DE2014880A1 - Process for making overbased complexes - Google Patents

Process for making overbased complexes

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Publication number
DE2014880A1
DE2014880A1 DE19702014880 DE2014880A DE2014880A1 DE 2014880 A1 DE2014880 A1 DE 2014880A1 DE 19702014880 DE19702014880 DE 19702014880 DE 2014880 A DE2014880 A DE 2014880A DE 2014880 A1 DE2014880 A1 DE 2014880A1
Authority
DE
Germany
Prior art keywords
component
overbased
acid
complex
carbon atoms
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
Application number
DE19702014880
Other languages
German (de)
Inventor
Paul Eldon Chagrin Falls Ohio Greenough (V.St.A.)
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lubrizol Corp
Original Assignee
Lubrizol Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Lubrizol Corp filed Critical Lubrizol Corp
Publication of DE2014880A1 publication Critical patent/DE2014880A1/en
Pending legal-status Critical Current

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Description

" Verfahren zur Herstellung überbasischer Komplexe n "Process for the preparation of overbased complexes n

Priorität? 27. März 1969, V.St.A., Nr. 811 204 4. Febr. 1970» V.8t.A., Nr. (noon nicht bekannt) Priority? March 27, 1969, V.St.A., No. 811 204 February 4, 1970 »V.8t.A., No. (noon unknown)

Überbasische Metallkomplexe sind bekannt. Solche Komplexe eignen sich beispielsweise als Schmierstoffzusätze, Anstrichtrockentüittel, Stabilisatoren für Kunststoffe, Emulgatoren oder Kost-, Schutzmittel ■> Besonders wertvoll sind sie wegen ihrer Detergent- bzw. Dispergierungswirkung und ihrer Fähigkeit zur Neutralisierung unerwünschter saurer Verbindungen, die sich z.B0 in Kurbelgehäuse-^ Schmier st jf fen während des Betriebs des betreffenden Motors bilden. Aus diesem Grunde gehören die vorgenannten überbasischen Metallkomplexe zu den gebräuchlichsten Schmierstoffzusätzen 0 In einigen fällen treten bei der Einverleibung dieser Komplexe in Schmierstoffe jedoch Probleme auf, wie die höhere Schaumbildungsneigung von Schmierstoffen, die Detergentien enthalten, oder die neigung solcher Schmierstoffe zum Trube^werden beim Stehen»Overbased metal complexes are known. Such complexes are suitable for example as lubricant additives Anstrichtrockentüittel, stabilizers for plastics, emulsifiers or Kost-, preservatives ■> Especially valuable they are because of their detergent- or Dispergierungswirkung and their ability to neutralize undesirable acid compounds derived eg 0 in crankcase ^ Lubricate points form during operation of the relevant engine. For this reason, include the aforementioned overbased metal complexes to the most common lubricant additives 0 but fell in some occur in the incorporation of these complexes in lubricants problems as the higher foaming tendency of lubricants containing detergents, or the inclination of such lubricants to Trube ^ are standing »

BADBATH

00984 0/212 200984 0/212 2

Aufgabe* der Erfindung ist es, ein neues Verfahren zur Herstellung überbasißcher Komplexe mit verbesserter öllöelichkeit und geringerer Schaumbildun&swirkung gegenüber Schmierstoffen und somit spezieller Eignung als Schmierstoffzusätze zur Verfugung zu stellen.The object of the invention is to provide a new method of production overbased complexes with improved oil solubility and lower foaming effect compared to lubricants and thus to provide special suitability as lubricant additives.

Gegenstand der Erfindung ist somit ein Verfahren zur Herstellung von überbasischen Komplexen, uas dadurch gekennzeichnet ist, dassThe invention thus relates to a process for the preparation of overbased complexes, which is characterized, among other things, that

P A) ein überbasischer Metallsulfonat-, Hetallsulfonat-carboxylat- oder iietallcarboxylat-Komplex bei Temperaturen von etwa 25°C bis zur Zersetzun^atemperatur des Keaktionsgemisches mitP A) an overbased metal sulfonate, metal sulfonate carboxylate or metal carboxylate complex at temperatures of about 25 ° C. to the decomposition temperature of the reaction mixture

B) einer der Gesamtbasizitat der Komponente A) (gemessen als mg/KOH/g Komponente A) höchstens entsprechenden tienge mindestens einer hochmolekularen, gegebenenfalls durch mindestens einen Arylrest und/oder mindestens einen polaren Rest substituierten, pro Carboxylgruppe mindestens etwa 25 aliphatische C-Atotae aufweisenden aliphatischen Mono- oder ^ Polycarbonsäuren ihrer Anhydride, Ester, Ammoniumsalze, Aminsalze, Amide oder Imide, behandelt wird.B) one of the total basicity of component A) (measured as mg / KOH / g component A) at most corresponding tienge at least one high molecular weight, optionally with at least one aryl radical and / or at least one polar one Radical substituted aliphatic mono- or aliphatic mono- or aliphatic atoms per carboxyl group having at least about 25 aliphatic carbon atoms ^ Polycarboxylic acids of their anhydrides, esters, ammonium salts, Amine salts, amides or imides.

Der Ausdruck "Komplex" besieht sich hier auf Uberbasische Metallsalze, die einen Metallüberschuss aufweisen, bezogen auf den in einem neutralen oder normalen Metallealz vorhandenen Metallanteil, Unter dem einen Komplex kennzeichnenden "Metallverhältnis" ist somit das Verhältnis der gesamten Metalläquivalente zu den in einem neutralen oder normalen Me Lallsalz auftretenden fletalläquivalenten zu verstehen, während die "Basen-Oesamtbasizität
zahl"/eines Komplexes die in mg ausgedrückte Gewientemenge KOH bedeutet, der gemäts der Titration 1 g dee Komplexes entspricht.
The term "complex" refers here to overbased metal salts which have an excess of metal, based on the proportion of metal present in a neutral or normal Metallealz normal Me Lallsalz occurring metal equivalents to understand, while the "base-Oesamtbasität
number "/ of a complex means the weight of KOH, expressed in mg, which, according to the titration, corresponds to 1 g of the complex.

0 0 9 8 A 0 / 2 1 2 20 0 9 8 A 0/2 1 2 2

Die Metalle, yon denen sich die erfindungegemäBS eingesetzten Uberbaeischen Komplexe ableiten, können Alkalimetalle, wie Natrium, Kalium oder Lithium, oder Erdalkalimetalle, vie Magnesium, StrontJ.ua, Barium oder Calcium, sein» Die von den Erdalkalimetallen, insbesondere Calcium, Barium und Hagneeium, abgeleiteten Komplexe werden erfindungsgemäss bevorzugt verwendet.The metals of which the invention is used Deriving superstitious complexes, alkali metals such as sodium, Potassium or lithium, or alkaline earth metals, such as magnesium, StrontJ.ua, barium or calcium, his »Those derived from the alkaline earth metals, especially calcium, barium and hagneeium Complexes are preferably used according to the invention.

Beispiele für bekannte, erfindungsgemäss ale Komponente A) einsetzbare überbasische Metallkomplexe sind jene Komplexe, die sich von öllösuchen Sulfonsäuren, öllöslichen Carbonsäuren oder entsprechenden Gemischen, wie den in den USA0-Patentsehriften 2 501 731, 2 616 904, 2 616 905, 2 616 906, 2 616 911,Examples of known, according to the invention ale component A) applicable overbased metal complexes are those complexes which are derived from öllösuchen sulfonic acids, oil-soluble carboxylic acids or mixtures appropriate, such as in the United States 0 -Patentsehriften 2,501,731, 2,616,904, 2,616,905, 2616 906, 2 616 911,

2 616 924, 2 616 925, 2 617 049, 2 777 874, 3 027 325,2 616 924, 2 616 925, 2 617 049, 2 777 874, 3 027 325,

3 256 1,86, 3 282 835, 3 384 585, 3 373 108, 3 365 396,3 256 1.86, 3 282 835, 3 384 585, 3 373 108, 3 365 396,

3 342 733, 3 320 162, 3 312 618 oder 3 318 809* beschriebenen Säuren oder Sauregemischen ableiten.3 342 733, 3 320 162, 3 312 618 or 3 318 809 * Derive acids or acid mixtures.

Ein Beispiel für ein besonders zweckiuässiges Verfahren zur Herstellung der er findung8gemäss einsetzbaren überbasischen Metall-An example of a particularly useful method of production according to the invention usable overbased metal

(A)
komplexe/besteht darin, dass eine öllöeliehe Sulfonsäure, wie eine synthetisch hergestellte Didodecylbenzoleulfoneäure, mit einem Überschuss Calciumoxid, z.B. 10 Äquivalenten CaO/ Äquivalent Säure, einen Pronotor, wie Methanol und/oder Heptylphenol und einen Lösungsmittel, wie Mineralöl, bei Temperaturen von 50 bis 150°C vermischt wird-und das Reaktionsgemisch anechliessend bis zur Erzielung einer homogenen Masse mit Kohlendioxid behandelt wird» Von Sulfonsäuren und/oder Carbonsäuren abgeleitete Komplexe sind z.B. nach dem in der USAo-Patentschrift 3 312 618 erläuterten Verfahren herstellbar. Ein weiteres Beispiel für ein solches Verfahren ist die Herstellung eines Mag-
(A)
Complex / consists in the fact that an oil-like sulfonic acid, such as a synthetically produced didodecylbenzenesulfonic acid, with an excess of calcium oxide, e.g. 10 equivalents CaO / equivalent acid, a pronotor, such as methanol and / or heptylphenol and a solvent, such as mineral oil, at temperatures from 50 to 150 ° C. and the reaction mixture is then treated with carbon dioxide until a homogeneous mass is obtained. Complexes derived from sulfonic acids and / or carboxylic acids can be prepared, for example, by the process explained in US Pat. Another example of such a process is the manufacture of a mag-

00 9 84 0/2122 -00 9 84 0/2122 -

-.C- ',,, BAD ORIGINAL-.C- ',,, BAD ORIGINAL

~4~ 20H880~ 4 ~ 20H880

nesiumsulfonatkomplexes, wobei ein Gemisch aue einer Sulfonsäure oder ihrem noriaalen Kagnesiumsalz, einem Überschuss an hagnesiumoxid, V.asser, sowie vorzugsweise einem Alkohol, wie Methanol, mit Kohlendioxid behandelt wird.nesiumsulfonatkomplexes, where a mixture aue a sulfonic acid or its norial magnesium salt, an excess of magnesium oxide, water, and preferably an alcohol such as methanol, is treated with carbon dioxide.

Sie Carbonsäuren, die sich zur Herstellung von erfindungsge— mäss als Komponente A) einsetzbaren Sulfonat-carboxylat-Komplexen und Carboxylat-Komplexen, d.h. von Komplexen eignen, die beispielsweise nach den vorgenannten Verfahren aus einem Gemisch einer Sulfonsäure mit einer Carbonsäure oder aus einer Carbonsäure allein anstatt aus einer Sulfonsäure hergestellt werden, sind öllösliche Carbonsäuren. Beispiele dafür sind hauptsächlich fettsäuren mit etwa 12 bis etwa 24 aliphatischen C-Atomen, wie Palmitin», Stearin-, Myrietin-, öl-, Linol-, Laurin- oder Behensäure. Es können auch cyclische Carbonsäuren verwendet werden, wie aromatische oder cycloaliphatische Carbonsäuren. Die geeigneten aromatischen Carbonsäuren weisen eine benzolartige Struktur auf, d.h. sie leiten sich beispielsweise von Benzol oder Naphthalin ab, und besitzen mindestens einen öllösich machenden Heat mit insgesamt mindestens etwa 15 bis 18, vorzugsweise etwa 15 bis etwa 200 C-Atomen· Beispiele für solche aromatische Carbonsäuren sind Stearylbenzoseäure, Phenylstearinsäure, durch einen oder mehrere Vfeohsreste mit mindestens etwa 18 C-Atomen substituierte Benzo·- oder Maphth allnalurta and Cetyloxybensc«säuren. Geeignete cycloaliphatische Carbonsäuren weisen etwa 12 bis etwa 30 C-Atome auf. Beispiele für solche Säuren sind Erdölnaphthensäuren, Cety!cyclohexancarbonsäuren, Dilauryldekahydronaphthalincarbonsäuren und Dioctylcyclopentancarbonsäuren. Die den vorgenannten Carbonsäuren entsprechendenYou carboxylic acids, which are used in the production of inventive According to sulfonate-carboxylate complexes and carboxylate complexes which can be used as component A), i.e. of complexes which be prepared, for example, by the aforementioned method from a mixture of a sulfonic acid with a carboxylic acid or from a carboxylic acid alone instead of a sulfonic acid, are oil-soluble carboxylic acids. Examples are mainly fatty acids with about 12 to about 24 aliphatic carbon atoms, such as Palmitin », stearin, myrietin, oil, linoleum, laurin or Behenic acid. Cyclic carboxylic acids can also be used such as aromatic or cycloaliphatic carboxylic acids. The suitable aromatic carboxylic acids have a benzene-like structure, i.e. they are derived, for example, from benzene or naphthalene, and have at least one oil soluble making heat with a total of at least about 15 to 18, preferably about 15 to about 200 carbon atoms · Examples of such aromatic carboxylic acids are stearylbenzoic acid, phenylstearic acid, by one or more Vfeohsreste with at least about 18 carbon atoms substituted benzo or maphth allnalurta and Cetyloxybene acids. Suitable cycloaliphatic carboxylic acids have about 12 to about 30 carbon atoms. Examples of such acids are petroleum naphthenic acids, Cety! Cyclohexanecarboxylic acids, Dilauryldekahydronaphthalenecarboxylic acids and dioctylcyclopentanecarboxylic acids. Those corresponding to the aforementioned carboxylic acids

009840/2122009840/2122

Thiocarbonsäuren, bei denen eines oder beide Sauerstoffatome der Carboxylgruppe durch eines bzw. zvei Schwefelatome ersetzt sind, sind ebenfalls geeignet.Thiocarboxylic acids in which one or both oxygen atoms of the carboxyl group are replaced by one or two sulfur atoms are also suitable.

Wenn sich die überbasischen Metallkomplexe der Komponente A) von einem Sulfonsäure-Carbonsäure-Gemisch ableiten, enthält diesee Gemisch 1 bis 5 Äquivalente, vorzugsweise 1 bis 2 Äquivalente der Sulfonsäure(n) pro Äquivalent der Carbonsäure(n).If the overbased metal complexes of component A) derive from a sulfonic acid-carboxylic acid mixture, this mixture contains 1 to 5 equivalents, preferably 1 to 2 equivalents of the sulfonic acid (s) per equivalent of the carboxylic acid (s).

Im allgemeinen werden im Verfahren der Erfindung als Komponente A) überbasische Metallkomplexe mit Metallverhältnissen von 1,1 bis etwa 30, vorzugsweise von 2 bis 20, eingesetzt.In general, as a component in the process of the invention A) overbased metal complexes with metal ratios from 1.1 to about 30, preferably from 2 to 20, are used.

Überbasische Metallkomplexe mit einer Basenzahl von mindestens etwa 70 werden erfindungsgemäss bevorzugt.Overbased metal complexes with a base number of at least about 70 are preferred according to the invention.

Ein wichtiges Merkmal des Verfahrens der Erfindung ist die Behandlung des Komplexes nach »seiner Bildung mit der hochmolekularen Carbonsäure oder ihrem Derivat (Komponente B). Die Bezeichnung "hochmolekulare Carbonsäure'* bezieht sich hier auf al 1-phatische Carbonsäuren, die eine Durchschnittszahl von mindestens etwa 25 aliphatischen C-Atomen pro Carboxylgruppe aufweisen« Beispiele für solche Carbonsäuren sind gegebenenfalls durch polare Reste substituierte von Alkanen oder Alkenen abgeleitete Carbonsäuren. Diese Säuren können entweder acyclische ■oder cyclische Carbonsäuren sein, sowie Arylreste als Subetituenten aufweisen« Beispiele für die polaren Substituenten sind Chlor-, Brom- und Jodatome sowie Äther- und Nitrogruppen. Die Säuren können Mono- oder Polycarbonsäuren, wie Di-, Trioder Te tracer bpneäur en, ZoBo substituierte Bernsteinsäuren,An important feature of the process of the invention is the treatment of the complex after »its formation with the high molecular weight carboxylic acid or its derivative (component B). The term "high molecular weight carboxylic acid" * refers here to al 1-phatic carboxylic acids which have an average number of have at least about 25 aliphatic carbon atoms per carboxyl group. Examples of such carboxylic acids are, where appropriate Carboxylic acids derived from alkanes or alkenes substituted by polar radicals. These acids can be either acyclic ■ or cyclic carboxylic acids, and also have aryl radicals as sub-substituents «Examples of the polar substituents are chlorine, bromine and iodine atoms as well as ether and nitro groups. The acids can be mono- or polycarboxylic acids, such as di-, tri or tetracer acidic acids, ZoBo-substituted succinic acids,

"■009.840/2122"■ 009.840 / 2122

20U88020U880

Maleinsäuren oder Malonsäuren, sein. Beispiele für erfinduz%egemäse bevorzugte hochmolekulare Carbonsäuren (B) eina die in der USA.-Patentschrift 3 219 666 beschriebenen Carbonsäuren· Die durch Kohlenwasserstoffreste mit mindestens etwa 50 aliphatischen C-Atomen substituierten hochmolekularen Carbonsäuren werden bevorzugt, insbesondere jene, deren Kohlenwasserstoffreste etwa 60 bis etwa 50G0 aliphatische C-Atome aufweisen. Auch die Säureanhydride und andere Säurederivate, aus denen die Säuren selbst gewinnbar sind, wie die in der USA»-Patentschrift 3 219 666 beschriebenen Derivate, sind erfindungsgemäss verwendbare Maleic acids or malonic acids. Examples of inventions preferred high molecular weight carboxylic acids (B) in U.S. Patent 3,219,666. The carboxylic acids described by hydrocarbon radicals with at least about 50 aliphatic High molecular weight carboxylic acids substituted with carbon atoms preferred, especially those whose hydrocarbon radicals have about 60 to about 50G0 aliphatic carbon atoms. Also the Acid anhydrides and other acid derivatives from which the acids themselves can be obtained, such as those in the USA »patent 3,219,666 described derivatives can be used according to the invention

Eine erfiüüun^sgeiaäss als Komponente B) besonders bevorzugte Klasse hochmolekularer Carbonsäuren bzw. ihrer Derivate sind die kohlenwaseerstoffsubstituierten Bernsteinsäuren und deren Anhydride, die etwa 50 bis im allgemeinen etwa 5000 aliphatische C-Atome aufweisen und die beispielsweise in der USAo-Patentschrift 3 219 666 beschrieben sind. Beispiele für solche Bernsteinsäuren bzw0 ihre Derivate sind Polyisobutenyl-(MgWo«760) bernsteinsäure, Polyisobutenyl (Mgw.«9OC) bernsteinsäure, Poljpropenyl (Mgw.=70C) bernsteinsäureanhydrid una Polyisobutenyl (Mgw.-1500) bernsteinsäure. Beiepiele für weitere erfindungsgemäss geeignete Carbonsäuren und ihre Derivate sind die durch Umsetzung eines halogenieren Kohlenwasserstoffs, wie chloriertes Polyisobuten (g.B. eines Molekularge-A class of high molecular weight carboxylic acids or their derivatives that are particularly preferred as component B) are the carbon-substituted succinic acids and their anhydrides, which have about 50 to generally about 5000 aliphatic carbon atoms and which are described, for example, in US Pat. No. 3,219,666 are. Examples of such succinic acids or 0 derivatives are polyisobutenyl (MgWO "760) succinic acid, polyisobutenyl (MGW." 9OC) succinic acid, Poljpropenyl (MGW. = 70C) succinic anhydride una polyisobutenyl (Mgw.-1500) succinic acid. Examples of other carboxylic acids suitable according to the invention and their derivatives are those obtained by reacting a halogenated hydrocarbon, such as chlorinated polyisobutene (gB of a molecular weight

wichts von 1000) mit einer (^-ungesättigten Carbonsäure, wie Acryl- oder Methacrylsäure oder einer eine solche Säure bildenden Verbindung, wie AcrylSäuremethylester, erhalten werden. Solche Säuren bzw. ihre Derivate werden in der USA «,-Patent-weight of 1000) with a (^ -unsaturated carboxylic acid, such as Acrylic or methacrylic acid or a compound which forms such an acid, such as methyl acrylate, can be obtained. Such acids or their derivatives are in the USA «, patent

0098A0/21220098A0 / 2122

"7" 201A880" 7 " 201A880

schrift 3 374 174 beschrieben.3 374 174.

Das Verfahren der Erfindung Kann bei jeder beliebigen Semperatur, beispielsweise bei Temperaturen von 250C bis zur Zersetzung temperatur des Reaktionsgemischeβ, durchgeführt werden. Vorzugsweise wird bei Temperaturen von etwa 50 bis etwa 25O0C, insbesondere von etwa 50 bis etwa 15O0C, gearbeitet. In einigen Fällen ist es zweckmässig, das Verfahren der Erfindung in Gegenwart eines Lösungejuittels, wie Benzol, Toluol, Schwerbenzin oder Mineralöl, durchzuführen.Be carried out the method of the invention may be temperature at any Semperatur, for example at temperatures of 25 0 C up to the decomposition of the Reaktionsgemischeβ. Is preferably carried out at temperatures of from about 50 to about 25O 0 C, in particular from about 50 to about 15O 0 C,. In some cases it is advantageous to carry out the process of the invention in the presence of a solvent such as benzene, toluene, heavy gasoline or mineral oil.

Xm Verfahren der Erfindung kann zur Behandlung des Komplexes (Komponente A) ein solcher Anteil der hochmolekularen Carbonsäure oder ihres Derivats (Komponente B) verwendet werden, dass dieser der OesaatbasizitHt (ausgedrückt durch die Basenzahl) des überbasischen Hetallkomplexes (A) entspricht. £8 wird jedoch häufig lediglich ein Anteil der Komponente B) verwendet, der höchstens 9C #, vorzugsweise höchstens 40 # der .Oesamtbasizltfit des Komplexes entspricht. Ee werden im allgemeinenThe method of the invention can be used to treat the complex (Component A) such a proportion of the high molecular weight carboxylic acid or its derivative (component B) is used that This is the basicity of the acid (expressed by the base number) of the overbased metal complex (A). 8 pounds will however often only a portion of component B) used, the at most 9C #, preferably at most 40 # of the total basic fit of the complex. Ee will in general 0,1 bis 10 Gew.-^, vorzugsweise 1 bis 10 Gew.-Jt, insbesondere 30.1 to 10% by weight, preferably 1 to 10% by weight, in particular 3

(B) bis 5 Gew.-^ der Carbonsäure oder ihres Derivats ,- bezogen(B) to 5 wt .- ^ of the carboxylic acid or its derivative , - based auf die eingesetzte hen&e des überbaeiechen Hetallkomplexee (A)on the inserted height of the covered metal complex (A)

Wenn im Verfahren der Erfindung als Komponente B) die Aminsalze, Ammoniumsalze, Imide, Amide oder Ester der* vorgenannten Carbonsäuren eingesetzt werden, sind die relativen Anteile dieser Verbindungen, bezogen auf die eingesetzte Menge des Uberbasischen Metallkomplexes, von Bedeutung. Ia allgemeinen soll der Anteil der vorgenannten Säurederivate 1 bie 25 1At vorzugsweise 5 bisIf the amine salts, ammonium salts, imides, amides or esters of the aforementioned carboxylic acids are used as component B) in the process of the invention, the relative proportions of these compounds, based on the amount of the overbased metal complex used, are important. In general, the proportion of the aforementioned acid derivatives should be 1 to 25 1 at, preferably 5 to

0.09-840/2122 ■■■0.09-840 / 2122 ■■■

-8~ 20U880 -8 ~ 20U880

10 $> der OesamtbasisltXt ties Komplexes entsprechen. Ein aueserhalb dee vorgenannten Bereichs liegender Anteil des Säurederivate ist für eine wirksame Behandlung des Komplexes nach dem Verfahren der Erfindung ungeeignet. Derivate der hochmolekularen Carbonsäuren sind in den USA.-Patentechriften 3 219 666, 3 374 174 und 3 381 022 beschrieben. Die In der USA-Patentschrift 3 219 666 beschriebenen Acylierungsprodukte von Aminen, speziell die von den hochmolekularen Bernsteinsäure!! einerseits und Ammoniak, Monoamineu und Alkylenpolyaminen andererseits abgeleiteten Produkte, eowie die in der USA.-Patentschrift 3 331 022 beecnriebenen Ester sind im Verfahren der Erfindung besonders vorteilhaft als Komponente B) einsetzbar. Bei Verwendung von Acylierung&produkten von Aminen oder von Estern als Derivate hochmolekularer Carbonsäuren (B) soll das erfindungsgtmäsBe Verfahren bei Temperaturen von etwa 100 bis etwa 25C C durchgeführt werden.10 $> correspond to the OesamtbasisltXt ties complex. A proportion of the acid derivative which is outside the abovementioned range is unsuitable for an effective treatment of the complex according to the process of the invention. Derivatives of the high molecular weight carboxylic acids are described in U.S. Patents 3,219,666, 3,374,174 and 3,381,022. The acylation products of amines described in US Pat. No. 3,219,666, especially those of the high molecular weight succinic acid !! on the one hand and ammonia, monoamines and alkylenepolyamines on the other hand, and the esters described in US Pat. No. 3,331,022, can be used particularly advantageously as component B) in the process of the invention. When using acylation products of amines or esters as derivatives of high molecular weight carboxylic acids (B), the process according to the invention should be carried out at temperatures from about 100 to about 25C.

Die erfindungsgemäss hergestellten j überThe j produced according to the invention over

basischen Komplexe eignen sich als Zusatzstoffe für Schmierstoffe, die für den Gebrauch in Motorkurbelgehäusen, Triebwerken, Zahnradgetrieben, Fahrgestellen, Drehmomentwandlern und anderen Einrichtungen für Kraftfahrzeuge sowie in industriellen Maschinen, Baumaschinen, iüsenbmhnlpkoeotiven und Schiffen vorgesehen sind. Die erfindun^sgemäss hergestellten Komplexe eignen sich ferner als Zusatzstoffe für Bitueenemuleionen und insektizide Mittel, als Stabiliaatoren für Weichmacher und Kunststoffe, als Zusatzstoffe für Anstrichmittel, Rostschutzmittel, Konservierungsöle, Schneiaule, Spülöle und Gerbstoffe, als aaulgatoren, als antiseptische Reini-basic complexes are suitable as additives for lubricants intended for use in engine crankcases, Engines, gear drives, chassis, torque converters and other devices for motor vehicles as well as in industrial machines, construction machinery, iüsenbmhnlpkoeotiven and ships are provided. The complexes prepared according to the invention are also suitable as additives for bituminous emulsions and insecticidal agents, as stabilizers for Plasticizers and plastics, as additives for paints, anti-rust agents, preservative oils, snow owls, flushing oils and tannins, as aaulgators, as antiseptic cleaners

009840/2122009840/2122

gungsmittel, als fettspaltende Mittel, als Flotierun0smittel sowie als Zusatzstoffe für Kraft- bzw„ Brennstoffe, wie Benzin, Heizöle oder Gasöl,restriction means, as lipolytic agents, as Flotierun 0 smittel and as additives for fuels or "fuels, such as gasoline, fuel oils or gas oil

Bei ihrer Verwendung als Scinaierst off zusätze werden die erfindungsgemäss hergestellten ' überbasischen , komplexe im allgemeinen in Konzentrationen von etwa C1I bis etwa 20 Gew.-ji, bezogen auf den Schmierstoff, eingesetzt„ Bei Schmierstoffen für das Kurbelgehäuse von Benzinmotoren werden optimale Konzentrationen von etwa 0,1 bis etwa 10 Gewo-?6, bei Schmierstoffen für_das Kurbelgehäuse von Dieselmotoren von etwa 1 bis etwa 20 Gew,-# verwendet. In Kraft»«- bzw,--Brennstoff en werden dieerfindungsgemäss hergestellten Produkte in einer Konzentration von 0,0001 bis etwa 2 Gew.-^ eingesetzt.When used as scinaierst off additives, the 'overbased, complexes produced according to the invention are generally used in concentrations of about C 1 to about 20% by weight, based on the lubricant about 0.1 to about 10 percent by o -? 6, wherein lubricants für_das crankcase of diesel engines, from about 1 to about 20 wt, - # used. In Kraft "" - or - fuels, the products manufactured according to the invention are used in a concentration of 0.0001 to about 2% by weight.

Die erfindungsgemäss hergestellten überbasischen Komplexe können mit guter Wirkung in den verschiedensten Schmierstoffen eingesetzt werden, deren Basiskomponentenverschiedene Öle mit einer Viskosität sind, die ihre Verwendung als Schmieröle gestattet, wie natürliche oder synthetische Öle oder geeignete Gemische. Die vorgenannten Schmierstoffe sind, wie erwähnt, hauptsächlich Schmieröle für Otto- und Dieselmotoren, wie Lastwagen- und sonstige Kraftfanrzeugmotoren, Zweitaktmotoren, Flugzeugkolbenmotoren sowie Schiffs- und üisenbahndieselmotoren. Aber auch z.B. Schmierstoffe für" automatische Getriebe, Aphsenschmierstoffe, Zahnradgetriebeöle, Metallbearbeitungsschmierstoffe oder Hydrauliköle und andere Schmieröle und -fette können durch Elnvefieibune, <ier erfindungsgemäss hergestellten überbaeischen lComplexe als Zusatzstoffe verbessert werden.The overbased complexes prepared according to the invention can used with good effect in a wide variety of lubricants the base components of which are different oils with a Viscosities that permit their use as lubricating oils, such as natural or synthetic oils or suitable mixtures. The aforementioned lubricants are, as mentioned, mainly lubricating oils for gasoline and diesel engines, such as truck and other motor vehicle engines, two-stroke engines, aircraft piston engines as well as marine and railway diesel engines. But also e.g. lubricants for "automatic gears, aphse lubricants, Gear transmission oils, metalworking lubricants or hydraulic oils and other lubricating oils and greases can get through Elnvefieibune, <ier coverings produced according to the invention lComplexes can be improved as additives.

009840/2122009840/2122

20U88020U880

Natürlich vjrkoniruende öle sinu sowohl tierische und pflanzliche Öle, wie Kicinusöl oder Speckbl, als auch Iö8unosmittelraffinierte ouer säureraffinierte Mineralschmieröle des paraffin-, naphthen- oder gemischtbaeischen Typs. Aus Kohle oder ölschiefer gewonnene öle mit einer Viskosität, die ihre Verwenaung als Schmierstoffe gestattet, sind ebenfalls als Baeiaöle geeignet. Beispiele für synthetische Schmieröle sind Öle auf der Grundlage von gegebenenfalls halogensubstituierten Kohlenwasserstoffen, wie Olefin-ilomo- und -Copolymerisate, z.B. Polybutene,Naturally mixed oils include both animal and vegetable oils, such as kicinus oil or bacon oil, as well as oil-refined or acid-refined mineral lubricating oils of the paraffin, naphthen or mixed-vegetable type. Oils obtained from coal or oil shale with a viscosity that allows them to be used as lubricants are also suitable as base oils. Examples of synthetic lubricating oils are oils based on optionally halogen-substituted hydrocarbons, such as olefin polymers and copolymers, e.g. polybutenes,

W Polypropylene,Propylen-Isobuten-Copolymerisate oaer chlorierte Polybutene, Alkylbenzole, z.B. Dottecylbenzole, Tetradecylbenzo-Ie, Dinonylbenzole ouer Di-(2-äthylhexyl)-benzole, und Polyphenyle, wie Diphenyle oder Terphenyle. Alkylenoxid-Homo- und -Copolymerisate und ihre Derivate, deren endständige Hydroxylgruppen ZoB, durch Veresterung oder Verätherung modifiziert wurden, sind eine weitere Klaase bekannter synthetischer Schmieröle. Beispiele dafür sind die durch Polymerisation von Äthylen- oder Propylenoxid hergestellten Öle, die Alkyl- und W polypropylenes, propylene-isobutene copolymers or chlorinated polybutenes, alkylbenzenes, for example dottecylbenzenes, tetradecylbenzenes, dinonylbenzenes or di- (2-ethylhexyl) -benzenes, and polyphenyls, such as diphenyls or terphenyls. Alkylene oxide homo- and copolymers and their derivatives, the terminal hydroxyl groups of which have been modified by esterification or etherification, are another class of known synthetic lubricating oils. Examples are the oils produced by the polymerization of ethylene oxide or propylene oxide, the alkyl and

^ Aryläther dieser Polyoxyalkylen-Polymerisate, wie Polyisopropylenglykolnie thy lather mit einem Durchschnittemolekulargewicht von 1000, Polyäthylenglykoldiphenylather mit einem Molekulargewicht von 500 bis IQOC- oder Polypropylenglykoldiäthyläther mit einem Molekulargewicht von 1000 bis 15CC, und ihre Ester mit Mono- und Polycarbonsäuren, wie die Essigsäureester, Gemische von Estern mit C, „-Fettsäuren oder der Diester^ Aryl ethers of these polyoxyalkylene polymers, such as polyisopropylene glycol thy lather with an average molecular weight of 1000, polyethylene glycol diphenyl ether with a molecular weight from 500 to IQOC or polypropylene glycol diethyl ether with a molecular weight of 1000 to 15CC, and their Esters with mono- and polycarboxylic acids, such as the acetic acid esters, mixtures of esters with C 1 -C fatty acids or the diesters

3-a3-a

einer C1--Carbonsäure des l'etraäthylenglykol&o Eine weitere Klasse geeigneter synthetischer Schmieröle sind die Ester von Dicarbonsäuren, wie der BenζοId!carbonsäuren, der Bernstein-, Malein-, Azelain-, Kork-, Sebacin-, Pumar-, Adipin- und dera C 1 carboxylic acid of tetraethylene glycol & o Another class of suitable synthetic lubricating oils are the esters of dicarboxylic acids, such as the BenζοId! carboxylic acids, the succinic, maleic, azelaic, cork, sebacic, pumar, adipic and the

J ' ;^i-j Q09840/2122 OAr> J '; ^ ij Q09840 / 2122 OAr>

BAD ORIGINALBATH ORIGINAL

" n ~ 20U880" n ~ 20U880

dlmeren Linoleäure mit Alkoholen, vie Butanol, Hexanol, Laurinalkohol, 2-Äthylhexanol ouer Pentaerythrit« Spezielle Beispiele für diese Ester sind Adipinsäuredibutyl-, Sebacinsäure-di-(2-äthylhexyl)-, Fumarsäure-di-n-hexyl-, Sebacinsäuredioctyl-, Azelainsäurediisooctyl-, Azelainsäuredlisodecyl-, Phthalsäuredioctyl-, Phthalsäuredidecyl- und SebacinBäuredieikosylester, sowie der 2-Äthylhexyldiester der dimeren Linoleäure und der durch Umsetzung von 1 Hol Sebacinsäure mit 2 Mol Tetraäthylenglykol unu 2 Mol 2-Äthylcapronsaure hergestellte.-aster. Öle auf der Grundlage von Silikonen, wie die Polyalkyl-, Pölyaryl-, Polyalkoxy- oder Polyaryloxyeiloxan- und-silikatöle, z.B. Tetraäthyls'ilikat, Tetraisopropyleilikat, Tetra-2-äthylhexylsilikat, Tetra-(4-metnyl-2-tetraäthyl)-eilikat, Tetra-p-terto-butylphenyleilikat, Hexyl-(4-Bethyl-2-pentoxy)-dieiloxant. die PoIymethylsiloxane oder die Polymetnylpheny!siloxane, sind eine weitere Klasse geeigneter synthetischer Schmierstoffe. Weitere synthetische Schmieröle sind die flüssigen iister von Phosphorsäuren, wie Trikre8ylphoephat, Trioctylphoephat oder Dekanphoephoneäurediäthylester, sowie polymerisiert« Tetrahydrofurane»Linoleic acid with alcohols such as butanol, hexanol, lauric alcohol, 2-ethylhexanol or pentaerythritol. Specific examples of these esters are adipic acid dibutyl, sebacic acid di- (2-ethylhexyl), fumaric acid di-n-hexyl, sebacic acid dioctyl, Azelaic acid diisooctyl, azelaic acid diisodecyl, phthalic acid dioctyl, phthalic acid decyl and sebacic acid diicosyl ester, as well as the 2-ethylhexyl diester of dimeric linoleic acid and the reaction of 1 part of sebacic acid with 2 mol of tetraethylene glycol and 2 mol of tetraethylene glycol. Oils based on silicone, such as the polyalkyl, polyaryl, polyalkoxy or polyaryloxyeiloxane and silicate oils, for example tetraethylsilicate, tetraisopropylsilicate, tetra-2-ethylhexylsilicate, tetra- (4-methyl-2-tetraethyl) -particle , Tetra-p-terto-butylphenyl silicate, hexyl- (4-ethyl-2-pentoxy) -dieiloxane t . the polymethylsiloxanes or the polymethylpheny / siloxanes are another class of suitable synthetic lubricants. Other synthetic lubricating oils are the liquid iisters of phosphoric acids, such as tricreylphoephate, trioctylphoephate or decanephoephone acid diethyl ester, as well as polymerized "tetrahydrofurans"

Die erfinciunLBgemäss her^eetellten Komplexe können, wie erwähnt, Schmierstoffen sowie Kraft- und Brennstoffen auchBueamaen ait anderen Zusatzstoffen einverleibt werden, wie zusätzliche aschehaltige oder aschefreie Detergentien t The erfinciunLBgemäss can ^ eetellten Complex ago, as mentioned, auchBueamaen lubricants and fuels ait other additives incorporated are as additional ash-containing or ash-free detergents t Viskositätsindex-Verbesserer, Stjckpunkteerniedriger, zusätzliche Antischaummittel, Hochdruckzu&ätze, Rottschutzalttel, Oxydatlonsinhibitoren, reibungaverbeesernde Kittel oder Korrosionsinhibitoren.Viscosity index improvers, item lowerers, additional Antifoam agents, high pressure additives, anti-rotting agents, oxidation inhibitors, anti-friction gowns or corrosion inhibitors.

009840/2122 BAD009840/2122 B AD

~l2~~ l2 ~ 20H88020H880

die zusätzlichen
21 <
the additional
21 <

Beispiele fiir/aschehaltigenDetergentien sind öllösliche neutrale und überbasische Salze organischer Phosphorsäuren, die mindestens eine unmittelbare Kohlenstoff-Phosphor-Binaung enthalten, wie sie durch Behandlung von Clefin-Polymerisaten, z.B. Polyisobuten mit einem Molekulargewicht von 1000, mit einem Phosphorierun^sniittel, wie PhosphortriChlorid, Phosphorheptaeulfiü, Phoephorpentasulfid, Phosphortrichloriu und Schwefel, weisser Phosphor und ein Schwefelhalo^eniü, ouer Phosphorthio- ^ Chlorid hergestellt werden« Die zumeist verwendeten Salze solcher Säuren sind die natrium-, Kalium-, Lithium-, Calcium-, Magnesium-, Strontium- und Bariumsalze. Zu den aschefreien Detergentien gehören auch die Acylierun^sprodukte von Aminen, wie sie z0B. in den USA.-Patentscuriften 3 172 892, 3 219 666 und 3 272 546 beschrieben sind.Examples of ash-containing detergents are oil-soluble, neutral and overbased salts of organic phosphoric acids which contain at least one direct carbon-phosphorus bond, as obtained by treating Clefin polymers, e.g. polyisobutene with a molecular weight of 1000, with a phosphorus agent such as phosphorus trichloride, Phosphorheptaeulfiü, Phoephorpentasulfid, Phosphortrichloriu and sulfur, white phosphorus and a sulfur halo ^ eniü, ouer phosphorothio ^ chloride are produced. The mostly used salts of such acids are the sodium, potassium, lithium, calcium, magnesium, strontium and Barium salts. To the ash-free detergents and the Acylierun ^ include sprodukte of amines, as described, for example, in the 0-USA. Patentscuriften 3,172,892, 3,219,666 and 3,272,546 are described.

Beispielt für Hochdruckzusätze und Korroeions- bzw. Oxydationsinhibitoren sind aliphatieche Chlorkohlenwasserstoffe, wie chloriertes Vrachs, organische Sulfide und Polysulfide, wie Benzyl- ^ disulfid, Bis-CchlorbenzylJ-disulfid, Dibutyltetrasulfid, sulfuriertes Spermöl, sulfuricrter ölsäuremethylester, sulfurierte Alkylphenole, sulfuriertes Dipenten oder sulfuriertes Terpen, phosphoeulfurierte Kohlenwasserstoffe, wie das Umsetzun^epro-Example for high pressure additives and corrosion and oxidation inhibitors are aliphatic chlorinated hydrocarbons, such as chlorinated Vrachs, organic sulfides and polysulfides, such as benzyl ^ disulfide, bis-chlorobenzyl-disulfide, dibutyl tetrasulfide, sulfurized Sperm oil, sulfurized oleic acid methyl ester, sulfurized Alkylphenols, sulfurized dipentene or sulfurized terpene, phosphoeulfurized hydrocarbons, such as the conversion

dukt eines Phosphorsulfids mit Terpentin,product of a phosphorus sulfide with turpentine,

Ester uer phosphorigen Säure, hauptsächlich X)I- und Trihyürocarbylphosphite, wie Dibutylph »ephit, x>iheptylphoephit, Dicyclohexylphosphit oaer Peritylphenylphoephit,una Metall-thiocarbauate, wie Zinkdioctylaitniooarbauat, und Dithiophoephate der iieteile der II. Gruppe des periodischen Systems, wie Zinkdicyclohexyldithiophoephat, Zinkdioctyldithiophosphat,Esters of phosphorous acid, mainly X) I- and Trihyurocarbyl phosphites, such as dibutylph »ephite, x> iheptylphoephite, Dicyclohexylphosphit or Peritylphenylphoephit, a Metall-Thiocarbauate, such as zinc dioctylaitniooarbauat, and dithiophoephate the iieteile of the II. group of the periodic table, like zinc dicyclohexyldithiophoephat, Zinc dioctyl dithiophosphate,

009840/2122009840/2122

Cadmiumdinonyldithiophosphat oder das Zinksal3 einer durch Umsetzung von Phosphorpentasulfid mit einem Gemisch aus 65 Mol-# Isobutanol und 35 Mol-# primärem Amylalkohol hergestellten Dithiophosphorsäure.Cadmium dinonyl dithiophosphate or the zinc salt of a reaction of phosphorus pentasulfide with a mixture of 65 mol # isobutanol and 35 mol # primary amyl alcohol Phosphorodithioic acid.

Beispiele für Antischaummittel sind Polymethaorylsäurealkylester, die Kondensationsprodukte eines Alkylphenols mit Formaldehyd und einem Amin, fluorierte Kohlenwasserstoff-Polymerisate und polymere Alkyl- und Aralkylsiloxane.Examples of antifoam agents are polymethaoryl acid alkyl esters, the condensation products of an alkylphenol with formaldehyde and an amine, fluorinated hydrocarbon polymers and polymeric alkyl and aralkyl siloxanes.

Die Beispiele erläutern die Erfindung. .The examples illustrate the invention. .

Beispiel 1example 1

Es wird eine. Mineralöllösung eines überbasischen Calciumkoaplexes hergestellt, indem ein Gemlsoh aus einer Alkylbenzolsulfonsäure (hgw. = 470), einem Calciumalkylphenolat, einer Alkoholmischung (Methanol, Butanol und Pentanol) und Calciumoxid im Überschuss (5,6 Äquivalente GaO/ Äquivalent der Säure) mit Kohlendioxid behandelt wird. Die Lösung weist einen Schwefelgehalt von 1,7 i°y einen Calciumgehalt von 12,6 # und eine Basenzahl von 336 auf. 950 g dieser Lösung werden dann bei 25 C mit 50 g eines durch einen Polyisobutenylrest mit einem holekulargewicht von 1000 substituierten Bernsteinsäureanhydrids, das eine Verseifungezahl von 100 aufweist, versetzt., Das erhaltene Gemisch wird gerührt, auf 1500C erhitzt, 30 Hinuten lang bei 150 C gehalten und schliesslich filtrierte Das filtrat weist eine Basenzahl von 315 auf und bnthält 35»4 MineralöleIt will be a. Mineral oil solution of an overbased calcium complex produced by treating a mixture of an alkylbenzenesulfonic acid (hgw. = 470), a calcium alkylphenolate , an alcohol mixture (methanol, butanol and pentanol) and calcium oxide in excess (5.6 equivalents GaO / equivalent of the acid) with carbon dioxide . The solution has a sulfur content of 1.7 ° i y a calcium content of 12.6 # and a base number of 336. 950 g of this solution are then incubated at 25 C with 50 g of a by a polyisobutenyl radical with a holekulargewicht 1000 substituted succinic anhydride having a Verseifungezahl of 100, was added., The resulting mixture is stirred, heated to 150 0 C, 30 Hinuten at Maintained at 150 C and finally filtered. The filtrate has a base number of 315 and contains 35 »4 mineral oils

Beispiel 2Example 2

950 g einer Lösung eines Uberbasisohen, mit Kohlendioxid be-"950 g of a solution of an overbased oil, loaded with carbon dioxide

handelten Calciumsalzes einer Alkylbenzolsulfonsäure .„..-... 0098Α0/2Ί22 traded calcium salt of an alkylbenzenesulfonic acid. "..-... 0098Α0 / 2Ί22

« 425) in Mineralöl (Basenzahl » 4Cb, Calciumgehalt 15,2 #, Schwefelgehalt * 1,4 #)werdenbei 57°C mit 50 g dee PolyiBobutenylbernsteinBäureanhydrids vom Beispiel 1 versetzt. Das erhaltene Gemisch wird 39 Minuten lang bei 55 bis 570C und aneohltessend 3C hinuten lang bei 152 bia 1530C gerührt und schliesslich bei 1500C filtriert. Das Piltrat weist eine Basenzahl von 387 auf und enthält 43,7 > Mineralöl.«425) in mineral oil (base number» 4Cb, calcium content 15.2 #, sulfur content * 1.4 #) are mixed with 50 g of the polybobutenyl amber anhydride from Example 1 at 57 ° C. The resulting mixture is stirred for 39 minutes at 55 to 57 0 C and aneohltessend 3C hinuten at 152 bia 153 0 C, and finally filtered at 150 0 C. The Piltrat has a base number of 387 and contains 43.7 > mineral oil.

Beispiel 3Example 3

iSin Gemisch aus 753 Gew.-teilen i'dneralöl, 1440 Gew.-teilen Xylol, 84 Gew.-teilen einer im Handel erhältlichen Fettsäuremischun^ (Säurezahl « 200), 59C Gew.-teilen einer Alkylbenzol-8ulfoneaure (MgW0 = 500) und 263 Gew.-teilen Wagneeiuaoxid wird auf 600C erhitzt und danach mit 360 Gew.-teilen Methanol und 180 Gew»-teilen wasser versetzt. Das erhaltene Gemisch wird bei Temperaturen von 65 bis 980C mit Kohlendioxid behandelt, wobei Methanol und Wasser in Form eines azeotrop siedenden Gemisches abdestilliert werden0 Anschliessend werden weitere 180 Gew„-teile Wasser zugesetzt, und die Behandlung mit Kohlendioxid wird 210 Minuten lang bei Temperaturen von 87 bis 900C fortgesetzt« Danach wird das Reaktionsgemisch unter einem Lruck von 20 Torr auf 16O0C erhitzt und bei 16O0C filtriert. Man erhält einen überbasischen, mit Kohlendioxid behandelten Magneeiumsulfonat-Carboxylat-Komplex (Ausbeute = 78,1?6), der 7,69 ^ Magnesium und 1,67 $ Schwefel enthält und jine Baeenzahl von 336 aufweist. 950 Gew.-teile dieses Komplexes werden mit 50 Gew.-teilen des Polyieobutenylbernsteinsäureanhydrids von Beispiel 1 versetzt, und das erhaltene Gemisch wird 30 Minuten lang auf 1500C erhitzt und anschliessenci filtriert. Sie Basenzahl aee dabei er-In a mixture of 753 parts by weight of i'dneral oil, 1440 parts by weight of xylene, 84 parts by weight of a commercially available fatty acid mixture (acid number <200), 59C parts by weight of an alkylbenzene-8ulfoneaure (MgW 0 = 500 ) and 263 parts by weight of Wagneeiuaoxid is heated to 60 0 C and then mixed with 360 parts by weight of methanol and 180 parts by weight of water. The mixture obtained is treated at temperatures 65 to 98 0 C with carbon dioxide, methanol and water in the form of an azeotropic boiling mixture are distilled off 0 then be further 180 wt "parts of water was added, and the treatment with carbon dioxide at 210 minutes temperatures "continued from 87 to 90 0 C. Thereafter, the reaction mixture is heated under a Lruck of 20 Torr to 16O 0 C and filtered at 16O 0 C. The result is a overbased, treated with carbon dioxide Magneeiumsulfonat-carboxylate complex (yield = 78.1? 6) containing 7.69 ^ 1.67 $ magnesium and sulfur and having jine Baeenzahl of 336th 950 parts by weight of this complex are mixed with 50 parts by weight of the Polyieobutenylbernsteinsäureanhydrids of Example 1, and the resulting mixture is heated for 30 minutes at 150 0 C and anschliessenci filtered. You base number aee

009840/2122009840/2122

haltenen Produkte beträgt 315held products is 315

Beispiel 4Example 4

Ein Gemisch aus 66,7 g einer Mineralöllösung eines von einer Alkylbenzolsulfonsäure (Mgw. * 500) abgeleiteten überbasischen, mit Kohlendioxid behandelten Calciumsulfonatkomplexes, der 15»5 f> Calcium und 1,56 i> Schwefel enthält unu eine Basenzahl ▼on 410 aufweist, 33,3 g einer -Mineralöllosung eines von einer Alkylbenzolsulfonsäure (Mgw. = 5CC) abgeleiteten überbasischen, mit Kohlendioxid behandelten Calciumsulfonatkomplexes, der 4,7 'J- Calcium und 2,63 W Schwefel enthält und eine Basenzahl von 84,5 aufweist, C,15 g einer 50 i~igen Lösung eines PoIyeiloxan-Antischaummittels in Kerosin und 0,25 g einer 10 ?Uigen Lösung eines weiteren Polysiloxan-Antieohaummittele in Kerosin wird mit 3 g eines durch einen Polyieobutenylreet mit einem Molekulargewicht von ICOO substituierten Bernsteinsäureanhydrids, das eine Verseifungszahl von 100 aufweist, versetzt. Das dabei erhaltene Gemisch wird bei Temperaturen von 60 bis 7O0C gerührt, A mixture of 66.7 g of a mineral oil solution of an overbased, carbon dioxide-treated calcium sulfonate complex derived from an alkylbenzenesulfonic acid (Mgw. * 500), which contains 15 »5 f> calcium and 1.56 i> sulfur and has a base number ▼ on 410, 33.3 g of a mineral oil solution of an overbased, carbon dioxide-treated calcium sulfonate complex derived from an alkylbenzenesulfonic acid (Mgw. = 5CC), which contains 4.7 % calcium and 2.63 W sulfur and has a base number of 84.5, C. , 15 g of a 50 i ~ strength solution of a PoIyeiloxan antifoam in kerosene and 0.25 g of a 10? Uigen solution of another polysiloxane Antieohaummittele in kerosene is charged with 3 g of a by a Polyieobutenylreet having a molecular weight of ICOO substituted succinic anhydride having a Has saponification number of 100, offset. The mixture obtained in this way is stirred at temperatures from 60 to 7O 0 C,

Beispiel 5Example 5

950 g einer hineralöllösung eines von einer Alkylbenzoleulfoneaure (Mgw. β 440) abgeleiteten Uberbasischen, mit Kohlendioxid behandelten Calciumsulfonatkomplexes, der 13,55 % Calcium und 1,81 j6 Schwefel enthält und eine Basenzahl von 345 aufweist, wird mit 50 g einer durch einen hochmolekularen Polyisobutenylrest substituierten Ilonocarbonsäure, die eine Säurezahl von 48 aufweist und durch Krhitzen eines chlorierten Polyisobutene mit einem Durchschnittsmolekulargewicht von ICOO und einem Chlorgehalt von 4,3 Ί» mit Acrylsäure hergestellt wurde, ver-950 g of a hineralöllösung one of a Alkylbenzoleulfoneaure (MGW. Β 440) derived Uberbasischen, treated with carbon dioxide Calciumsulfonatkomplexes containing 13.55% calcium and 1.81 j6 sulfur and having a base number of 345, is charged with 50 g of a high molecular weight by a Polyisobutenyl radical substituted ilonocarboxylic acid, which has an acid number of 48 and was prepared by heating a chlorinated polyisobutenes with an average molecular weight of ICOO and a chlorine content of 4.3 Ί » with acrylic acid.

00 9840/212200 9840/2122

20148602014860

setzt. Das erhaltene Gemisch wird auf Temperaturen von 150 bis 16O°C erhitzt, wobei Stickstoff mit einer Geschwindigkeit τοη 56,6 Liter/h eingeleitet wird. Mach Filtration erhält man ein Gemisch mit einer Basenzahl von 318.puts. The mixture obtained is heated to temperatures of 150 to 16O ° C heated, with nitrogen at a rate τοη 56.6 liters / h is introduced. After filtration, a mixture with a base number of 318 is obtained.

Beispiel 6Example 6

Ein UemiBCh aus 906 g einer Öllösung einer Alkylbeneolsulfoneäure mit einem Durohschnittemolekulargewicht von 460 bis 480 (1,5 Äquivalent), 564 g Mineralöl, 600 g Toluol, 95,7 g (4,4 Äquivalent) Magnesiumoxid und 120 g Wasser wird 7 Stunden lang bei Temperaturen von etwa 78 bis 850C mit Kohlendioxid bexiandelt (74,9 Liter COg/h). Das mit Kohlendioxid behandelte Produkt wird duroh Erhitzen auf 165°C unter einem Jruck von 20 Torr von flüchtigen Anteilen befreit und danach filtriert. Das Piltrat ist eine öllösung eines überbasischen, mit Kohlendioxid behandelten Magnesiumsulfonat-Komplexee, der ein Metallverhält· nie von 3,1 aufweist und 15,27 i> Magnesiumsulfatasche und 2,66 i> Schwefel enthält, sowie eine Basenzahl von 98 aufweist. 95 g dieses Komplexes werden mit 5 g des Polyisobutenylbernsteinsäureanhydrids vom Beispiel 1 versetzt, und das erhaltene Gemisoh wird bei 15O0C gerührt und danach filtriert.A UemiBCh of 906 g of an oil solution of an alkylbeneol sulfonic acid having a durometer molecular weight of 460 to 480 (1.5 equivalent), 564 g of mineral oil, 600 g of toluene, 95.7 g (4.4 equivalent) of magnesium oxide and 120 g of water is used for 7 hours at temperatures of about 78 to 85 0 C bexiisiert with carbon dioxide (74.9 liters of COg / h). The product treated with carbon dioxide is freed from volatile constituents by heating to 165 ° C. under a pressure of 20 torr and then filtered. The Piltrat is an oil solution comprising an overbased, treated with carbon dioxide, magnesium sulfonate Komplexee, comprising a metal behaves · never of 3.1 and containing 15.27 i> Magnesium sulfate ash and 2.66 i> sulfur and a base number of 98th 95 g of this complex are mixed with 5 grams of the polyisobutenyl succinic anhydride from Example 1 was added, and the Gemisoh is stirred at 15O 0 C and then filtered.

Beispiel 7Example 7

950 g einer Mineralöllösung eines von einer Mahagonieulfonsäure abgeleiteten Uberbasisohen, mit Kohlendioxid behandelten CaI-ciumsulfonat-Komplexes, der 12,0 J* Calcium und 1,7β ?ί Schwefel enthält unci eine Basenzanl von 300 aufweist, werden mit 83 g einer 60 i^-igen HineralöllÖsung eines Ammoniumsalzeβ einer PoIyisobutenylbernsteinsäure 'Stickstoffgehalt « 0,66 %) , versetzt. ba.B erhaltene Gemisch wird 30 Minuten lang auf 16O°C950 g of a mineral oil solution of a calcium sulfonate complex which is derived from a mahogany sulfonic acid and has been treated with carbon dioxide, which contains 12.0% calcium and 1.7% sulfur and has a base number of 300, is mixed with 83 g of a 60% -igen back oil solution of an ammonium salt of a polyisobutenylsuccinic acid 'nitrogen content' 0.66 %) . The mixture obtained in ba.B is heated to 160 ° C. for 30 minutes

009840/2122009840/2122

erhitzt, und die erhaltene Masse wird filtriert. Das Piltrat enthält 24 Öl.heated, and the resulting mass is filtered. The Piltrat contains 24 i "oil.

Beispiel 8Example 8

Eine Mineralöllösung eines von einer Mahagonisulfoneäure abgeleiteten überbasischen, mit Kohlendioxid behandelten Calciumkomplexes, uer 15,5 Ψ Calcium und 1,35 i> Schwefel enthält und eine Basenzahl von 400 aufweist, wird bei Temperaturen von 100 bis 120 C bis zur Erzielung einer homogenen Masse mit 2 Gew.-#, bezogen auf den Komplex, · des Monomethylesters jenerA mineral oil solution of an overbased derived from a Mahagonisulfoneäure, treated with carbon dioxide, calcium complex, uer 15.5 Ψ calcium and 1.35 i> sulfur and having a base number of 400 is performed at temperatures of 100 to 120 C until obtaining a homogeneous mass with 2 wt .- #, based on the complex, · of the monomethyl ester of that

vonfrom

Polyisobutenylbernßteinsäure vermischt, der sioh Cas Bernsteinsäureanhydrid von Beispiel 1 ableitet.Polyisobutenylsuccinic acid mixed, the sioh Cas succinic anhydride derived from example 1.

Beispiel 9Example 9

936 g einer Mineralöllösung eines von einer Alkylbenzolsulfonsäure (Hgw* »440) abgeleiteten überbasischen, mit Kohlendioxid behandelten Calciumkomplexes, der 13,55 $> Calcium und 1,81 °?> Schwefel enthält, und eine Basenzahl von 345 aufweist, werden mit 64 g einer 78 j^-i^en Mineralöllösunt, eines Polyieobutenylbernsteinsäureimids mit einem Stickstoffgehalt von 1 i> versetzt. -Das erhaltene Gemisch wird 1 Stunde lang auf Temperatüren von 150 bis 1600O erhitzt und anschlieesend filtrierte Das FiItrat weist eine Basenzahl von 326 auf und enthält 22,4 °l· Mineralöl»936 g of a mineral oil solution of an overbased, carbon dioxide-treated calcium complex derived from an alkylbenzenesulfonic acid (Hgw *> 440), which contains 13.55 $> calcium and 1.81 °?> Sulfur, and has a base number of 345, are added with 64 g a 78 j ^ -i ^ en mineral oil solution, a polyieobutenyl succinic acid imide with a nitrogen content of 1 i> added. The mixture obtained is heated to temperatures of 150 to 160 0 O for 1 hour and then filtered. The filtrate has a base number of 326 and contains 22.4 ° l · mineral oil »

Beispiel 10Example 10

Ein Gemisch aus 1400 g einer Mineralöllöeung eines von einer Erdölsulfonsäure (Mgw. = 450) abgeleiteten überbaeischen, mitA mixture of 1400 g of a mineral oil solution one of one Petroleum sulfonic acid (Mgw. = 450) derived overbaeischen, with

ttbeivttbeiv

Kohlendioxid behandelten Galciumkomplexee (10/baeißChe Metalläquivalente), der 15,5 "h Calcium und 1,35 ^ Schwefel enthält und Carbon dioxide treated Galciumkomplexee (10 / baeißChe metal equivalents), the 15.5 "h calcium and 1.35 ^ sulfur contains and

00 98AO/ 2 12 200 98AO / 2 12 2

20Η88020Η880

eine Bas^enzahl von 400 aufweist, und 1650 g (3 Äquivalent) einer Polyisobutenylbernsteinßäure mit einer Säurezahl von 102 wird biß zur Erzielung einer homogenen Hasse auf 1500C erhitzt und anschliessend filtriert.has a base number of 400, and 1650 g (3 equivalents) of a polyisobutenylsuccinic acid with an acid number of 102 is heated to 150 ° C. to achieve a homogeneous Hasse and then filtered.

Beispiel 11Example 11

Ein Gemisch aus 2576 g Mineralöl, 240 g (1,85 Äquivalent) Octanol, 74C g (20,0 Äquivalent) Calciumhydroxyd, 2304 g (8 Äquivalent) Ölsäure und 392 g(12,3 Äquivalent) Methanol wird unter Rühren etwa 30 Minuten lang auf etwa 500G erhitzt und anschliessend etwa 210 Minuten lang bei Temperaturen von 5C bis 6O0C mit Kohlendioxid (74,9 Liter CO2/h) behandelt. Das erhaltene Gemisch wird auf 150°C erhitzt und filtriert. Das FiI-A mixture of 2576 g mineral oil, 240 g (1.85 equivalent) octanol, 74C g (20.0 equivalent) calcium hydroxide, 2304 g (8 equivalent) oleic acid and 392 g (12.3 equivalent) methanol is stirred for about 30 minutes heated at about 50 0 G and then treated about 210 minutes at temperatures of 5C to 6O 0 C with carbon dioxide (CO 2 74.9 liter / h). The resulting mixture is heated to 150 ° C. and filtered. The FiI

enthäXt einen
trat überbasischen Calciuaoleat-Komplex, der 24,1 > Sulfatasche enthält und ein Metallverhältnis von 2,5 sowie eine Neutralisationszahl (sauer) von 2,0 aufweist.
Contains one
occurred overbased calcium oleate complex, which contains 24.1> sulfated ash and has a metal ratio of 2.5 and a neutralization number (acidic) of 2.0.

Dieser überbasische Ualciumoleatkomplex wird nun wie der überbasische, mit Kohlendioxid behandelte Calciumkomplex von Beif spiel 1 nach dem Verfahren von Beispiel 1 mit dem Polyisobutenylbernsteinsautfeanhydrid behandelte Es wird ein ,' überbasische r Calciumkomplex erhalten.This overbased ualcium oleate complex is now like the overbased, carbon dioxide-treated calcium complex of Example 1 according to the method of Example 1 with the polyisobutenyl succinic anhydride treated An overbased calcium complex is obtained.

Die Beispiele A bis £ beziehen sioh auf Schmierstoffe, denen die nach üem Verfahren der Erfindung hergestellten überbasischen . Komplexe einverleibt wurden.Examples A to £ relate to lubricants that the overbased ones produced by the process of the invention. Complexes were incorporated.

Beispiel AExample A.

SAE 30-Mineralschmieröl, enthaltend 20,2 f> des Produkte vonSAE 30 mineral lubricating oil, containing 20.2 % of the products of

Beispiel IoExample Io

009840/2122009840/2122

;-19- 201A880; - 19 - 201A880

ι ■ι ■

Beiapiel BBeiapiel B

SAE 30-Mineralschmieröl, enthaltend 17,1 # dee Produkts vonSAE 30 mineral lubricating oil containing 17.1 # of the product of

Beitjpiel 2.Example 2.

Be ie pi el CExample C

SAE 50-Mineralschmieröl, enthaltend 20,4 #des Produkt8 vonSAE 50 mineral lubricating oil containing 20.4 # of the product8 of

Beiepiel 3.Example 3.

Beispiel DExample D

SAE 30-Mineral8Chmieröl, enthaltend 2 jt des Produkte von Beispiel 4.SAE 30 mineral oil, containing 2 parts of the product from Example 4.

Beispiel EExample E.

SAE ^C-Mineralsohmieröl, enthaltend 15 f> dee Produkte von Beiepiel 11.SAE ^ C-Mineralsohmieröl containing 15 f> dee products Beiepiel 11th

Aus Tabelle I Bind die LÖBlichkeiteeigenachaften von erfindungBgemäse hergestellten überbasischeTable I shows the solubility properties of overbased products made according to the invention

Komplexen(Probe I, III, V und VII) sowie zum Vergleich jene der als Ausgangsmaterialien verwendeten Komplexe/selb&t (Probe 11, IV, Vl und VIII) ersichtlich. Aus diesem Vergleich ist die Wirkung der hochmolekularen Carbonsäuren bew. ihrer Derivate (B) zur Verbesserung der öllöslichkeit der Uberbaslscnen hetallkomplexe erkennbar. Die Probe IX veranschaulicht die Unwirksamkeit eines vorweg hergestellten Metallsalzes der hoch-Complexes (sample I, III, V and VII) and for comparison those of the complexes / selb & t used as starting materials (Sample 11, IV, VI and VIII) can be seen. From this comparison is the effect of the high molecular weight carboxylic acids and their derivatives (B) to improve the oil solubility of the overbased oils metal complexes recognizable. Sample IX illustrates the ineffectiveness of a previously prepared metal salt of the high-

- (BJ) molekularen Carbon6äure/als Mittel zur Behandlung des Uberbasiechen He-tal!komplexes (A). - (BJ) molecular carboxylic acid / as an agent for the treatment of the overbased He-tal! Complex (A).

009840/2122009840/2122

Tabelle ITable I.

Probesample

geprüfte Substanztested substance

Konzentration ie Mineralschmieröl, Gew.^ Concentration ie mineral lubricating oil, wt

Produkt vonProduct of
In BeispielIn example
Beispiel 1example 1
1 eingesetzter Komplex1 inserted complex
50 f> 50 f> 10 *10 * 1 f 1 f
II.
IIII
Produkt vonProduct of
In BeispielIn example
Beispiel 2Example 2
2 eingesetzter Komplex2 inserted complex
k
k
k
k
kk
mm
IIIIII
IVIV
Produkt vonProduct of
In BeiepielIn example
Beispiel 3Example 3
3 eingesetzter Komplex3 inserted complex
k
k
k
k
k
t, ft
k
t, ft
kk
11
VV
VIVI
k
B -
k
B -
k
β
k
β
k
β
k
β

VII Durch Vermischen von 90 Gew.-teilen eines überbasischen mit Kohlendioxid behandelten Calciumsulfonat-Komplexes (Basenzahl ·= 345» .Schwefelgehalt - 1,8 si) mit 10 Gew,-teilen des Polyieobutenylbernsteinsäureanhydrids von Beiepiel 1 bei 160 C hergestelltes ProduktVII By mixing 90 parts by weight of an overbased calcium sulfonate complex treated with carbon dioxide (base number = 345 ».Sulfur content - 1.8 si) with 10 parts by weight of the polyobutenylsuccinic anhydride from Example 1 160 C manufactured product

VIII Der zur Herstellung des Produkts unter (VII) eingesetzte KomplexVIII The complex used to prepare the product under (VII)

IX Ein ueia Produkt unter (VII) entsprechendes Produkt, wobei jedoch anstelle des Bernsteineäureanhydride das CalcluKSalz der entsprechenden Bernsteinsäure verwendet wurdeIX An ueia product under (VII) corresponding product, however instead of succinic anhydride, the calculus salt of the corresponding Succinic acid was used

k =k = klarclear t st s trübecloudy mm » mittlere»Middle one
Sedimentationsedimentation
1 =1 = leicht trübe slightly cloudy β »β » geringelow
Sedimentär .Sedimentary.
tiontion
88th » stark«" strong"
Sedimentationsedimentation

009840/2122009840/2122

Die niedrige Schaumbildungswirkung der nach dem Verfahren derThe low foaming effect of the

Erfindung hergestellten überbasischInvention manufactured overbased

(Ibis 3) (Ibis 3)

K omplexe wird anhand eines aus 3 Durchgängen/bestehenden Prüfverfahrens aufgezeigte Jeder Durchgang dieses Verfahrens besteht aus folgenden zwei Stufen:C omplex is based on a 3-pass / test procedure Each cycle of this procedure consists of the following two stages:

x zur Schaumbildung x for foam formation

a) Einleiten von LUft/in eine iiineralscliniierölprobe, der .a) Introduction of air into a mineral sclining oil sample, the.

jeweils 2 Gew.-'/i des zu prüfenden Zusatzstoffes einverleibt wurden, und Bestimmung des Schauravoluinens (in ml) unmittelbar nach dem Einleiten der Luft;in each case 2% by weight of the additive to be tested were incorporated, and determination of the Schauravoluinen (in ml) immediately after introducing the air;

b) Wiederholung der Stufe a) nach 2 Wochen langer Lagerung der Ö.lprobe.b) Repetition of step a) after 2 weeks of storage of the Oil sample.

Der Durchgang 1) wird bei Raumtemperatur durchgeführt und die Lagerung erfolgt ebenfalls bei flaumtemperatur. Der Durchgang 2) wird bei etwa 930C an einer friscnen Probe durchgeführt, die Lagerühgeteinperatur beträgt etwa 380C0 Der Durchgang 3) wird wiederum bei Raumtemperatur durchgeführt, wobei die bereits im Durchgang 2) geprüfte Probe verwendet wird.Run 1) is carried out at room temperature and storage is also carried out at fluff temperature. The passage 2) where the checked already in the pass 2) sample is used is carried out at about 93 0 C at a friscnen sample Lagerühgeteinperatur is about 38 0 C 0 The passage 3) is carried out in turn at room temperature.

Tabelle II zeigt die Ergebnisse der vorstehend beschriebenen Prüfung, Das während der Prüfung gemessene Schauravoiuinen wird in ml angegeben. Es wird das Schaumvolumen, das in einer ein erfindungsgemäes hergestelltes Produkt enthaltenden Probe erzeugtTable II shows the results of those described above Exam, which will be the show avoiuinen measured during the exam given in ml. It is the foam volume, which in an inventive produced product containing sample generated

inin

wird, mit dem Schaumvolumen einer Probe verglichen, die jenen Komplex enthält, der als Ausgangem&terial (A) für das vorgenannte Produkt eingesetzt wurde. is compared with the foam volume of a sample that contains the complex that was used as the starting material (A) for the aforementioned product.

BAD ORlQlNAL 009840/2122 BAD ORlQINAL 009840/2122

20U88020U880

l\l \
DJDJ
Tabelle IITable II in Beispiel 4 ein
gesetzter Komplex (A)
in example 4
set complex (A)
2)
a J
toj
2)
a J
toj
O
460
O
460
3]3]
SS.
erzeugtes Schaumvolumen, oilgenerated foam volume, oil 25
260
25th
260
Durchgang
Stufe
Stufe
Passage
step
step
Produkt yon
Beispiel 4
Product of
Example 4
20
220
20th
220
Durchgang
Stufe
Stufe
Passage
step
step
O
O
O
O
Durchgang
Stufe
Stufe
Passage
step
step
10
130
10
130
O
20
O
20th

Pie Wirksamkeit von Schmierstoffen, denen erfindun^sgemäes hergestellte überbaeisehe Komplexe einverleibt wurden, wird nach einem Aluminiumplattentest ("Panel Coker Test")» bescnrieben von Raymond N. JollePie effectiveness of lubricants, which according to the invention manufactured over-building complexes were incorporated, is after an aluminum plate test ("Panel Coker Test") »described by Raymond N. Jolle

im Vortrag br. 23, Section V des 5· WelterdölJcongreeses £L959j, untersucht. Bei aieseni Test wird eine Probe von jeweils 350 g des jeweiligen Öls in den Behälter der Prüfvorrichtung eingebracht. Die Prüfvorrichtung ist mit einer Spritzvorrichtung ausgestattet. Sowohl der Behälter als auch die Probe werden bei kaumtemperatur gehalten, und oberhalb der Probe befinaet eich eine Aluminiumplatte mit den Abmessungen 3,6 cm χ 8,9 ca χ 0,635 cm. Durch diese Platte wird der Behälter luftdicht abgeschlossen. Die Temperatur*1 des Ölbehälters bzw, jene der Platte werden iw Bereicn von Jlfc biß 1240C bzw. im Bereioh von 299 bis 31O0C gehalten. Die Spritzvorrichtung wird 1* 1/2 Minuten lang betrieben, vobei uie Ölprobe auf die sandgestrahlte Oberfläche de: ?lac ■ ^.»spitzt wird, Anschliessenö wird das Bespritzen unteioro» ynd dl·-. Hit» wird 9C Sekunden lang der Hitzeeinwirkung, 4»u.t^ östi^t. Der vorgenannte Cyolus wiru über eine Ge-in the lecture br. 23, Section V des 5 · WelterdölJcongreeses £ L959j . In the case of aieseni test, a sample of 350 g each of the respective oil is placed in the container of the test device. The test device is equipped with a spray device. Both the container and the sample are kept at a low temperature, and an aluminum plate with the dimensions 3.6 cm 8.9 approx χ 0.635 cm is attached above the sample. The container is hermetically sealed by this plate. The temperature * 1 of the oil container and that of the plate are kept in the range from Jlfc to 124 0 C or in the range from 299 to 31O 0 C. The spraying device is operated for 1 1/2 minutes, during which the oil sample is pointed onto the sand-blasted surface, then the spraying is unteioro »ynd dl · -. Hit »is for 9C seconds of exposure to heat, 4» ut ^ osti ^ t. The aforementioned Cyolus is about a

saatdauer τοπ 4 Stunden wiederholt, und danach wird die Vorrichtung abgekühlt. Sehliesslich wird die Aluminiumplatte, herausgenommen, ait Schwerbenein gewaschen und untersucht. Die theraieche Beständigkeit der geprüften ö!probe wird mittels der Untersuchung der Platte bestimmt und gemäss den Ablagerungen, die eich auf dieser Platte angesammelt haben, bewertet. Die Ergebnisse dieser Bewertung werden mittels einer Zahlenskala, die Ton O bis 10 reicht, wiedergegeben·"O" bedeutet dabei eine ▼ollständige Bedeckung der Platte ait Ablagerungen, während "10" die vollständige Abwesenheit solcher Ablagerungen anzeigt.sowing time τοπ repeated 4 hours, and then the device is cooled. Finally, the aluminum plate is removed, washed and examined with difficulty. The thermal resistance of the tested Ö! Sample is determined by means of the Examination of the plate determined and evaluated according to the deposits that have accumulated on this plate. the Results of this evaluation are shown using a number scale ranging from 0 to 10. "O" means one ▼ omplete coverage of the plate ait deposits, while "10" indicates the complete absence of such deposits.

Die Ergebnisse des "Panel Coker Tests" sind aus Tabelle III ersichtlich. Die Proben (1) bzw. (3) entsprechen den Schmierstoffen von Beispiel A bzw« B, die erfindunöSgemäss hergestellte Produkte enthalten, die Proben (2) bzw. (4) Schmierstoffen, denen uie wetallkoaiplexe(A· bzw. B') einverleibt wurden, die als Ausgangsmaterialien für uie vorgenannten Produkte herangezogen wurden. Jede Scjunierstoff probe enthält eine so bemesEene !.enge des jeweiligen Zusatzstoffes, dass eine Basenzahl von 65 erzielt wird·The results of the "Panel Coker Test" are shown in Table III. Samples (1) and (3) correspond to the lubricants of example A and B, which are produced according to the invention Products contain the samples (2) or (4) lubricants, to which uie wetallkoaiplexe (A · or B ') were incorporated, the were used as starting materials for the aforementioned products. Each fabric sample contains one of these dimensions ! .length of the respective additive that a base number of 65 is achieved

Tabelle HITable HI

"Panel Coker Test" Probe Bewertung*»ahl "Panel Coker Test" sample evaluation * »ahl

(1) Schmierstoff von Beispiel A 9(1) Lubricant from example A 9

(2) Schmierstoff, enthaltend Komplex A1 4(2) Lubricant containing complex A 1 4

(3) Schmierstoif von Beispiel B 8(3) Lubricant from Example B 8

(4) Schmierstoff,enthaltend Komplex B1 6(4) Lubricant containing complex B 1 6

009840/2122009840/2122

Claims (14)

20U880 Patentansprüche20U880 claims 1.) Verfahren zur Herstellung von Uberbasischen Konplexen,1.) Process for the production of uberbased complexes, dadurch gekennzeichnet, dasscharacterized in that A) ein Uberbasischer Metallsulf onat-, Metallsulf onat-oarboxylat- oder Metallcarboxylat-Komplex bei Temperaturen von etwa 250C bis zur Zersetzungstemperatur des Reafctlonsgemisches mitA) an overbased Metallsulfonat-, Metallsulfonat-oarboxylat- or metal carboxylate complex at temperatures of about 25 0 C up to the decomposition temperature of the Reafctlonsgemisches * B) einer der Oesamtbaslzltät der Komponente A) (gemessen als mg KOH/g Komponente A) höchstens entsprechenden Menge Mindestens einer hochmolekularen, gegebenenfalls durch mindestens einen Arylrest und/oder mindestens einen polaren Rest substituierten, pro Carboxylgruppe mindestens etwa 25 aliphatische C-Atome aufweisenden aliphatischen Mono- oder Polycarbonsäure oder ihrer Anhydride, Ester, Ammoniumsalze,. Aminsalze, Amide oder Imide, behandelt wird.* B) one of the total baseline of component A) (measured as mg KOH / g component A) at most a corresponding amount of at least one high molecular weight, optionally through at least one aryl radical and / or at least one polar Radical substituted, aliphatic mono- or polycarboxylic acid or its anhydrides, esters, ammonium salts ,. Amine salts, amides or imides. 2.) Verfahren nach Anspruch 1, dadurch gekenn-W zeichnet, dass als Komponente A) mindestens ein überbasischer Erdalkali-, vorzugsweise Calciumsulfonat-, -sulfonetcarboxylat oder -carboxylÄt-Koeplex verwendet wird.2.) A process according to claim 1, characterized marked W is characterized in that as component A) at least one overbased alkaline earth metal, preferably, calcium sulfonate, or -sulfonetcarboxylat -carboxylÄt-Koeplex is used. 3.) Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass sieh der tiberbasische Metallkomplex (Komponente A) von einer alkylierten Arylsulfonstture mit Mindestens etwa 15 aliphatischen C-Atomen ableitet.3.) The method according to claim 1 or 2, characterized in that see the tiberbasische metal complex (component A) of an alkylated Arylsulfonstture with at least derives about 15 aliphatic carbon atoms. 0098AO/21220098AO / 2122 4.) Verfahren nach Anspruch 1 bis 3, dadurch g e k e η η zeichnet« dass als Komponente A) ein überbasischer Calclumsulfonat-Komplex verwendet wird, der aus a) einem mit Kohlendioxid behandelten überbasischen Calciumalkylbenzolsulfonat mit einer Basenzahl von etwa 400 und b) einen mit Kohlendioxid behandelten Uberbasischen Calciumalkylbenzolsulfonat mit einer Basenzahl von etwa 80 besteht, wobei das Gewichtsverhältnis a) : b) etwa 1 : 1 bis etwa 10 : 1 beträgt.4.) Method according to claim 1 to 3, characterized in that g e k e η η « that as component A) an overbased calcium sulfonate complex is used, which is composed of a) one with Carbon dioxide treated calcium overbased alkyl benzene sulfonate with a base number of about 400 and b) one with carbon dioxide treated overbased calcium alkylbenzenesulfonate with a Base number of about 80, the weight ratio a): b) being about 1: 1 to about 10: 1. 5.) Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, dass als Komponente A) ein Kohlendioxid behandelter überbasischer Magnesiumsulfonat-carboxylat-Komplex verwendet wird.5.) Method according to claim 1 to 3, characterized in that that a carbon dioxide treated as component A) overbased magnesium sulfonate carboxylate complex used will. 6.) Verfahren nach Anspruch 1 bis 5, dadurch gekennzeichnet, dass der überbasische Metallkomplex (Komponente A^ sich von mindestens einer etwa 12 bis etwa 24 aliphatische C-Atome aufweisenden Fettsäure und/oder mindestens einer aromatischen, durch mindestens einen öllöslich machenden Rest mit mindestens etwa 15 bis 18 C-Atomen, vorzugsweise etwa 15 bis etwa 200 C-Atomen, substituierten Carbonsäure und/oder mindestens einer etwa 12 bis etwa 30 C-Atome aufweisenden oycloaliphatisohen Carbonsäure ableitet.6.) The method according to claim 1 to 5, characterized in that the overbased metal complex (Component A ^ ranges from at least one about 12 to about 24 aliphatic carbon atoms having fatty acid and / or at least one aromatic, by at least one oil-solubilizing acid Remainder with at least about 15 to 18 carbon atoms, preferably about 15 to about 200 carbon atoms, substituted carboxylic acid and / or at least one having about 12 to about 30 carbon atoms derives oycloaliphatisohen carboxylic acid. 7-) Verfahren nach Anspruch 1 bis 6, dadurch gekennzeichnet, dass sich der überbasische Metallkomplexe (Komponente A) von einem Säuregemisch ableitet, das pro Kquivalent der Carbonsäure(n) 1 bis 5 Äquivalente, vorzugsweise7-) Method according to claim 1 to 6, characterized in that that the overbased metal complexes (Component A) derived from a mixture of acids, the per Kequivalent of the carboxylic acid (s) 1 to 5 equivalents, preferably 009840/2122009840/2122 1 bis 2 Äquivalente der Sulfonsäure(n) aufweist«Has 1 to 2 equivalents of the sulfonic acid (s) « 8.) Verfahren nach Anspruch 1 bis 7» dadurch gekennzeichnet, dass der Uberbasische Metallkomplex (Komponente A) eine Basenzahl von mindestens etwa 70, vorzugsweise von etwa 300 bis etwa 500, aufweist.8.) The method according to claim 1 to 7 »characterized in that the uberbasische metal complex (component A) has a base number of at least about 70, preferably of about 300 to about 500. 9.) Verfahren nach Anspruch 1 bis 8, dadurch gekennzeichnet, dass der Uberbasische Metallkomplex (Komponente A) ein Metallverhältnis von 1,1 bis etwa 30, vorzugsweise von 2 bis 20, aufweist.9.) The method according to claim 1 to 8, characterized in that the overbased metal complex (component A) has a metal ratio of 1.1 to about 30, preferably from 2 to 20. 10.) Verfahren nach Anspruch 1 bis 9, dadurch gekennzeichnet, dass als Komponente B) eine durch einen PoIyisobutenylrest mit einer Durchschnittszahl von mindestens etwa 50, vozugsweise etwa 60 bis 5000 C-Atomen substituierte Bernsteinsäure, die vorzugsweise ein Molekulargewicht von etwa 700 bis etwa 5000 aufweist, oder ihr Anhydrid verwendet wird.10.) The method according to claim 1 to 9, characterized in that as component B) one by a polyisobutenyl radical with an average number of at least about 50, preferably about 60 to 5000 carbon atoms substituted succinic acid, which preferably has a molecular weight of about 700 to about 5000, or its anhydride is used. 11.) Verfahren nach Anspruch 1 bis 10, dadurch gekennzeichnet, dass 0,1 bis 10 Gew.-^, vorzugsweise 3 bis 5 0ew.-# der Komponente B^, bezogen auf die Komponente A), verwendet werden.11.) The method according to claim 1 to 10, characterized in that 0.1 to 10 wt .- ^, preferably 3 to 5 0ew .- # of component B ^, based on component A), can be used. 12.) Verfahren nach Anspruch 1 bis 11, dadurch gekennzeichnet, dass ein Anteil von 1 bis 25#* vorzugsweise 5 bis 10# Gesamtbasisitat des - Uberbasisehen Metallkomplexes12.) The method according to claim 1 to 11, characterized in that a proportion of 1 to 25 # * is preferably 5 to 10 # total basis of the overbased metal complex (JComponeii ve A antspreohenden Menge eines Amlnsalzes, Ammonlum-(JComponeii ve A antspreohenden amount of an amine salt, ammonium QQ9840/2122QQ9840 / 2122 BAD ORlQINAI,BAD ORlQINAI, -27.- 2ÖU880-27.- 2ÖU880 salzes. Imide, Amids oder Esters einer hochmolekularen aliphatischen Carbonsäure (Komponente B) verwendet wird.salt. Imide, amide or ester of a high molecular weight aliphatic carboxylic acid (component B) is used. 13.) Verfahren nach Anspruch 1 bis 12, dadurch gekenn ζ ei ohne t( dass bei Temperaturen von etwa bis etwa 2500C, vorzugsweise von etwa 50 bis etwa 1500Q gearbeitet wird.13.) The method of claim 1 to 12, characterized labeled in ζ ei without t (that at temperatures of about 0 to about 250 C, is preferably carried out from about 50 to about 150 0 Q. 14.) Verfahren nach Anspruch 1 bis 15, dadurch gekennzei ohne t, dass es in Gegenwart eines Lösungsmittels durchgeführt wird.14.) The method according to claim 1 to 15, characterized marked without t that it is in the presence of a Solvent is carried out. 15·) Verwendung der naoh Anspruch 1 bis ΙΛ hergestellten überbasischen Komplexe als Zusatzstoffe in Schmierstoffen, Kraft- und Brennstoffen.15 ·) Use of the overbased complexes produced according to claims 1 to ΙΛ as additives in lubricants, fuels and fuels. 009840/2122009840/2122
DE19702014880 1969-03-27 1970-03-26 Process for making overbased complexes Pending DE2014880A1 (en)

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