EP0011224A1 - Lubricating and cooling agent - Google Patents

Lubricating and cooling agent Download PDF

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Publication number
EP0011224A1
EP0011224A1 EP79104352A EP79104352A EP0011224A1 EP 0011224 A1 EP0011224 A1 EP 0011224A1 EP 79104352 A EP79104352 A EP 79104352A EP 79104352 A EP79104352 A EP 79104352A EP 0011224 A1 EP0011224 A1 EP 0011224A1
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EP
European Patent Office
Prior art keywords
weight
ammonium polyphosphate
additive
coolant
lubricant
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.)
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EP79104352A
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German (de)
French (fr)
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EP0011224B1 (en
Inventor
Michael Ahlgrim
Gerhard Dr. Mietens
Franz-Josef Dr. Dany
Joachim Dr. Kandler
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Hoechst AG
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Hoechst AG
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/24—Compounds containing phosphorus, arsenic or antimony
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02—Water
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085—Phosphorus oxides, acids or salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/22—Acids obtained from polymerised unsaturated acids
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/068—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings having amino groups bound to polycyclic aromatic ring systems, i.e. systems with three or more condensed rings
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/221—Six-membered rings containing nitrogen and carbon only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/225—Heterocyclic nitrogen compounds the rings containing both nitrogen and oxygen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/225—Heterocyclic nitrogen compounds the rings containing both nitrogen and oxygen
    • C10M2215/226—Morpholines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/30—Heterocyclic compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • 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
    • C10M2223/041—Triaryl phosphates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • 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
    • C10M2223/043—Ammonium or amine salts thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • 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
    • C10M2223/047—Thioderivatives not containing metallic elements
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2225/00—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2225/00—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2225/02—Macromolecular compounds from phosphorus-containg monomers, obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/22—Metal working with essential removal of material, e.g. cutting, grinding or drilling
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/241—Manufacturing joint-less pipes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/242—Hot working
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/243—Cold working
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C10N2040/245—Soft metals, e.g. aluminum
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C10N2040/246—Iron or steel
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/244—Metal working of specific metals
    • C10N2040/247—Stainless steel

Definitions

  • the invention relates to an additive suitable for metalworking in phosphate-based lubricants and coolants.
  • the additive according to the invention is particularly suitable for metalworking processes in which extremely high pressures and temperatures occur, e.g. Milling, extruding or drawing and rolling processes in cold or hot condition.
  • lubricants and coolants which reduce the frictional resistance between the workpiece and the tool in order to reduce wear and increase production.
  • These lubricants and coolants generally consist of lubricating oils to which wear and corrosion-inhibiting additives have been added.
  • DE-OS 16 44 875 proposes an aqueous coolant which contains 0.1-20% by weight of a polyoxyalkylene Lenglykolpolyesters be added to a dimeric fatty acid. It has been found that the organic constituent oxidizes and / or evaporates on the tool due to the occasional high heat development and prevents the formation of a sliding layer.
  • DE-OS 16 44 9o8 describes lubricants containing iron and / or zinc pyrophosphate.
  • DE-OS 2o 48 537 proposes a high-temperature lubricant based on a binder and a solvent, to which salts of ortho- and / or polyphosphoric acid with sodium and / or potassium and / or zinc and / or aluminum and / or boron are mixed .
  • a lubricant and coolant is produced by adding ortho- or condensed phosphates of alkali metals and metal oxides.
  • Inorganic and organic phosphorus compounds as additives in lubricating oils or water are therefore part of the prior art.
  • orthophosphoric or polyphosphoric acid as an additive in lubricating oils, but also in particular in water, severe corrosion occurs which can be reduced by neutralization with alkali metal hydroxide or amines.
  • neutralizing the free acids a reduction in the lubrication must be accepted and the bases added can lead to undesired thickening, which considerably reduces the cooling effect.
  • the invention has for its object to provide an additive for metalworking, which has improved high-pressure properties and anti-wear properties on the basis of lubricating oils or water.
  • the object is achieved according to the invention in that a long-chain ammonium polyphosphate is added to the lubricant and coolant as an additive.
  • ammonium polyphosphate is one of the general formula used, in which n corresponds to an integer from 50 to 1000, in particular from 300 to 800, and R denotes an ammonium group.
  • ammonium polyphosphate up to 20%, in particular up to 5%, of the ammonium groups can be replaced by hydrogen.
  • ammonium polyphosphate can be used as an additive in lubricating oils or water in the form of a liquid, suspension or paste.
  • ammonium polyphosphate is added to the lubricant and coolant in an amount of 0.1 to 30, preferably 2 to 10,% by weight.
  • ammonium polyphosphate can be used as an additive in combination with surfactants and / or anti-foaming agents and / or dyes and / or rust inhibitors and / or phosphate esters.
  • Mineral lubricating oils such as paraffin-based or naphthen-based distillate oils with a viscosity between e.g. 6 and 60cSt at 60 ° C and / or synthetic lubricating oils, such as polyolefins and / or ester oils and / or polyoxyalkylenes, can be used.
  • Nonionic detergents such as polyoxyethylene stearate or polyoxyethylene monobutyl ether in amounts between 1 and 20% by weight of the lubricant and coolant have proven particularly useful as surface-active substances.
  • Siloxanes can be added to the lubricant and coolant as anti-foaming agents, e.g. Polymethylsiloxane in an amount of 5 - 25 ppm.
  • benzotriazole or ethyl succinic acid can be added as a rust inhibitor in amounts of about 200 ppm.
  • phosphate esters for example ammonium salt of the mixture of mono- and dioleyl phosphoric acid or di-n-propyldithiophosphoric acid or tricresyl phosphate in amounts of 0.01 to 10% by weight of the lubricant and coolant, the effect of ammonium polyphosphate based on lubricating oils can be synergistic be improved.
  • ammonium polyphosphate as an additive in lubricants and coolants.
  • the invention is not restricted to these examples; this applies in particular to the admixture of further additives which improve the lubricant and coolant.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

Langkettiges Ammoniumpolyphosphat ist ein gutes Additiv in Schmier- und Kühlmitteln bei Metallbearbeitungen, die unter extrem hohen Drücken und Temperaturen durchgeführt werden. Die Polyphosphatkette soll 50 bis 1000 Phosphoratome enthalten. Bis zu 20% der Ammoniumgruppen sind durch Wasserstoff ersetzbar. Das Additiv wird dem Schmierund Kühlmittel in einer Menge von 0,1 bis 30 Gew% zugesetzt.Long-chain ammonium polyphosphate is a good additive in lubricants and coolants for metalworking that is carried out under extremely high pressures and temperatures. The polyphosphate chain is said to contain 50 to 1000 phosphorus atoms. Up to 20% of the ammonium groups can be replaced by hydrogen. The additive is added to the lubricant and coolant in an amount of 0.1 to 30% by weight.

Description

Die Erfindung betrifft ein für die Metallbearbeitung geeignetes Additiv in Schmier- und Kühlmitteln auf Phosphatbasis. Das erfindungsgemäße Additiv eignet sich besonders für Metallbearbeitungsverfahren, bei denen extrem hohe Drücke und Temperaturen auftreten, wie z.B. Fräsen, Extrudieren oder Zieh- und Walzvorgänge im kalten oder heißen Zustand.The invention relates to an additive suitable for metalworking in phosphate-based lubricants and coolants. The additive according to the invention is particularly suitable for metalworking processes in which extremely high pressures and temperatures occur, e.g. Milling, extruding or drawing and rolling processes in cold or hot condition.

Es ist bekannt, zur Verschleißverminderung und Produktionserhöhung Schmier- und Kühlmittel zu verwenden, die den Reibungswiderstand zwischen dem Werkstück und Werkzeug verkleinern. Diese Schmier- und Kühlmittel bestehen im allgemeinen aus Schmierölen, denen verschleiß- und korrosionshemmende Additive zugesetzt sind.It is known to use lubricants and coolants which reduce the frictional resistance between the workpiece and the tool in order to reduce wear and increase production. These lubricants and coolants generally consist of lubricating oils to which wear and corrosion-inhibiting additives have been added.

So wird in der DE-OS 16 44 875 ein wäßriges Kühlmittel vorgeschlagen , welchem 0,1 - 20 Gew·% eines Polyoxialkylenglykolpolyesters einer dimeren Fettsäure zugesetzt werden. Es hat sich herausgestellt, daß der organische Bestandteil durch die punktuell auftretende große Hitzeentwicklung an dem Werkzeug oxidiert und/oder verdampft und den Aufbau einer Gleitschicht verhindert.For example, DE-OS 16 44 875 proposes an aqueous coolant which contains 0.1-20% by weight of a polyoxyalkylene Lenglykolpolyesters be added to a dimeric fatty acid. It has been found that the organic constituent oxidizes and / or evaporates on the tool due to the occasional high heat development and prevents the formation of a sliding layer.

In der DE-OS 16 44 9o8 werden Schmierstoffe mit einem Gehalt an Eisen- und/oder Zinkpyrophosphat beschrieben.DE-OS 16 44 9o8 describes lubricants containing iron and / or zinc pyrophosphate.

In der DE-OS 2o 48 537 wird ein Hochtemperaturschmierstoff auf der Grundlage eines Binders und eines Lösungsmittels vorgeschlagen, dem Salze der Ortho- und/oder Polyphosphorsäure mit Natrium und/oder Kalium und/oder Zink und/oder Aluminium und/oder Bor zugemischt sind.DE-OS 2o 48 537 proposes a high-temperature lubricant based on a binder and a solvent, to which salts of ortho- and / or polyphosphoric acid with sodium and / or potassium and / or zinc and / or aluminum and / or boron are mixed .

Gemäß der AT-PS 278 223 wird ein Schmier- und Kühlmittel hergestellt durch Zusatz von Ortho-oder kondensierten Phosphaten von Alkalimetallen und Metalloxiden.According to AT-PS 278 223, a lubricant and coolant is produced by adding ortho- or condensed phosphates of alkali metals and metal oxides.

Anorganische und organische Phosphorverbindungen als Additive in Schmierölen oder Wasser gehören somit zum Stand der Technik. Bei der Verwendung von Ortho- bzw. Polyphosphorsäure als Additiv in Schmierölen, aber auch insbesondere in Wasser, treten starke Korrosionen ein, die durch eine Neutralisation mit Alkalihydroxid oder Aminen reduziert werden können. Bei der Neutralisation der freien Säuren muß eine Reduzierung der Schmierung in Kauf genommen werden und es kann durch die zugesetzten Basen zu einer unerwünschten Eindickung kommen, wodurch die Kühlwirkung erheblich reduziert wird.Inorganic and organic phosphorus compounds as additives in lubricating oils or water are therefore part of the prior art. When using orthophosphoric or polyphosphoric acid as an additive in lubricating oils, but also in particular in water, severe corrosion occurs which can be reduced by neutralization with alkali metal hydroxide or amines. When neutralizing the free acids, a reduction in the lubrication must be accepted and the bases added can lead to undesired thickening, which considerably reduces the cooling effect.

Durch die Zugabe von Phosphorsäureestern ist die Herstellung von neutralen, homogenen Schmier- und Kühlmitteln möglich. Aus Erfahrung weiß man, daß ein Zusammenhang besteht zwischen der Schmierwirkung und dem Phosphorgehalt des Schmier- und Kühlmittels. Je höher der Phosphorgehalt ist, desto bessere Ergebnisse werden mit dem Schmier- und Kühlmittel erzielt. Beim Zusatz von Phosphorsäureestern ist der Phosphorgehalt im Schmier- und Kühlmittel begrenzt, da die verwendbaren Phosphorsäureester im P-Gehalt höchstens 13,4 Gew/ betragen können, vgl. DE-OS 21 45 296.The addition of phosphoric acid esters makes it possible to produce neutral, homogeneous lubricants and coolants. Experience has shown that there is a connection between the lubricating effect and the phosphorus content of the lubricant and coolant. The higher the phosphorus content, the better results are achieved with the lubricant and coolant. When phosphoric acid esters are added, the phosphorus content in the lubricant and coolant is limited, since the usable phosphoric acid esters in the P content can be a maximum of 13.4% by weight, cf. DE-OS 21 45 296.

Es hat sich gezeigt, daß die bisher vorgeschlagenen Schmierund Kühlmittel verbesserungsbedürftig sind. Einerseits weisen die bisherigen Schmiermittel nur eine unzureichende Kühlwirkung bei dem Werkzeug auf, andererseits müssen die auf dem Werkstück aufgesinterten Metalloxid-Phosphat-Gläser in einer nachfolgenden Ätzstufe durch eine Säurebehandlung entfernt werden.It has been shown that the previously proposed lubricants and coolants are in need of improvement. On the one hand, the previous lubricants only have an insufficient cooling effect on the tool, on the other hand, the metal oxide-phosphate glasses sintered onto the workpiece have to be removed in a subsequent etching stage by an acid treatment.

Der Erfindung liegt die Aufgabe zugrunde, ein Additiv für die Metallbearbeitung zu schaffen, welches auf der Grundlage von Schmierölen oder Wasser verbesserte Hochdruckeigenschaften und verschleißhemmende Eigenschaften aufweist.The invention has for its object to provide an additive for metalworking, which has improved high-pressure properties and anti-wear properties on the basis of lubricating oils or water.

Die Aufgabe wird gemäß der Erfindung dadurch gelöst, daß dem Schmier- und Kühlmittel als Additiv ein langkettiges Ammoniumpolyphosphat zugesetzt wird.The object is achieved according to the invention in that a long-chain ammonium polyphosphate is added to the lubricant and coolant as an additive.

Als Ammoniumpolyphosphat wird ein solches der allgemeinen Formel

Figure imgb0001
verwendet, in der n einer ganzen Zahl von 50 bis 1000, insbesondere von 300 bis 800, entspricht und R eine Ammoniumgruppe bedeutet.The ammonium polyphosphate is one of the general formula
Figure imgb0001
 used, in which n corresponds to an integer from 50 to 1000, in particular from 300 to 800, and R denotes an ammonium group.

Bei dem Ammoniumpolyphosphat können bis zu 20 %, insbesondere bis zu 5 %, der Ammoniumgruppen durch Wasserstoff ersetzt sein.In the ammonium polyphosphate, up to 20%, in particular up to 5%, of the ammonium groups can be replaced by hydrogen.

Als Additiv kann das Ammoniumpolyphosphat in Schmierölen oder Wasser in Form einer Flüssigkeit, Suspension oder Paste angewendet werden.The ammonium polyphosphate can be used as an additive in lubricating oils or water in the form of a liquid, suspension or paste.

Das Ammoniumpolyphosphat wird dem Schmier- und Kühlmittel in einer Menge von 0,1 bis 30, vorzugsweise von 2 bis 10, Gew% zugesetzt.The ammonium polyphosphate is added to the lubricant and coolant in an amount of 0.1 to 30, preferably 2 to 10,% by weight.

Das Ammoniumpolyphosphat kann als Additiv verwendet werden in Kombination mit grenzflächenaktiven Stoffen und/ oder Antischaummitteln und/oder Farbstoffen und/oder Rostinhibitoren und/oder Phosphatestern.The ammonium polyphosphate can be used as an additive in combination with surfactants and / or anti-foaming agents and / or dyes and / or rust inhibitors and / or phosphate esters.

Als Schmierölgrundlage können mineralische Schmieröle, wie paraffinbasische oder naphtenbasische Destillatöle mit einer Viskosität zwischen z.B. 6 und 60cSt bei 60°C und/oder synthetische Schmieröle, wie Polyolefine und/oder Esteröle und/oder Polyoxialkylene, verwendet werden.Mineral lubricating oils, such as paraffin-based or naphthen-based distillate oils with a viscosity between e.g. 6 and 60cSt at 60 ° C and / or synthetic lubricating oils, such as polyolefins and / or ester oils and / or polyoxyalkylenes, can be used.

Als grenzflächenaktive Stoffe haben sich insbesondere nichtionische Detergentien, wie Polyoxiäthylenstearat oder Polyoxiäthylenmonobutyläther in Mengen zwischen 1 bis 20 Gew% des Schmier- und Kühlmittels bewährt.Nonionic detergents such as polyoxyethylene stearate or polyoxyethylene monobutyl ether in amounts between 1 and 20% by weight of the lubricant and coolant have proven particularly useful as surface-active substances.

Als Antischaummittel können dem Schmier- und Kühlmittel Siloxane zugesetzt werden, z.B. Polymethylsiloxan in einer Menge von 5 - 25 ppm.Siloxanes can be added to the lubricant and coolant as anti-foaming agents, e.g. Polymethylsiloxane in an amount of 5 - 25 ppm.

Als Rostinhibitor können z.B. Benzotriazol oder Äthylbernsteinsäure in Mengen von etwa 200 ppm zugemischt werden. Durch den Zusatz von Phosphatestern, z.B. Ammoniumsalz des Gemisches der Mono- und Dioleylphosphorsäure oder der Di-n-propyldithiophosphorsäure oder Trikresylphosphat in Mengen von 0,01 bis 10 Gew% des Schmier- und Kühlmittels, kann die Wirkung von Ammoniumpolyphosphat auf Basis von Schmierölen synergistisch verbessert werden.For example, benzotriazole or ethyl succinic acid can be added as a rust inhibitor in amounts of about 200 ppm. By adding phosphate esters, for example ammonium salt of the mixture of mono- and dioleyl phosphoric acid or di-n-propyldithiophosphoric acid or tricresyl phosphate in amounts of 0.01 to 10% by weight of the lubricant and coolant, the effect of ammonium polyphosphate based on lubricating oils can be synergistic be improved.

Es hat sich gezeigt, daß bei der Heißbearbeitung von Metallen ein Ammoniumpolyphosphat mit einer mittleren Kettenlänge von n = 500 bis 1000, insbesondere von n = 600 bis 800, eingesetzt werden kann, wie es z.B. hergestellt wird gemäß der DE-PS 23 3o 174.It has been shown that an ammonium polyphosphate with an average chain length of n = 500 to 1000, in particular n = 600 to 800, can be used in the hot working of metals, as it is e.g. is produced according to DE-PS 23 3o 174.

Für die Kaltbearbeitung von Metallen, wo speziell großer Wert auf eine gute Kühlung des Werkzeuges und Werkstückes gelegt wird, eignet sich als Additiv besonders ein Ammoniumpolyphosphat mit einer mittleren Kettenlänge von n = 50 bis 400, insbesondere von n = 300 - 400, wie es z.B. hergestellt wird gemäß der DE-PS 17 67 2o5.An ammonium polyphosphate with an average chain length of n = 50 to 400, in particular of n = 300 - 400, is particularly suitable as an additive for cold machining of metals, where great importance is attached to good cooling of the tool and workpiece. is produced according to DE-PS 17 67 2o5.

Die folgenden Beispiele dienen der Erläuterung der Eigenschaften des Ammoniumpolyphosphats als Additiv in Schmierund Kühlmitteln. Die Erfindung ist nicht auf diese Beispiele beschränkt, das gilt insbesondere der Zumischung weiterer, das Schmier- und Kühlmittel verbessernder Zusätze.The following examples illustrate the properties of ammonium polyphosphate as an additive in lubricants and coolants. The invention is not restricted to these examples; this applies in particular to the admixture of further additives which improve the lubricant and coolant.

Die Prüfung der Schmier- und Kühlmittel erfolgte gemäß der DIN 51 350 im Shell-Vierkugel-Apparat sowie mit der Reibverschleißwaage nach Reichert.The lubricants and coolants were tested in accordance with DIN 51 350 in the Shell four-ball device and with the friction wear balance according to Reichert.

Beispiel 1example 1

2,5 Gewichtsteile Ammoniumpolyphosphat wurden in 97,5 Gewichtsteilen Wasser aufgeschlämmt. Ammoniumpolyphosphat wurde gemäß DE-PS 17 67 2o5 bei 330 - 340°C getempert und hatte eine mittlere Kettenlänge von n = 300 - 400 und eine Körnung von <63/u.
Das Testergebnis auf der Reibverschleißwaage ist in Tabelle 1 aufgeführt.2.5 parts by weight of ammonium polyphosphate were slurried in 97.5 parts by weight of water. Ammonium polyphosphate was annealed according to DE-PS 17 67 2o5 at 330 - 340 ° C and had an average chain length of n = 300 - 400 and a grain size of <63 / u.
T e stergebnis on the friction wear is listed in Table 1 below.

Vergleichsbeispiel 1 aComparative Example 1 a

3,0 Gewichtsteile Phosphatester eines Handelsproduktes auf Basis von Phenol mit 6 Äthylenoxid-Einheiten wurden mit
97,0 Gewichtsteilen Wasser gemischt. Das Testergebnis auf der Reibschleißwaage ist in Tabelle 1 aufgeführt.3.0 parts by weight of phosphate ester of a commercial product based on phenol with 6 ethylene oxide units were with
97.0 parts by weight of water mixed. The test result on the friction wear balance is listed in Table 1.

Vergleichsbeispiel 1 bComparative Example 1 b

Die Schmierwirkung von reinem Wasser wurde bestimmt. Das Testergebnis auf der Reibverschleißwaage ist in der Tabelle 1 aufgeführt.

Figure imgb0002
The lubricating effect of pure water was determined. The test result on the friction wear balance is listed in Table 1.
Figure imgb0002

Beispiel 2Example 2

5 Gewichtsteile Ammoniumpolyphosphat wurden in 95 Gewichtsteilen naphtenbasischem Öl (Coray 90 (R), Fa. Esso AG) suspendiert. Ammoniumpolyphosphat wurde gemäß DE-PS 17 67 2o5 hergestellt und hatte eine Kettenlänge von n = 300 - 400 und eine Korngröße von < 63/u.
Das Testergebnis mit dem Shell-Vierkugel-Apparat ist in Tabelle 2 aufgeführt.5 parts by weight of ammonium polyphosphate were suspended in 95 parts by weight of naphthenic oil (Coray 90 (R), Esso AG). Ammonium polyphosphate was produced according to DE-PS 17 67 2o5 and had a chain length of n = 300-400 and a grain size of <63 / u.
The test result with the Shell four-ball apparatus is shown in Table 2.

Vergleichsbeispiel 2 aComparative Example 2 a

Die Schmierwirkung von reinem naphtenbasischen Öl (Coray 90 (R)) wurde bestimmt.
Das Testergebnis mit dem Shell-Vierkugel-Apparat.ist in Tabelle 2 aufgeführt.The lubricity of pure naphthenic oil (Coray 90 (R) ) was determined.
The test result with the Shell Four Ball Apparatus is shown in Table 2.

Beispiel 3Example 3

2,5 Gewichtsteile Ammoniumpolyphosphat(gemäß Beispiel 2) und 2,5 Gewichtsteile Phosphatester auf Basis von Oleylalkohol mit 5 Äthylenoxid-Einheiten wurden in 95 Gewichtsteilen naphtenbasischem Öl (Coray 90 (R)) gelöst.2.5 parts by weight of ammonium polyphosphate (according to Example 2) and 2.5 parts by weight of phosphate ester based on oleyl alcohol with 5 ethylene oxide units were dissolved in 95 parts by weight of naphthenic oil (Coray 90 (R)).

Vergleichsbeispiel 3 aComparative Example 3 a

5 Gewichtsteile Phosphatester auf Basis von Oleylalkohol mit 5 Äthylenoxid-Einheiten wurden in 95 Gewichtsteilen naphtenbasischem Öl (Coray 90 (R)) gelöst.
Das Testergebnis mit dem Shell-Vierkugel-Apparat ist in Tabelle 2 aufgeführt.

Figure imgb0003
5 parts by weight of phosphate ester based on oleyl alcohol with 5 ethylene oxide units were dissolved in 95 parts by weight of naphthenic oil (Coray 90 (R)).
The test result with the Shell four-ball apparatus is shown in Table 2.
Figure imgb0003

Beispiel 4Example 4

In der beigefügten Zeichnung sind die Tiefziehversuchsergebnisse nach Erichsen dargestellt. Durch den Zusatz von Ammoniumpolyphosphat tritt eine deutliche Zunahme des Ziehweges ein. Mit einer Suspension von 30 Gewichtsteilen Ammoniumpolyphosphat (Exolit 263 (R), Fa. Hoechst AG) in 70 Gewichtsteilen naphtenbasischem Öl (Coray 90 (R)) erhält man bei einem Ziehverhältnis von 2,27 (Rondendurchmesser 75 mm; Ziehstempel 33 mm 0) einen Näpfchenzug ohne Abriß. Nur mit Coray 90 (R) kommt es bei einem Ziehverhältnis von 2,27 bereits zum Abriß bei einer Ziehung von 18,4 mm.The Erichsen thermoforming test results are shown in the attached drawing. The addition of ammonium polyphosphate leads to a significant increase in the drawing path. A suspension of 30 parts by weight of ammonium polyphosphate (Exolit 263 (R), Hoechst AG) in 70 parts by weight of naphthenic oil (Coray 90 (R) ) gives a draw ratio of 2.27 (round diameter 75 mm; punch 33 mm 0) a cell pull without demolition. Only with Coray 90 (R) with a draw ratio of 2.27 does a tear occur with a draw of 18.4 mm.

Beispiel 5Example 5

10 Gewichtsteile Ammoniumpolyphosphat (Exolit 263 (R), Fa. Hoechst AG) werden unter starkem Rühren in 80 Gewichtsteilen naphtenbasischem Öl (Coray 90 (R)) suspendiert und auf 100°C erwärmt. In diese erwärmte Suspension werden 5 Gewichtsteile eines Oxialkohols (Genapol - X - 050 (R), Fa. Hoechst AG) und 5 Gewichtsteile eines Oxiparaffins (Wachs OP., Fa. Hoechst AG) eingerührt. Nach Abkühlung erhält man ein Schmierfett. Das Testergebnis mit der Reibverschleißwaage ergab einen Flächendruck von 3,266 bar bei 0 Geräuschmeter. Die Messung wurde im flüssigen Zustand der Paste bei 65°C durchgeführt.10 parts by weight of ammonium polyphosphate (Exolit 263 (R), Hoechst AG) are suspended in 80 parts by weight of naphthenic oil (Coray 90 (R) ) with vigorous stirring and heated to 100 ° C. 5 parts by weight of an oxy alcohol (Genapol - X - 05 0 ( R ), Hoechst AG) and 5 parts by weight of an oxiparaffin (wax OP., Hoechst AG) are stirred into this heated suspension. After cooling, a grease is obtained. The test result with the friction wear scale showed a surface pressure of 3.266 bar at 0 noise meter. The measurement was carried out in the liquid state of the paste at 65 ° C.

Claims (6)

1. Additiv in Schmier- und Kühlmitteln für die Metallbearbeitung auf Phosphatbasis, dadurch gekennzeichnet, daß die Phosphatbasis ein langkettiges Ammoniumpolyphosphat ist.1. Additive in lubricants and coolants for metalworking based on phosphate, characterized in that the phosphate base is a long-chain ammonium polyphosphate. 2. Additiv nach Anspruch 1, dadurch gekennzeichnet, daß ein Ammoniumpolyphosphat der chemischen Formel
Figure imgb0004
verwendet wird, in der n einer ganzen Zahl von 50 bis 1000, insbesondere von 300 bis 800, entspricht und R eine Ammoniumgruppe bedeutet.2. Additive according to claim 1, characterized in that an ammonium polyphosphate of the chemical formula
Figure imgb0004
 is used, in which n corresponds to an integer from 50 to 1000, in particular from 300 to 800, and R denotes an ammonium group. 3. Additiv nach Anspruch 2, dadurch gekennzeichnet, daß in dem Ammoniumpolyphosphat bis zu 20 %, insbesondere bis zu 5 % der Ammoniumgruppen durch Wasserstoff ersetzt sind.3. Additive according to claim 2, characterized in that in the ammonium polyphosphate up to 20%, in particular up to 5% of the ammonium groups are replaced by hydrogen. 4. Additiv nach einem der Ansprüche 1 - 3, dadurch gekennzeichnet, daß es in Schmierölen oder Wasser in Form einer Flüssigkeit, Suspension oder Paste angewendet wird.4. Additive according to one of claims 1-3, characterized in that it is used in lubricating oils or water in the form of a liquid, suspension or paste. 5. Additiv nach Anspruch 4, dadurch gekennzeichnet, daß es dem Schmier- und Kühlmittel in einer Menge von 0,1 bis 30 Gew%, vorzugsweise von 2 bis 10 Gew%, zugesetzt wird.5. Additive according to claim 4, characterized in that it is added to the lubricant and coolant in an amount of 0.1 to 30% by weight, preferably 2 to 10% by weight. 6. Additiv nach einem der Ansprüche 4 und 5, dadurch gekennzeichnet, daß es in Kombination mit grenzflächenaktiven Stoffen und/oder Antischaummitteln und/oder Farbstoffen und/oder Rostinhibitoren und/oder Phosphatestern angewendet wird.6. Additive according to one of claims 4 and 5, characterized in that it is used in combination with surface-active substances and / or anti-foaming agents and / or dyes and / or rust inhibitors and / or phosphate esters.
EP79104352A 1978-11-20 1979-11-07 Lubricating and cooling agent Expired EP0011224B1 (en)

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