DE1040729B - Grease and process for its manufacture - Google Patents
Grease and process for its manufactureInfo
- Publication number
- DE1040729B DE1040729B DEE13282A DEE0013282A DE1040729B DE 1040729 B DE1040729 B DE 1040729B DE E13282 A DEE13282 A DE E13282A DE E0013282 A DEE0013282 A DE E0013282A DE 1040729 B DE1040729 B DE 1040729B
- Authority
- DE
- Germany
- Prior art keywords
- lubricating
- molecular weight
- high molecular
- lubricating grease
- carboxylic acid
- 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.)
- Pending
Links
Classifications
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- C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
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- C10M2201/08—Inorganic acids or salts thereof
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- C10M2201/081—Inorganic acids or salts thereof containing halogen
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
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- 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
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- 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/08—Thiols; Sulfides; Polysulfides; Mercaptals
- C10M2219/082—Thiols; Sulfides; Polysulfides; Mercaptals containing sulfur atoms bound to acyclic or cycloaliphatic carbon atoms
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
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- 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
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/042—Metal salts thereof
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- 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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/02—Unspecified siloxanes; Silicones
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
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- 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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/043—Siloxanes with specific structure containing carbon-to-carbon double bonds
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- 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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/044—Siloxanes with specific structure containing silicon-to-hydrogen bonds
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- 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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
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- 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
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- 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
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- 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
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- 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
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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Description
DEUTSCHESGERMAN
Die Erfindung betrifft Schmierfette, die sich besonders zur Hochtemperaturschmierung sowie zur Schmierung von Wälzlagern bei höheren und auch bei normalen Betriebstemperaturen eignen.The invention relates to lubricating greases which are particularly suitable for high-temperature lubrication and for lubrication of rolling bearings at higher and also at normal operating temperatures.
Es ist bekannt, hochdruckbeständige, konsistente Schmierfette auf Grundlage von Ölen und Seifen herzustellen, indem man den konsistenten Fetten geringe Mengen an Sulfaten, Sulfiten, Thiosulfaten, Phosphaten oder Boraten zusetzt. Hierbei können die genannten Salze auch während der Herstellung der Fette durch Mitverwendung von freier Säure und der entsprechenden Basenmenge erzeugt werden.It is known to produce high-pressure-resistant, consistent lubricating greases based on oils and soaps, by giving the consistent fats small amounts of sulfates, sulfites, thiosulfates, phosphates or borates added. The salts mentioned can also be used during the production of the fats of free acid and the corresponding amount of base.
Ferner ist es bekannt, daß man den Tropfpunkt von Schmierfetten erhöhen kann, indem man dem Reaktionsgemisch bei der Fettherstellung, solange es sich noch auf hoher Temperatur befindet, ein anorganisches Nitrit zusetzt. It is also known that the dropping point of greases can be increased by adding the reaction mixture to the grease production while it is still on high temperature, an inorganic nitrite adds.
Die vorliegende Erfindung macht nicht von derartigen Zusätzen zu Sqhmierfetten Gebrauch, sondern basiert auf der Verwendung eines durch Umsetzung einer Kombination mehrerer Säuren und einer Metallbase erzeugten Fettverdickers.The present invention does not make use of such additives to Sqhmierfetten, but is based on the use of one produced by reacting a combination of several acids and a metal base Fat thickener.
Die Anwendung von Kombinationen hochmolekularer Fettsäuren und niedrigmolekularer Carbonsäuren in verschiedenen Molverhältnissen als Fettverdicker ist bereits bekannt. Kürzlich wurde auch die Anwendung starker anorganischer Säuren in Verbindung mit hoch- und medrigmolekularen Carbonsäuren zur Herstellung wirksamer Fettverdicker vorgeschlagen, TJm den fertigen Schmierfetten eine genügende Stabilität und sonstige vorteilhafte Beschaffenheit zu verleihen, wurden diese Säuregemische im allgemeinen mit alkalischen Erden neutralisiert, wobei Calcium besonders bevorzugt wurde. Die niedrigmolekulare Carbonsäure, z.B. Essigsäure, wurde hierbei als notwendiger Bestandteil angesehen, wenn man zu einem beständigen Schmierfett gelangen wollte, das sich zur Anwendung bei höheren Temperaturen und unter hohen Belastungen eignet.The use of combinations of high molecular weight fatty acids and low molecular weight carboxylic acids in different Molar ratios as a fat thickener is already known. Recently, the application has also become stronger inorganic acids in connection with high and medium molecular weight carboxylic acids for the production of effective Fat thickener proposed that the finished lubricating greases have sufficient stability and others To impart a favorable texture, these acid mixtures were generally made with alkaline earths neutralized, with calcium being particularly preferred. The low molecular weight carboxylic acid, e.g. acetic acid, was seen as a necessary component, if you wanted to get a permanent grease that could be used at higher temperatures and suitable under high loads.
Es hat sich nun herausgestellt, daß man ausgezeichnete Schmierfette erhält, wenn man die niedrigmolekulare Carbonsäure vollständig durch Salpetersäure ersetzt und das Schmierfett durch gemeinsame Neutralisation eines Gemisches von hochmolekularer Fettsäure und Salpetersäure in einem Schmieröl mit 'einer Alkalibase herstellt. Wie nachstehend gezeigt wird, sind für die Zwecke der Erfindung die Salpetersäure und die Alkalimetalle den niedrigmolekularen Carbonsäuren bzw, den Erdalkalimetallen durchaus nicht gleichwertig.It has now been found that excellent lubricating greases are obtained by using the low molecular weight Carboxylic acid is completely replaced by nitric acid and the grease by common neutralization of one Mixture of high molecular weight fatty acid and nitric acid in a lubricating oil with an alkali base. As will be shown below, for purposes of the invention, the nitric acid and alkali metals are the Low molecular weight carboxylic acids or alkaline earth metals are by no means equivalent.
Es ist nicht genau bekannt, welche Umsetzungen mit der Salpetersäure bei -.der gemeinsamen Neutralisation
mit den hochmolekularen Carbonsäuren stattfinden. Gewisse Anzeichen deuten darauf hin, daß die Salpetersäure
vor der Neutralisation mit der Alkalibase mit den Organischen Verbindungen reagiert. Für den vorliegenden
Schmierfett und Verfahren
zu seiner HerstellungIt is not exactly known which reactions with the nitric acid take place during the joint neutralization with the high molecular weight carboxylic acids. Certain signs indicate that the nitric acid reacts with the organic compounds before neutralization with the alkali base. For the present grease and procedure
for its manufacture
Anmelder:Applicant:
Esso Research, and Engineering Company, Elizabeth, N. J. (V. St. A.)Esso Research, and Engineering Company, Elizabeth, N. J. (V. St. A.)
Vertreter: B. Maemecke, Berlin-Iichterfelde West,Representative: B. Maemecke, Berlin-Iichterfelde West,
und Dr. W. Kühl, Hamburg 36, Esplanade 36 a,and Dr. W. Kühl, Hamburg 36, Esplanade 36 a,
PatentanwältePatent attorneys
Beanspruchte Priorität:Claimed priority:
V. St. v. Amerika vom 30. November 1955V. St. v. America November 30, 1955
Zweck genügt es, festzustellen, daß die Salpetersäure zur Herstellung ausgezeichneter Schmierfette beiträgt.Suffice it to say that nitric acid contributes to the manufacture of excellent lubricating greases.
Das erfindungsgemäße Schmierfett auf Grundlage eines Schmieröls ist daher dadurch gekennzeichnet, daß es als Verdicker ein mit einer Alkalibase gemeinsam neutralisiertes Gemisch von Salpetersäure und -einer hochmolekularen C12- bis Cgo-Carbonsäure enthält.The lubricating grease according to the invention based on a lubricating oil is therefore characterized in that it contains, as a thickener, a mixture of nitric acid and a high molecular weight C 12 to C 12 carboxylic acid which has been neutralized jointly with an alkali base.
Man kann die Salpetersäure im Rahmen der Erfindung entweder in konzentrierter Form oder als verdünnte Lösung anwenden. Im letzteren Fall kann die Konzentration der Salpetersäure in der wäßrigen Lösung im Bereich von etwa 6 bis 99,9 Gewichtsprozent liegen. Im allgemeinen arbeitet man jedoch mit der konstant siedenden Säure des Handels, die etwa 70°/0 HNO3 enthält. Die Menge der bei dem Fettherstellungsverfahren nach der Erfindung angewendeten Salpetersäure liegt im Bereich von 1 bis 8, vorzugsweise von etwa 2 bis 5 Gewichtsprozent des fertigen Schmierfettes. In the context of the invention, nitric acid can be used either in concentrated form or as a dilute solution. In the latter case, the concentration of nitric acid in the aqueous solution can range from about 6 to 99.9 percent by weight. In general, however, of commerce, containing about 70 ° / 0 HNO 3 works with the constant boiling acid. The amount of nitric acid employed in the grease manufacturing process of the invention is in the range of 1 to 8, preferably about 2 to 5 percent by weight of the finished grease.
Für die Zwecke der Erfindung eignen-sich hochmolekulare aliphatische Carbonsäuren mit 12 bis 30, vorzugsweise etwa 18 bis 22 C-Atomen im Molekül. Oiese Säuren können von gesättigten -ader ungesättigten, in der Isiatur vorkommenden oder synthetischen Stoffen abgeleitet sein. Bevorzugt werden die normalerweise zur Herstellung der üblichen Schmierfette verwendeten Fettsäuren, insbesondere die stärker gesättigten Monocarbonsäuren. Beispiele für solche Säuren sind Laurinsäure, Myristinsäure, Palmitinsäure, Stearinsäure, Mono- und -Polyoxystearinsäuren, Arachinsäure sowie hydrierte Fischölsäuren und Talgsäuren. Man kann jedoch auch mit un-High molecular weight ones are suitable for the purposes of the invention aliphatic carboxylic acids with 12 to 30, preferably about 18 to 22 carbon atoms in the molecule. These acids can of saturated -vein unsaturated, in the Isiature occurring or synthetic substances. They are normally preferred for manufacture the fatty acids used in the usual lubricating greases, especially the more saturated monocarboxylic acids. Examples of such acids are lauric acid, myristic acid, palmitic acid, stearic acid, mono- and polyoxystearic acids, Arachidic acid as well as hydrogenated fish oleic acids and tallow acids. However, one can also use un-
409 657M20409 657M20
gesättigten Fettsäuren, wie Oleinsäure, Ricinolsäure und ähnlichen Säuren, arbeiten. Von diesen hochmolekularen Fettsäuren verwendet man zur Herstellung der Schmierfette nach der Erfindung etwa 5 bis 20, vorzugsweise etwa 8 bis 15 Gewichtsprozent, bezogen auf das fertige Schmierfett.Saturated fatty acids, such as oleic acid, ricinoleic acid, and similar acids, work. Of these high molecular weight Fatty acids are used for the preparation of the lubricating greases according to the invention about 5 to 20, preferably about 8 to 15 percent by weight, based on the finished lubricating grease.
Das Molverhältnis von Salpetersäure zu hochmolekularer Carbonsäure soll zwischen etwa 1:5 und vorzugsweise 2:1 liegen. Besonders bevorzugt wird ein Molverhältnis von etwa 1:1.The molar ratio of nitric acid to high molecular weight carboxylic acid should be between about 1: 5 and preferably 2: 1. A molar ratio is particularly preferred of about 1: 1.
Geeignete Metallbasen zur Neutralisation dieser Säuregemische sind die Hydroxyde und Carbonate der Alkalimetalle Natrium, Kalium und Lithium. Natriumhydroxyd wird besonders bevorzugt. Nach dem erfindungsgemäßen Verfahren arbeitet man gewöhnlich mit etwa 2 bis 10 Gewichtsprozent Metallhydroxyd oder -carbonat, bezogen auf das fertige Schmierfett. Gegebenenfalls kann man auch mit Gemischen der obigen Metalle arbeiten.Suitable metal bases for neutralizing these acid mixtures are the hydroxides and carbonates of the alkali metals Sodium, potassium and lithium. Sodium hydroxide is particularly preferred. According to the invention Processes are usually carried out with about 2 to 10 percent by weight metal hydroxide or carbonate, based on on the finished grease. If appropriate, you can also work with mixtures of the above metals.
Die als flüssige Phase bei der Herstellung der erfindungsgemäßen Schmierfette verwendeten Schmieröle ao können entweder die üblicherweise zur Fettherstellung dienenden Mineralöle oder synthetische Schmieröle sein. Allgemein sollen die Mineralöle und synthetischen Öle eine Viskosität im Bereich von etwa 7,5 bis 435 cSt bei 37,80C und etwa 1,2 bis 47 cSt bei 98,9°C, einen ASTM-Stockpunkt von etwa — 6,7 bis — 59 C, einen Flammpunkt von etwa 177 bis 343° C und einen Viskositätsindex von etwa 0 bis 60 besitzen; man kann jedoch auch mit Schmierölen eines Viskositätsindex von 100 oder darüber hinaus arbeiten.The lubricating oils ao used as the liquid phase in the production of the lubricating greases according to the invention can either be the mineral oils customarily used for the production of grease or synthetic lubricating oils. Generally are the mineral oils and synthetic oils have a viscosity in the range of about 7.5 to 435 cSt at 37.8 0 C and about 1.2 to 47 cSt at 98.9 ° C, an ASTM pour point of about - 6.7 to -59 C, a flash point of about 177 to 343 ° C and a viscosity index of about 0 to 60; however, it is also possible to work with lubricating oils with a viscosity index of 100 or more.
Das Schmierfett nach der Erfindung enthält 50 bis 90, vorzugsweise etwa 70 bis 85 Gewichtsprozent Mineralschmieröl und bzw. oder synthetisches Schmieröl und 10 bis 50, vorzugsweise etwa 15 bis 30 Gewichtsprozent der aus den oben angegebenen Säuregemischen und der Metallbase erhaltenen Reaktionsprodukte.The lubricating grease according to the invention contains 50 to 90, preferably about 70 to 85 percent by weight of mineral lubricating oil and / or synthetic lubricating oil and 10 to 50, preferably about 15 to 30 percent by weight of the reaction products obtained from the above-mentioned acid mixtures and the metal base.
Die Schmierfette nach der Erfindung können allgemein durch gemeinsame Neutralisation eines Gemisches von Salpetersäure und hochmolekularen Carbonsäuren in einem Schmieröl hergestellt werden. Das gemeinsam neutralisierte Gemisch wird dann auf etwa 177 bis 288° C, vorzugsweise etwa 230 bis 288° C, erhitzt und darauf zu einem Schmierfett gekühlt. Das gekühlte Fett kann fertig verarbeitet werden, indem man es durch eine Gaulin-Homogenisiervorrichtung, eine Morehouse-Mühle oder eine andere zu diesem Zweck geeignete Homogenisiervorrichtung bei Drücken von etwa 210 bis 560 kg/cm2 und bei hohen Schergeschwindigkeiten im Bereich von etwa 100 000 bis 500 000 Sek.-1 hindurchschickt.The lubricating greases of the invention can generally be prepared by co-neutralizing a mixture of nitric acid and high molecular weight carboxylic acids in a lubricating oil. The co-neutralized mixture is then heated to about 177 to 288 ° C, preferably about 230 to 288 ° C, and then cooled to a grease. The chilled fat can be finished by passing it through a Gaulin homogenizer, Morehouse mill or other suitable homogenizer at pressures of about 210-560 kg / cm 2 and at high shear rates in the range of about 100,000 round sends to 500,000 secs. 1
Das bevorzugte Verfahren zur Herstellung der erfindungsgemäßen Schmierfette besteht darin, daß man die hochmolekulare Carbonsäure in einem direkt beheizten Fettkessel in der Gesamtmenge der Schmierölgrundlage oder einem Teil derselben dispergiert und die Dispersion auf etwa 43 bis 65° C erwärmt. Sobald die hochmolekulare Carbonsäure vollständig geschmolzen ist, setzt man die Salpetersäure und dann sofort die Metallbase unter Rühren zu. Zur Abtreibung des Wassers erhitzt man dann weiter auf etwa 127 bis 154° C. Nach der Dehydratisierung setzt man gegebenenfalls den Rest des Schmieröls zu und erhitzt auf etwa 204 bis 260° C. Das Erhitzen wird dann unterbrochen und das Fett rasch unter Rühren gekühlt. Bei etwa 93° C kann man beliebige der üblichen Schmiermittelzusätze, wie Oxydationsverzögerer, Korrosionsinhibitoren, Metalldeaktivatoren, Hochdruckzusätze, Mittel zur Verbesserung der fadenziehenden Eigenschaft u. dgl., zugeben. Dann kühlt man das Fett weiter auf etwa 50 bis 82° C und nimmt die Fertigverarbeitung in einer Gaulin-Homogenisiervorrichtung oder einer Morehouse-Mühle vor.The preferred method of making the lubricating greases of the invention is that high molecular carboxylic acid in a directly heated fat tank in the total amount of the lubricating oil base or a portion thereof and the dispersion is heated to about 43 to 65 ° C. Once the high molecular weight Carboxylic acid is completely melted, add the nitric acid and then immediately the metal base with stirring to. To remove the water, heat is then continued to around 127 to 154 ° C. After dehydration If necessary, the remainder of the lubricating oil is added and the mixture is heated to about 204 to 260 ° C. The heating is then carried out interrupted and the fat quickly cooled while stirring. At about 93 ° C you can use any of the usual lubricant additives, such as oxidation retardants, corrosion inhibitors, metal deactivators, extreme pressure additives, agents to improve the thread-pulling property and the like. Then you cool the fat further down to about 50 to 82 ° C and takes the final processing in a Gaulin homogenizer or a Morehouse mill before.
Wenn ein Teil des Schmieröls aus einem verseifbaren synthetischen Öl besteht, dispergiert man vorzugsweise die Reaktionsteilnehmer zunächst in einem Mineralöl oder in demjenigen Teil des Schmieröls, der aus unverseifbarem synthetischem Öl besteht, und fügt erst dann das verseifbare synthetische Öl zu dem Fettansatz hinzu, wenn dieser gekühlt worden ist. Besteht jedoch das verwendete Schmieröl vollständig aus einem verseifbaren synthetischen Schmieröl, so ist es ratsam, das Reaktionsgemisch zunächst bei einer verhältnismäßig niedrigen Temperatur, z. B. 104 bis 150° C, zu dehydratisieren, bevor man es zur Bildung des erfindungsgemäßen Schmierfettes auf eine Temperatur von etwa 204° C erhitzt.When part of the lubricating oil consists of a saponifiable synthetic oil, it is preferred to disperse the reactants first in a mineral oil or in that part of the lubricating oil that consists of unsaponifiable synthetic oil, and only then adds the saponifiable Synthetic oil is added to the fat base when it has been cooled. However, there is the one used Lubricating oil is made entirely from a saponifiable synthetic lubricating oil, so it is advisable to use the reaction mixture initially at a relatively low temperature, e.g. B. 104 to 150 ° C to dehydrate before it to Formation of the grease according to the invention heated to a temperature of about 204 ° C.
Ein Schmierfett nach der Erfindung wurde aus den folgenden Bestandteilen hergestellt:A grease according to the invention was made from the following ingredients:
* Säuregemisch, welches bezüglich seines Molekulargewichts und Sättigungsgrades technischer Stearinsäure entspricht.* Acid mixture which corresponds to technical stearic acid in terms of its molecular weight and degree of saturation.
** Das Fett enthält außerdem noch: 0,80 Gewichtsprozent Natrium-Er dölsulfonat und 0,50 °/0 Salicylaläthylendiamin.** The fat also contains 0.80 weight percent sodium He dölsulfonat and 0.50 ° / 0 Salicylaläthylendiamin.
HerstellungManufacturing
Schmierfett A. Etwa zwei Drittel der gesamten Mineralschmierölmenge und die Gesamtmenge der hydrierten Fischölsäuren wurden in einen direkt beheizten Fettkessel aufgegeben und auf etwa 54° C erwärmt. Sobald die hydrierten Fischölsäuren vollständig geschmolzen waren, wurde die Salpetersäure als konzentrierte Lösung zugesetzt. Unmittelbar darauf wurde unter beständigem Rühren 40°/0ige wäßrige Natronlauge zugegeben. Dann wurde die Mischung auf etwa 150° C erhitzt. Nach vollständiger Abtreibung des Wassers wurde der Rest des Mineralschmieröls zugesetzt. Dann wurde weiter auf etwa 250° C erhitzt. Sobald diese Temperatur erreicht war, wurde das Erhitzen unterbrochen und das Fett schnell unter Rühren gekühlt. Das Phenyl-a-naphthylamin wurde bei etwa 93° C zugesetzt. Dann wurde das Fett in einer Gaulin-Homogenisiervorrichtung bei etwa 65° C fertig verarbeitet. Lubricating grease A. Approximately two thirds of the total amount of mineral lubricating oil and the total amount of hydrogenated fish oleic acids were placed in a directly heated fat kettle and heated to about 54 ° C. When the hydrogenated fish oleic acids were completely melted, the nitric acid was added as a concentrated solution. Immediately thereafter strength with constant stirring to 40 ° / 0 aqueous sodium hydroxide was added. The mixture was then heated to about 150 ° C. After the water was completely aborted, the remainder of the mineral lubricating oil was added. The heating was then continued to about 250 ° C. As soon as this temperature was reached, the heating was stopped and the fat was rapidly cooled with stirring. The phenyl-a-naphthylamine was added at about 93 ° C. Then the fat was processed in a Gaulin homogenizer at about 65 ° C.
Schmierfett B. Das Kalkhydrat, die Stearinsäure und das Mineralschmieröl wurden in einen direkt beheizten Fettkessel aufgegeben und unter Rühren auf etwa 50° C erwärmt. Dann wurde die Salpetersäure zugesetzt und das Gemisch auf etwa 260° C erhitzt. Das Erhitzen wurde sodann unterbrochen und das Fett unter Rühren auf etwa 93° C gekühlt. Darauf wurde das Phenyl-a-naphthylamin zugesetzt. Das Fett wurde weiter auf etwa 82° C gekühlt und schließlich in einer Gauün-Homogemsiervorrichtung bei etwa 455 kg/cm2 fertig verarbeitet.Lubricating grease B. The hydrated lime, stearic acid and mineral lubricating oil were placed in a directly heated fat kettle and heated to about 50 ° C. while stirring. The nitric acid was then added and the mixture heated to about 260 ° C. The heating was then interrupted and the fat was cooled to about 93 ° C. with stirring. The phenyl-a-naphthylamine was then added. The fat was cooled further to about 82 ° C. and finally processed in a Gauün homogenizer at about 455 kg / cm 2 .
Schmierfett C. Das Rüböl und die Hälfte des Mineralöls wurden in einem direkt beheizten Fettkessel miteinander gemischt und auf 50° C erwärmt. Dann wurde 40%igeGrease C. The rapeseed oil and half of the mineral oil were mixed together in a directly heated fat kettle and heated to 50 ° C. Then it became 40%
wäßrige Natronlauge zugesetzt und das Gemisch auf 1500C erhitzt. Sobald die Schaumbildung nachgelassen hatte und das meiste Wasser abgetrieben war, wurde während des weiteren Erhitzens auf 260° C der Rest des Schmieröls langsam hinzugefügt. Bei 204° C findet eine zweite Reaktion unter Schaumentwicklung und Volurnenvermehrungaqueous sodium hydroxide solution was added and the mixture heated to 150 0 C. Once the foaming had subsided and most of the water had driven off, the remainder of the lubricating oil was slowly added while further heating to 260 ° C. At 204 ° C a second reaction takes place with foam development and increase in volume
statt. Es wurde weiter erhitzt, bis die Schaumbildung nachgelassen hatte. Dann wurde das Fett unter Rühren auf 120° C gekühlt. Hierauf wurde das Phenyl-a-naphthylamin zugesetzt und das Fett weiter auf 82 bis 93° C gekühlt. Schließlich wurde das Fett filtriert, homogenisiert und verpackt.instead of. The heating was continued until the foaming had subsided. Then the fat was stirring cooled to 120 ° C. This was followed by the phenyl-a-naphthylamine added and the fat further cooled to 82 to 93 ° C. Finally the fat was filtered, homogenized and packed.
Eigenschaftenproperties
Aussehen Appearance
Tropfpunkt, 0C Drop point, 0 C
Penetration bei 25° C, mm/10Penetration at 25 ° C, mm / 10
Ruhpenetration Resting penetration
Walkpenetration nach 60 Stoßen Walk penetration after 60 thrusts
Walkpenetration nach 100 000 Stoßen Walk penetration after 100,000 hits
Norma Hoffman-Oxydationsprüfung (Stunden bis zumNorma Hoffman oxidation test (hours up to
Druckabfall um 0,35 kg/cm2) Pressure drop by 0.35 kg / cm 2 )
Schmierdauer, Stunden (10 000 U/Min.; 121° C) Lubrication time, hours (10,000 rpm; 121 ° C)
WasserlöslichkeitWater solubility
Wassertemperatur oberhalb 66° C Water temperature above 66 ° C
Wassertemperatur unterhalb 66° C Water temperature below 66 ° C
Radlagerprüfung (6 Stunden; 104° C; 660 U/Min.) Wheel bearing test (6 hours; 104 ° C; 660 rpm)
Phasenänderungen bis zu 204° C Phase changes up to 204 ° C
4-Kugel-Abnutzungsprüfung nach Shell; Schrammendurchmesser,
mm (1800 U/Min.; 10 kg; 1 Stunde; 750C) ausgezeichnet
210Shell 4-ball wear test; Scratch diameter, mm (1800 rpm; 10 kg; 1 hour; 75 0 C) excellent
210
165
175
340165
175
340
>400
>1553*> 400
> 1553 *
löslich
unlöslich
genügendsoluble
insoluble
enough
keineno
0,540.54
ausgezeichnetexcellent
halbflüssigsemi-liquid
* Der Wert beruht nicht auf dem Versagen der Schmierung, sondern die Prüfung wurde abgebrochen;
Schmierfett befanden sich noch in gutem Zustande.* The value is not based on the failure of the lubrication, but the test was aborted;
The grease was still in good condition.
ausgezeichnet 260excellent 260
190 200190 200
345345
232 1200 bis 2000232 1200 to 2000
löslich löslich genügend wird tropfenförmig und gummiartig bei 135 bis 150°soluble soluble enough becomes teardrop-shaped and rubbery at 135 to 150 °
0,550.55
die Lager und dasthe bearings and that
Man bemerkt, daß das der vorliegenden Erfindung entsprechende Schmierfett A nicht nur im Vergleich mit den aus hoch- und niedrigmolekularen Carbonsäuren mit oder ohne Mineralsäuren hergestellten Schmierfetten offensichtliche wirtschaftliche Vorteile bietet, sondern diesen Schmierfetten auch technisch überlegen ist, wie sich aus einem Vergleich mit Schmierfett C ergibt. Ferner zeigen die obigen Werte, daß die Verwendung einer Alkalibase an Stelle einer Erdalkalibase ein wichtiges Merkmal der Erfindung ist.It is noted that the grease A according to the present invention is not only in comparison with the lubricating greases made from high and low molecular weight carboxylic acids with or without mineral acids offers obvious economic advantages, but is also technically superior to these greases, like results from a comparison with grease C. Furthermore, the above values show that the use of a Alkali base rather than alkaline earth base is an important feature of the invention.
Werden etwas weichere Schmierfette als das Schmierfett A benötigt, so erhält man diese durch Mischen des homogenisierten oder nicht homogenisierten Schmierfettes A mit weiterem Schmieröl von der gleichen oder einer verschiedenen Viskosität. Der Erläuterung dieser Ausführungsform dient das folgende Beispiel:If slightly softer greases than grease A are required, these can be obtained by mixing the homogenized or non-homogenized lubricating grease A with further lubricating oil of the same or a different viscosity. The following example is used to explain this embodiment:
Bestandteile GewichtsprozentComponents by weight
Hydrierte Fischölsäuren 6,00Hydrogenated fish oleic acids 6.00
Salpetersäure (71 %) 1,90Nitric acid (71%) 1.90
Natriumhydroxyd 1,85Sodium hydroxide 1.85
Phenyl-a-naphthylamin 0,50Phenyl-a-naphthylamine 0.50
MineralschmierölMineral lubricating oil
9 cStbei98,9°C 39,759 cSt at 98.9 ° C 39.75
11,6 cSt bei 98,9° C (hydrofmiert) 50,0011.6 cSt at 98.9 ° C (hydrated) 50.00
HerstellungManufacturing
Das nach Beispiel 1 fertig verarbeitete Schmierfett A wurde mit der gleichen Menge eines hydrofinierten Destillatöles unter schwachem Erwärmen auf 66° C innig gemischt. Die Mischung wurde dann in einer Gaulin-Homogenisiervorrichtung bei 420 kg/cm2 fertig verarbeitet, filtriert und verpackt.The finished lubricating grease A according to Example 1 was intimately mixed with the same amount of a hydrofined distillate oil with gentle heating to 66.degree. The mixture was then processed in a Gaulin homogenizer at 420 kg / cm 2 , filtered and packaged.
Eigenschaftenproperties
Aussehen ausgezeichnetesAppearance excellent
gleichmäßigeseven
Produkt Penetration bei 25° C, mm/10Product penetration at 25 ° C, mm / 10
Ruhpenetration 265Resting penetration 265
Walkpenetration nach 60 Stoßen 290Walk penetration after 60 thrusts 290
WalkpenetrationWalk penetration
nach 100 000 Stoßen 375after 100,000 hits 375
Tropfpunkt, ° C 193Drop point, 193 ° C
Claims (8)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US550173A US2967151A (en) | 1955-11-30 | 1955-11-30 | Utilization of phosphoric acid in the preparation of greases |
Publications (1)
Publication Number | Publication Date |
---|---|
DE1040729B true DE1040729B (en) | 1958-10-09 |
Family
ID=24196045
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DEE13282A Pending DE1040729B (en) | 1955-11-30 | 1956-11-27 | Grease and process for its manufacture |
Country Status (4)
Country | Link |
---|---|
US (1) | US2967151A (en) |
DE (1) | DE1040729B (en) |
FR (1) | FR1165150A (en) |
GB (1) | GB793684A (en) |
Families Citing this family (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3196109A (en) * | 1962-03-01 | 1965-07-20 | Exxon Research Engineering Co | Lubricating grease containing boron nitride |
US3318807A (en) * | 1963-05-13 | 1967-05-09 | Texaco Inc | Lubricating greases containing finely divided inorganic metal salts and method of preparation therefor |
US3389085A (en) * | 1964-03-31 | 1968-06-18 | Exxon Research Engineering Co | Lubricants containing mixed metal salts of mono- and polybasic acids |
US3344065A (en) * | 1965-01-25 | 1967-09-26 | Molykote Produktions G M B H | Extreme pressure lubricants |
US4107058A (en) * | 1977-08-19 | 1978-08-15 | Exxon Research & Engineering Co. | Pressure grease composition |
US4787992A (en) * | 1986-02-18 | 1988-11-29 | Amoco Corporation | Calcium soap thickened front-wheel drive grease |
US5126062A (en) * | 1991-01-15 | 1992-06-30 | Nch Corporation | Calcium sulfonate grease and method of manufacture |
AU710294B2 (en) * | 1995-09-12 | 1999-09-16 | Lubrizol Corporation, The | Lubrication fluids for reduced air entrainment and improved gear protection |
BR112013013581A2 (en) * | 2010-12-06 | 2019-09-24 | Skf Ab | grease composition, mechanical component, use of grease composition, and method for preparing a grease composition |
CN104024162B (en) | 2011-10-31 | 2017-11-28 | Nch公司 | Calcium hydroxy apetite base sulfoacid calcium fat or oil composition and preparation method thereof |
US9458406B2 (en) | 2011-10-31 | 2016-10-04 | Nch Corporation | Calcium hydroxyapatite based sulfonate grease compositions and method of manufacture |
US9976102B2 (en) | 2011-10-31 | 2018-05-22 | Nch Corporation | Composition and method of manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents |
US9976101B2 (en) | 2011-10-31 | 2018-05-22 | Nch Corporation | Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents |
US10519393B2 (en) | 2016-05-18 | 2019-12-31 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
US10392577B2 (en) | 2016-05-18 | 2019-08-27 | Nch Corporation | Composition and method of manufacturing overbased sulfonate modified lithium carboxylate grease |
US10087387B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
US10087391B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent |
US10087388B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid |
US11661563B2 (en) | 2020-02-11 | 2023-05-30 | Nch Corporation | Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE850051C (en) * | 1940-09-24 | 1952-09-22 | Steinkohlenbergwerk Rheinpreus | Process for producing high pressure resistant, consistent lubricating greases |
GB718391A (en) * | 1952-01-30 | 1954-11-10 | Shell Refining & Marketing Co | Improvements in and relating to lubricating greases |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2417431A (en) * | 1945-03-31 | 1947-03-18 | Union Oil Co | Lubricants |
US2417430A (en) * | 1945-03-31 | 1947-03-18 | Union Oil Co | Lubricants |
US2417433A (en) * | 1945-04-23 | 1947-03-18 | Union Oil Co | Lubricating composition |
US2513680A (en) * | 1949-01-18 | 1950-07-04 | Socony Vacuum Oil Co Inc | Lime base grease |
US2846392A (en) * | 1953-10-21 | 1958-08-05 | Exxon Research Engineering Co | Metal soap-salt complexes and lubricants containing same |
-
1955
- 1955-11-30 US US550173A patent/US2967151A/en not_active Expired - Lifetime
-
1956
- 1956-11-23 GB GB35864/56A patent/GB793684A/en not_active Expired
- 1956-11-27 DE DEE13282A patent/DE1040729B/en active Pending
- 1956-11-29 FR FR1165150D patent/FR1165150A/en not_active Expired
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE850051C (en) * | 1940-09-24 | 1952-09-22 | Steinkohlenbergwerk Rheinpreus | Process for producing high pressure resistant, consistent lubricating greases |
GB718391A (en) * | 1952-01-30 | 1954-11-10 | Shell Refining & Marketing Co | Improvements in and relating to lubricating greases |
Also Published As
Publication number | Publication date |
---|---|
FR1165150A (en) | 1958-10-20 |
US2967151A (en) | 1961-01-03 |
GB793684A (en) | 1958-04-23 |
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