EP2032679A2 - Graphite-free high-temperature lubricant - Google Patents

Graphite-free high-temperature lubricant

Info

Publication number
EP2032679A2
EP2032679A2 EP07765571A EP07765571A EP2032679A2 EP 2032679 A2 EP2032679 A2 EP 2032679A2 EP 07765571 A EP07765571 A EP 07765571A EP 07765571 A EP07765571 A EP 07765571A EP 2032679 A2 EP2032679 A2 EP 2032679A2
Authority
EP
European Patent Office
Prior art keywords
mixture
fatty acid
temperature lubricant
lubricant according
pyrophosphate
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.)
Granted
Application number
EP07765571A
Other languages
German (de)
French (fr)
Other versions
EP2032679B1 (en
Inventor
Steffen Bugner
Ralf Giskow
Bernd Schneider
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.)
Chemische Fabrik Budenhiem KG
Original Assignee
Chemische Fabrik Budenhiem KG
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 Chemische Fabrik Budenhiem KG filed Critical Chemische Fabrik Budenhiem KG
Priority to EP14198677.8A priority Critical patent/EP2878661A1/en
Priority to SI200731628T priority patent/SI2032679T1/en
Priority to PL07765571T priority patent/PL2032679T3/en
Publication of EP2032679A2 publication Critical patent/EP2032679A2/en
Application granted granted Critical
Publication of EP2032679B1 publication Critical patent/EP2032679B1/en
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • 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
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085—Phosphorus oxides, acids or salts
    • C10M2201/0853—Phosphorus oxides, acids or salts used as base material
    • 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
    • C10M2201/087—Boron 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
    • 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
    • C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
    • 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
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • 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
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08—Resistance to extreme temperature
    • 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
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/40—Low content or no content compositions
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/08—Solids

Definitions

  • the present invention relates to a high-temperature lubricant for the hot processing of metals.
  • graphite Many lubricants for hot deformation of metals contain graphite because of its good lubricating properties.
  • graphite has significant disadvantages, such. Example, the inclusion of graphite carbon in the machined metal surface, whereby the composition and the properties of the metal surface can be changed.
  • graphite is undesirable for occupational hygiene reasons, because the graphite powder is easily atomized into the ambient atmosphere and represents a health hazard to nearby people by inhalation of graphite powder.
  • the object of the present invention was to provide a high-temperature lubricant with good flow and flow behavior for scale dissolution on heated metal surfaces, applied in powder form allows good coverage of the metal surface and even after prolonged storage under production conditions still good trickle and Has flow properties without strong clumping and avoids the use of graphite.
  • a high-temperature lubricant for the hot processing of metals consisting of a mixture of pulverulent materials, the mixture containing at least the following constituents:
  • the mixture according to the invention with the components (a), (b), (c) and (d) is particularly suitable as a lubricant for the hot processing of metals. It is understood that the lubricant according to the invention may contain further constituents, as long as they do not significantly adversely affect the desired advantageous properties.
  • Secondary and / or tertiary calcium phosphate compounds have surprisingly proven to be particularly suitable flow aids in a high-temperature lubricant of the type according to the invention for the hot processing of metals.
  • Monocalcium phosphate is unsuitable because it leads to clumping when humid.
  • the calcium phosphate compound of the high-temperature lubricant according to the invention is under Hxdroxylapatit [Ca 5 (PO 4) OH S] and tricalcium phosphate [Ca 3 (PO 4) 2] is selected, wherein Hxdroxylapatit is particularly preferred.
  • the mixture of the high-temperature lubricant according to the invention also contains a fatty acid or a fatty acid salt in combination with the other constituents. It has surprisingly been found that by using a fatty acid or a fatty acid salt, the agglomeration of the fine powder can be significantly reduced and the storage stability can be improved. Without the applicant thereby being bound to a theory, it becomes assumed that the fatty acid or fatty acid salt attaches to the grains of one or more other components of the mixture and thus prevents or reduces clumping of the grains, prevents moisture from the grains and thereby the storage stability and the flow behavior of the lubricant improved.
  • the fatty acid or the fatty acid salt is selected from saturated and unsaturated fatty acids having 6 to 26 carbon atoms or their salts. Particular preference is given to the fatty acid or the fatty acid salt among caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, margaric acid, stearic acid, arachic acid, behenic acid, lignoceric acid, cerotic acid, palmitoleic acid, oleic acid, elaidic acid, vaccenic acid, icosenoic acid, erucic acid, nervonic acid, Linoleic acid, linolenic acid, arachidonic acid, timnodonic acid, clupanodonic acid or salts thereof.
  • the fatty acid or the fatty acid salt is stearic acid or its salt, in particular magnesium stearate.
  • the fatty acid or the fatty acid salt is present at a temperature> 30 0 C as a solid.
  • the high-temperature lubricant according to the invention contains as further constituent boric acid, a boric acid salt (borate) and / or a mineral containing boric acid (borate).
  • boric acid H 3 BO 3
  • borax Na 2 B 4 O 5 (OH) 4 SH 2 O or Na 2 B 4 O 7 I OH 2 O
  • further sodium borates such as Na 2 B 4 O 7 OH 2 O, Na 2 B 4 O 7 (anhydrous), sodium metaborate [NaBO 2 4H 2 O] and boric anhydride [B 2 O 3 ].
  • boric acid a boric acid salt (borate) and / or a mineral containing a boric acid (borate) improves the uniform distribution of the lubricant on the metal surface and reduces scale formation. At high metalworking temperatures, the high temperature lubricant forms a melt.
  • the high-temperature lubricant according to the invention contains as further constituent condensed alkali metal phosphates, preferably condensed sodium or potassium phosphates or mixtures thereof, more preferably polyphosphates and / or pyrophosphates and / or metaphosphates or mixtures thereof.
  • the constituents of the mixture have an average particle size of ⁇ 150 ⁇ m. Preference is given to an average particle size of the constituents of the mixture of ⁇ 100 ⁇ m, more preferably of ⁇ 50 ⁇ m. Due to the small mean particle sizes of the constituents of the mixture according to the invention, the flow and flow behavior of the high-temperature lubricant according to the invention compared to known lubricants is significantly improved, facilitates the spraying on surfaces as a powder and ensures better and more uniform layer formation or occupancy on the metal surface. At the same time, the combination of the constituents of the mixture according to the invention prevents or reduces clumping which has regularly occurred in the case of lubricants according to the prior art with small grain sizes and has led to considerable disadvantages.
  • the constituents of the mixture of the high-temperature lubricant according to the invention have an average particle size of> 3 ⁇ m, preferably ⁇ 10 ⁇ m, particularly preferably> 15 ⁇ m. It has been found that too small average grain sizes can only be produced very costly and under relatively high costs and, on the other hand, they also increase the tendency to clumping again. An average grain size in the range of 20 to 50 microns has therefore proved to be optimal.
  • the secondary or tertiary calcium phosphate compound (a) is in an amount of 0.1 to 15% by weight, preferably 0.5 to 10% by weight, more preferably 1 to 5 Wt .-% in the mixture.
  • the fatty acid or fatty acid salt (b) is present in an amount of from 0.1 to 15% by weight, preferably from 1 to 10% by weight, more preferably from 3 to 7 Wt .-% in the mixture.
  • boric acid, boric acid salt (borate) and / or a mineral (c) containing boric acid (c) are present in an amount of from 5 to 30% by weight, preferably from 10 to 25% by weight. %, more preferably from 15 to 20 wt .-% in the mixture.
  • the high-temperature lubricant according to the invention is polyphosphate and / or pyrophosphate and / or metaphosphate (d) in an amount of 60 to 95 wt .-%, preferably from 70 to 85 wt .-%, particularly preferably from 75 to 80 wt .-% in the mixture.
  • the average particle size of the mixture or constituents of the mixture of the high-temperature lubricant according to the invention is determined by means of a Cilas Model 715/920 laser granulometer from Cilas. Inc. Approximately 80 mg of sample is suspended in 2-propanol and the measurement is made one minute after preparation of the suspension according to the manufacturer's instructions.

Abstract

The invention relates to a high-temperature lubricant for the heat treatment of metals, said lubricant consisting of a mixture of pulverulent materials. The aim of the invention is to provide a high-temperature lubricant with good free-flowing properties and behaviour for dissolving scale on heated metallic surfaces, said lubricant being applied in a powder form and enabling a good covering of the metallic surface, having good free-flowing properties without much agglutination even after a long storage period under production conditions, and avoiding the use of graphite. To this end, the mixture contains at least the following components: a) a secondary and/or tertiary calcium phosphate compound, b) a fatty acid or a fatty acid salt, c) boric acid, a boric acid salt (borate) and/or a mineral containing a boric acid salt (borate) and d) condensed alkali phosphate. The constituents of the mixture have an average particle size of 150 µm and the lubricant does not contain any added graphite.

Description

Graphitfreier Hochtemperatur-Schmierstoff Graphite-free high-temperature lubricant
Die vorliegende Erfindung betrifft einen Hochtemperatur-Schmierstoff für die Heißverarbeitung von Metallen.The present invention relates to a high-temperature lubricant for the hot processing of metals.
Hintergrund der ErfindungBackground of the invention
Beim Warmverformen von Metallen, insbesondere von Stahl, in einem Temperaturbereich von 700- 13000C kommt es an der erhitzten Metalloberfläche an der Umgebungsluft zur Zunderbildung. Bei Warmwalzverfahren von Stahl zur Herstellung von nahtlosen Rohren wird ein Vollmaterial durchstoßen und ein Hohlblock gebildet, der anschließend in nachfolgenden Walzschritten elongiert wird. Hier ist die Gefahr von Zunderbildung auf der erhitzten Metalloberfläche des Hohlblocks während der Überführung zu dem Elongierprozeß besonders hoch. Bei den nachfolgenden Walzschritten kann dieser Zunderanfall zu Innenfehlern des nahtlosen Rohres führen. Aus diesem Grund wird der anfallende Zunder beispielsweise mit Druckluft oder Inertgas ausgeblasen. Zusätzlich werden unterschiedlichste Substanzen in Pulverform als Schmier- oder Beizmittel auf die Innenoberfläche der Hohlblöcke aufgebracht. Beispiele für solche Schmier- oder Beizmittel enthalten Graphit, Bornitrid, Molybdänsulfid, Silikate oder Erdalkaliphosphate sowie Mischungen davon.When hot forming metals, especially steel, in a temperature range of 700- 1300 0 C occurs on the heated metal surface in the ambient air to the formation of scale. In hot rolling of steel for the production of seamless tubes, a solid material is pierced and a hollow block is formed, which is then elongated in subsequent rolling steps. Here, the risk of scale formation on the heated metal surface of the hollow block during the transfer to the Elongierprozeß is particularly high. In the subsequent rolling steps, this scale attack can lead to internal defects of the seamless pipe. For this reason, the resulting scale is blown out, for example, with compressed air or inert gas. In addition, a wide variety of substances are applied in powder form as a lubricant or mordant to the inner surface of the hollow blocks. Examples of such lubricants or mordants include graphite, boron nitride, molybdenum sulfide, silicates or alkaline earth phosphates and mixtures thereof.
Viele Schmiermittel für die Heißverformung von Metallen enthalten Graphit aufgrund seiner guten Schmiereigenschaften. Allerdings hat Graphit erhebliche Nachteile, wie z. B. die Aufnahme von Graphitkohlenstoff in die bearbeitete Metalloberfläche, wodurch die Zusammensetzung und die Eigenschaften der Metalloberfläche verändert werden können. Darüber hinaus ist Graphit aus arbeitshygienischen Gründen unerwünscht, da das Graphitpulver leicht in die Umgebungsatmosphäre zerstäubt wird und für in der Nähe arbeitende Personen eine Gesundheitsgefährdung durch Einatmen des Graphitpulvers darstellt.Many lubricants for hot deformation of metals contain graphite because of its good lubricating properties. However, graphite has significant disadvantages, such. Example, the inclusion of graphite carbon in the machined metal surface, whereby the composition and the properties of the metal surface can be changed. In addition, graphite is undesirable for occupational hygiene reasons, because the graphite powder is easily atomized into the ambient atmosphere and represents a health hazard to nearby people by inhalation of graphite powder.
Weiterhin besitzen viele bekannte Schmiermittel aufgrund ihrer physikalischen Eigenschaften und Korngrößen kein gutes Riesel- bzw. Fließverhalten. Ein grobes Material mit hohen Korngrößen führt häufig zu einer unzureichenden und ungleichmäßigen Belegung der Metalloberfläche und damit zu einer schlechten Zunderreduzierung. Bekannte feinkörnige Materialien mit kleinen Korngrößen, bei- spielsweise unter 50 μm, neigen häufig zu Verklumpung, insbesondere bei Lagerung, weshalb sie nur schwer als Pulver auf die Metalloberfläche aufgesprüht werden können. Eine feinere Körnung hätte jedoch den Vorteil, daß eine bessere Schichtbildung erreicht werden kann, jedoch wird dieser Vorteil bei bekannten Zusammensetzungen mit feiner Körnung durch die starke Neigung zur Verklumpung wieder zunichte gemacht. Aufgabe der ErfindungFurthermore, many known lubricants due to their physical properties and grain sizes no good trickle or flow behavior. A coarse material with high particle sizes often leads to an insufficient and uneven coverage of the metal surface and thus to a poor scale reduction. Known fine-grained materials with small particle sizes, for example less than 50 μm, often tend to clump together, especially during storage, which is why they are difficult to spray onto the metal surface as a powder. However, a finer grain size would have the advantage that a better layer formation can be achieved, but this advantage is nullified in known compositions with fine grain by the strong tendency to clumping again. Object of the invention
Die Aufgabe der vorliegenden Erfindung bestand daher darin, einen Hochtemperatur-Schmierstoff mit gutem Riesel- und Fließverhalten zur Zunderauflösung auf erhitzten Metalloberflächen bereitzu- stellen, der in Pulverform aufgebracht eine gute Belegung der Metalloberfläche erlaubt und auch nach längerer Lagerung unter Produktionsbedingungen noch gute Riesel- und Fließeigenschaften ohne starke Verklumpung aufweist und der die Verwendung von Graphit vermeidet.The object of the present invention was to provide a high-temperature lubricant with good flow and flow behavior for scale dissolution on heated metal surfaces, applied in powder form allows good coverage of the metal surface and even after prolonged storage under production conditions still good trickle and Has flow properties without strong clumping and avoids the use of graphite.
Beschreibung der Erfindung Gelöst wird diese Aufgabe erfindungsgemäß durch einen Hochtemperatur-Schmierstoff für die Heißverarbeitung von Metallen, bestehend aus einem Gemisch von feinpulverigen Materialien, wobei das Gemisch wenigstens die folgenden Bestandteile enthält:DESCRIPTION OF THE INVENTION This object is achieved according to the invention by a high-temperature lubricant for the hot processing of metals, consisting of a mixture of pulverulent materials, the mixture containing at least the following constituents:
(a) eine sekundäre und/oder tertiäre Calciumphosphatverbindung,(a) a secondary and / or tertiary calcium phosphate compound,
(b) eine Fettsäure oder ein Fettsäuresalz, (c) Borsäure, ein Borsäuresalz (Borat) und/oder ein Borsäuresalz (Borat) enthaltendes Mineral und(b) a fatty acid or a fatty acid salt, (c) boric acid, a borate salt (borate) and / or a boric acid borate containing mineral, and
(d) kondensierte Alkaliphosphate, und wobei die Bestandteile des Gemischs eine mittlere Korngröße von < 150 μm aufweisen und der Schmierstoff keinen Zusatz von Graphit enthält.(D) condensed alkali metal phosphates, and wherein the components of the mixture have a mean particle size of <150 microns and the lubricant contains no addition of graphite.
Es hat sich überraschenderweise gezeigt, daß sich das erfindungsgemäße Gemisch mit den Bestandteile (a), (b), (c) und (d) als Schmierstoff für die Heißverarbeitung von Metallen besonders gut eignet. Es versteht sich, daß der erfindungsgemäße Schmierstoff weitere Bestandteile enthalten kann, soweit diese die gewünschten vorteilhaften Eigenschaften nicht wesentlich nachteilig beein- flussen.It has surprisingly been found that the mixture according to the invention with the components (a), (b), (c) and (d) is particularly suitable as a lubricant for the hot processing of metals. It is understood that the lubricant according to the invention may contain further constituents, as long as they do not significantly adversely affect the desired advantageous properties.
Sekundäre und/oder tertiäre Calciumphosphatverbindungen haben sich überraschenderweise als besonders geeignete Rieselhilfsmittel in einem Hochtemperatur-Schmierstoff der erfindungsgemäßen Art für die Heißverarbeitung von Metallen erwiesen. Monocalciumphosphat ist ungeeignet, da es bei Luftfeuchte zu Verklumpung führt. Ganz besonders bevorzugt ist die Calciumphosphatverbindung des erfindungsgemäßen Hochtemperatur-Schmierstoffes unter Hxdroxylapatit [Ca5(PO4)SOH] und Tricalciumphosphat [Ca3(PO4)2] ausgewählt, wobei Hxdroxylapatit besonders bevorzugt ist.Secondary and / or tertiary calcium phosphate compounds have surprisingly proven to be particularly suitable flow aids in a high-temperature lubricant of the type according to the invention for the hot processing of metals. Monocalcium phosphate is unsuitable because it leads to clumping when humid. Most preferably, the calcium phosphate compound of the high-temperature lubricant according to the invention is under Hxdroxylapatit [Ca 5 (PO 4) OH S] and tricalcium phosphate [Ca 3 (PO 4) 2] is selected, wherein Hxdroxylapatit is particularly preferred.
Das Gemisch des erfindungsgemäßen Hochtemperatur-Schmierstoffs enthält weiterhin eine Fett- säure oder ein Fettsäuresalz in Kombination mit den übrigen Bestandteilen. Es hat sich überraschenderweise gezeigt, daß durch die Verwendung einer Fettsäure oder eines Fettsäuresalzes die Verklumpung des feinkörnigen Pulvers erheblich verringert und die Lagerungsbeständigkeit verbessert werden können. Ohne daß sich die Anmelderin hierdurch an eine Theorie gebunden fühlt, wird angenommen, daß sich die Fettsäure oder das Fettsäuresalz an die Körner eines oder mehrerer weiterer Bestandteile des Gemisches anlagert und auf diese Weise eine Verklumpung der Körner verhindert oder vermindert, Feuchtigkeit von den Körnern abhält und dadurch die Lagerungsbeständigkeit sowie das Riesel- bzw. Fließverhalten des Schmierstoffs verbessert.The mixture of the high-temperature lubricant according to the invention also contains a fatty acid or a fatty acid salt in combination with the other constituents. It has surprisingly been found that by using a fatty acid or a fatty acid salt, the agglomeration of the fine powder can be significantly reduced and the storage stability can be improved. Without the applicant thereby being bound to a theory, it becomes assumed that the fatty acid or fatty acid salt attaches to the grains of one or more other components of the mixture and thus prevents or reduces clumping of the grains, prevents moisture from the grains and thereby the storage stability and the flow behavior of the lubricant improved.
In einer bevorzugten Ausführungsform des erfindungsgemäßen Hochtemperatur-Schmierstoffs ist die Fettsäure bzw. das Fettsäuresalz unter gesättigten und ungesättigten Fettsäuren mit 6 bis 26 Kohlenstoffatomen bzw. deren Salzen ausgewählt. Besonders bevorzugt ist die Fettsäure bzw. das Fettsäuresalz unter Kapronsäure, Kaprylsäure, Kaprinsäure, Laurinsäure, Myristinsäure, Palmitin- säure, Margarinsäure, Stearinsäure, Arachinsäure, Behensäure, Lignocerinsäure, Cerotinsäure, Palmitoleinsäure, Ölsäure, Elaidinsäure, Vaccensäure, Icosensäure, Erucasäure, Nervonsäure, Li- nolsäure, Linolensäure, Arachidonsäure, Timnodonsäure, Clupanodonsäure bzw. deren Salzen, ausgewählt. Ganz besonders bevorzugt ist die Fettsäure bzw. das Fettsäuresalz Stearinsäure bzw. deren Salz, insbesondere Magnesiumstearat. Voraussetzung für die Auswahl ist, daß die Fettsäure bzw. das Fettsäuresalz bei einer Temperatur > 300C als Feststoff vorliegt.In a preferred embodiment of the high-temperature lubricant according to the invention, the fatty acid or the fatty acid salt is selected from saturated and unsaturated fatty acids having 6 to 26 carbon atoms or their salts. Particular preference is given to the fatty acid or the fatty acid salt among caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, margaric acid, stearic acid, arachic acid, behenic acid, lignoceric acid, cerotic acid, palmitoleic acid, oleic acid, elaidic acid, vaccenic acid, icosenoic acid, erucic acid, nervonic acid, Linoleic acid, linolenic acid, arachidonic acid, timnodonic acid, clupanodonic acid or salts thereof. Most preferably, the fatty acid or the fatty acid salt is stearic acid or its salt, in particular magnesium stearate. Prerequisite for the selection is that the fatty acid or the fatty acid salt is present at a temperature> 30 0 C as a solid.
Der erfindungsgemäße Hochtemperatur-Schmierstoff enthält als weiteren Bestandteil Borsäure, ein Borsäuresalz (Borat) und/oder ein Borsäuresalz (Borat) enthaltendes Mineral. Besonders bevorzugt sind Borsäure [H3BO3], Borax [Na2B4O5(OH)4 SH2O bzw. Na2B4O7 I OH2O], weitere Natriumborate, wie Na2B4O7 OH2O, Na2B4O7 (wasserfrei), Natriummetaborat [NaBO24H2O] und Borsäureanhydrid [B2O3]. Die erfindungsgemäße Verwendung von Borsäure, einem Borsäuresalz (Borat) und/oder einem ein Borsäuresalz (Borat) enthaltenden Mineral verbessert die gleichmäßige Verteilung des Schmiermittels auf der Metalloberfläche und reduziert die Zunderbildung. Bei den hohen Temperaturen der Metallverarbeitung bildet der Hochtemperatur-Schmierstoff eine Schmelze.The high-temperature lubricant according to the invention contains as further constituent boric acid, a boric acid salt (borate) and / or a mineral containing boric acid (borate). Particularly preferred are boric acid [H 3 BO 3 ], borax [Na 2 B 4 O 5 (OH) 4 SH 2 O or Na 2 B 4 O 7 I OH 2 O], further sodium borates, such as Na 2 B 4 O 7 OH 2 O, Na 2 B 4 O 7 (anhydrous), sodium metaborate [NaBO 2 4H 2 O] and boric anhydride [B 2 O 3 ]. The use according to the invention of boric acid, a boric acid salt (borate) and / or a mineral containing a boric acid (borate) improves the uniform distribution of the lubricant on the metal surface and reduces scale formation. At high metalworking temperatures, the high temperature lubricant forms a melt.
Der erfindungsgemäße Hochtemperatur-Schmierstoff enthält als weiteren Bestandteil kondensierte Alkaliphosphate, vorzugsweise kondensierte Natrium- oder Kaliumphosphate oder Gemische davon, besonders bevorzugt Polyphosphate und/oder Pyrophosphate und/oder Metaphosphate oder Gemische davon. Ganz besonders bevorzugt sind Dinatriumpyrophosphat [Na2H2P2O7], Trinatriumpy- rophosphat [Na3HP2O7], Tetranatriumpyrophosphat [Na4P2O7], Natriumtripolyphosphat [Na5P3O-Io], Natriumtrimetaphosphat [(NaPO3)3], Natriumpolyphosphat [(NaPO3)n], Dikaliumpyrophosphat [K2H2P2O7], Trikaliumpyrophosphat [K3HP2O7], Tetrakaliumpyrophosphat [K4P2O7], Kaliumtripo- lyphosphat [K5P3Oio], Kaliumtrimetaphosphat [(KPO3)3] und/oder Kaliumpolyphosphat [(KPO3)n], am bevorzugtesten Natriumtripolyphosphat [Na5P3OiO]. Es hat sich gezeigt, daß die Verwendung eines Polyphosphats und/oder eines Pyrophosphats und/oder eines Metaphosphats in dem Gemisch des erfindungsgemäßen Hochtemperatur-Schmierstoffs mit Vorteil unter anderem zur Zunderauflösung beiträgt. - A -The high-temperature lubricant according to the invention contains as further constituent condensed alkali metal phosphates, preferably condensed sodium or potassium phosphates or mixtures thereof, more preferably polyphosphates and / or pyrophosphates and / or metaphosphates or mixtures thereof. Very particular preference is given to disodium pyrophosphate [Na 2 H 2 P 2 O 7 ], trisodium pyrophosphate [Na 3 HP 2 O 7 ], tetrasodium pyrophosphate [Na 4 P 2 O 7 ], sodium tripolyphosphate [Na 5 P 3 O- I o], Sodium trimetaphosphate [(NaPO 3 ) 3 ], sodium polyphosphate [(NaPO 3 ) n ], dipotassium pyrophosphate [K 2 H 2 P 2 O 7 ], tripotassium pyrophosphate [K 3 HP 2 O 7 ], tetrapotassium pyrophosphate [K 4 P 2 O 7 ], Potassium tripolyphosphate [K 5 P 3 Oio], potassium trimetaphosphate [(KPO 3 ) 3 ] and / or potassium polyphosphate [(KPO 3 ) n ], most preferably sodium tripolyphosphate [Na 5 P 3 Oi O ]. It has been found that the use of a polyphosphate and / or a pyrophosphate and / or a metaphosphate in the mixture of the high-temperature lubricant according to the invention advantageously contributes, inter alia, to the scale dissolution. - A -
In dem erfindungsgemäßen Hochtemperatur-Schmierstoff weisen die Bestandteile des Gemischs eine mittlere Korngröße von < 150 μm auf. Bevorzugt ist eine mittlere Korngröße der Bestandteile des Gemischs von < 100 μm, besonders bevorzugt von < 50 μm. Durch die geringen mittleren Korngrößen der Bestandteile des erfindungsgemäßen Gemischs wird das Riesel- und Fließverhalten des erfindungsgemäßen Hochtemperatur-Schmierstoffs gegenüber bekannten Schmierstoffen erheblich verbessert, das Aufsprühen auf Oberflächen als Pulver erleichtert und eine bessere und gleichmäßigere Schichtbildung bzw. Belegung auf der Metalloberfläche gewährleistet. Gleichzeitig wird durch die Kombination der erfindungsgemäßen Bestandteile des Gemischs eine Verklumpung verhindert oder vermindert, die bei Schmierstoffen nach dem Stand der Technik mit kleinen Korn- großen regelmäßig aufgetreten ist und zu erheblichen Nachteilen geführt hat.In the high-temperature lubricant according to the invention, the constituents of the mixture have an average particle size of <150 μm. Preference is given to an average particle size of the constituents of the mixture of <100 μm, more preferably of <50 μm. Due to the small mean particle sizes of the constituents of the mixture according to the invention, the flow and flow behavior of the high-temperature lubricant according to the invention compared to known lubricants is significantly improved, facilitates the spraying on surfaces as a powder and ensures better and more uniform layer formation or occupancy on the metal surface. At the same time, the combination of the constituents of the mixture according to the invention prevents or reduces clumping which has regularly occurred in the case of lubricants according to the prior art with small grain sizes and has led to considerable disadvantages.
Es ist weiterhin bevorzugt, wenn die Bestandteile des Gemischs des erfindungsgemäßen Hochtemperatur-Schmierstoffs eine mittlere Korngröße von > 3 μm, vorzugsweise ≥ 10 μm, besonders bevorzugt > 15 μm aufweisen. Es hat sich erwiesen, daß zu geringe mittlere Korngrößen zum einen nur sehr aufwendig und unter verhältnismäßig hohen Kosten herstellbar sind und sie zum anderen auch die Neigung zur Verklumpung wieder erhöhen. Eine mittlere Korngröße im Bereich von 20 bis 50 μm hat sich daher als optimal erwiesen.It is further preferred if the constituents of the mixture of the high-temperature lubricant according to the invention have an average particle size of> 3 μm, preferably ≥ 10 μm, particularly preferably> 15 μm. It has been found that too small average grain sizes can only be produced very costly and under relatively high costs and, on the other hand, they also increase the tendency to clumping again. An average grain size in the range of 20 to 50 microns has therefore proved to be optimal.
In einer bevorzugten Ausführungsform des erfindungsgemäßen Hochtemperatur-Schmierstoffs ist die sekundäre oder tertiäre Calciumphosphatverbindung (a) in einer Menge von 0,1 bis 15 Gew.-%, vorzugsweise von 0,5 bis 10 Gew.-%, besonders bevorzugt von 1 bis 5 Gew.-% in dem Gemisch enthalten.In a preferred embodiment of the high temperature lubricant of the present invention, the secondary or tertiary calcium phosphate compound (a) is in an amount of 0.1 to 15% by weight, preferably 0.5 to 10% by weight, more preferably 1 to 5 Wt .-% in the mixture.
In einer weiteren bevorzugten Ausführungsform des erfindungsgemäßen Hochtemperatur- Schmierstoffs ist die Fettsäure bzw. das Fettsäuresalz (b) in einer Menge von 0, 1 bis 15 Gew.-%, vorzugsweise von 1 bis 10 Gew.-%, besonders bevorzugt von 3 bis 7 Gew.-% in dem Gemisch enthalten.In a further preferred embodiment of the high-temperature lubricant according to the invention, the fatty acid or fatty acid salt (b) is present in an amount of from 0.1 to 15% by weight, preferably from 1 to 10% by weight, more preferably from 3 to 7 Wt .-% in the mixture.
In einer weiteren bevorzugten Ausführungsform des erfindungsgemäßen Hochtemperatur- Schmierstoffs ist Borsäure, Borsäuresalz (Borat) und/oder ein Borsäuresalz (Borat) enthaltendes Mineral (c) in einer Menge von 5 bis 30 Gew.-%, vorzugsweise von 10 bis 25 Gew.-%, besonders bevorzugt von 15 bis 20 Gew.-% in dem Gemisch enthalten.In a further preferred embodiment of the high-temperature lubricant according to the invention, boric acid, boric acid salt (borate) and / or a mineral (c) containing boric acid (c) are present in an amount of from 5 to 30% by weight, preferably from 10 to 25% by weight. %, more preferably from 15 to 20 wt .-% in the mixture.
In einer weiteren bevorzugten Ausführungsform des erfindungsgemäßen Hochtemperatur- Schmierstoffs ist Polyphosphat und/oder Pyrophosphat und/oder Metaphosphat (d) in einer Menge von 60 bis 95 Gew.-%, vorzugsweise von 70 bis 85 Gew.-%, besonders bevorzugt von 75 bis 80 Gew.-% in dem Gemisch enthalten. Lagerverhalten, Agglomeratbildung und FeuchteaufnahmeIn a further preferred embodiment of the high-temperature lubricant according to the invention is polyphosphate and / or pyrophosphate and / or metaphosphate (d) in an amount of 60 to 95 wt .-%, preferably from 70 to 85 wt .-%, particularly preferably from 75 to 80 wt .-% in the mixture. Storage behavior, agglomeration and moisture absorption
Zur Prüfung der Verklumpungsneigung unter Produktionsbedingungen wurden Lagerversuche verschiedener Mischungen unter Produktionsbedingungen durchgeführt. Dafür wurden 150 g Probe im Klimaschrank (Typ 3821/15 der Firma Feutron) bei konstant 300C und 80% relativer Luftfeuchte für 0 h, 67 h und 96 h gelagert und anschließend ihre Agglomeratbildung (Rieselfähigkeit) in einem Siebtest sowie ihre Feuchteaufnahme anhand der Gewichtszunahme gegenüber der ursprünglichen Einwaage bestimmt.To test the tendency to agglomerate under production conditions, storage trials of various mixtures were carried out under production conditions. For 150 g sample in the climatic chamber were (type 3821/15 the company Feutron) constant at 30 0 C and 80% relative humidity for 0 h, 67 h and 96 h stored and then their agglomeration (flowability) in a sieve as well as their moisture absorption based the weight gain compared to the original weight determined.
Erst die Gesamtbeurteilung von kombiniertem Lager- und Rieselverhalten einer jeweiligen Mischung läßt eine Aussage über ihre Qualität und Eignung unter Produktionsbedingungen zu. Die Ergebnisse der Untersuchung verschiedener Mischungen sind in Tabelle 1 gezeigt.Only the overall assessment of combined storage and trickling behavior of a particular mixture can be a statement about their quality and suitability under production conditions. The results of the examination of various mixtures are shown in Table 1.
KorngrößenbestimmungParticle size determination
Die Bestimmung der mittleren Korngröße des Gemischs bzw. der Bestandteile des Gemischs des erfindungsgemäßen Hochtemperatur-Schmierstoffs erfolgt mittels eines Laser-Granulometers Cilas Modell 715/920 der Firma Cilas U.S. Inc. Circa 80 mg Probe werden in 2-Propanol suspendiert und die Messung eine Minute nach Herstellung der Suspension gemäß der Anleitung des Herstellers durchgeführt.The average particle size of the mixture or constituents of the mixture of the high-temperature lubricant according to the invention is determined by means of a Cilas Model 715/920 laser granulometer from Cilas. Inc. Approximately 80 mg of sample is suspended in 2-propanol and the measurement is made one minute after preparation of the suspension according to the manufacturer's instructions.
Tabelle 1Table 1
Rieselfähigkeit und Feuchteaufnahme nach unterschiedlicher Lagerdauer unter ProduktionsbedingungenFree-flowing and moisture absorption after different storage periods under production conditions
Siebbedingungen: Probenmenge 2 g + Feuchtaufnahmemenge; Vibrationsamplitude 1 Skalenteil; Vibrationsdauer 70 sek. Screening conditions: Sample amount 2 g + moisture pickup amount; Vibration amplitude 1 scale part; Vibration duration 70 sec.

Claims

PATENTANSPRÜCHE
1. Hochtemperatur-Schmierstoff für die Heißverarbeitung von Metallen, bestehend aus einem Gemisch von feinpulverigen Materialien, wobei das Gemisch wenigstens die folgenden Be- standteile enthält:1. High-temperature lubricant for the hot processing of metals, consisting of a mixture of pulverulent materials, the mixture containing at least the following constituents:
(a) eine sekundäre und/oder tertiäre Calciumphosphatverbindung,(a) a secondary and / or tertiary calcium phosphate compound,
(b) eine Fettsäure oder ein Fettsäuresalz,(b) a fatty acid or a fatty acid salt,
(c) Borsäure, ein Borsäuresalz (Borat) und/oder ein Borsäuresalz (Borat) enthaltendes Mineral und (d) kondensierte Alkaliphosphate, und wobei die Bestandteile des Gemischs eine mittlere Korngröße von < 150 μm aufweisen und der Schmierstoff keinen Zusatz von Graphit enthält.(c) boric acid, a boric acid borate and / or borate salt and (d) condensed alkali phosphates, and wherein the components of the mixture have a mean grain size of <150 μm and the lubricant does not contain added graphite.
2. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch ge- kennzeichnet, daß Bestandteil (c) unter Borsäure [H3BO3], Borax [Na2B4O5(OH)4 SH2O bzw.2. High-temperature lubricant according to one of the preceding claims, character- ized in that component (c) under boric acid [H 3 BO 3 ], borax [Na 2 B 4 O 5 (OH) 4 SH 2 O or
Na2B4O7 I OH2O], Natriumboraten, wie Na2B4O7 OH2O, Na2B4O7 (wasserfrei), Natriummetaborat [NaBO24H2O] und Borsäureanhydrid [B2O3] und Gemischen davon ausgewählt ist.Na 2 B 4 O 7 I OH 2 O], sodium borates such as Na 2 B 4 O 7 OH 2 O, Na 2 B 4 O 7 (anhydrous), sodium metaborate [NaBO 2 4H 2 O] and boric anhydride [B 2 O 3 ] and mixtures thereof.
3. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß Bestandteil (d) unter kondensierten Natrium- oder Kaliumphosphaten o- der Gemischen davon, bevorzugt unter Polyphosphaten und/oder Pyrophosphaten und/oder Metaphosphaten oder Gemischen davon, besonders bevorzugt unter Dinatriumpyrophosphat [Na2H2P2O7], Trinatriumpyrophosphat [Na3HP2O7], Tetranatriumpyrophosphat [Na4P2O7], Natriumtripolyphosphat [Na5P3O-Io], Natriumtrimetaphosphat [(NaPO3)3], Natriumpolyphosphat [(NaPO3)n], Dikaliumpyrophosphat [K2H2P2O7], Trikaliumpyrophosphat [K3HP2O7], Tetrakaliumpyrophosphat [K4P2O7], Kaliumtripolyphosphat [K5P3Oio], Kaliumtrimetaphosphat [(KPO3)3], Kaliumpolyphosphat [(KPO3)n] oder Gemischen davon ausgewählt ist, wobei Bestandteil (d) am bevorzugtesten Natriumtripolyphosphat [Na5P3Oio] ist.3. High-temperature lubricant according to one of the preceding claims, characterized in that component (d) under condensed sodium or potassium phosphates o- mixtures thereof, preferably polyphosphates and / or pyrophosphates and / or metaphosphates or mixtures thereof, more preferably disodium pyrophosphate [Na 2 H 2 P 2 O 7 ], trisodium pyrophosphate [Na 3 HP 2 O 7 ], tetrasodium pyrophosphate [Na 4 P 2 O 7 ], sodium tripolyphosphate [Na 5 P 3 O- I o], sodium trimetaphosphate [(NaPO 3 ) 3 ], Sodium polyphosphate [(NaPO 3 ) n ], dipotassium pyrophosphate [K 2 H 2 P 2 O 7 ], tripotassium pyrophosphate [K 3 HP 2 O 7 ], tetrapotassium pyrophosphate [K 4 P 2 O 7 ], potassium tripolyphosphate [K 5 P 3 Oio ], Potassium trimetaphosphate [(KPO 3 ) 3 ], potassium polyphosphate [(KPO 3 ) n ], or mixtures thereof, wherein component (d) is most preferably sodium tripolyphosphate [Na 5 P 3 Oio].
4. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß die Calciumphosphatverbindung unter Hxdroxylapatit [Ca5(PO4)3OH] und Tricalciumphosphat [Ca3(PO4)2] ausgewählt ist, wobei Hxdroxylapatit besonders bevorzugt ist.4. High-temperature lubricant according to one of the preceding claims, characterized in that the calcium phosphate compound under Hxdroxylapatit [Ca 5 (PO 4 ) 3 OH] and tricalcium phosphate [Ca 3 (PO 4 ) 2 ] is selected, with Hxdroxylapatit is particularly preferred.
5. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß die Fettsäure bzw. das Fettsäuresalz unter gesättigten und ungesättigten Fettsäuren mit 6 bis 26 Kohlenstoffatomen bzw. deren Salzen, vorzugsweise unter Kapron- säure, Kaprylsäure, Kaprinsäure, Laurinsäure, Myristinsäure, Palmitinsäure, Margarinsäure, Stearinsäure, Arachinsäure, Behensäure, Lignocerinsäure, Cerotinsäure, Palmitoleinsäure, Ölsäure, Elaidinsäure, Vaccensäure, Icosensäure, Erucasäure, Nervonsäure, Linolsäure, Linolensäure, Arachidonsäure, Timnodonsäure, Clupanodonsäure bzw. deren Salzen, ausge- wählt ist, vorausgesetzt daß die Fettsäure bzw. das Fettsäuresalz bei einer Temperatur >5. High-temperature lubricant according to one of the preceding claims, characterized in that the fatty acid or the fatty acid salt among saturated and unsaturated fatty acids having 6 to 26 carbon atoms or their salts, preferably below Kapron- acid, caprylic, capric, lauric, myristic, palmitic, margaric, stearic, arachidic, behenic, lignoceric, cerotic, palmitoleic, oleic, elaidic, vaccenic, icosenoic, erucic, nervonic, linoleic, linolenic, arachidonic, timnodonic, clupanodonic acids and their derivatives Salts, is selected, provided that the fatty acid or the fatty acid salt at a temperature
300C als Feststoff vorliegt.30 0 C is present as a solid.
6. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß die Fettsäure bzw. das Fettsäuresalz Stearinsäure bzw. deren Salz ist.6. High-temperature lubricant according to one of the preceding claims, characterized in that the fatty acid or the fatty acid salt is stearic acid or its salt.
7. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß die sekundäre oder tertiäre Calciumphosphatverbindung (a) in einer Menge von 0,1 bis 15 Gew.-%, vorzugsweise von 0,5 bis 10 Gew.-%, besonders bevorzugt von 1 bis 5 Gew.-% in dem Gemisch enthalten ist.7. High-temperature lubricant according to one of the preceding claims, characterized in that the secondary or tertiary calcium phosphate compound (a) in an amount of 0.1 to 15 wt .-%, preferably from 0.5 to 10 wt .-%, especially preferably from 1 to 5 wt .-% is contained in the mixture.
8. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß die Fettsäure bzw. das Fettsäuresalz (b) in einer Menge von 0,1 bis 15 Gew.-%, vorzugsweise von 1 bis 10 Gew.-%, besonders bevorzugt von 3 bis 7 Gew.-% in dem Gemisch enthalten ist.8. High-temperature lubricant according to one of the preceding claims, characterized in that the fatty acid or the fatty acid salt (b) in an amount of 0.1 to 15 wt .-%, preferably from 1 to 10 wt .-%, particularly preferably from 3 to 7% by weight is contained in the mixture.
9. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß Borsäure, Borsäuresalz (Borat) und/oder ein Borsäuresalz (Borat) enthaltendes Mineral (c) in einer Menge von 5 bis 30 Gew.-%, vorzugsweise von 10 bis 25 Gew.- %, besonders bevorzugt von 15 bis 20 Gew.-% in dem Gemisch enthalten ist.9. High-temperature lubricant according to one of the preceding claims, characterized in that boric acid, boric acid (borate) and / or a boric acid (borate) containing mineral (c) in an amount of 5 to 30 wt .-%, preferably from 10 to 25% by weight, more preferably from 15 to 20% by weight, is contained in the mixture.
10. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß Polyphosphat und/oder Pyrophosphat und/oder Metaphosphat (d) in einer Menge von 60 bis 95 Gew.-%, vorzugsweise von 70 bis 85 Gew.-%, besonders bevorzugt von 75 bis 80 Gew.-% in dem Gemisch enthalten ist.10. High-temperature lubricant according to one of the preceding claims, characterized in that polyphosphate and / or pyrophosphate and / or metaphosphate (d) in an amount of 60 to 95 wt .-%, preferably from 70 to 85 wt .-%, especially preferably from 75 to 80 wt .-% is contained in the mixture.
1 1. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß die Bestandteile des Gemischs eine mittlere Korngröße von < 100 μm, vorzugsweise ≤ 50 μm ausweisen.1 1. High-temperature lubricant according to one of the preceding claims, characterized in that the constituents of the mixture have an average particle size of <100 microns, preferably ≤ 50 microns.
12. Hochtemperatur-Schmierstoff nach einem der vorangegangenen Ansprüche, dadurch gekennzeichnet, daß die Bestandteile des Gemischs eine mittlere Korngröße von > 3 μm, vorzugsweise ≥ 10 μm, besonders bevorzugt > 15 μm aufweisen. 12. High-temperature lubricant according to one of the preceding claims, characterized in that the constituents of the mixture have an average particle size of> 3 microns, preferably ≥ 10 microns, more preferably> 15 microns.
EP07765571.0A 2006-06-28 2007-06-22 Graphite-free high-temperature lubricant Not-in-force EP2032679B1 (en)

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EP (2) EP2878661A1 (en)
CN (1) CN101479369B (en)
AR (1) AR061694A1 (en)
DE (1) DE102006030113B4 (en)
ES (1) ES2532847T3 (en)
PL (1) PL2032679T3 (en)
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CN102559337A (en) * 2010-12-28 2012-07-11 张红芬 Lubricating agent for high-temperature core rod and preparation method thereof
DE102013102897A1 (en) 2013-03-21 2014-09-25 Chemische Fabrik Budenheim Kg Composition for protection against scale and as a lubricant for the hot processing of metals
RU2536820C1 (en) * 2013-09-10 2014-12-27 Открытое акционерное общество "Российский научно-исследовательский институт трубной промышленности" (ОАО "РосНИТИ") Product for hot pressure treatment of metals
WO2017112701A1 (en) 2015-12-22 2017-06-29 Zogenix International Limited Metabolism resistant fenfluramine analogs and methods of using the same
RU2020128323A (en) 2015-12-22 2020-10-06 Зодженикс Интернэшнл Лимитед FENFLURAMINE COMPOSITIONS AND METHODS FOR THEIR PREPARATION
IL290727B2 (en) 2016-08-24 2023-12-01 Zogenix International Ltd Formulation for inhibiting formation of 5-ht 2b agonists and methods of using same
CN106544149B (en) * 2016-11-08 2019-10-18 北京科技大学 A kind of liquid-solid mixed lubrication agent and preparation method thereof strengthened based on graphene
FR3064198B1 (en) 2017-03-23 2021-10-01 Air Liquide France Ind DEVICE FOR INJECTING A CRYOGENIC FLUID THROUGH THE BOTTOM OF A MIXER
US10682317B2 (en) 2017-09-26 2020-06-16 Zogenix International Limited Ketogenic diet compatible fenfluramine formulation
JP2021526507A (en) 2018-05-11 2021-10-07 ゾゲニクス インターナショナル リミテッド Compositions and Methods for Treating Sudden Death Induced by Seizures
WO2019241005A1 (en) 2018-06-14 2019-12-19 Zogenix International Limited Compositions and methods for treating respiratory depression with fenfluramine
EP4121500B1 (en) * 2020-03-16 2023-10-18 Chemische Fabrik Budenheim KG Composition for lubricating and/or descaling during hot working of metals
US11612574B2 (en) 2020-07-17 2023-03-28 Zogenix International Limited Method of treating patients infected with severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2)
CN111909762B (en) * 2020-08-18 2022-06-28 烟台开发区阳光工贸有限责任公司 Water-soluble high-temperature-resistant lubricant for hot rolling of steel pipe

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RU2009102453A (en) 2010-08-10
DE102006030113A1 (en) 2008-01-03
AR061694A1 (en) 2008-09-17
CN101479369B (en) 2013-05-01
US8940672B2 (en) 2015-01-27
SI2032679T1 (en) 2015-04-30
RU2458111C2 (en) 2012-08-10
WO2008000700A3 (en) 2008-02-28
US20100298181A1 (en) 2010-11-25
ES2532847T3 (en) 2015-04-01
EP2032679B1 (en) 2015-01-07
DE102006030113B4 (en) 2009-02-12
PL2032679T3 (en) 2015-06-30
EP2878661A1 (en) 2015-06-03
WO2008000700A2 (en) 2008-01-03
CN101479369A (en) 2009-07-08

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