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US20030164205A1 - Hot rolling process for rolling aluminium and aluminium alloys sheets - Google Patents

Hot rolling process for rolling aluminium and aluminium alloys sheets Download PDF

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Publication number
US20030164205A1
US20030164205A1 US10/182,490 US18249002A US2003164205A1 US 20030164205 A1 US20030164205 A1 US 20030164205A1 US 18249002 A US18249002 A US 18249002A US 2003164205 A1 US2003164205 A1 US 2003164205A1
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United States
Prior art keywords
water
hot rolling
oil composition
emulsion
rolling process
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Abandoned
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US10/182,490
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English (en)
Inventor
Francis Prince
Jean-Yves Claire
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M129/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/68Esters
    • C10M129/72Esters of polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00Lubricating compositions containing more than 10% water
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02Hydroxy compounds
    • C10M2207/021Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix 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
    • C10M2207/126Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/02Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2215/042Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04Phosphate esters
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/24Emulsion properties
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • C10N2040/242Hot working
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • C10N2040/244Metal working of specific metals
    • C10N2040/245Soft metals, e.g. aluminum

Definitions

  • the present invention relates to a hot rolling process for rolling aluminium and aluminium alloys sheets.
  • the invention also relates to a water-soluble aluminium and aluminium hot rolling oil composition, to a oil-in-water emulsion prepared therewith and to the use of said oil-in-water emulsion in a hot rolling process.
  • the aluminium and aluminium alloys rolling industry expresses the need to maximize the efficiency of their rolled metal manufacturing process. In general terms, this means that there is a wish to operate at higher rolling speeds and to produce more marketable products per operating shift. Additionally, there is also a wish to minimize the number of passes through the mill taken to achieve a given level of reduction. Both these routes require that quality and surface finish be not compromised.
  • the invention thus provides an oil composition for hot rolling mills that affords the following customer benefits:
  • the invention is effective on any type of hot rolling, be it reversible or not, on breakdown, tandem and combination mills.
  • the invention exhibits high reduction and rolling capabilities while providing an excellent strip surface finish when rolling at high speed.
  • the invention provides a hot rolling process for rolling aluminium and aluminium alloys sheets, comprising applying an effective amount of an oil-in-water emulsion comprising water and a water-soluble oil composition comprising a base stock oil and, based on the total weight of the water-soluble oil composition, from 1 to 80% and preferably from 3 to 30% by weight of di(2-ethylhexyl) adipate ester.
  • the oil composition further comprises, based on the total weight of the composition, from 0,05 to 20%, preferably from 0,1 to 5% by weight of a non-ionic surfactant, such as an ethylene oxide addition polymer.
  • a non-ionic surfactant such as an ethylene oxide addition polymer.
  • An example of such an ethylene oxide addition polymer is the ethylene oxide addition polymer sold by the company ICI under tradename Hypermerc® A60.
  • the oil composition further comprises, based on the total weight of the composition, from 1 to 30%, preferably from 5 to 20% of oleic acid. It is actually believed that the free oleic acid provides a better surface finish to the aluminium or aluminium alloy strip.
  • the invention further provides a water-soluble aluminium and aluminium alloys hot rolling oil composition.
  • the invention further provides a process for preparing the water-soluble oil composition.
  • the invention further provides an oil-in-water emulsion containing the oil composition and a process for preparing this emulsion.
  • the invention provides the use of the water-soluble oil composition of the invention to prepare emulsions intended to be used in a aluminium or aluminium alloy hot rolling process.
  • the invention provides the use of the emulsion in a hot rolling process.
  • FIG. 1 is a graph showing the applied rolling force versus the number of passes, first, when an emulsion of the prior art and then when an emulsion of the invention are used.
  • FIG. 2 is a graph showing the applied net rolling power versus the number of passes, first, when an emulsion of the prior art and then when an emulsion of the invention are used.
  • the water-soluble oil compositions of the invention are neat oil concentrates generally intended to be diluted in water to give oil-in-water emulsions.
  • the base stock oil is any oil typically used in the field of hot rolling. It can be paraffinic or naphthenic.
  • Paraffinic base oils are made from crude oils that have relatively high alkane contents (high paraffin and isoparaffin contents). Typical crudes are from the Middle East, North Sea, US mid-continent. The manufacturing process requires aromatics removal (usually by solvent extraction) and dewaxing. Paraffinic base oils are characterized by their good viscosity/temperature characteristics, i.e. high viscosity index, adequate low-temperature properties and good stability. They are often referred to as solvent neutrals, where solvent means that the base oil has been solvent-refined and neutral means that the oil is of neutral pH. An alternative designation is high viscosity index (HVI) base oil. They are available in full range of viscosities, from light spindle oils to viscous brightstock.
  • HVI high viscosity index
  • Naphthenic base oils have a naturally low pour point, are wax-free and have excellent solvent power. Solvent extraction and hydrotreatment can be used to reduce the polycyclic aromatic content.
  • a preferred base oil is a mixture of paraffinic and naphthenic oils.
  • the base oil typically has a viscosity from 7 to 150 cSt at 40° C., and preferably from 20 to 50 cSt at 40° C.
  • the water-soluble oil composition preferably comprises a trialkanolamine (C 2-4 ), preferably triethanolamine, the amount of which being such that all bindable trialkanolamine is bound to a part only of the oleic acid.
  • the aim of this embodiment is to ensure that there remains free oleic acid in the oil composition.
  • the water-soluble oil composition may comprise classical additives, such as surfactants, coupling agents or cosurfactants, friction reducing agents or lubricity agents, corrosion inhibitors or anti-oxidants, extreme-pressure and anti-wear agents, bactericides and fungicides, anti-foaming agents, anti-rust agents.
  • classical additives such as surfactants, coupling agents or cosurfactants, friction reducing agents or lubricity agents, corrosion inhibitors or anti-oxidants, extreme-pressure and anti-wear agents, bactericides and fungicides, anti-foaming agents, anti-rust agents.
  • anti-foaming agents are silicone based, especially polydimethylsiloxane.
  • Examples of corrosion inhibitors are hindered phenols and zinc dialkyldithiophosphates (ZDDP).
  • Examples of extreme-pressure and anti-wear agents are dilauryl phosphate, didodecyl phosphite, trialkylphosphate such as tri(2-ethylhexyl)phosphate, tricresylphosphate (TCP), zinc dialkyl(or diaryl)dithiophosphates (ZDDP), phospho-sulphurized fatty oils, zinc dialkyldithiocarbamate), mercaptobenzothiazole, sulphurized fatty oils, sulphurized terpenes, sulphurized oleic acid, alkyl and aryl polysulphides, sulphurized sperm oil, sulphurized mineral oil, sulphur chloride treated fatty oils, chlornaphta xanthate, cetyl chloride, chlorinated paraffinic oils, chlorinated paraffin wax sulphides, chlorinated paraffin wax, and zinc dialkyl(or diaryl)dithi
  • corrosion inhibitors or anti-oxidants are radical scavengers such as phenolic antioxidants (sterically hindered), aminic antioxidants, organo-copper salts, hydroperoxides decomposers, butylated hydroxytoluene.
  • radical scavengers such as phenolic antioxidants (sterically hindered), aminic antioxidants, organo-copper salts, hydroperoxides decomposers, butylated hydroxytoluene.
  • anti-rust agents are amine derivatives of alkenyl succinic anhydride.
  • friction reducing agents/lubricity agents are fatty acids (C 12-20 ) like lauric acid, oleic acid, palmitic acid, alkyl(C 6-10 ) alkylate(C 12-20 ) esters like di(2-ethyl-hexyl) adipate.
  • the balance being a mixture of naphthenic and paraffinic lube base oils.
  • the oil composition is prepared by blending the base oil and the other ingredients, preferably under stirring or with any mixing device, whilst controlling the temperature so that is does not exceed 50° C., and more preferably, 35° C.
  • An oil-in-water emulsion is prepared by diluting under stirring the oil composition of the invention in water. It is preferred to use deionized water which may previously have been warmed to around 35° C.
  • the emulsion generally comprises water and, based on the total volume of the emulsion, from 0.5 to 30%, preferably from 1 to 15%, by volume, of the oil composition.
  • the aluminium alloys to which the invention applies are any aluminum alloys, including 1000, 2000, 3000, 5000, 6000, 7000 series.
  • the hot rolling process can be the classical process.
  • the rolled metal temperature is generally around 600-650° C. for breakdown mills and around 400-500° C. for tandem mills.
  • the process is preferably carried out on a breakdown rolling mill, on a tandem rolling mill or on a finishing rolling mill.
  • the instant oil composition allows a significant reduction of the number of passes. With conventional prior art oils, the number of passes was typically 13.
  • the oil composition of the invention allows lowering this number to two passes, which is a significant improvement.
  • the emulsion preferably comprises, based on the total volume of the emulsion, from 2 to 4% by volume of the oil composition.
  • the emulsion preferably comprises, based on the total volume of the emulsion, from 5 to 7% by volume of the oil composition.
  • a composition is prepared by mixing the ingredients of Table 1 in the order in which they appear in this table.
  • the temperature is be maintained at a maximum of 35° C. to ensure a complete dissolution and homogeneisation of the ingredients without impairing the properties of the emulsion.
  • An emulsion is prepared by diluting under stirring the oil composition of Table 1 in deionized water prewarmed to 35° C. The characteristics of the obtained emulsion are given in Table 3. TABLE 3 Typical Emulsion Method characteristics Stability of the 6% Mobil 1) 1% cream (v/v) emulsion (at room temperature, for 20 hours) pH value of fresh 5% ASTM E 8.3 (v/v) emulsion at 20° C. 70-90
  • a blank is first prepared by diluting a prior art oil composition which has the composition set out in Table 4: TABLE 4 Ingredients Content (wt %) Paraffinic base oil (25 cSt at 40° C.) 48.5 Naphthenic base oil (115 cSt at 40° C.) 13.0 Naphthenic base oil (8 cSt at 40° C.) 20.0 Ditertiobutyl paracresol 0.2 Organic fatty acid (C 12 to C 18 ) 11.6 Dialkylene glycol 2.1 Trialkanol amine (C 2 to C 4 ) 2.6 Trialkylphosphate ester (C 3 to C 10 ) 2.0
  • Two emulsions are prepared by respectively diluting the oil compositions of the invention and of the prior art in dionized water.
  • motor output 45 kW or 67 kW
  • ingot dimensions 305 ⁇ 610 ⁇ 1650 mm
  • emulsion temperature 50° C.
  • a 100 cm (4-inch) thick block of AA5182 was given 5 rolling passes using the following nominal pass schedule. Mill speed was 18.3 m/min. All passes were in the east to west rolling direction. The mill gap setpoints were recorded for the first emulsion tested and then duplicated for the remaining emulsions. These settings were 1.27 mm below the nominal desired exit thickness on each pass.
  • Nominal Pass Schedule Pass 1 100 mm-83 mm Pass 2 83 mm-65 mm Pass 3 65 mm-50 mm Pass 4 50 mm-37 mm Pass 5 37 mm-25 mm
  • FIG. 1 is a graph showing the applied rolling force (in tons) applied on an aluminium alloy AA5182 versus the number of passes.
  • FIG. 2 is a graph showing the applied net rolling power (total power minus bearing losses, in kW) versus the number of passes.
  • a pilot anodizing line was used to anodize approximately 150 mm of the length of the 25 mm thick and 5 mm thick pieces (see above point 6) to highlight pickup and surface appearance.
  • the procedure was:
  • a plexiglass, gasketed fixture was attached and sealed to the center of the top work roll. This fixture includes a reservoir covering an area of 20.26 square centimeters of the roll surface.

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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)
  • Lubricants (AREA)
  • Metal Rolling (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)
US10/182,490 2000-02-08 2001-02-07 Hot rolling process for rolling aluminium and aluminium alloys sheets Abandoned US20030164205A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP00400351.3 2000-02-08
EP00400351A EP1123967A1 (de) 2000-02-08 2000-02-08 Wasserlösliche Zusammensetzungen für Warmwalzen von Aluminium und Aluminiumlegierungen

Publications (1)

Publication Number Publication Date
US20030164205A1 true US20030164205A1 (en) 2003-09-04

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US10/182,490 Abandoned US20030164205A1 (en) 2000-02-08 2001-02-07 Hot rolling process for rolling aluminium and aluminium alloys sheets

Country Status (10)

Country Link
US (1) US20030164205A1 (de)
EP (2) EP1123967A1 (de)
JP (1) JP2003522279A (de)
CN (1) CN1398291A (de)
AT (1) ATE276337T1 (de)
AU (2) AU4831001A (de)
BR (1) BR0108161A (de)
CA (1) CA2397841A1 (de)
DE (1) DE60105570T2 (de)
WO (1) WO2001059040A1 (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050181956A1 (en) * 2004-01-23 2005-08-18 Limited Liability Company "Vmpauto" Plating concentrate
US20060281646A1 (en) * 2003-03-03 2006-12-14 Oleksiak Thomas P Additive for cold rolling lubricants
WO2010009326A1 (en) * 2008-07-16 2010-01-21 Fata Hunter, Inc. Method for twin roll casting of aluminum clad magnesium
US11945008B2 (en) * 2018-03-27 2024-04-02 Hydro Aluminum Rolled Products Gmbh Roller cleaning method and roller cleaning machine

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US6818609B2 (en) 2002-08-21 2004-11-16 Houghton Technical Corp. Metal deformation compositions and uses thereof
JP2005187650A (ja) * 2003-12-25 2005-07-14 Nippon Oil Corp 金属加工用油剤
DE102007001190A1 (de) * 2007-01-05 2008-07-10 Wet-Protect-Gmbh Zusammensetzung zum Schutz vor Feuchtigkeit, insbesondere Korrosionsschutz
DE102007001189A1 (de) * 2007-01-05 2008-07-10 Wet-Protect-Gmbh Zusammensetzung zum Schutz vor Feuchtigkeit, insbesondere Korrosionsschutz
CN102746924B (zh) * 2011-04-22 2014-04-09 中国石油化工股份有限公司 一种铝热轧油
CN102757848B (zh) * 2011-04-29 2014-04-23 中国石油化工股份有限公司 水溶性轧制液组合物及其用途
CN106433916A (zh) * 2016-09-21 2017-02-22 广西大学 一种环境友好铝及其合金热粗轧乳化液的组合物
CN107325871B (zh) * 2017-07-25 2020-03-13 山东迈拓凯尔新材料科技有限公司 一种用于铝合金板带材热轧工艺的润滑剂
CN107267271B (zh) * 2017-07-25 2020-03-13 山东迈拓凯尔新材料科技有限公司 一种用于铝合金板带材热轧工艺的润滑剂
CN115302134B (zh) * 2022-03-17 2024-08-06 山东迈拓凯尔新材料科技有限公司 一种用于焊接用铝箔的表面防护组合物

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060281646A1 (en) * 2003-03-03 2006-12-14 Oleksiak Thomas P Additive for cold rolling lubricants
US20050181956A1 (en) * 2004-01-23 2005-08-18 Limited Liability Company "Vmpauto" Plating concentrate
US7375060B2 (en) * 2004-01-23 2008-05-20 Vmpauto Plating concentrate
WO2010009326A1 (en) * 2008-07-16 2010-01-21 Fata Hunter, Inc. Method for twin roll casting of aluminum clad magnesium
US20100015469A1 (en) * 2008-07-16 2010-01-21 Romanowski Christopher A Method for twin roll casting of aluminum clad magnesium
US8122940B2 (en) * 2008-07-16 2012-02-28 Fata Hunter, Inc. Method for twin roll casting of aluminum clad magnesium
US11945008B2 (en) * 2018-03-27 2024-04-02 Hydro Aluminum Rolled Products Gmbh Roller cleaning method and roller cleaning machine

Also Published As

Publication number Publication date
CA2397841A1 (en) 2001-08-16
ATE276337T1 (de) 2004-10-15
CN1398291A (zh) 2003-02-19
AU2001248310B2 (en) 2005-01-27
AU4831001A (en) 2001-08-20
BR0108161A (pt) 2003-01-21
EP1268719A1 (de) 2003-01-02
EP1268719B1 (de) 2004-09-15
EP1123967A1 (de) 2001-08-16
JP2003522279A (ja) 2003-07-22
DE60105570T2 (de) 2005-09-29
WO2001059040A1 (en) 2001-08-16
DE60105570D1 (de) 2004-10-21

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