EP0398201A1 - Compositions et procédé pour la préparation de métaux destinés au travail à froid - Google Patents

Compositions et procédé pour la préparation de métaux destinés au travail à froid Download PDF

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Publication number
EP0398201A1
EP0398201A1 EP90108988A EP90108988A EP0398201A1 EP 0398201 A1 EP0398201 A1 EP 0398201A1 EP 90108988 A EP90108988 A EP 90108988A EP 90108988 A EP90108988 A EP 90108988A EP 0398201 A1 EP0398201 A1 EP 0398201A1
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EP
European Patent Office
Prior art keywords
solution
concentration
complexing agent
component
lubricating
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.)
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Application number
EP90108988A
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German (de)
English (en)
Inventor
Paul A. Kulongowski
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Henkel Corp
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Henkel Corp
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Publication of EP0398201A1 publication Critical patent/EP0398201A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment
    • 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
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/04—Hydroxy compounds
    • C10M129/06—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/08—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least 2 hydroxy groups
    • 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
    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
    • C10M129/40—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms monocarboxylic
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • 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
    • C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M133/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M133/08—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M145/00—Lubricating compositions characterised by the additive being a macromolecular compound containing oxygen
    • C10M145/18—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/24—Polyethers
    • C10M145/26—Polyoxyalkylenes
    • C10M145/28—Polyoxyalkylenes of alkylene oxides containing 2 carbon atoms only
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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    • C10M145/18—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/24—Polyethers
    • C10M145/26—Polyoxyalkylenes
    • C10M145/30—Polyoxyalkylenes of alkylene oxides containing 3 carbon atoms only
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    • C10M145/24—Polyethers
    • C10M145/26—Polyoxyalkylenes
    • C10M145/34—Polyoxyalkylenes of two or more specified different types
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    • C10M173/00—Lubricating compositions containing more than 10% water
    • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02—Water
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    • 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
    • C10M2207/02—Hydroxy compounds
    • C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
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    • 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
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • 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
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    • 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
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    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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    • 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
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    • 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
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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    • 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
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/105—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only
    • 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
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/107—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of two or more specified different alkylene oxides covered by groups C10M2209/104 - C10M2209/106
    • C—CHEMISTRY; METALLURGY
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2215/042—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
    • C—CHEMISTRY; METALLURGY
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
    • C—CHEMISTRY; METALLURGY
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/241—Manufacturing joint-less pipes
    • C—CHEMISTRY; METALLURGY
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
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    • C10N2040/242—Hot working
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
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    • C10N2040/243—Cold working
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    • C10N2040/245—Soft metals, e.g. aluminum
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    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/01—Emulsions, colloids, or micelles
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    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • the present invention relates to compositions and methods for lubricating phosphated metal surfaces prior to drawing or other cold forming processes on the lubricated metal.
  • phosphating from solutions that contain zinc ions, and sometimes also contain calcium, nickel, manganese, copper, and/or other divalent metal ions, is preferred as the phosphating step.
  • An aqueous solution of alkali metal soap capable of reacting with zinc phosphate to produce a very favorable form of zinc stearate called "reacted lube" in situ on the surface, is generally preferred for the lubrication stage.
  • the reactive lubrication process can be improved by using aqueous lubricating solutions that, in addition to soluble metallic soaps having aliphatic anions with 8 to 22 carbon atoms and hydrolysis resistant complexing agents as taught by Nuss, contain water soluble or dispersible organic compounds that are stable in solution or dispersion under normal conditions of applying lubricant to phosphated surfaces and that contain at least one hydroxyl or ether oxygen for each eight carbon atoms.
  • This latter component is referred to briefly hereinafter as "OSOC” (for "oxygen­ated soluble organic compound”).
  • OSOC oxygen only oxygen atom of a carboxyl or car­boxylate group is considered to be an ether or hydroxyl oxygen.
  • the OSOC component molecules contain at least one hydroxyl or ether oxygen for each two carbon atoms.
  • the water soluble soap to be used in this invention may be any material known for such a use in the art, including technical sodium stearate containing from 40 to 90 % of C18 soaps, as used in some examples of the Nuss patent noted above, but technical mixtures including a higher proportion of sodium stearate are generally most highly preferred.
  • the complexing agent similarly may be any material known as such in the art, but preferably is selected from the group consisting of ethylene diaminetetraacetic acid (hereinafter “EDTA”) and its salts, nitrilotriacetic acid (hereinafter “NTA”) and its salts, N-­hydroxyethylethylene diaminetriacetic acid (hereinafter “NEDTA”) and its salts, diethylene triamine pentaacetic acid and its salts, diethanol glycine, and a material having CAS Registry No.
  • EDTA ethylene diaminetetraacetic acid
  • NDA nitrilotriacetic acid
  • NEDTA N-­hydroxyethylethylene diaminetriacetic acid
  • diethylene triamine pentaacetic acid and its salts diethanol glycine
  • the OSOC component is preferably selected from the group consisting of alkylene glycols, polyalkylene glycols, glycol ethers, ethoxylated alcohols, polymers and copolymers of ethylene oxide and propylene oxide, and glycerin.
  • mixtures of materials from the preferred group are equally as preferred as single chemical types of materials, unless otherwise noted.
  • PEG 4000 Poly(ethylene glycol), hereinafter "PEG 4000”
  • the ratio of the concentration of the complexing agent to the concentra­tion of the OSOC component lie within the range of 1 - 5, more preferably within the range of 2.5 to 3.5, and most preferably within the range of 2.9 - 3.1.
  • concentration of reactive soap in the solutions according to the invention lie within the range of 5 to 150 g/L of solution.
  • concentrations of complexing agent are determined by balancing several considerations, as noted further below.
  • a process embodiment of this invention may be per­formed by contacting a suitable phosphated surface with a lubricating solution according to the invention, as gener­ally described above. It is believed that there is no advantage from the presence of the complexing agent in the very early stages of use of a freshly prepared lubricating solution, before any significant amounts of divalent metal ions have accumulated in the lubricating solution as a result of its exposure to a phosphated surface.
  • An ideal lubricating process would maintain a consistent, high coating weight level of reacted lube, avoid the introduction into the lubricating solution of byproducts that interfere with the desired reaction between constituents of the phosphate coating and constituents of the lubricating solution, and remove little or none of the phosphate coating that was on the metal when it entered the lubricating solution.
  • No actual lubricating solution known can accomplish such ideal lubrication, but preferable practical baths tend toward maximizing the ratio of reacted lube coating weight to conversion coating loss, with consideration toward optimizing the ratio of reacted lube coating weight to unreacted lube coating weight.
  • the most preferred embodiments of the process according to the invention utilize complexing agents and OSOC component in lubricating baths from near the beginning of use of a freshly made bath.
  • satisfactory operating conditions can generally be attained by selecting an upper bound on the concentration of "titratable metals", as defined exactly below, and by adding complexing agent after each measurement of titratable metals concentration that is higher than the selected upper limit.
  • the amount of complexing agent should be at least sufficient to bring the concentration of titratable metals under a selected upper limit value.
  • the best upper limit value may be determined most precisely from experience with each particular lubricating solution composition and type of base metal and phosphate coating lubricated, but in general an upper limit of 0.05 % by weight or less is preferred.
  • lubricating processes and solutions according to this invention should be controlled, from the beginning of use of a freshly made solution, so that the concentration of titratable metals never rises above its selected upper limit during the entire period of use of a lubricating solution according to the invention. Therefore, it is more preferable to add sufficient complexing agent, after each measurement of titratable metals, to bring the titratable metals concentration below two-thirds or less of its upper limit value immediately after addition, and to measure the titratable metals concentration sufficiently often so as to assure that the concentration never rises above the selected upper limit. It is generally most preferable in such situations to add sufficient complexing agent to bring the titratable metals concentration below 0.01 % by weight after each measurement of a higher value for this concentration.
  • the process according to this invention may also be usefully embodied by starting with a conventional lubricating solution, containing little or no complexing agent, that has already been used for phosphating to a sufficient extent to accumulate a concentration of titratable metals greater than the desired upper limit for processes according to this invention.
  • a conventional lubricating solution containing little or no complexing agent, that has already been used for phosphating to a sufficient extent to accumulate a concentration of titratable metals greater than the desired upper limit for processes according to this invention.
  • Such a large amount of complexing agent may cause excessive conversion coating losses during lubricating.
  • the process according to the invention is preferably continued in the same general manner as described above for embodiments in which complexing agent is added to the lubricating solution from the beginning of its use, except that the additions of complexing agent should be limited so that they do not reduce the concentration of titratable metals below three-quarters of their concentration after the initial addition of complexing agent.
  • the OSOC component preferably should be added to the lubricating solution at the same time as the complexing agent, in sufficient amount to maintain the ratio between these two components within the already stated preferred range.
  • the temperature of the lubricating solution and the time of contact between the lubricating solution and the phosphated surface in any process according to this inven­tion are generally within the range of such conditions as used in the art for reactive lubrication.
  • the temperature is usually preferably between 70 and 90° C and the time of contact between 1 and 10 minutes.
  • the temperature of the lubricating solutions was maintained at 79° C, and phosphated metal specimens were contacted with the solution for 5 minutes, then dried for 15 minutes in an oven maintained at 121° C.
  • the test specimens were Type 1010 cold rolled steel that had been phosphated by use of Bonderite® 181x, a commercial zinc phosphating solution available from the Parker+Amchem Division of Henkel Corpor­ation, Madison Heights, Michigan, in a solution maintained with a total acid number of 30 points.
  • the average phosphate coating weight was 12.8 grams per square meter of surface (g/m2) for all the panels except those used in Experiment 5, for which the average coating weight was 21 g/m2.
  • Read mg Fe from a standard curve is obtained by the following procedure: To a series of 100-ml glass-stoppered cylinders, add 0, 0.5, 1.0, 1.5, and 2.0 ml of "Standard Solution 91", a solution of 0.03 % by weight ferrous sulfate and 2 % by weight sulfuric acid in water. These amounts correspond to 0, 0.5, 0.1, 0.15, and 0.2 mg Fe. Then add 5 ml of "Reagent Solution 65" and 10 ml of "Indicator 19" to each cylinder. Dilute to 100 ml with deionized water and mix by upending twice.
  • the "titratable metals" concentration of the solution is then defined as: % Zn + (1.64)(% Ca + Mg) + (1.16)(% Fe).
  • the viscosity of the lubricating solutions was measured with a #2 Zahn Cup.
  • Coating weights and other related characteristics of the samples are defined and/or were determined as follows:
  • An initial lubricating solution as freshly made up consisted of 3.6 % by weight in water of a sodium soap mixture that was made by neutralizing with sodium hydroxide a technical fatty acid mixture that is at least 95 % stearic acid.
  • Solution No. 1 was this freshly made solution, while solutions Nos. 2 - 5 had been aged through actual use to lubricate phosphated surfaces. Characteris­tics of the solutions at the start are given in Table 1. The following experiments were then performed:
  • Experiment 2 shows the effect the addition of EDTA tetrasodium salt has on the coating process.
  • solution #4 contains the highest level of metal ions.
  • the amount of nonreacted lube greatly increases, due to the increase in solution viscosity from 14 to 16 seconds.
  • Experiment 3 shows how the polyethylene glycol not only returns the solution to a lower viscosity but also improves the ratio of reacted lube to nonreacted lube and of reacted lube to conversion coating loss.
  • the nonreacted lube weights came down while the much more desirable reacted lube weights increased, even though the conversion coating loss stayed about the same.
  • Experiment 4 shows how the proper initial addition of EDTA tetrasodium salt and polyethylene glycol should preferably be based on the initial divalent metal ion concentration to optimize coating weights.
  • the addition of large amounts of EDTA tetrasodium salt, as exemplified by the third addition in this experiment, will increase conversion coating loss but will not improve lube coating weights very much, once substantially all of the divalent metal cations present have been complexed.
  • the second addition of complexing agent thus leaves this particular solution with more desirable lubricating properties overall than are produced by the third addition, even though the concentration of titratable metals remains well above 0.01 % by weight after the second addition but is below that after the third addition.
  • this third addition of EDTA brings the solution outside the most preferred range of complexing agent concentrations, even though still within the scope of the invention.
  • the invention can be useful in solutions containing up to 0.2 weight % of such titratable divalent metal ions.

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EP90108988A 1989-05-18 1990-05-12 Compositions et procédé pour la préparation de métaux destinés au travail à froid Withdrawn EP0398201A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6852678B2 (en) 1996-11-18 2005-02-08 Mec International Corporation Water-based lubricants containing sulfur as a coordinating atom and uses thereof
US6858568B2 (en) 2000-12-21 2005-02-22 Mec International Corporation Metal lubricants containing a bridge complex

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW385332B (en) * 1997-02-27 2000-03-21 Idemitsu Kosan Co Refrigerating oil composition
CN1058519C (zh) * 1997-06-23 2000-11-15 中国石化兰州炼油化工总厂 含破乳剂的船用曲轴箱油组合物

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4199381A (en) * 1977-08-16 1980-04-22 Oxy Metal Industries Corporation Preparation of metals for cold forming
US4688411A (en) * 1984-05-21 1987-08-25 Sumitomo Metal Industries, Inc. Method for continuous drawing of wire rod
US4728373A (en) * 1985-09-19 1988-03-01 Nihon Parkerizing Co., Ltd. Solution and process for cold forming titanium
US4780153A (en) * 1987-02-06 1988-10-25 Guhde Donald J Chromium-containing low-cure coating composition
EP0291891A1 (fr) * 1987-05-16 1988-11-23 Nihon Parkerizing Co., Ltd. Procédé pour appliquer des couches de conversion sur le titane

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4199381A (en) * 1977-08-16 1980-04-22 Oxy Metal Industries Corporation Preparation of metals for cold forming
US4688411A (en) * 1984-05-21 1987-08-25 Sumitomo Metal Industries, Inc. Method for continuous drawing of wire rod
US4728373A (en) * 1985-09-19 1988-03-01 Nihon Parkerizing Co., Ltd. Solution and process for cold forming titanium
US4780153A (en) * 1987-02-06 1988-10-25 Guhde Donald J Chromium-containing low-cure coating composition
EP0291891A1 (fr) * 1987-05-16 1988-11-23 Nihon Parkerizing Co., Ltd. Procédé pour appliquer des couches de conversion sur le titane

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6852678B2 (en) 1996-11-18 2005-02-08 Mec International Corporation Water-based lubricants containing sulfur as a coordinating atom and uses thereof
US6858568B2 (en) 2000-12-21 2005-02-22 Mec International Corporation Metal lubricants containing a bridge complex

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ZA903494B (en) 1991-02-27
CN1047331A (zh) 1990-11-28
BR9002320A (pt) 1991-08-06
CA2017014A1 (fr) 1990-11-18
JPH02305897A (ja) 1990-12-19
AU624710B2 (en) 1992-06-18
AU5507390A (en) 1990-11-22

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