CA1272181A - Process for preparing suspensions of solid lubricants - Google Patents

Process for preparing suspensions of solid lubricants

Info

Publication number
CA1272181A
CA1272181A CA000518992A CA518992A CA1272181A CA 1272181 A CA1272181 A CA 1272181A CA 000518992 A CA000518992 A CA 000518992A CA 518992 A CA518992 A CA 518992A CA 1272181 A CA1272181 A CA 1272181A
Authority
CA
Canada
Prior art keywords
suspension
colloid mill
process according
sec
water
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 - Fee Related
Application number
CA000518992A
Other languages
French (fr)
Inventor
Hans-Rudolf Staub
Hansjorg Furrer
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.)
Lonza AG
Original Assignee
Lonza AG
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 Lonza AG filed Critical Lonza AG
Application granted granted Critical
Publication of CA1272181A publication Critical patent/CA1272181A/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • 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

Abstract

PROCESS FOR PREPARING SUSPENSIONS OF SOLID LUBRICANTS

ABSTRACT OF THE DISCLOSURE

A process is disclosed for preparing a suspension of a solid lubricant which is 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

.1 The invention relates to a process ~or suspending solid lubricants, which are used in non-cutting hot forming of metals, said lubricants containiny graphite and polymers in water as a carrier liquid.
Solid lubricants for the non cutting forming of metals at high temperatures are known from Swiss Published Patent Specifications Nos. 596,294 and 609,728. Such lubricants contain graphite, polymers, suspension auxiliary agents and optionally other auxiliary agents, such as bactericides, which form a suspension with water. The addition of bactericides has been necessary to avoid a bacterial decomposition of the suspended solid lubricant during storage; the suspension au~iliary agents serve the purpose of keeping the liquid and solid constituents in homogeneous mixture over longer periods. The solid lubricant suspension is consumed during processing, i.e., the water on the tool of the workpieces evaporates and the polymer portion burns off. In the processing of the solid lubricants, the bacterial additions also are subjected to evaporation, which in view of their possible toxicity is undesirable and, together with the suspension auxiliary agents, form an undesirable, non-lubricating part of the solid lubricant formulation.
The main object of the invention is to provide a process for producing a homogeneous, stable, solid lubricant suspension, containing a carrier liq~lid, such as water, graphite and polymers, directly at the site of use, without the addition of bactericides and with a suspension auxiliary agent content which is as small as possible.
Accordingly, the invention provides a process for preparing a suspension of at least one solid lubricant, which is used in the non-cutting hot-forming of metals, said lubricant containing graphite and at least one polymer in water as a carrier liquid, comprising suspending the constituents of the solid lubricant in the water in a colloid mill, said suspension having a solid lubricant content of 1 to 70 weight percent, said suspension containing 1 to 90 weight percent of graphite and 1 to 50 .~

weight percent of at lest one polymer, and wa~er bein~
present as a carrier liquid in an amount at leas~c sufficient to allow said suspension of at least one solid lubricant to be formed, and immediately thereafter subjecting said suspension to a further mixing process in an intensive mixer, thereby processing said suspension to a stable suspension.
For performing the process, the dry, premixed constituents of the solid lubricant and water can be brought together in a colloid mill. By the phrase "dry premixed constituents" is meant the mixture of graphite, polymer and optional additions, such as suspension auxiliary agents, film stabilizers, optionally also wetting agents and inorganic additives.
Additives such as wetting agents, solvents, film-forming agents, pH stabilizer, soluble inorganic salts (e.g., phosphates), etc., have already been added to the water.
In a further embodiment of the invention, the water and optionally the stated additives, such as suspension auxiliary agents, wetting agents, solvents, etc., together with the polymer, e.g., as a plastic dispersion, are premixed and then the mixture is fed into the colloid mill with the graphite, which is optionally homogeneously mixed, e.g., with suspension auxiliary agents, film stabilizers, etc.
The invention further provides an apparatus for carrying out the process of the invention, which comprises a colloid mill and an intensive mixer installed immediately downstream thereof, the colloid mill exhibitiny a clearance of 0.01 to 3 mm and operating with a peripheral speed of 10 to 40 m/sec, and the intensive mixer being a mixer with at least a co-rotating agitator blade shaft or counter-rotating agitator blade shafts or comprising an agitator ball mill, a jet mixer or a screw mixer and the residence time of the material mixed in the intensive mixer being 60 to 3000 seconds.

2a Generally speaking, existing commercially available apparatus can be used as the colloid mill, whereby adjustments may be necessary for special purposes and in view of the properties of the products to be produced. Such adjustments include dimensioning the drive powder conveyers, li~uid and powder intakes and valves, strippers and switching devices. The clearance between the rotor and housing should be 0.01 to 3 mm and the peripheral speed, calculated from the rotor periphery and revolutions, should be 10 to 4Q m/sec.
According to the process of the invention, suspensions with a solid content of 1 to 70 percent by weight can be produced. The possibility of attaining such high solid contents was all the more surprising since the individual constituents of the solid lubricant exhibit very low bulk densities. For graphite, such densities are 0.2 to 0.5 kg/l, for the polymers and additives they are 0.2 to 0.7 kg/l, and for a typical dry mixture they are 0.2 to 0.5 kg/l. Thus, for a 25 percent by weight suspension,the volume of the solid lubricant is already greater than the volume of the water necessary for production of the suspension.

B

With the use of the colloi.d mill accordiny to the invention, one can reli.ably avoid lumping of -the solid.
The.residue time of the components in the mixi.ng area of the colloid mill is advantageously in the range of 0.01 to 5 seconds.
However, the stabi.l.ity of suspensions so produced is limited and the soli.ds qui.ckl.y settl.e. An immediate reprocessing of the suspension in an intensive mixer, which has an average residence time oE 60 to 3000 sec., preferably 150 to 300 sec., provides stable suspensions.
Suitable intensi.ve mixers are advan-tageously mixers with at least a co-rotating agitator bl.ade shaf-t or counter-rotating agi.tator blade shafts, agita-tor ball mills, jet mixers or screw mixers, preferably in cascade arrangement. If the constituents, such as the solid lubricant and water, for example, were mixed only in an i.ntensive mixer for the solid lubrican-t suspension, lumping and inhomogeneity i.n the suspension can nei.ther be prevented nor eli.minated.
By the arrangement according to the invention of connecting a colloi.d mill and intensive mixer downstream from each other, it is possible to obtain from the carrier liquid and the solids a completely lump-free, homogeneous solid suspension, the constituents of which are completely wet and, to the extent that they are sui.table for the purpose, are decomposed. A suspension produced in this way is lump-free and has a considerably extended residence time, measured against the -type and amount o~the suspension auxiliary agent, and a sedimentation of the solids occurs only after considerably longer ti.mes than would be possi.ble in the case of a mixing and suspending wi.-th only one of the mixers placed one af-ter the o-ther according to the invention.
The solid lubri.cants to be used i.n -the process of the invention are known, e.g., from Swiss Published Patent Specifications Nos. 596,294 and 609,728. Accordingly, -the initial materials to be used comprise a-t least a solid lubricant, preEerably graphite, especia~.l.y -those yraphites with a hi.gh purity, for example over 90 percent, and an average grain size of not more than 300 m:icrometers. The best results can be obtained wi-th graphi.te of 96 to 99.5 percent purity and an average grain size o:E :l00 micrometers.
Optionally, mol.ybdenum disulEi.de, CaE2 or BN a.lone or in mi.xture with graphi.te can be used analogously in -the framework of this i.nvention.
The useful polymers are organic products which decompose residue-free on heati.ng, and i.nclude, for example, alkylene homopolymers or copolymers. They include homo and copolymers of alkenes (monoolefins, diolefins, e-tc.), vinyl esters, vinyl alcohols, unsaturated dibasic acids and esters (dicarboxylic acids and esters), alkyl esters and acyclic acids and esters. The alkylene homopol.ymer or copolymer can be, for example, polyethylene, polymethyl me-thacrylate, polystyrene, polybutadi.ene, polyvinyl acetate, polyvinyl propionate, a copolymer of methyl methacrylate and styrene, a copolymer of methyl methacrylate and alpha-methyl styrene, polydiallyl phthalate~ polypropylene,a copolymer of styrene and butadiene, polymethyl methacrylate, a copolymer of vinyl acetate and di.butyl maleate, a copolymer of vinyl acetate and ethylene, or polyi.sobutylene.
~seful suspension auxi.li.ary agen-t materials include polysaccharides, such as starches, celluloses, i.nulin, glycogen, agar, levan, diquinone, pectin, lignin and araban, alkylcelluloses, such as methyl, ethyl, propyl and butyl celluloses, alginates, such as sodium alginate, potassium alginate, propyleneglycol algi.nate and ammonium alginate, and mi.x-tures of such substances.
The homogeneous aqueous dispersion should contain 1 to 70 percent by wei.ght of the solid lubricant and exhibi.t a viscosi-ty of 100 to 30000 cp a-t 5 to 50C. To achieve the desired viscosi.ty for -the di.spersion, an organi.c sta-bilizer, opti.onally con-tai.ned i.n the solid l.ubricant, can be adequate. But i.t is also possible to control -the viscosity by a thickener or a mi.x-ture of thickeners. Of the series of suitable thickeners, e.y., water-soluble polysaccharides, alkylcellu]oses, polyv:inyl a~cohols, polyarylates, polyvinylpyrrolidone~ and optionally even inorganic substances, especially minerals, such as clays or silicic acid, are suitab]e.
Other addi-tives can be inorganic additives including, for example, boron compounds, polyphosphates and alkali silicates, alone or in admixture with one another. Polyphos-phates in insoluble or slightly soluble form also belong to this group. Preferably Madrell salts or Kurrol salts are used as the polyphosphates. In this case, there are involved compounds of the type (NaPO3)n, with n being 6 to 50,000, preferably 6 to 10,000. The boron compound can be used in soluble form or preferab]y in sllgh-tly soluble or insoluble form. Borax, boric acid, B2O3, KB5O84-H2O or zinc borate can be used as the boron compound.
The applicable al~ali silicate to be used is pre-Eerably a sodium silicate or potassium silicate with an SiO2 content of between 21 and 47 percent.
For reliable wetting of the powdery solid lubricant mixture, it can be helpful to add a wet-ting agent -to the mixture and~or water. Examples of such wetting agents are alkylaryl sulfonates, fatty acid amines, soaps from fats, substi-tuted amides of alkyl phospha-tes, sulfonated esters of dicarboxylic acids, sulfona-ted fatty amides, alkylamines, sodium alkyl sulfates, aliphatic amino esters, polyethers such as polyoxyethylene and polyoxypropylene, sulfonated high phenols and naphthalene sulfona-tes.
The solid lubricant suspensions to be produced according to the process oE -the invention can contain as solid components, for example, 1 to 90 percent by weigh-t of solid Lubricant, preferably graphite, 1 -to 50 percent by weight of polymer, l to 80 percent by weight oE inorganic additive and 0.2 to 80 percent by weigh-t of an organic stabilizing agen-t.
Water is used as the carrier liquid. Optional additions to the water are, for example, wet-ting agents and solvents such as al.cohols, esters, ketones and aldehydes.
Such additions to the wa-ter can be useful, :for example, for quickly bringi.ng into suspension the soli.~ ].ubr:Lcant and thus the graphite that is extremely difficult to wet, or to quickly solubi.lize or swell the pol.ymer port.i.on.
The solid lubri.cants are sui.table for high-temperature application at temperatures of 300 to 1300C, for example, for lubricating a tool, e.g., mandrel, mandrel rod or die and workpiece, for example, ball or pipe, in hot forming i.n the so-callea "multiple pipe mi.lls," continuous trains, pilger mills, ~ssel trains, push bench installations, extrusion presses or headi.ng presses, and i.n rolli.ng mi]l trains for shape and sheet rolli.ng. The preferred ma-terials available for working in this case are iron and steel.
The suspension produced accordi.ng to the process of the invention is applied to the ho-t workpiece or hot tool or roll by spreading, brushi.ng or preferably by sprayi.ng, whereby the carrier liqui.d, in this case water, and optional volatile additives evaporate and leave a water-resistant, graphite-containing melted film of polymer. The wa-ter resistance of the film is required -to be able to cool the surface coated with the solid lubricant, if necessary.
The film-forming properties are the essential feature of the solid lubricant. These properties are shown not only at the use si.te, i.e., on the workpi.ece or tool, but also during mi.xi.ny, i.e., in the con-tact of the solids and then especially of the polymers with the water. It is therefore all the more surpri.si.ng tha-t it is now possible according to the process of -the inven-tion to mix with water in a lump-free and homogeneous manner, a material which is extremely di.fficult to wet, such as graphite, and a polymer wi.th strongly fi.lm-forming to adhering properties, whereby the formi.ng film must then be water-resistant. In the process, this is aggravated by -the fact that the volume of the solids because of their low bulk density can exceed -the volume of the water.
Finally, the suspension, measured ayainst the amoun-t of ~,~Dd~7%~

the addi-tion of suspension auxiliary agents, must be extremely stable and must not show any separation or sedimentation over longer periods.
The inven-tion further comprises the device for carrying out the process according to the invention, which consists of a colloid mill and an intensive mixer installed immediately downstream thereof.
The colloid mill usually has a clearance of 0.01 to 3 mm and is usually operated with rotational speeds of 10 to 40 m~sec. The entire installation is advantageously designed for a throughput of 25 to 1200 kg/h and more preferably of 25 to 2000 kg/h, of material. The accompanying Figure shows diagrammatically a device according to an embodiment of the invention. A colloid mill l consists essentially of a housing 2 and a rotor 3, which can be placed in motion by a drive 4. From a storage vessel 5, a graphite~polymer mixture or graphite alone, respectively with the other possible additives, and by a feed ~ the water~ optionally in admixture with the polymer and other op-tional additives, are fed into the colloid mill 1.
Immediately after discharge 7 of the colloid mill through a hose 8, the premixed suspension is fed into an intensive mixer 9, (represented by way of illustration as a blade agitator lO arranged in cascade form). After the intensive mixer 9, a storage vessel 11 can be provided which can be equipped with a filling level gauge to turn the installation on and off according to the filling level.

Claims (13)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for preparing a suspension of at least one solid lubricant, which is used in the non-cutting hot-forming of metals, said lubricant containing graphite and at least one polymer in water as a carrier liquid, comprising suspending the constituents of the solid lubricant in the water in a colloid mill, said suspension having a solid lubricant content of 1 to 70 weight percent, said suspension containing 1 to 90 weight percent of graphite and 1 to 50 weight percent of at lest one polymer, and water being present as a carrier liquid in an amount at least sufficient to allow said suspension of at least one solid lubricant to be formed, and immediately thereafter subjecting said suspension to a further mixing process in an intensive mixer, thereby processing said suspension to a stable suspension.
2. A process according to claim 1, wherein the dry premixed constituents of the solid lubricant and water are brought together in the colloid mill.
3. A process according to claim 1, wherein the graphite and the polymer premixed in the water are fed into the colloid mill.
4. A process according to claim 3, wherein the colloid mill exhibits a clearance of 0.01 to 3 mm.
5. A process according to claim 4, wherein the colloid mill is operated with a peripheral speed of 10 to 40 m/sec.
6. A process according to claim 5, wherein the residence time of the material being mixed in the intensive mixer is 60 to 3000 sec.
7. A process according to claim 1 or 2, wherein the colloid mill exhibits a clearance of 0.01 to 3 mm.
8. A process according to claim 1 or 2, wherein the colloid mill is operated with a peripheral speed of 10 to 40 m/sec.
9. A process according to claim 1 or 2, wherein the colloid mill is operated with a peripheral speed of 15 to 20 m/sec.
10. A process according to claim 1 or 2, wherein the residence time of the material being mixed in the intensive mixer is 60 to 3000 sec.
11. A process according to claim 1 or 2, wherein the residence time of the material being mixed in the intensive mixer is 150 to 300 sec.
12. An apparatus for performing the process according to claim 1, which comprises a colloid mill and an intensive mixer installed immediately downstream thereof, the colloid mill exhibiting a clearance of 0.01 to 3 mm and operating with a peripheral speed of 10 to 40 m/sec, and the intensive mixer being a mixer with at least a co-rotating agitator blade shaft or counter-rotating agitator blade shafts or comprising an agitator ball mill, a jet mixer or a screw mixer and the residence time of the material mixed in the intensive mixer being 60 to 3000 seconds.
13. An apparatus according to claim 12, wherein the residence time of said material is 150 to 300 seconds.
CA000518992A 1985-10-02 1986-09-25 Process for preparing suspensions of solid lubricants Expired - Fee Related CA1272181A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CHGES.4249/85 1985-10-02
CH4249/85A CH665847A5 (en) 1985-10-02 1985-10-02 METHOD FOR SUSPENDING SOLID LUBRICANTS.

Publications (1)

Publication Number Publication Date
CA1272181A true CA1272181A (en) 1990-07-31

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ID=4272580

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000518992A Expired - Fee Related CA1272181A (en) 1985-10-02 1986-09-25 Process for preparing suspensions of solid lubricants

Country Status (14)

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US (1) US4735734A (en)
EP (1) EP0218989B1 (en)
JP (1) JPS6291229A (en)
CN (1) CN1006400B (en)
AT (1) ATE60249T1 (en)
CA (1) CA1272181A (en)
CH (1) CH665847A5 (en)
CS (1) CS261247B2 (en)
DD (1) DD249858A5 (en)
DE (1) DE3677127D1 (en)
ES (1) ES2020173B3 (en)
PL (1) PL261617A1 (en)
SU (1) SU1498378A3 (en)
ZA (1) ZA867265B (en)

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Also Published As

Publication number Publication date
CS261247B2 (en) 1989-01-12
CN1006400B (en) 1990-01-10
EP0218989A3 (en) 1989-04-26
CN86106627A (en) 1987-04-01
DD249858A5 (en) 1987-09-23
EP0218989A2 (en) 1987-04-22
ATE60249T1 (en) 1991-02-15
PL261617A1 (en) 1987-12-28
US4735734A (en) 1988-04-05
ES2020173B3 (en) 1991-08-01
EP0218989B1 (en) 1991-01-23
CH665847A5 (en) 1988-06-15
CS706186A2 (en) 1988-04-15
DE3677127D1 (en) 1991-02-28
SU1498378A3 (en) 1989-07-30
ZA867265B (en) 1987-05-27
JPS6291229A (en) 1987-04-25

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