EP0218989A2 - Method for suspending solid lubricants - Google Patents

Method for suspending solid lubricants Download PDF

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Publication number
EP0218989A2
EP0218989A2 EP86113474A EP86113474A EP0218989A2 EP 0218989 A2 EP0218989 A2 EP 0218989A2 EP 86113474 A EP86113474 A EP 86113474A EP 86113474 A EP86113474 A EP 86113474A EP 0218989 A2 EP0218989 A2 EP 0218989A2
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Prior art keywords
colloid mill
water
mixer
sec
suspension
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EP86113474A
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German (de)
French (fr)
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EP0218989B1 (en
EP0218989A3 (en
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Hans-Rudolf Staub
Hansjörg Furrer
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Lonza AG
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Lonza AG
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80Mixing plants; Combinations of mixers
    • B01F33/82Combinations of dissimilar mixers
    • B01F33/821Combinations of dissimilar mixers with consecutive receptacles

Definitions

  • the invention relates to a method for suspending solid lubricants which are used in the non-cutting hot forming of metals, containing graphite and polymers in water as the carrier liquid.
  • solid lubricants for non-cutting metal forming at high temperatures are known, containing graphite, polymers, suspension aids and optionally other aids, such as bactericides, which form a suspension with water.
  • the addition of the bactericides is necessary to avoid bacterial decomposition of the solid lubricant suspension during storage;
  • the suspension auxiliaries serve the purpose of keeping the liquid and solid constituents in a homogeneous mixture even over long periods.
  • the solid lubricant suspension is used up during processing, ie the water evaporates on the tool of the workpieces, the polymer component burns off.
  • the bactericidal additives When processing the solid lubricants, the bactericidal additives are also subject to evaporation, which is undesirable in view of their possible toxicity and together with the suspension aids they form a not inconsiderable non-lubricating part of the solid lubricant formulation.
  • the object of the present invention was to propose a method which makes it possible to in a homogeneous and stable solid lubricant suspension containing a carrier liquid usually water, graphite and polymers to be produced directly at the point of use, without the addition of bactericides and with the lowest possible level of suspension aids.
  • a carrier liquid usually water, graphite and polymers
  • the dry, premixed components of the solid lubricant and the water can be combined in the colloid mill.
  • the mixture of graphite, the polymer and any additives, such as suspension aids, film stabilizers, and optionally also wetting agents and inorganic additives, is referred to as dry, premixed constituents.
  • additives such as e.g. Wetting agents, solvents, film formers, pH stabilizers, soluble inorganic salts (e.g. phosphates) etc. should be added beforehand.
  • the water optionally with the additives mentioned, such as suspensions Sion aids, wetting agents or solvents, etc.
  • the polymer for example as a plastic dispersion
  • this mixture is fed in the colloid mill with the graphite, which is optionally homogeneously mixed with, for example, suspension aids, film stabilizers, etc.
  • the gap between the rotor and housing can be 0.01 to 3 mm; the peripheral speed, calculated from the rotor circumference and speed, can range from 10 to 40 m / sec. be.
  • Suspensions with a solids content of 1 to 70% by weight can be prepared by the process according to the invention.
  • the possibility of achieving such high solids contents in the suspension was more surprising to us than the individual components of the solid lubricant have very low bulk densities. These are 0.2 to 0.5 kg / l for graphite, 0.2 to 0.7 kg / l for the polymers and additives and, for example, 0.2 to 0.5 kg / l for a typical dry mixture .
  • the volume of the solid lubricant is greater than the volume required to produce the suspension.
  • the residence time of the components in the mixing area of the colloid mill is expediently in the range from 0.01 to 5 seconds.
  • Suitable intensive mixers are expediently mixers with at least one co-rotating impeller shaft or counter-rotating impeller shafts, agitator ball mills, guide jet mixers or screw mixers, preferably in a cascade arrangement. If the constituents, ie the solid lubricant and the water, were mixed to form the solid lubricant suspension, for example, only in an intensive mixer, lump formation and inhomogeneity in the suspension could neither be avoided nor eliminated.
  • Solid lubricants to be produced by the process according to the invention are known, for example, from CH-PS 596 294 and 609 728. Accordingly, the starting materials used are at least one solid lubricant, preferably graphite, in particular those graphites with high purity, for example over 90%, and an average grain size of no more than 300 microns. The best results can be achieved with the graphite of 96 to 99.5% purity and an average grain size of 100 micrometers. If appropriate, the use of molybdenum disulfide, CaF 2 or BN alone or in a mixture with graphite is conceivable in the context of the present invention.
  • Polymers are understood as meaning the organic products which decompose without leaving any heat, for example alkylene homopolymers or copolymers. These include the homo- and copolymers of alkenes (monoolefins, diolefins, etc.), vinyls ters, vinyl alcohols, unsaturated dibasic acids and esters (dicarboxylic acids and esters), alkyl esters and acyclic acids and esters.
  • the alkylene homopolymer or copolymer can be polyethylene, polymethyl methacrylate, polystyrene, polybutadiene, polyvinyl acetate, polyvinyl propionate, a copolymer of methyl methacrylate and styrene, a copolymer of methyl methacrylate and alphamethylstyrene, polydiallyl phthalate, polypropylene, a copolymer of styrene and butadiene, and polymethyl methacrylate Dibutyl maleate, a copolymer of vinyl acetate and ethylene and polyisobutylene.
  • the polymers mentioned can be used alone or in a mixture with one another dry or, if appropriate, as a dispersion.
  • substances from the group of polysaccharides such as starch, celluloses, inulin, glycogen agar, levan, dichinone, pectin, lignin and araban can be used as suspension aids.
  • Methyl, ethyl, propyl and butyl celluloses, or alginates such as sodium alginate, potassium alginate, propylene glycol alginate and ammonium alginate, or mixtures of the substances can be used.
  • the solid lubricant When used, the solid lubricant should be present as a 1 to 70% by weight homogeneous aqueous dispersion and have a viscosity of 100 to 30,000 cp at 5 to 50 ° C.
  • an organic stabilizer which may be present in the solid lubricant may also be sufficient.
  • a thickener e.g. water-soluble polysaccharides, alkyl celluloses, polyvinyl alcohols, polyarylates, polyvinyl pyrrolidone, optionally also inorganic substances, in particular minerals, such as clays or silica.
  • additives can be inorganic additives and selected from the range of boron compounds, polyphosphates and alkali silicates, alone or as a mixture with one another. These compounds include polyphosphate in insoluble or poorly soluble form. Madrell's salts or Kurrol's salts are preferably used as polyphosphates. These are compounds of the type (Na PO 3 ) n with n - 6 to 50,000, preferably 6 - 10,000. The boron compound can be used in soluble and preferably in poorly soluble or insoluble form.
  • borax boric acid
  • B203 KB 5 O 8 .4H 2 O
  • zinc borate can be used as the boron compound.
  • the alkali silicate used is preferably a sodium water glass or potassium water glass with an SiO 2 content between 21 and 47%.
  • wetting agent For a safe wetting of the powdery solid lubricant mixture, it can be helpful to add a wetting agent to the mixture and / or the water.
  • wetting agents are alkyl aryl sulfonates, fatty acid amines, fatty soaps, substituted amides of alkyl phosphates, sulfonated esters of dicarboxylic acids, sulfonated fatty amides, alkyl amines, sodium alkyl sulfates, aliphatic amine esters, polyethers such as polyoxyethylene and polyoxypropylene, sulfonated high phenols or naphthalenesulfonates.
  • the solid lubricant suspensions to be produced by the process according to the invention can contain, for example, 1 to 90% by weight solid lubricant, preferably graphite, 1 to 50% by weight polymer, 1 to 80% by weight inorganic additive and 0.2 to 80% by weight of an organic stabilizer as a solid component contain.
  • Water is used as the carrier liquid, with any additives to the water, such as wetting agents, solvents, e.g. Alcohols, esters, ketones or aldehydes are included.
  • additives in the water may be necessary, for example, to quickly bring the solid lubricant and thereby the extremely poorly wettable graphite into suspension or, for example, to quickly dissolve or swell the polymer portion.
  • the solid lubricants are suitable for high temperature applications, at temperatures from 300 to 1300 ° C, for example for the lubrication of tools such as mandrels, mandrel bars or dies and workpieces, for example blanks or tubes, in hot forming in so-called “multiple pipe mills", continuous lines, mitral mills, Assel lines, push bench systems, bar presses or upsetting presses, and in rolling lines for profile and sheet metal rolling.
  • the preferred materials for processing are iron and steel.
  • the suspension produced by the method of the invention is by brushing, brushing and preferably by spraying onto the hot workpiece or tool.
  • the carrier liquid in this case the water, and any volatile additives evaporate and leave a waterproof, graphite-containing melt film from the polymer.
  • the water resistance of the film is required in order to be able to cool the surface coated with the solid lubricant if necessary.
  • the film-forming properties are an essential feature of the solid lubricant. However, these do not show up at the place of application, i.e. on the workpiece or tool, but already during mixing, i.e. when the solids and then especially the polymers come into contact with the water.
  • the invention further comprises the device for carrying out the method according to the invention, consisting of a colloid mill and an intensive mixer immediately downstream.
  • the colloid mill can have a gap width of 0.01 to 3 mm and can with peripheral speeds of 10 to 40 rcVsec. operate.
  • the entire system is suitably designed for throughputs of 25 to 1200 kg / h and preferably up to 2000 kg / h of material.
  • the colloid mill 1 consists essentially of the housing 2 and the rotor 3, which is set in motion by the drive 4.
  • the graphite / polymer mixture or the graphite alone, in each case with the further possible additives, and the water 6, possibly in a mixture with the polymer and other possible additives, is fed into the colloid mill 1 from a storage vessel 5.
  • a storage vessel 11 can be provided, which can be equipped with a level meter and switches the system on and off according to the level.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Lubricants (AREA)
  • Forging (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Chemically Coating (AREA)

Abstract

Solid lubricants which are used in the non-cutting hot forming of metals. Lubricants containing graphite and polymers are presuspended in a colloid mill in water as a carrier liquid and immediately thereafter are subjected to a further mixing process in an intensive mixer, thereby being processed to a stable suspension.

Description

Die Erfindung betrifft ein Verfahren zum Suspendieren von Festschmierstoffen, die bei der spanlosen Warmumformung von Metallen Anwendung finden, enthaltend Graphit und Polymere in Wasser als Trägerflüssigkeit.The invention relates to a method for suspending solid lubricants which are used in the non-cutting hot forming of metals, containing graphite and polymers in water as the carrier liquid.

Aus den CH-PS 596 294 und 609 728 sind Festschmierstoffe für die spanlose Metallumformung bei hohen Temperaturen bekannt, enthaltend Graphit, Polymerisate, Suspensionshilfsmittel und gegebenenfalls weitere Hilfsmittel, wie Bakterizide, die mit Wasser eine Suspension bilden. Der Zusatz der Bakterizide ist notwendig um eine bakterielle Zersetzung der Festschmierstoffsuspension bei der Lagerung zu vermeiden; die Suspensionshilfsmittel erfüllen den Zweck, die flüssigen und festen Bestandteile auch über längere Zeiträume in homogener Mischung zu halten. Die Festschmierstoffsuspension braucht sich während der Verarbeitung auf, d.h. das Wasser verdampft auf dem Werkzeug der Werkstücke, der Polymeranteil brennt ab. Bei der Verarbeitung der Festschmierstoffe unterliegen die bakteriziden Zusätze ebenfalls einer Verdampfung, was in Anbetracht deren möglicher Giftigkeit unerwünscht ist und zusammen mit den Suspensionshilfsmitteln bilden sie einen nicht unerheblichen nichtschmierenden Teil der Festschmierstofformulation.From C H -PS 596 294 and 609 728 solid lubricants for non-cutting metal forming at high temperatures are known, containing graphite, polymers, suspension aids and optionally other aids, such as bactericides, which form a suspension with water. The addition of the bactericides is necessary to avoid bacterial decomposition of the solid lubricant suspension during storage; The suspension auxiliaries serve the purpose of keeping the liquid and solid constituents in a homogeneous mixture even over long periods. The solid lubricant suspension is used up during processing, ie the water evaporates on the tool of the workpieces, the polymer component burns off. When processing the solid lubricants, the bactericidal additives are also subject to evaporation, which is undesirable in view of their possible toxicity and together with the suspension aids they form a not inconsiderable non-lubricating part of the solid lubricant formulation.

Aufgabe vorliegender Erfindung war es, ein Verfahren vorzuschlagen, das es ermöglicht, eine homogene und stabile Festschmierstoffsuspension, enthaltend eine Trägerflüssigkeit, in der Regel Wasser, Graphit und Polymere, unmittelbar am Ort des Verbrauchs herzustellen, ohne Zusatz von Bakteriziden und mit einem möglichst geringen Gehalt an Suspensionshilfsmitteln.The object of the present invention was to propose a method which makes it possible to in a homogeneous and stable solid lubricant suspension containing a carrier liquid usually water, graphite and polymers to be produced directly at the point of use, without the addition of bactericides and with the lowest possible level of suspension aids.

Erfindungsgemäss wird das dadurch erreicht, dass die Bestandteile des Festschmierstoffes und Wasser als Trägerflüssigkeit in einer Kolloidmühle vorsuspendiert werden und unmittelbar anschliessend in einem Intensivmischer einem weiteren Mischprozess unterworfen und dabei zu einer stabilen Suspension verarbeitet werden.This is achieved according to the invention in that the constituents of the solid lubricant and water as the carrier liquid are pre-suspended in a colloid mill and then immediately subjected to a further mixing process in an intensive mixer and thereby processed into a stable suspension.

Zur Ausführung des Verfahrens können die trockenen, vorgemischten Bestandteile des Festschmierstoffes und das Wasser in der Kolloidmühle zusammengeführt werden.To carry out the process, the dry, premixed components of the solid lubricant and the water can be combined in the colloid mill.

Als trockene, vorgemischte Bestandteile wird die Mischung von Graphit, dem Polymer und allfälligen Zusätzen, wie Suspensionshilfsmitteln, Filmstabilisatoren, gegebenenfalls auch Netzmitteln und anorganischen Additive, bezeichnet.The mixture of graphite, the polymer and any additives, such as suspension aids, film stabilizers, and optionally also wetting agents and inorganic additives, is referred to as dry, premixed constituents.

Dem Wasser können allenfalls auch Zusätze, wie z.B. Netzmittel, Lösungsmittel, Filmbildner, pH-Stabilisator, lösliche anorganische Salze (z.B. Phosphate) usw. schon vorgängig beigefügt werden.At most, additives such as e.g. Wetting agents, solvents, film formers, pH stabilizers, soluble inorganic salts (e.g. phosphates) etc. should be added beforehand.

In einer weiteren Ausführungsform der Erfindung kann das Wasser, gegebenenfalls mit den genannten Zusätzen, wie Suspensionshilfsmitteln, Netzmitteln oder Lösungsmitteln usw., zusammen mit dem Polymer, z.B. als Kunststoff-Dispersion, vorgemischt werden und diese Mischung in der Kolloidmühle mit dem Graphit, der gegebenenfalls mit z.B. Suspensionshilfsmitteln, Filmstabilisatoren usw. homogen vermischt ist, zugeführt werden.In a further embodiment of the invention, the water, optionally with the additives mentioned, such as suspensions Sion aids, wetting agents or solvents, etc., are premixed together with the polymer, for example as a plastic dispersion, and this mixture is fed in the colloid mill with the graphite, which is optionally homogeneously mixed with, for example, suspension aids, film stabilizers, etc.

Als Kolloidmühle können an sich handelsübliche Geräte angewendet werden, wobei sich für den speziellen Zweck und im Hinblick auf die Eigenschaften der zu verarbeitenden Produkte Anpassungen notwendig sein können. Zu solchen Anpassungen gehören die Dimensionierung des Antriebes, Pulverförderer, Flüssigkeits-und Pulvereinlässe und -ventile, Abstreifer und Schaltvorrichtungen.Commercially available devices can be used as a colloid mill, although adjustments may be necessary for the special purpose and with regard to the properties of the products to be processed. Such adaptations include the dimensioning of the drive, powder conveyor, liquid and powder inlets and valves, wipers and switching devices.

Die Spaltweite zwischen dem Rotor und Gehäuse kann 0,01 bis 3 mm betragen; die Umfangsgeschwindigkeit, errechnet aus Rotorumfang und Drehzahl kann 10 bis 40 m/sec. betragen.The gap between the rotor and housing can be 0.01 to 3 mm; the peripheral speed, calculated from the rotor circumference and speed, can range from 10 to 40 m / sec. be.

Nach dem erfindungsgemässen Verfahren können Suspensionen mit einem Feststoffgehalt von 1 bis 70 Gew.% hergestellt werden. Die Möglichkeit, derart hohe Feststoffgehalte in der Suspension zu erzielen, war unser überraschender, als die einzelnen Bestandteile des Festschmierstoffes sehr niedrige Schüttgewichte aufweisen. Diese liegen für Graphit bei 0,2 bis 0,5 kg/l, für die Polymere und Zusätze bei 0,2 bis 0,7 kg/1 und beispielsweise für eine typische trockene Mischung bei 0,2 bis 0,5 kg/l. Somit ist schon für eine 25 Gew.%ige Suspension das Volumen des Festschmierstoffes grösser als das Volumen zur Herstellung der Suspension benötigten Wassers.Suspensions with a solids content of 1 to 70% by weight can be prepared by the process according to the invention. The possibility of achieving such high solids contents in the suspension was more surprising to us than the individual components of the solid lubricant have very low bulk densities. These are 0.2 to 0.5 kg / l for graphite, 0.2 to 0.7 kg / l for the polymers and additives and, for example, 0.2 to 0.5 kg / l for a typical dry mixture . Thus, for a 25% by weight Sus pension the volume of the solid lubricant is greater than the volume required to produce the suspension.

Mit dem erfindungsgemässen Einsatz der Kolloidmühle gelingt es, eine Klumpenbildung der Feststoffe sicher zu vermeiden. Die Verweildauer der Komponenten im Mischbereich der Kolloidmühle liegt zweckmässig im Bereich von 0,01 bis 5 sec.With the use of the colloid mill according to the invention, it is possible to reliably avoid clumping of the solids. The residence time of the components in the mixing area of the colloid mill is expediently in the range from 0.01 to 5 seconds.

Die Stabilität derart hergestellter Suspensionen ist jedoch beschränkt und die Feststoffe sedimentieren rasch. Eine unmittelbare Weiterbehandlung der Suspension in einem Intensivmischer, wobei eine durchschnittliche Verweilzeit von 60 bis 3000 sec., vorzugsweise 150 bis 300 sec., eingehalten werden soll, führt zu stabilen Suspensionen.However, the stability of suspensions produced in this way is limited and the solids sediment rapidly. Immediate further treatment of the suspension in an intensive mixer, with an average residence time of 60 to 3000 seconds, preferably 150 to 300 seconds, to result in stable suspensions.

Geeignete Intensivmischer sind zweckmässig Mischer mit wenigstens einer gleichläufigen Rührflügelwelle oder gegenläufigen Rührflügelwellen, Rührwerkskugelmühlen, Leitstrahlmischer oder Schneckenmischer, vorzugsweise in kaskadenförmiger Anordnung. Würden die Bestandteile, also der Festschmierstoff und das Wasser, beispielsweise nur in einem Intensivmischer zu der Festschmierstoffsuspension vermischt, liesse sich eine Klumpenbildung und Inhomogenität in der Suspension weder vermeiden noch beheben.Suitable intensive mixers are expediently mixers with at least one co-rotating impeller shaft or counter-rotating impeller shafts, agitator ball mills, guide jet mixers or screw mixers, preferably in a cascade arrangement. If the constituents, ie the solid lubricant and the water, were mixed to form the solid lubricant suspension, for example, only in an intensive mixer, lump formation and inhomogeneity in the suspension could neither be avoided nor eliminated.

Durch die erfindungsgemässe Anordnung, dem Nacheinanderschalten einer Kolloidmühle und einem Intensivmischer gelingt es, aus der Trägerflüssigkeit und den Feststoffen eine völlig klumpenfreie, homogene Feststoffsuspension zu erhalten, deren Bestandteile vollständig benetzt und soweit dazu geeignet, aufgeschlossen sind. Eine derart hergestellte Suspension ist klumpenfrei und hat eine, gemessen an der Art und Menge des Suspensionshilfsmittels, wesentlich verlängerte Standzeit und eine Sedimentation der Feststoffe tritt erst nach wesentlich längeren Zeiträumen auf, als das bei einem Mischen und Suspendieren mit nur einem der erfindungsgemäss nacheinander angeordneten Mischer möglich wäre.As a result of the arrangement according to the invention, the sequential connection of a colloid mill and an intensive mixer, it is possible to obtain a completely lump-free, homogeneous solid suspension from the carrier liquid and the solids, its existence parts are completely wetted and, if appropriate, open-minded. A suspension produced in this way is lump-free and has a significantly longer service life, measured in terms of the type and amount of suspension aid, and sedimentation of the solids only occurs after considerably longer periods of time than when mixing and suspending with only one of the mixers arranged in succession according to the invention it is possible.

Nach dem erfindungsgemässen Verfahren herzustellende Festschmierstoffe sind z.B. bekannt aus den CH-PS 596 294 und 609 728. Entsprechend sind die zur Anwendung gelangenden Ausgangsmaterialien wenigstens ein Festschmierstoff, bevorzugt Graphit, insbesondere solche Graphite mit hoher Reinheit, beispielsweise über 90%, und einer durchschnittlichen Korngrösse von nicht mehr als 300 Mikrometer. Die besten Ergebnisse lassen sich mit dem Graphit von 96 bis 99,5% Reinheit und einer durchschnittlichen Korngrösse von 100 Mikrometer erzielen. Gegebenenfalls ist die Anwendung von Molybdändisulfid, CaF2 oder BN allein oder im Gemisch mit Graphit sinngemäss im Rahmen vorliegender Erfindung denkbar.Solid lubricants to be produced by the process according to the invention are known, for example, from CH-PS 596 294 and 609 728. Accordingly, the starting materials used are at least one solid lubricant, preferably graphite, in particular those graphites with high purity, for example over 90%, and an average grain size of no more than 300 microns. The best results can be achieved with the graphite of 96 to 99.5% purity and an average grain size of 100 micrometers. If appropriate, the use of molybdenum disulfide, CaF 2 or BN alone or in a mixture with graphite is conceivable in the context of the present invention.

Unter Polymeren werden die sich in Wärme rückstandsfrei zersetzenden organischen Produkte, beispielsweise Alkylenhomopolymere oder -copolymere verstanden. Dazu zählen die Homo- und Copolymere von Alkenen (Monoolefine, Diolefine etc.), Vinylestern, Vinylalkoholen, ungesättigte dibasischen Säuren und Estern (Dicarboxylsäuren und -ester), Alkylestern und acyclische Säuren und Estern.Polymers are understood as meaning the organic products which decompose without leaving any heat, for example alkylene homopolymers or copolymers. These include the homo- and copolymers of alkenes (monoolefins, diolefins, etc.), vinyls ters, vinyl alcohols, unsaturated dibasic acids and esters (dicarboxylic acids and esters), alkyl esters and acyclic acids and esters.

Das Alkylenhomopolymer oder -copolymer kann Polyethylen, Polymethylmethacrylat, Polystyrol, Polybutadien, Polyvinylacetat, Polyvinylpropionat, ein Copolymer aus Methylmethacrylat und Styrol, ein Copolymer aus Methylmethacrylat und Alphamethylstyrol, Polydiallylphthalat, Polypropylen, ein Copolymer aus Styrol und Butadien, Polymethylmethacrylat, ein Copolymer aus Vinylacetat und Dibutylmaleinat, ein Copolymer aus Vinylacetat und Ethylen und Polyisobutylen, sein.The alkylene homopolymer or copolymer can be polyethylene, polymethyl methacrylate, polystyrene, polybutadiene, polyvinyl acetate, polyvinyl propionate, a copolymer of methyl methacrylate and styrene, a copolymer of methyl methacrylate and alphamethylstyrene, polydiallyl phthalate, polypropylene, a copolymer of styrene and butadiene, and polymethyl methacrylate Dibutyl maleate, a copolymer of vinyl acetate and ethylene and polyisobutylene.

Die genannten Polymere können allein oder im Gemisch untereinander trocken oder geeignetenfalls als Dispersion angewendet werden.The polymers mentioned can be used alone or in a mixture with one another dry or, if appropriate, as a dispersion.

Als Suspensionshilfsmittel können beispielsweise Stoffe aus der Gruppe Polysaccharide, wie Stärke, Cellulosen, Inulin, Glycogen Agar, Levan, Dichinon,_ Pectin, Lignin und Araban, ferner können Alkylcellulosen, wie z.B. Methyl-, Ethyl-, Propyl- und Butylcellulosen, oder Alginate, wie Natriumalginat, Kaliumalginat, Propylenglykolalginat und Ammoniumalginat, oder Gemische der Substanzen angewendet werden.For example, substances from the group of polysaccharides such as starch, celluloses, inulin, glycogen agar, levan, dichinone, pectin, lignin and araban can be used as suspension aids. Methyl, ethyl, propyl and butyl celluloses, or alginates such as sodium alginate, potassium alginate, propylene glycol alginate and ammonium alginate, or mixtures of the substances can be used.

Der Festschmierstoff soll bei deren Anwendung als 1 bis 70 Gew- %ige homogene wässrige Dispersion vorliegen und eine Viskosität von 100 bis 30000 cp bei 5 bis 50°C aufweisen.When used, the solid lubricant should be present as a 1 to 70% by weight homogeneous aqueous dispersion and have a viscosity of 100 to 30,000 cp at 5 to 50 ° C.

Um die Viskosität der Dispersion zu erreichen, kann auch ein gegebenenfalls im Festschmierstoff enthaltener organischer Stabilisator ausreichend sein. Es ist aber auch möglich, durch einen Verdicker oder ein Gemisch von Verdickern die Viskosität zu steuern. Aus der Reihe von geeigneten Verdickern eignen sich z.B. wasserlösliche Polysaccharide, Alkylcellulosen, Polyvinylalkohole, Polyarylate, Polyvinylpyrrolidon, gegebenenfalls noch anorganische Substanzen, insbesondere Mineralien, wie Tone oder Kieselsäure.To achieve the viscosity of the dispersion, an organic stabilizer which may be present in the solid lubricant may also be sufficient. However, it is also possible to control the viscosity by means of a thickener or a mixture of thickeners. From the range of suitable thickeners, e.g. water-soluble polysaccharides, alkyl celluloses, polyvinyl alcohols, polyarylates, polyvinyl pyrrolidone, optionally also inorganic substances, in particular minerals, such as clays or silica.

Weitere Zusätze können anorganische Additive sein und aus der Reihe der Borverbindungen, der Polyphosphate und der Alkalisilikate, allein oder in Mischung untereinander gewählt werden. Zu diesen Verbindungen gehören Polyphosphat in unlöslicher oder schwerlöslicher Form. Vorzugsweise kommen als Polyphosphate Madrell'sche Salze oder Kurrol'sche Salze zur Anwendung. Dabei handelt es sich um Verbindungen der Art (Na PO3)n mit n - 6 bis 50'000, vorzugsweise 6 - 10'000. Die Borverbindung kann in löslicher und vorzugsweise in schwerlöslicher oder unlöslicher Form angewendet werden.Other additives can be inorganic additives and selected from the range of boron compounds, polyphosphates and alkali silicates, alone or as a mixture with one another. These compounds include polyphosphate in insoluble or poorly soluble form. Madrell's salts or Kurrol's salts are preferably used as polyphosphates. These are compounds of the type (Na PO 3 ) n with n - 6 to 50,000, preferably 6 - 10,000. The boron compound can be used in soluble and preferably in poorly soluble or insoluble form.

Als Borverbindung können beispielsweise Borax, Borsäure, B203, KB5O8·4H2O oder Zinkborat angewendet werden.For example, borax, boric acid, B203, KB 5 O 8 .4H 2 O or zinc borate can be used as the boron compound.

Das zur Anwendung gelangende Alkalisilikat ist bevorzugt ein Natronwasserglas oder Kaliwasserglas mit einem Si02-Gehalt zwischen 21 und 47%.The alkali silicate used is preferably a sodium water glass or potassium water glass with an SiO 2 content between 21 and 47%.

Zur sicheren Benetzung des pulverigen Festschmierstoffgemisches kann es hilfreich sein, dem Gemisch und/oder dem Wasser ein Netzmittel zuzufügen. Beispiele von solchen Netzmitteln sind Alkylarylsulfonate, Fettsäureamine, Fettseifen, substituierte Amide der Alkylphosphate, sulfonierte Ester der Dicarboxylsäuren, sulfonierte Fettamide, Alkylamine, Natriumalkylsulfate, aliphatische Aminester, Polyether, wie Polyoxyethylen und Polyoxypropylen, sulfonierte hohe Phenole oder Naphthalensulfonate.For a safe wetting of the powdery solid lubricant mixture, it can be helpful to add a wetting agent to the mixture and / or the water. Examples of such wetting agents are alkyl aryl sulfonates, fatty acid amines, fatty soaps, substituted amides of alkyl phosphates, sulfonated esters of dicarboxylic acids, sulfonated fatty amides, alkyl amines, sodium alkyl sulfates, aliphatic amine esters, polyethers such as polyoxyethylene and polyoxypropylene, sulfonated high phenols or naphthalenesulfonates.

Die nach dem erfindungsgemässen Verfahren herzustellenden Festschmierstoffsuspensionen können beispielsweise als Feststoffkomponente 1 bis 90 Gew.% Festschmierstoff, vorzugsweise Graphit, 1 bis 50 Gew.% Polymer, 1 bis 80 Gew.% anorganischen Zusatz und 0,2 bis 80 Gew.% eines organischen Stabilisierungsmittels enthalten.The solid lubricant suspensions to be produced by the process according to the invention can contain, for example, 1 to 90% by weight solid lubricant, preferably graphite, 1 to 50% by weight polymer, 1 to 80% by weight inorganic additive and 0.2 to 80% by weight of an organic stabilizer as a solid component contain.

Als Trägerflüssigkeit wird Wasser angewendet, wobei allfällige Zusätze zum Wasser, wie Netzmittel, Lösungsmittel, wie z.B. Alkohole, Ester, Ketone oder Aldehyde, miteingeschlossen sind. Derartige Zusätze im Wasser können notwendig sein, um beispielsweise den Festschmierstoff und dabei den äusserst schlecht benetzbaren Graphit rasch in Suspension zu bringen oder beispielsweise den Polymeranteil rasch anzulösen oder anzuquellen.Water is used as the carrier liquid, with any additives to the water, such as wetting agents, solvents, e.g. Alcohols, esters, ketones or aldehydes are included. Such additives in the water may be necessary, for example, to quickly bring the solid lubricant and thereby the extremely poorly wettable graphite into suspension or, for example, to quickly dissolve or swell the polymer portion.

Die Festschmierstoffe eignen sich für eine Hochtemperaturanwendung, bei Temperaturen von 300 bis 1300°C, beispielsweise für die Schmierung von Werkzeug, z.B. Dorn, Dornstange oder Matrize und Werkstücke, beispielsweise Luppe oder Rohr, bei der Warmumformung in sogenannten "multiple pipe mills", Kontistrassen, Pilgerschrittwalzwerken, Asselstrassen, Stossbankanlagen, Stangenpressen oder Anstauchpressen, und in Walzstrassen zum Profil- und Blechwalzen. Die bevorzugt zur Bearbeitung gelangenden Materialien sind dabei Eisen und Stahl.The solid lubricants are suitable for high temperature applications, at temperatures from 300 to 1300 ° C, for example for the lubrication of tools such as mandrels, mandrel bars or dies and workpieces, for example blanks or tubes, in hot forming in so-called "multiple pipe mills", continuous lines, pilgrim step rolling mills, Assel lines, push bench systems, bar presses or upsetting presses, and in rolling lines for profile and sheet metal rolling. The preferred materials for processing are iron and steel.

Die nach dem Verfahren der Erfindung hergestellte Suspension wird durch Aufstreichen, Aufbürsten und bevorzugt durch Aufsprühen auf das heisse Werkstück oder das heisse Werkzeug resp. Walze aufgetragen, wobei die Trägerflüssigkeit, in vorliegendem Falle das Wasser, und allfällige flüchtige Zusätze verdampfen und einen wasserfesten, graphithaltigen Schmelzfilm aus dem Polymer zurücklassen. Die Wasserfestigkeit des Filmes wird gefordert, um nötigenfalls die mit dem Festschmierstoff beschichtete Oberfläche kühlen zu können.The suspension produced by the method of the invention is by brushing, brushing and preferably by spraying onto the hot workpiece or tool. Roll applied, the carrier liquid, in this case the water, and any volatile additives evaporate and leave a waterproof, graphite-containing melt film from the polymer. The water resistance of the film is required in order to be able to cool the surface coated with the solid lubricant if necessary.

Wesentliches Merkmal des Festschmiermittels sind die filmbildenden Eigenschaften. Diese zeigen sich aber nicht erst am Anwendungsort, also auf dem Werkstück oder Werkzeug, sondern schon während des Mischens, also bei der Berührung der Feststoffe und dann insbesondere der Polymere mit dem Wasser.The film-forming properties are an essential feature of the solid lubricant. However, these do not show up at the place of application, i.e. on the workpiece or tool, but already during mixing, i.e. when the solids and then especially the polymers come into contact with the water.

Es ist deshalb umso überraschender, dass es nun gelingt, nach dem Verfahren der Erfindung einen extrem schlecht benetzbaren Stoff, wie Graphit, und ein Polymer mit stark filmbildenden bis klebenden Eigenschaften, wobei der sich ausbildende Film anschliessend wasserfest sein muss, mit Wasser klumpenfrei und homogen zu mischen. Erschwerend kommt beim Verfahren hinzu, dass das Volumen der Feststoffe aufgrund deren niedrigen Schüttgewichtes das Volumen des Wassers übertreffen können. Schliesslich muss die Suspension, gemessen an der Menge des Zusatzes von Suspensionshilfsmitteln, extrem stabil sein und darf über längere Zeiträume keine Entmischung oder Sedimentation zeigen.It is therefore all the more surprising that it is now possible, according to the process of the invention, to use an extremely poorly wettable substance, such as graphite, and a polymer with strong film-forming to adhesive properties, with the film which forms finally must be waterproof, mix with water lump-free and homogeneously. To make matters in the process, adding that the volume of solids due to their low S chüttgewichtes the volume may exceed the water. Finally, the suspension, measured by the amount of suspension aids added, must be extremely stable and must not show segregation or sedimentation over long periods.

Die Erfindung umfasst weiters die Vorrichtung zur Ausführung des erfindungsgemässen Verfahrens, bestehend aus einer Kolloidmühle und einem unmittelbar nachgeordneten Intensivmischer.The invention further comprises the device for carrying out the method according to the invention, consisting of a colloid mill and an intensive mixer immediately downstream.

Die Kolloidmühle kann eine Spaltweite von 0,01 bis 3 mm aufweisen und kann mit Umfangsgeschwindigkeiten von 10 bis 40 rcVsec. betrieben werden. Die ganze Anlage ist zweckmäßig für Durchsätze von 25 bis 1200 kg/h und vorzugsweise bis 2000 kg/h Material ausgelegt.The colloid mill can have a gap width of 0.01 to 3 mm and can with peripheral speeds of 10 to 40 rcVsec. operate. The entire system is suitably designed for throughputs of 25 to 1200 kg / h and preferably up to 2000 kg / h of material.

Die Abbildung gibt schematisch die erfindungsgemässe Vorrichtung wieder. Die Kolloidmühle 1 besteht im wesentlichen aus Gehäuse 2 und Rotor 3, der durch Antrieb 4 in Bewegung gesetzt wird. Aus einem Vorratsgefäss 5 wird das Graphit/Polymergemisch oder der Graphit allein, jeweils mit den weiteren möglichen Zusätzen, und durch die Zuführung 6 das Wasser, allenfalls im Gemisch mit dem Polymer und anderen allfälligen Zusätzen, in die Kolloidmühle 1 geführt. Unmittelbar nach dem Auslass 7 der Kolloidmühle, durch eine Schlauchleitung 8, wird die vorgemischte Suspension in einem Intensivmischer 9, hier beispielhaft dargestellt mit einem kaskadenförmig angeordneten Blattrührer 10, geleitet. Nach dem Intensivmischer 9 kann ein Vorratsgefäss 11 vorgesehen sein, das mit einem Füllstandsmesser ausgerüstet sein kann und entsprechend dem Füllstand die Anlage ein- und ausschaltet.The figure schematically shows the device according to the invention. The colloid mill 1 consists essentially of the housing 2 and the rotor 3, which is set in motion by the drive 4. The graphite / polymer mixture or the graphite alone, in each case with the further possible additives, and the water 6, possibly in a mixture with the polymer and other possible additives, is fed into the colloid mill 1 from a storage vessel 5. Immediately after the outlet 7 of the colloid mill, through a hose 8, the pre mixed suspension in an intensive mixer 9, shown here by way of example with a cascade-shaped blade stirrer 10. After the intensive mixer 9, a storage vessel 11 can be provided, which can be equipped with a level meter and switches the system on and off according to the level.

Claims (10)

1. Verfahren zum Suspendieren von Festschmierstoffen, die bei der spanlose Warmumformung von Metallen Anwendung finden, enthaltend Graphit und Polymere in Wasser als Trägerflüssigkeit, dadurch gekennzeichnet, dass die Bestandteile des Festschmierstoffes und Wasser in einer Kolloidmühle vorsuspendiert werden und unmittelbar anschliessend in einem Intensivmischer einem weiteren Mischprozess unterworfen und dabei zu einer stabilen Suspension verarbeitet werden.1. A method for suspending solid lubricants which are used in the non-cutting hot forming of metals, containing graphite and polymers in water as the carrier liquid, characterized in that the constituents of the solid lubricant and water are presuspended in a colloid mill and then immediately in another intensive mixer Subjected to the mixing process and processed into a stable suspension. 2. Verfahren nach Patentanspruch 1, dadurch gekennzeichnet, dass die trockenen, vorgemischten Festschmierstoffbestandteile und das Wasser in der Kolloidmühle zusammengeführt werden.2. The method according to claim 1, characterized in that the dry, premixed solid lubricant components and the water are brought together in the colloid mill. 3. Verfahren nach Patentanspruch 1, dadurch gekennzeichnet, dass der Graphit und das im Wasser vorgemischte Polymer in der Kolloidmühle zusammengeführt werden.3. The method according to claim 1, characterized in that the graphite and the polymer premixed in the water are brought together in the colloid mill. 4. Verfahren nach Patentansprüchen 1, 2 und 3, dadurch gekennzeichnet, dass die Kolloidmühle eine Spaltweite von 0,01 bis 3 mm aufweist.4. The method according to claims 1, 2 and 3, characterized in that the colloid mill has a gap width of 0.01 to 3 mm. 5. Verfahren nach Patentansprüchen 1, 2, 3 und 4, dadurch gekennzeichnet, dass die Kolloidmühle mit einer Umfangsgeschwindigkeit von 10 bis 40 m/sec., vorzugsweise 15 bis 20 m/sec., betrieben wird.5. The method according to claims 1, 2, 3 and 4, characterized in that the colloid mill is operated at a peripheral speed of 10 to 40 m / sec., Preferably 15 to 20 m / sec. 6. Verfahren nach Patentansprüchen 1, 2, 3, 4 und 5, dadurch gekennzeichnet, dass eine Suspension mit einem Feststoffgehalt von 1 bis 70 Gew.% hergestellt wird.6. The method according to claims 1, 2, 3, 4 and 5, characterized in that a suspension with a solids content of 1 to 70% by weight is produced. 7. Verfahren nach Patentansprüchen 1, 2, 3, 4, 5 und 6, dadurch gekennzeichnet, dass die Verweildauer des Mischgutes im Intensivmischer 60 bis 3000 sec., vorzugsweise 150 bis 300 sec., beträgt.7. The method according to claims 1, 2, 3, 4, 5 and 6, characterized in that the residence time of the material to be mixed in the intensive mixer is 60 to 3000 seconds, preferably 150 to 300 seconds. 8. Vorrichtung zur Ausführung des Verfahrens nach Patentansprüchen 1, 2, 3, 4, 5, 6 und 7, dadurch gekennzeichnet, dass die Vorrichtung aus einer Kolloidmühle und unmittelbar nachgeordnet einem Intensivmischer besteht.8. Device for performing the method according to claims 1, 2, 3, 4, 5, 6 and 7, characterized in that the device consists of a colloid mill and immediately downstream of an intensive mixer. 9. Vorrichtung nach Patentanspruch 8, dadurch gekennzeichnet, dass die Kolloidmühle eine Spaltweite von 0,01 bis 3 mm aufweist und mit einer Umfangsgeschwindigkeit von 10 bis 40 m/sec. betrieben wird.9. The device according to claim 8, characterized in that the colloid mill has a gap width of 0.01 to 3 mm and with a peripheral speed of 10 to 40 m / sec. is operated. 10. Vorrichtung nach Patentansprüchen 8 und 9, dadurch gekennzeichnet, dass der Intensivmischer, ein Mischer mit wenigstens einer gleichläufigen Rührflügelwelle oder gegenläufigen Rührflügelwellen ist, oder es sich um eine Rührwerkskugelmühle, einen Leitstrahlmischer oder einen Schneckenmischer handelt und die Verweildauer des Mischgutes im Intensivmischer 60 bei 3000 sec., vorzugsweise 150 bis 300 sec., beträgt.10. The device according to claims 8 and 9, characterized in that the intensive mixer is a mixer with at least one co-rotating impeller shaft or counter-rotating impeller shaft, or it is an agitator ball mill, a jet mixer or a screw mixer and the residence time of the mixed material in the intensive mixer 60 3000 sec., Preferably 150 to 300 sec.
EP86113474A 1985-10-02 1986-10-01 Method for suspending solid lubricants Expired - Lifetime EP0218989B1 (en)

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AT86113474T ATE60249T1 (en) 1985-10-02 1986-10-01 METHOD OF SUSPENSING SOLID LUBRICANTS.

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CH4249/85A CH665847A5 (en) 1985-10-02 1985-10-02 METHOD FOR SUSPENDING SOLID LUBRICANTS.

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ATE60249T1 (en) 1991-02-15
CN1006400B (en) 1990-01-10
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DE3677127D1 (en) 1991-02-28
JPS6291229A (en) 1987-04-25
PL261617A1 (en) 1987-12-28
DD249858A5 (en) 1987-09-23
CS706186A2 (en) 1988-04-15
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CA1272181A (en) 1990-07-31
US4735734A (en) 1988-04-05
EP0218989B1 (en) 1991-01-23
CS261247B2 (en) 1989-01-12
CN86106627A (en) 1987-04-01
EP0218989A3 (en) 1989-04-26
SU1498378A3 (en) 1989-07-30

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