EP0711821B1 - Salt precoat as lubricant carrier for metal forming - Google Patents

Salt precoat as lubricant carrier for metal forming Download PDF

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Publication number
EP0711821B1
EP0711821B1 EP95115908A EP95115908A EP0711821B1 EP 0711821 B1 EP0711821 B1 EP 0711821B1 EP 95115908 A EP95115908 A EP 95115908A EP 95115908 A EP95115908 A EP 95115908A EP 0711821 B1 EP0711821 B1 EP 0711821B1
Authority
EP
European Patent Office
Prior art keywords
salt
lubricant
precoat
acid
weight
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.)
Expired - Lifetime
Application number
EP95115908A
Other languages
German (de)
French (fr)
Other versions
EP0711821A1 (en
Inventor
Klaus-Dieter Nittel
Norbert Schwinke-Kruse
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.)
chemetal GmbH
Original Assignee
Metallgesellschaft AG
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Filing date
Publication date
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Publication of EP0711821A1 publication Critical patent/EP0711821A1/en
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Publication of EP0711821B1 publication Critical patent/EP0711821B1/en
Anticipated expiration legal-status Critical
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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
    • C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/04—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a macromolecular organic compound
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C9/00—Cooling, heating or lubricating drawing material
    • B21C9/02—Selection of compositions therefor
    • 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
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C—CHEMISTRY; METALLURGY
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    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
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    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/22—Carboxylic acids or their salts
    • C10M105/24—Carboxylic acids or their salts having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
    • C—CHEMISTRY; METALLURGY
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    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/22—Carboxylic acids or their salts
    • C10M105/26—Carboxylic acids or their salts having more than one carboxyl group bound to an acyclic carbon atom or cycloaliphatic carbon atom
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    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/20—Lubricating compositions characterised by the base-material being a macromolecular compound containing oxygen
    • C10M107/36—Polysaccharides, e.g. cellulose
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    • C10M2201/061—Carbides; Hydrides; Nitrides
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    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C10M2201/0623—Oxides; Hydroxides; Carbonates or bicarbonates used as base material
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    • C10M2201/0663—Molybdenum sulfide used as base material
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    • C10M2207/1253—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 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
    • 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
    • C10M2207/127—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 polycarboxylic
    • C10M2207/1273—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 polycarboxylic 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
    • 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
    • C10M2207/12—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
    • C10M2207/1293—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/16—Naphthenic acids
    • C10M2207/163—Naphthenic acids 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/18—Tall oil acids
    • C10M2207/183—Tall oil acids 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/20—Rosin acids
    • C10M2207/203—Rosin acids 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
    • 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
    • C10M2207/223—Acids obtained from polymerised unsaturated acids 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/24—Epoxidised acids; Ester derivatives thereof
    • C10M2207/243—Epoxidised acids; Ester derivatives thereof 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
    • 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
    • C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
    • C10M2209/123—Polysaccharides, e.g. cellulose, biopolymers used as base material
    • 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

Definitions

  • the invention relates to a lubricant carrier salt for relief the cold forming of workpieces made of iron or steel on the basis Boric acid and / or alkali borate and a method for relief the cold forming of workpieces made of iron or steel with the help this lubricant carrier salt.
  • Lubricants are also known which consist of neutral grease and / or oil, Alkali metal soap and alkali metal salt of boric acid exist (DE-B-23 30 806), alkali borate, alkali sulfate and silicate as well as chloride contain (GB 1 561 836) or a content of water-soluble Metal soap, alkali metal chloride, alkali metal sulfate and Have alkali metal borate (GB-A-2 003 923).
  • lubricant carrier salts are, for example, lime (Ca (OH) 2 ), iron hydroxide (Fe (OH) 2 ) and borax (Na 2 B 4 O 7 • 10 H 2 O) (D. Oppen "Chemical surface treatment as a means to facilitate cold forming” , Metall Structure (1982), pages 566 ff).
  • Borax in particular allows a high drawing speed.
  • its hygroscopicity is disadvantageous, so that the Drawability, e.g. of the wire, falls off and rust formation on the Wire surface is to be determined.
  • the reason for the loss Drawability is the one associated with increasing water absorption Loss of liability.
  • Another problem lies in the subsequent one Drying. E.g. the wire dries up, i.e. becomes from the applied borax the crystal water completely or only partially expelled, the borax layer loses its adhesion to the wire. The Drawability is no longer given.
  • the object of the invention is to provide a lubricant carrier salt Facilitating the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate provide the disadvantages of the known Does not have lubricant carrier salts, especially insensitive compared to the drying process and not after application or is only slightly hygroscopic.
  • the object is achieved by further developing the lubricant carrier salt of the type mentioned at the outset in accordance with the invention such that it contains aliphatic di- or tricarboxylic acid which is either unsubstituted or substituted by at least one OH group and / or an alkali salt thereof wherein the weight ratio of boric acid / alkali borate (calculated as H 3 BO 3 ) to carboxylic acid (calculated as citric acid) (5 to 15): 1.
  • aliphatic di- or tricarboxylic acid which is either unsubstituted or substituted by at least one OH group
  • carboxylic acid used must have at least one substitutable CH 2 or CH group.
  • di- or tricarboxylic acids are malonic acid, Maleic acid, succinic acid, tartaric acid and / or citric acid.
  • the lubricant carrier salt according to the invention should carboxylic acids used have a melting point above Have 100 ° C.
  • the film thickness of the applied lubricant carrier salt Another is to be able to set within certain limits advantageous embodiment of the invention, a Use lubricant carrier salt, which has an additional content of inorganic or organic thickener, preferably in Quantities from 0.5 to 5% by weight (based on the formulated Lubricant carrier salt).
  • Particularly suitable Thickeners are bentonite and / or polysaccharide.
  • Another advantageous embodiment of the invention consists in apply a lubricant carrier salt, which an additional Content of aluminate and / or silicate, preferably of metasilicate and / or disilicate, in amounts of 1 to 10% by weight (based on the ready-formulated lubricant carrier salt). This will achieved that applied to the workpiece Lubricant carrier salt receives a defined roughness and thus a defined amount of lubricant in the forming tool transported.
  • lubricant carrier salt which has an additional content dispersants, lubricants and / or rust inhibitors, preferably Soap, in a total amount of 2 to 15% by weight (based on the formulated lubricant carrier salt) and / or one additional content of titanium salt, preferably titanium phosphate, in Quantities from 10 to 100 mg / kg of lubricant carrier salt (calculated as Titanium).
  • additional content dispersants, lubricants and / or rust inhibitors preferably Soap
  • titanium salt preferably titanium phosphate
  • the lubricant carrier salts according to the invention are usually in the form of an aqueous solution or dispersion on the workpieces upset. Accordingly, a method is part of the invention to facilitate the cold forming of workpieces made of iron or Steel, which is characterized in that the Lubricant carrier salt with an aqueous solution or dispersion a concentration of 5 to 30% by weight and with a temperature of 80 to 100 ° C is applied by dipping or continuous process.
  • the application of the lubricant carrier salt can be applied to the bare Metal surface.
  • it is particularly useful according to a further advantageous embodiment of the inventive method before applying the Lubricant carrier salt with the workpieces made of iron or steel to be provided with a phosphate coating. This will e.g. at Multiple moves make contact between workpiece and tool effective prevented.
  • the invention is particularly suitable for wire drawing Cold upsetting, extrusion and ironing. Your special advantages are that it is on the workpieces applied lubricant carrier salt insensitive to one Over-drying is and practically no hygroscopic properties shows. The maximum water absorption after drying is 2% by weight.
  • a 15% by weight aqueous solution was prepared from the above-mentioned lubricant carrier salt, in which bundles of steel wire were immersed for 10 minutes at a temperature of 90 ° C. Following the immersion treatment, drying was carried out at 150 ° C. in a forced air oven. Due to the pretreatment mentioned, the steel wire had a lubricant carrier salt coating with a layer weight of 6 g / m 2 . After applying soap in front of the drawing die, the wire, which had an initial diameter of 5.5 mm, was formed in eight passes at a drawing speed of 8 m / sec to a final diameter of 1.9 mm. These results were reproducibly achieved with changing storage times of the wire coated with the lubricant carrier salt and partial overdrying.
  • the basis weight of the phosphate coating produced with the phosphating solution was 10 g / m 2 .
  • the lubricant carrier salt was applied from a 25% by weight solution heated to 90 ° C. in a continuous process, the contact time between steel wire and solution of the lubricant carrier salt being 15 seconds.
  • the lubricant carrier salt applied in this way had a weight of 4 g / m 2 .
  • the steel wire was then applied before the Drawing die in six passes at 6 m / sec from an initial 6 mm to 3.5 mm reshaped. Again, with different storage times and partial overdrying achieves reproducible results.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

Lubricant carrier salt is based on boric acid and/or alkali borate and contains aliphatic di- or tri-carboxylic acid (non)substd. by at least one OH group and their alkali salts The wt. ratio of boric acid/alkali borate (calc. as H3BO3) to carboxylic acid (calc. as citric acid) is 5-15:1. Also claimed is a process for facilitating cold forming of iron or steel workpieces, in which the lubricant carrier salt is applied as an aq. soln. or dispersion in a concn. of 5-30 wt. % and at 80-100 degrees C, to form a phosphate coating.

Description

Die Erfindung betrifft ein Schmiermittelträgersalz zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl auf Basis Borsäure und/oder Alkaliborat sowie ein Verfahren zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl mit Hilfe dieses Schmiermittelträgersalzes.The invention relates to a lubricant carrier salt for relief the cold forming of workpieces made of iron or steel on the basis Boric acid and / or alkali borate and a method for relief the cold forming of workpieces made of iron or steel with the help this lubricant carrier salt.

Es ist bekannt, die Kaltumformung von metallischen Werkstücken durch Verwendung von fettsauren Salzen (Seifen) zu erleichtern. Diese werden häufig in Form heißer, wäßriger Seifenlösungen auf die umzuformenden Werkstücke aufgebracht. In manchen Fällen, insbesondere wenn schwere Verformungsoperationen durchgeführt werden sollen, pflegt man vor der Aufbringung des Schmiermittels einen chemischen Überzug auf die Metalloberfläche aufzubringen, z.B. einen Phosphat-, Oxid-, Oxalat- oder Sulfidüberzug. In beiden Fällen, d.h. bei Aufbringung des Schmiermittels auf das blanke Werkstück oder auf das zuvor mit einem chemischen Überzug versehene Werkstück, soll das Schmiermittel einen gleichmäßigen Film ausbilden, der eine gute Trennschicht zwischen Werkstück und Werkzeug während der Umformungsbehandlung bildet.It is known to carry out the cold forming of metallic workpieces Facilitate use of fatty acid salts (soaps). This are often in the form of hot, aqueous soap solutions on the Workpieces to be formed applied. In some cases, especially if severe deformation operations are to be performed, maintain a chemical before applying the lubricant Apply coating to the metal surface, e.g. a phosphate, Oxide, oxalate or sulfide coating. In both cases, i.e. at Applying the lubricant to the bare workpiece or to the Workpiece previously provided with a chemical coating should do that Lubricants form an even film that is a good one Interface between workpiece and tool during the Forming treatment forms.

Neben der Applikation von Seifen auf blanke oder zuvor mit einem Konversionsüberzug versehene Werkstücke ist es auch bekannt, Schmiermittel zur Erleichterung der Kaltumformung einzusetzen, die ein Gemisch aus fettsauren Salzen und Alkalipyrophosphat und/oder Alkalitetraborat darstellen (DE-A-1 594 512). Hierbei soll ein Teil der Seifen fettsaures Salz von Lithium, Kalium, Ammonium, Calcium, Mangesium, Zink und/oder Aluminium sein.In addition to the application of soaps on bare or previously with a Conversion-coated workpieces, it is also known Use lubricants to facilitate cold forming, which a mixture of fatty acid salts and alkali pyrophosphate and / or Alkali tetraborate represent (DE-A-1 594 512). Here is a part the soaps fatty acid salt of lithium, potassium, ammonium, calcium, Mangesium, zinc and / or aluminum.

Auch sind Schmiermittel bekannt, die aus Neutralfett und/oder Öl, Alkalimetallseife sowie Alkalimetallsalz von Borsäure bestehen (DE-B-23 30 806), Alkaliborat, Alkalisulfat und Silikat sowie Chlorid enthalten (GB 1 561 836) oder aber einen Gehalt an wasserlöslicher Metallseife, Alkalimetallchlorid, Alkalimetallsulfat und Alkalimetallborat aufweisen (GB-A-2 003 923).Lubricants are also known which consist of neutral grease and / or oil, Alkali metal soap and alkali metal salt of boric acid exist (DE-B-23 30 806), alkali borate, alkali sulfate and silicate as well as chloride contain (GB 1 561 836) or a content of water-soluble Metal soap, alkali metal chloride, alkali metal sulfate and Have alkali metal borate (GB-A-2 003 923).

Weiterhin ist es bekannt, auf metallische Werkstücke sogenannte Schmiermittelträgersalze aufzubringen, die selbst nicht als Schmiermittel wirken, sondern eine Nachbehandlung z.B. durch Beseifung an der Ziehmaschine erfahren. Derartige Schmiermittelträgersalze sind beispielsweise Kalk (Ca(OH)2), Eisenhydroxid (Fe(OH)2) und Borax (Na2B4O7 • 10 H2O) (D. Oppen "Chemische Oberflächenbehandlung als Mittel zur Erleichterung der Kaltumformung", Metalloberfläche (1982), Seiten 566 ff).Furthermore, it is known to apply so-called lubricant carrier salts to metallic workpieces, which do not themselves act as lubricants, but rather undergo post-treatment, for example by soaping on the drawing machine. Such lubricant carrier salts are, for example, lime (Ca (OH) 2 ), iron hydroxide (Fe (OH) 2 ) and borax (Na 2 B 4 O 7 • 10 H 2 O) (D. Oppen "Chemical surface treatment as a means to facilitate cold forming" , Metallfläche (1982), pages 566 ff).

Insbesondere Borax erlaubt zwar eine hohe Ziehgeschwindigkeit. Nachteilig ist jedoch seine Hygroskopizität, so daß die Ziehfähigkeit, z.B. des Drahtes, abfällt und eine Rostbildung auf der Drahtoberfläche festzustellen ist. Der Grund für den Verlust an Ziehfähigkeit ist der mit der steigenden Wasseraufnahme verbundene Abfall der Haftung. Ein weiteres Problem liegt in der anschließenden Trocknung. Wird z.B. der Draht übertrocknet, d.h. wird aus dem aufgebrachten Borax das Kristallwasser ganz oder auch nur teilweise ausgetrieben, verliert die Boraxschicht ihre Haftung zum Draht. Die Ziehfähigkeit ist damit nicht mehr gegeben.Borax in particular allows a high drawing speed. However, its hygroscopicity is disadvantageous, so that the Drawability, e.g. of the wire, falls off and rust formation on the Wire surface is to be determined. The reason for the loss Drawability is the one associated with increasing water absorption Loss of liability. Another problem lies in the subsequent one Drying. E.g. the wire dries up, i.e. becomes from the applied borax the crystal water completely or only partially expelled, the borax layer loses its adhesion to the wire. The Drawability is no longer given.

Aufgabe der Erfindung ist es, ein Schmiermittelträgersalz zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl auf Basis Borsäure und/oder Alkaliborat bereitzustellen, das die Nachteile der bekannten Schmiermittelträgersalze nicht aufweist, insbesondere unempfindlich gegenüber dem Trockenprozeß ist und nach der Applikation nicht bzw. nur geringfügig hygroskopisch ist.The object of the invention is to provide a lubricant carrier salt Facilitating the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate provide the disadvantages of the known Does not have lubricant carrier salts, especially insensitive compared to the drying process and not after application or is only slightly hygroscopic.

Die Aufgabe wird gelöst, indem das Schmiermittelträgersalz der eingangs genannten Art entsprechend der Erfindung derart weitergebildet wird, daß es einen Gehalt an aliphatischer Di- oder Tricarbonsäure, die entweder nicht substituiert oder durch mindestens eine OH-Gruppe substituiert ist, und/oder ein Alkalisalz hiervon aufweist, wobei das Gewichtsverhältnis von Borsäure/Alkaliborat (berechnet als H3BO3) zu Carbonsäure (berechnet als Zitronensäure) (5 bis 15) : 1 beträgt.The object is achieved by further developing the lubricant carrier salt of the type mentioned at the outset in accordance with the invention such that it contains aliphatic di- or tricarboxylic acid which is either unsubstituted or substituted by at least one OH group and / or an alkali salt thereof wherein the weight ratio of boric acid / alkali borate (calculated as H 3 BO 3 ) to carboxylic acid (calculated as citric acid) (5 to 15): 1.

Die vorstehend verwendete Formulierung "aliphatische Di- oder Tricarbonsäure, die entweder nicht substituiert oder durch mindestens eine OH-Gruppe substituiert ist" bedeutet, daß die verwendete Carbonsäure mindestens eine substituierbare CH2- oder CH-Gruppe aufweisen muß.The wording used above "aliphatic di- or tricarboxylic acid which is either unsubstituted or substituted by at least one OH group" means that the carboxylic acid used must have at least one substitutable CH 2 or CH group.

Besonders geeignete Di- bzw. Tricarbonsäuren sind Malonsäure, Maleinsäure, Bernsteinsäure, Weinsäure und/oder Zitronensäure. Insbesondere sollten die im erfindungsgemäßen Schmiermittelträgersalz zum Einsatz gelangenden Carbonsäuren einen Schmelzpunkt oberhalb 100°C aufweisen.Particularly suitable di- or tricarboxylic acids are malonic acid, Maleic acid, succinic acid, tartaric acid and / or citric acid. In particular, the lubricant carrier salt according to the invention should carboxylic acids used have a melting point above Have 100 ° C.

Um die Filmdicke des aufgebrachten Schmiermittelträgersalzes innerhalb bestimmter Grenzen einstellen zu können, sieht eine weitere vorteilhafte Ausgestaltung der Erfindung vor, ein Schmiermittelträgersalz einzusetzen, das einen zusätzlichen Gehalt an anorganischem oder organischem Verdickungsmittel, vorzugsweise in Mengen von 0,5 bis 5 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz), aufweist. Besonders geeignete Verdickungsmittel sind Bentonit und/oder Polysaccharid. The film thickness of the applied lubricant carrier salt Another is to be able to set within certain limits advantageous embodiment of the invention, a Use lubricant carrier salt, which has an additional content of inorganic or organic thickener, preferably in Quantities from 0.5 to 5% by weight (based on the formulated Lubricant carrier salt). Particularly suitable Thickeners are bentonite and / or polysaccharide.

Eine weitere vorteilhafte Ausgestaltung der Erfindung besteht darin, ein Schmiermittelträgersalz aufzubringen, das einen zusätzlichen Gehalt an Aluminat und/oder Silikat, vorzugsweise von Metasilikat und/oder Disilikat, in Mengen von 1 bis 10 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz) aufweist. Hierdurch wird erreicht, daß das auf das Werkstück aufgebrachte Schmiermittelträgersalz eine definierte Rauhigkeit erhält und damit eine definierte Schmiermittelmenge in das Umformungswerkzeug transportiert.Another advantageous embodiment of the invention consists in apply a lubricant carrier salt, which an additional Content of aluminate and / or silicate, preferably of metasilicate and / or disilicate, in amounts of 1 to 10% by weight (based on the ready-formulated lubricant carrier salt). This will achieved that applied to the workpiece Lubricant carrier salt receives a defined roughness and thus a defined amount of lubricant in the forming tool transported.

Schließlich ist es von Vorteil, auf die Werkstücke ein Schmiermittelträgersalz zu applizieren, das einen zusätzlichen Gehalt an Dispergier-, Gleit- und/oder Rostschutzmitteln, vorzugsweise Seife, in einer Gesamtmenge von 2 bis 15 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz) und/oder einen zusätzlichen Gehalt an Titansalz, vorzugsweise an Titanphosphat, in Mengen von 10 bis 100 mg/kg Schmiermittelträgersalz (berechnet als Titan) besitzt. Die besonderen Vorzüge derartiger Zusätze bestehen darin, daß der Kontakt Werkstück/Werkzeug besonders effektiv verhindert wird.Finally, it is advantageous to work on the workpieces Apply lubricant carrier salt, which has an additional content dispersants, lubricants and / or rust inhibitors, preferably Soap, in a total amount of 2 to 15% by weight (based on the formulated lubricant carrier salt) and / or one additional content of titanium salt, preferably titanium phosphate, in Quantities from 10 to 100 mg / kg of lubricant carrier salt (calculated as Titanium). The special advantages of such additives exist in that the workpiece / tool contact is particularly effective is prevented.

Die erfindungsgemäßen Schmiermittelträgersalze werden üblicherweise in Form einer wäßrigen Lösung oder Dispersion auf die Werkstücke aufgebracht. Demzufolge ist Bestandteil der Erfindung ein Verfahren zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl, das dadurch gekennzeichnet ist, daß das Schmiermittelträgersalz aus einer wäßrigen Lösung oder Dispersion mit einer Konzentration von 5 bis 30 Gew.% und mit einer Temperatur von 80 bis 100°C im Tauchen oder Durchlaufverfahren aufgebracht wird.The lubricant carrier salts according to the invention are usually in the form of an aqueous solution or dispersion on the workpieces upset. Accordingly, a method is part of the invention to facilitate the cold forming of workpieces made of iron or Steel, which is characterized in that the Lubricant carrier salt with an aqueous solution or dispersion a concentration of 5 to 30% by weight and with a temperature of 80 to 100 ° C is applied by dipping or continuous process.

Die Applikation des Schmiermittelträgersalzes kann auf die blanke Metalloberfläche erfolgen. Besonders zweckmäßig ist es jedoch entsprechend einer weiteren vorteilhaften Ausgestaltung des erfindungsgemäßen Verfahrens, vor der Aufbringung des Schmiermittelträgersalzes die Werkstücke aus Eisen oder Stahl mit einem Phosphatüberzug zu versehen. Hierdurch wird z.B. bei Mehrfachzügen ein Kontakt zwischen Werkstück und Werkzeug wirksam verhindert.The application of the lubricant carrier salt can be applied to the bare Metal surface. However, it is particularly useful according to a further advantageous embodiment of the inventive method, before applying the Lubricant carrier salt with the workpieces made of iron or steel to be provided with a phosphate coating. This will e.g. at Multiple moves make contact between workpiece and tool effective prevented.

Die Erfindung eignet sich insbesondere zum Drahtzug, zum Kaltstauchen, zum Fließpressen und zum Abstreckziehen. Ihre besonderen Vorzüge liegen darin, daß das auf die Werkstücke aufgebrachte Schmiermittelträgersalz unempfindlich gegenüber einer Übertrocknung ist und praktisch keine hygroskopischen Eigenschaften zeigt. Die maximale Wasseraufnahme nach der erfolgten Trocknung beträgt 2 Gew.%.The invention is particularly suitable for wire drawing Cold upsetting, extrusion and ironing. Your special advantages are that it is on the workpieces applied lubricant carrier salt insensitive to one Over-drying is and practically no hygroscopic properties shows. The maximum water absorption after drying is 2% by weight.

Die Erfindung wird anhand der nachfolgenden Beispiele beispielsweise und näher erläutert.The invention is illustrated by the examples below and explained in more detail.

Beispiel 1example 1

Zum Einsatz gelangte ein Schmiermittelträgersalz, das folgende Bestandteile aufwies:

  • 50 Gew.% Borsäure (H3BO3)
  • 15 Gew.% Kaliumborat (K2B4O7•4H2O)
  • 10 Gew.% Natriumborat (Neobor, Na2B4O7•5H2O)
  • 5 Gew.% Natriumdisilikat (Na2Si2O5•xH2O)
  • 10 Gew.% Zitronensäure
  • 10 Gew.% Natriumstearat.
    • A lubricant carrier salt was used, which had the following components:
  • 50% by weight boric acid (H 3 BO 3 )
  • 15% by weight potassium borate (K 2 B 4 O 7 • 4H 2 O)
  • 10% by weight sodium borate (Neobor, Na 2 B 4 O 7 • 5H 2 O)
  • 5% by weight sodium disilicate (Na 2 Si 2 O 5 • xH 2 O)
  • 10% by weight of citric acid
  • 10% by weight sodium stearate.

    • Aus dem vorstehend genannten Schmiermittelträgersalz wurde eine 15 Gew.%ige wäßrige Lösung hergestellt, in der Bunde aus Stahldraht bei einer Temperatur von 90°C 10 min im Tauchen behandelt wurden. Im Anschluß an die Tauchbehandlung erfolgte eine Trocknung bei 150°C im Umluftofen. Der Stahldraht hatte aufgrund der genannten Vorbehandlung eine Schmiermittelträgersalzauflage mit einem Schichtgewicht von 6 g/m2. Nach dem Auftrag von Seife vor dem Ziehstein wurde der Draht, der einen anfänglichen Durchmesser von 5,5 mm hatte, in acht Zügen mit einer Ziehgeschwindigkeit von 8 m/sec auf einen Enddurchmesser von 1,9 mm umgeformt. Diese Ergebnisse wurden bei wechselnden Lagerzeiten des mit dem Schmiermittelträgersalz beschichteten Drahtes und teilweiser Übertrocknung reproduzierbar erreicht.A 15% by weight aqueous solution was prepared from the above-mentioned lubricant carrier salt, in which bundles of steel wire were immersed for 10 minutes at a temperature of 90 ° C. Following the immersion treatment, drying was carried out at 150 ° C. in a forced air oven. Due to the pretreatment mentioned, the steel wire had a lubricant carrier salt coating with a layer weight of 6 g / m 2 . After applying soap in front of the drawing die, the wire, which had an initial diameter of 5.5 mm, was formed in eight passes at a drawing speed of 8 m / sec to a final diameter of 1.9 mm. These results were reproducibly achieved with changing storage times of the wire coated with the lubricant carrier salt and partial overdrying.

    Beispiel 2Example 2

    Zur Vorbereitung von ebenfalls Stahldrähten wurde ein Schmiermittelträgersalz eingesetzt, das folgende Bestandteile enthielt:

  • 40 Gew.% Borsäure (H3BO3)
  • 35 Gew.% Kaliumborat (K2B4O7•4H2O)
  • 2,9 Gew.% Natriumdisilikat (Na2Si2O5•xH2O)
  • 10 Gew.% Zitronensäure
  • 0,1 Gew.% Titanylsulfat
  • 5 Gew.% Polysaccharid
  • 7 Gew.% Kaliumoleat.
    • A lubricant carrier salt was used to prepare steel wires, which contained the following components:
  • 40% by weight boric acid (H 3 BO 3 )
  • 35% by weight potassium borate (K 2 B 4 O 7 • 4H 2 O)
  • 2.9% by weight sodium disilicate (Na 2 Si 2 O 5 • xH 2 O)
  • 10% by weight of citric acid
  • 0.1% by weight of titanyl sulfate
  • 5% by weight polysaccharide
  • 7% by weight potassium oleate.

    • Vor der Aufbringung des Schmiermittelträgersalzes war der Stahldraht im Tauchen mit Hilfe von Salzsäure von Rost und Zunder befreit und nach gründlicher Wasserspülung 6 bis 10 min bei 45°C phosphatiert worden. Die Zusammensetzung der Phosphatierungslösung betrug:

  • 10,9 g/l Zink,
  • 2,1 g/l Mangan,
  • 2,0 g/l Eisen(II),
  • 0,5 g/l Calcium,
  • 0,5 g/l Nickel,
  • 0,01 g/l Kupfer,
  • 0,3 g/l Natrium,
  • 24,0 g/l Nitrat,
  • 10,6 g/l Phosphat (berechnet als P2O5),
  • 1,6 g/l Tetrafluoroborat,
  • 1,6 g/l Weinsäure und
  • 0,5 g/l Harnstoff.
    • Before the lubricant carrier salt was applied, the steel wire was freed of rust and scale by dipping with hydrochloric acid and phosphated at 45 ° C. for 6 to 10 minutes after thorough water rinsing. The composition of the phosphating solution was:
  • 10.9 g / l zinc,
  • 2.1 g / l manganese,
  • 2.0 g / l iron (II),
  • 0.5 g / l calcium,
  • 0.5 g / l nickel,
  • 0.01 g / l copper,
  • 0.3 g / l sodium,
  • 24.0 g / l nitrate,
  • 10.6 g / l phosphate (calculated as P 2 O 5 ),
  • 1.6 g / l tetrafluoroborate,
  • 1.6 g / l tartaric acid and
  • 0.5 g / l urea.

    • Das mit der Phosphatierungslösung erzeugte Flächengewicht des Phosphatüberzuges betrug 10 g/m2.The basis weight of the phosphate coating produced with the phosphating solution was 10 g / m 2 .

    Die Applikation des Schmiermittelträgersalzes erfolgte aus einer 25 Gew.%igen, auf 90°C erwärmten Lösung im Durchlaufverfahren, wobei die Kontaktdauer zwischen Stahldraht und Lösung des Schmiermittelträgersalzes 15 sec betrug. Das auf diese Weise aufgebrachte Schmiermittelträgersalz hatte ein Gewicht von 4 g/m2.The lubricant carrier salt was applied from a 25% by weight solution heated to 90 ° C. in a continuous process, the contact time between steel wire and solution of the lubricant carrier salt being 15 seconds. The lubricant carrier salt applied in this way had a weight of 4 g / m 2 .

    Anschließend wurde der Stahldraht nach Seifenauftrag vor dem Ziehstein in sechs Zügen mit 6 m/sec von anfänglich 6 mm auf 3,5 mm umgeformt. Auch hier wurden bei unterschiedlichen Lagerzeiten und teilweiser Übertrocknung reproduzierbare Ergebnisse erzielt.The steel wire was then applied before the Drawing die in six passes at 6 m / sec from an initial 6 mm to 3.5 mm reshaped. Again, with different storage times and partial overdrying achieves reproducible results.

    Claims (9)

    1. Lubricant salt precoat for facilitating the cold forming of work pieces made of iron or steel, based on boric acid and/or alkali borate, characterised by a content of aliphatic dicarboxylic or tricarboxylic acid having at least one CH2- or CH group, which is either not substituted or is substituted by at least one OH group, and/or of alkali salts thereof, wherein the weight ratio of boric acid/alkali borate (calculated as H3BO3) to carboxylic acid (calculated as citric acid) amounts to (5 to 15) : 1.
    2. Lubricant salt precoat according to claim 1, characterised by a content of malonic acid, maleic acid, succinic acid, tartaric acid and/or citric acid.
    3. Lubricant salt precoat according to claim 1 or 2, characterised by an additional content of inorganic or organic thickening agent, preferably in amounts of 0.5 to 5% by weight (with respect to the completely formulated lubricant salt precoat).
    4. Lubricant salt precoat according to claim 3, characterised by a content of bentonite and/or polysaccharide as thickening agent.
    5. Lubricant salt precoat according to one or more of claims 1 to 4, characterised by an additional content of aluminate and/or silicate, preferably metasilicate and/or disilicate, in amounts of 1 to 10% by weight (with respect to the completely formulated lubricant salt precoat).
    6. Lubricant salt precoat according to one or more of claims 1 to 5, characterised by an additional content of dispersing, lubricating and/or anti-rust agents, preferably of soap, in a total amount of 2 to 15% by weight (with respect to the completely formulated lubricant salt precoat).
    7. Lubricant salt precoat according to one or more of claims 1 to 6, characterised by an additional content of titanium salt, preferably titanium phosphate, in amounts, (calculated as titanium) of 10 to 100 mg/kg lubricant salt precoat.
    8. Method for facilitating the cold forming of work pieces made of iron or steel, characterised in that the lubricant salt precoat in accordance with one or more of claims 1 to 7 is applied from an aqueous solution or dispersion with a concentration of 5 to 30% by weight and with a temperature of 80 to 100°C in immersion or in a continuous operation.
    9. Method according to claim 8, characterised in that before the application of the lubricant salt precoat, a phosphate coating is generated on the work pieces made of iron or steel.
    EP95115908A 1994-11-11 1995-10-10 Salt precoat as lubricant carrier for metal forming Expired - Lifetime EP0711821B1 (en)

    Applications Claiming Priority (2)

    Application Number Priority Date Filing Date Title
    DE4440301A DE4440301A1 (en) 1994-11-11 1994-11-11 Lubricant carrier salt for metal forming
    DE4440301 1994-11-11

    Publications (2)

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    EP0711821A1 EP0711821A1 (en) 1996-05-15
    EP0711821B1 true EP0711821B1 (en) 2000-05-17

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    EP (1) EP0711821B1 (en)
    AT (1) ATE193049T1 (en)
    DE (2) DE4440301A1 (en)
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    UY24689A1 (en) * 1996-08-30 1997-09-08 Solutia Inc NEW WATER-SOLUBLE FLUIDS FOR METAL MACHINING
    USH2142H1 (en) * 1998-01-29 2006-01-03 Edward Elizondo Method for measuring the concentration of bodymaker lubricant in bodymaker coolant
    US6376433B1 (en) * 1999-07-13 2002-04-23 Century Chemical Corporation Process and product for lubricating metal prior to cold forming
    BR0113641A (en) * 2000-09-05 2003-10-14 Honda Motor Co Ltd Process-type aqueous lubricant used for highly efficient cold forging
    US7811975B2 (en) * 2002-10-25 2010-10-12 Ali Erdemir Metalworking and machining fluids
    US8082767B2 (en) * 2006-03-27 2011-12-27 Sumitomo Metal Industries, Ltd. Lubricant for hot metal working and powder lubricant composition for hot metal working
    TWI457432B (en) 2008-01-30 2014-10-21 Chemetall Gmbh Process for coating metallic surface with a wax-coataining lubricant composition
    TWI457433B (en) * 2008-01-30 2014-10-21 Chemetall Gmbh Process for coating metallic surfaces with a phosphate layer and then with a polymer lubricant layer
    TWI457431B (en) * 2008-01-30 2014-10-21 Chemetall Gmbh Process for coating a metallic surface with a lubricant composition
    CN114317077A (en) * 2021-12-23 2022-04-12 南京华舜润滑制品有限公司 Production process of wire-drawing lubricating powder
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    US5584945A (en) 1996-12-17
    DE4440301A1 (en) 1996-05-15
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    DE59508345D1 (en) 2000-06-21
    EP0711821A1 (en) 1996-05-15

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