hog molekylarvikt, sasom polyalkylmetakrylater, isobutylenpolymerer och alkylstyrenpolymerer, vax-naftalenkondensationsprodukter, alkylfenoler, sasom 2,6-di-tert.-butyl-4-metylfenol, oorganiska och organiska nitriter, sasom NaNO2 eller LiNO2 och di-isopropylammoniumnitrit eller dicyklohexylammoniumnitrit, organiska fosfiter, fosfater och fosfonater, sasom trikloretylfosfit och trikresylfosfat, fosforsulfid-olifin-reaktionsprodukter, sasom P2S-terpen-reaktionsprodukter, metallorganiska fosfater, sasom Caeller Zn-dicyklohexyltiofosfat eller metyleyklohexyltiolosfat, organiska sulfider, sasom vax-disulfid och etylenbistotylsulfid, samt monomera aminer, sasom oktadecylamin. LOsningsframjande medel fOr att framja losligheten av vissa av salterna enligt uppfinningen I smorjoljor, innefatta bl. a. langkedjiga alifatiska alkoholer och. fettsyror, sasom sLearylalkohol och oleinsyra, samt partiella estrar, sasom sorbitan-monooleat. Lubricating oil compositions of the invention may be modified by the introduction of minor amounts, such as 0.01-2%, of other additives, such as pour point depressants, antioxidants, fluorescent agents, corrosion inhibitors, oily agents and release agents. Such materials include high molecular weight polymers, such as polyalkyl methacrylates, isobutylene polymers and alkylstyrene polymers, wax-naphthalene condensation products, alkylphenols, such as 2,6-di-tert-butyl-4-methylphenol, inorganic and organic nitrites and di -isopropylammoniumnitrit or dicyclohexylammonium nitrite, organic phosphites, phosphates and phosphonates such as trikloretylfosfit and tricresyl phosphate, phosphorus-olifin reaction products, such P2S-terpene reaction products, metal organic phosphates, such Caeller Zn dicyklohexyltiofosfat or metyleyklohexyltiolosfat, organic sulfides such as wax-disulfide and etylenbistotylsulfid , and monomeric amines, such as octadecylamine. Solution-promoting agents for promoting the solubility of some of the salts according to the invention in lubricating oils, include e.g. a. long chain aliphatic alcohols and. fatty acids, such as sLearyl alcohol and oleic acid, and partial esters, such as sorbitan monooleate.
Normalt forbattra tillsatserna enligt uppfinningen aven utgangsoljans lastbarande egenskaper men dessa kunna em erforderligt ytterligare forbattras genom att tillsatta sma mangder, t. ex. c:a 0,5 vikt-%, oljelosliga alifatiska ditiokarbarnater ay tva'varda metaller ur periodiska systemets grupp II, exempelvis zink- eller kadmium-diamylditiokarbamat. Normally the additives according to the invention also improve the load-bearing properties of the starting oil, but these can be further improved if necessary by adding small amounts, e.g. about 0.5% by weight, oil-soluble aliphatic dithiocarbonates of two-valent metals of the Periodic Table Group II, for example zinc or cadmium diamyldithiocarbamate.
Tillsalserna kunna aven anvandas i samband med detergenter, sasom kalcium- eller bariumnaft a sulfonater. The additives can also be used in conjunction with detergents, such as calcium or barium naphtha and sulfonates.
Foljande exempel illustrera beredningen av de nya salterna enligt uppfinningen. The following examples illustrate the preparation of the novel salts of the invention.
Exempel 1. Example 1.
Den anvanda polymera aminen hade fram.- stallts genom sampolymerisering av en bland-fling av 12 vikt-% metylmetakrylat, 23 vikt-% tekniskt stearylmetakrylat, 60 vikt-% tekniskt laurylmetakrylat och 5 vikt-% 2-inety1-5-vinyl-pyridin genom den i belgiska patentet 563 612 beskrivna metoden. 3 viktdelar air denna sampolymer lostes 110 viktdelar bensen on ett ringa Overskott av saltsyra (raknat pa kvavehalten) tillsattes, Blandningen upphettades med aterloppskylning under en DeanStark-overdel till dess att intet ytterligare vat-ten franskildes. Till bensenlosningen sattes en kvantitativ mangd av natriumsaltet av dinonylfosfat. Natriumklorid utfalldes och fraufiltrerades. Filtratet destillerades under reducerat tryck for avlagsnande av bensenen, och de sista sparen avlagsnades pa angbad vid ett tryck av 0,1 ram Hg. Aterstoclen utgjordes av den polymera aminens dinonylfosfat. The polymeric amine used had been prepared by copolymerizing a mixture of 12% by weight of methyl methacrylate, 23% by weight of technical stearyl methacrylate, 60% by weight of technical lauryl methacrylate and 5% by weight of 2-methyl-5-vinyl-pyridine by the method described in Belgian patent 563 612. 3 parts by weight of this copolymer dissolved 110 parts by weight of benzene on a slight excess of hydrochloric acid (shaved on the nitrogen content) was added. The mixture was heated by refluxing under a DeanStark upper part until no additional water was separated. To the benzene solution was added a quantitative amount of the sodium salt of dinonyl phosphate. Sodium chloride precipitated and was filtered off. The filtrate was distilled under reduced pressure to remove the benzene, and the last traces were removed on a steam bath at a pressure of 0.1 .mu.m Hg. The backstock was the dinonyl phosphate of the polymeric amine.
Exempel 2. Example 2.
Den i exempel 1 beskrivna polymera aminen lostes i bensen och ett overskott av koncentrerad saltsyra tillsattes. Oyerskottet av saltsyra Mover det som erfordrades for bildande av amin-hydrold.orid-salt av sampolymeren airdestillerades, varvid det narvarande vattnet avenledes avlagsnades genom azeotrop destillation med anvandande av en Dean & Starkoverdel. Den resulterande losningen kyldes till e:a 60° C och darpa tillsattes en losning av natrium-di(3,5,5-trimetylhex.y1),ditiofosfat (teoretiska mangden baserad pa den ursprungliga sampolymerens halt av basiskt kvave). Blandningen omri3rdes under 30 ml-fluter vid 60° C. Bensenlosningen filtrerades sedan den kallnat f6r avlagsnande av natriumklorid soul uppstatt under saltbildningen. Efter avlagsnande air lOsningsmedlet vid reduce-rat tryck pa angba.d erh011s den polymera aminens dinonylditiofosfat. The polymeric amine described in Example 1 was dissolved in benzene and an excess of concentrated hydrochloric acid was added. The excess hydrochloric acid excess of that required for the formation of the amine hydride chloride salt of the copolymer was air distilled, the present water being removed by azeotropic distillation using a Dean & Stark supernatant. The resulting solution was cooled to about 60 ° C and then a solution of sodium di (3,5,5-trimethylhexyl), dithiophosphate (theoretical amount based on the basic nitrogen content of the original copolymer) was added. The mixture was stirred under 30 ml of flute at 60 ° C. The benzene solution was filtered after it had cooled to remove sodium chloride soul formed during the salt formation. After deprotection of the solvent under reduced pressure on angba.d, the dinonyldithiophosphate of the polymeric amine is obtained.
Exempel 3. 34 viktdelar av en polymer amin innehallande 0,22 mekv. hasiskt kvave per gram och framstalld air E. L du Pont de Nemours & Co. saint i handeln said under beteckningen LOA 564 lostes i 50 volymdelar av en mineralisk smorjolja med en viskositet av 65 sekunder Redwood I vid 60° C. Losningen upphettades till 100,0 C och ekvivalenta mangden (2,1 viktdelar) fast dikresylvatefosfat tillsattes, varvid erholls en losning av fosfatet av den polymera aminen i smorjoljan. Example 3. 34 parts by weight of a polymeric amine containing 0.22 meq. hashish suffocation per gram and produced air E. L du Pont de Nemours & Co. saint in the trade said under the designation LOA 564 was dissolved in 50 parts by volume of a mineral lubricating oil with a viscosity of 65 seconds Redwood I at 60 ° C. The solution was heated to 100.0 ° C and the equivalent amount (2.1 parts by weight) of solid dicresylvate phosphate was added, a solution of the phosphate of the polymeric amine in the lubricating oil is obtained.
Smorjoljekompositioner enligt uppfinningen askadliggoras av foljande exempel: Komposition A Saltet enligt excmpel 14 vikt-% Mineralisk smorjolja med en viskositet air 65 sekunder Redwood I yid 60° Crest Komposition B Saltet enligt exempel 14 vikt-% Antioxidant said under be- teckningen AN-20,75 vikt-% Smorjolj arest Komposition C Saltet enligt exempel 14 vikt-% Antioxidant said under be- teckningen AN-20,75 vikt-% Smorjoljarest Nedanstaende tabell visar den viskositetsokning i procent hos utgangsoljan, som ernatts med komposition A vid Ire temperaturer: 38° C99° C130° C 394658 Man ser salunda att saud enlig foreliggande uppfinning medfOr en mycket kraftigare 4— — f5rtjockning av utgan.gsoljan vid hoga An vid Mega temperaturer. Lubricating oil compositions according to the invention are ash-damaged by the following examples: Composition A The salt according to example 14% by weight Mineral lubricating oil with a viscosity air 65 seconds Redwood I yid 60 ° Crest Composition B The salt according to example 14% by weight Antioxidant said under the designation AN-20, 75% by weight Lubricating oil residue Composition C The salt according to Example 14% by weight Antioxidant said under the designation AN-20.75% by weight Lubricating oil residue The table below shows the percentage increase in viscosity of the starting oil obtained with composition A at Irish temperatures: 38 ° C99 ° C130 ° C 394658 It can thus be seen that according to the present invention a very thicker 4— - thickening of the starting oil at high An at Mega temperatures.
Komposition B underkastades ett slitageprov i en bilmotor och visade darvid nastan 80 Vo minskning av kamaxelforslitningen j am-fort med en liknande komposition, i vilken saltet enligt exemplet ersatts med en sampolymer av vinylpyrrolidon ()eh laurylmetakrylat. Aven vid faststallande av hogtrycksegenskaperna i en D4-ball-machine visade kompositionen forbattrade egenskaper jamfiirt med den liknande kompositionen. Vidare visade kompositionerna B och C goda lagtemperaturegenskaper vid anvandning i bilmotorer, vilket framgick am avsaknaden av slambildning. Composition B was subjected to a wear test in a car engine, thereby showing almost 80 Vo reduction of the camshaft wear compared with a similar composition, in which the salt according to the example was replaced with a copolymer of vinylpyrrolidone () or lauryl methacrylate. Even when determining the high pressure properties of a D4 ball machine, the composition showed improved properties compared to the similar composition. Furthermore, compositions B and C showed good layer temperature properties when used in car engines, as evidenced by the lack of sludge formation.
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