WO2000052226A1 - Composition and process for treating metal surfaces - Google Patents
Composition and process for treating metal surfaces Download PDFInfo
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- WO2000052226A1 WO2000052226A1 PCT/US2000/005766 US0005766W WO0052226A1 WO 2000052226 A1 WO2000052226 A1 WO 2000052226A1 US 0005766 W US0005766 W US 0005766W WO 0052226 A1 WO0052226 A1 WO 0052226A1
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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
- C10N2040/243—Cold working
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/20—Metal working
- C10N2040/244—Metal working of specific metals
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/20—Metal working
- C10N2040/244—Metal working of specific metals
- C10N2040/245—Soft metals, e.g. aluminum
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/20—Metal working
- C10N2040/244—Metal working of specific metals
- C10N2040/246—Iron or steel
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/20—Metal working
- C10N2040/244—Metal working of specific metals
- C10N2040/247—Stainless steel
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/32—Wires, ropes or cables lubricants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/34—Lubricating-sealants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Definitions
- This invention relates to treatment of a metal surface with an aqueous liquid composition that, before and/or during drying of the liquid composition into place on the surface, spontaneously reacts with the metal surface, without any application of electromot- ive force from an external source, to produce on the metal a surface with better corrosion resistance than the original untreated metal surface More particularly, this invention is related to a process that provides a corrosion protective treatment that also provides lubricating qualities, so that mechanical deformation of the surface can be more readily accomplished, without unacceptable damage to the surface, than can the same me- chanical deformation of the original untreated metal surface.
- the metal surface treated is an alloy of zinc and aluminum, and/or the lubricating quality of the surface is sufficiently good that a metal sheet or coil having at least one surface modified by the treatment can be roll formed and/or press molded without unacceptable surface damage and without the use of any additional lubricant material on the part of the treated metal surface that is being mechanically deformed.
- Aluminum-zinc alloy coated steel sheets are steel sheets which have been coated with an alloy which consists of 4 - 75 % by weight of aluminum, the remainder being mainly zinc with traces of other components such as silicon, magnesium, cerium, lanthanum, or the like.
- low aluminum-zinc alloy coated steel sheets which are coated with an alloy consisting of 4 - 10 % by weight of aluminum, the remainder consisting mainly of zinc with traces of magnesium, cerium, and/or lanthanum
- high aluminum-zinc alloy coated steel sheets which are coated with an alloy consisting of 55 % by weight of aluminum, 43.4 % by weight of zinc, and 1.6 % by weight of silicon.
- the corrosion resistance is improved by a factor of some 1 5 - 2 times in the case of the low aluminum-zinc coated steel sheets and by a factor of some 3 - 6 times in the case of the high aluminum-zinc alloy coated steel sheets.
- the high aluminum-zinc alloy coated steel sheets also have heat reflecting properties and excel- lent resistance to heat.
- these aluminum-zinc alloy coated steel sheets have found wide application as building materials in the form of roofing and walling materials in civil engineering applications, e g , as guard rails, sound insulating barriers, anti-snow fencing, or drainage gullies, as materials for automo- biles, domestic appliances, and industrial machinery and, after having been painted, as replacements for painted steel sheets.
- the coated layer on these aluminum-zinc alloy coated steel sheets provides less effective lubrication than does the substantially pure zinc such as is found on the surface of hot-dip galvanized steel when roll forming or press molding these materials.
- the surface of aluminum-zinc alloy is more susceptible to damage; the coated layer may become fused onto the forming rolls or the pressing dies as a result of the heat which is generated by friction during such operations; and metal powder which has become detached from the aluminum-zinc alloy coated sheet steel may become attached to the forming rolls or the pressing dies. This powder may accumulate in the corner parts of a molded product, or it may cause defects that blemish the external appearance of the product.
- the surface may be so slippery that an initially cylindrical coil of the finished material can readily be distorted by the force of -gravity into a cone shape unless it is maintained strict- ly horizontal at all times when not mechanically restrained from such shape deformation; anything placed on an inclined surface of the coated lubricated material can more readily slip off than if the oil or wax were not present; and, if a coating is to be applied to the aluminum-zinc coated steel sheet after the shaping process, it is usually essential that all of the lubricating oil should be cleaned from the surface before applying any subse- quent coating. Removing a lubricating oil or wax from the surface to a sufficient degree to assure uniformly good adhesion of the coating applied over it often is very difficult.
- the lubricating oil becomes attached to the forming rolls or the pressing dies and if, at a later time, surface coated steel sheet is shaped using these same forming rolls or pressing dies, the lubricating oil often is transferred to the coated surfaces of these coated steel sheets, which are thereby stained. Any metal powder which is produced during the shaping process can become attached to the coated surface by way of the lubricating oil, so that it is necessary to clean the forming rolls or pressing dies thoroughly before carrying out such operations in order to prevent the occurrence of this type of contamination; such cleaning is very troublesome.
- a major object of this invention is to provide a surface layer on metal substrates, particularly those of aluminum-zinc alloy, that will more reliably permit press and/or roll forming without the need for any additional lubrication with materials that (i) diminish the adhesion or blemish the surface appearance of a subsequently applied coating and/or (ii) make the surface so slippery as to cause substantial practical difficulties in further processing or use of the metal with a surface treatment formed according to this invention.
- materials that (i) diminish the adhesion or blemish the surface appearance of a subsequently applied coating and/or (ii) make the surface so slippery as to cause substantial practical difficulties in further processing or use of the metal with a surface treatment formed according to this invention.
- aqueous liquid composition that comprises, preferably consists essentially of, or more preferably consists of, water and the following components: (A) dissolved, dispersed, or both dissolved and dispersed organic film-forming resin; (B) dissolved, dispersed, or both dissolved and dispersed wax that is not part of immediately previously recited component (A); and
- a "dissolved, dispersed, or both dissolved and dispersed film-forming resin” means a material that satisfies the following condition: when: (i) the resin is dissolved, dispersed, or both dissolved and dispersed in an aqueous medium to form a liquid solution/dispersion that contains at least
- melt is defined as a substance that: (i) is a plastic solid at 25 °C under normal atmospheric pressure and (ii) melts in contact with the natural ambient atmosphere without visually evident decomposition at a temperature that is at least 55 °C.
- Component (A) preferably is selected from resins that, after drying from any solution/dispersion in which they may initially be present, are not soluble in water at 25 °C to an extent greater than, with increasing preference in the order given, 1.0, 0.5, 0.20, 0.10, 0.050, 0.020, 0.010, 0.0050, 0.0020, 0.0010, 0.00050, 0.00020, or 0.00010 % of the resin in water.
- component (A) preferably is selected from polymers of vinyl monomers selected from the group consisting of hydrocarbons, halohydrocarbons, acrylic acid, methacrylic acid, maleic acid, and all esters, amides, and nitriles of organic acids. (Whether before or after polymerization, salts of any of these acids are to be understood as equivalent to the acids themselves.) If these polymers, as is usually preferred, have as low a solubility in water before drying as they are preferred to have after drying, the resins will be predominantly dispersed rather than dissolved in the treatment composition. In such dispersions, a surfactant is normally required as a dispersing agent.
- surfactants commonly used for this purpose in some (but not all) commercially supplied latexes, the preferred source for component (A), have not been observed to have any harmful effect on the properties of the compositions prepared with latexes containing them and if present are part of optional component (E) as described above, unless they are copolymerized into the polymer resin itself, in which instance they are part of component (A).
- component (A) is selected from polymers of monomers selected from the group consisting of acrylic acid, methacrylic acid, maleic acid, the esters of all of these acids, acrylonitrile, methacrylonitrile, acrylamide, and methacrylamide and still more preferably, in such polymers, the total number of millimoles of carboxylic acid and carboxylate salt moieties per gram of the dried resin is at least, with increasing prefer- ence in the order given, 0.030, 0.040, 0.050, 0.070, 0.080, 0.090, 0.100, 0.110, 0.120,
- 0.130, 0.135, or 0.140 independently preferably is not more than, with increasing preference in the order given, 1.5, 1 .0, 0.50, 0.40, 0.35, 0.30, 0.27, 0.24, 0.22, 0.200, 0.190, 0.180, 0.170, or 0.160.
- polymers of component (A) preferably have a glass transition temperature that is not more than, with increasing preference in the order given, 30, 27, 25, 23, 21 , 19, 17, or 15 °C.
- a wax to be used as component (B) in a composition or process according to this invention preferably is predominantly an organic substance selected from the group consisting of hydrocarbons, halohydrocarbons, halocarbons, alcohols, ethers, carboxylic acids, esters of carboxylic acids, ketones, and aldehydes. More preferably, the wax is polyethylene. Most if not all of the preferred waxes have scant solubility in water, and therefore are preferably added as dispersions to a mixture that constitutes, or after further additions will constitute, a composition according to the invention. Commercially available dispersions with fine dispersed particle size are preferably used.
- the average particle size of a dispersion of wax that is part of component (B) in a composition according to the invention preferably is not more than, with increasing preference in the order given, 50, 40, 30, 20, 10, 5, 2, 1 .0, 0.5, 0.20, 0.15, 0.12, 0.10, 0.08, or 0.06 micrometres.
- a dispersing agent required for a stable dispersion of this type; the dispersing agents in some but not all commercially supplied dispersions do not have any detrimental effect on a composition or process according to the invention; and when a dispersing agent for the wax component in a composition used according to the invention is present, this dispersing agent usually forms part of optional component (E).
- the melting point of a wax used in this in- vention preferably is at least, with increasing preference in the order given, 57, 65, 75,
- wax component (B) A substantial amount of wax component (B) is required to obtain the maximum resistance to damage in forming the finished product, but too large a fraction of wax can be disadvantageous.
- too much wax may reduce the corrosion resistance, if the wax by itself does not form a continuous protective coating as the acrylic component (A) does, make a substrate surface so slippery that it is very difficult to keep it coiled and/or to keep anything placed on an inclined surface of the coated substrate from sliding off; and/or cause undesired adhesion of the coated surface to another surface with which it is in contact, especially if the wax is low in melting point and the coated surface is exposed to heat while or shortly before it is in contact with another surface from which it is desired later to separate it.
- the ratio by mass, on a dried basis, of wax component (B) to acrylate component (A) preferably is at least, with increasing preference in the order given, 0.020:1 .00, 0.040-1.00, 0.050:1.00, 0.060:1 .00, 0.065:1.00, 0.070:1.00, 0.075:1.00, 0.080:1.00, 0.085.1 00, 0.090:1.00, 0.095:1.00, 0.100.1.00, or
- 0.103:1.00 and independently preferably is not more than, with increasing preference in the order given, 0.50:1.00, 0.40:1.00, 0.30:1.00, 0.25-1 00, 0.20:1.00, 0.15:1.00, 0.13:1.00, or 0.1 1 :1.00.
- Any water soluble source of hexavalent chromium atoms may be used to provide necessary component (C) according to the invention.
- Examples include chromic acid
- ammonium bichromate potassium bichromate, sodium bichromate, ammonium chromate, potassium chromate, sodium chromate, and the like
- ammonium salts and/or chromic acid is preferred, in order to avoid the presence in a composition according to the invention of any non-volatile alkali component.
- ammonium salts are preferred for at least part of component (C), but they are, at least for economy, preferably formed in situ by adding aqueous ammonia to an aqueous solution of chromic acid.
- the concentration of chromium in a composition according to the invention is usually measured as its stoichiomet ⁇ c equivalent as CrO 3 , and this stoichiomet ⁇ c equivalent preferably has a ratio to the concentration of component (A) (on a dry basis) in the same composition that is at least, with increasing preference in the order given, 0.0010:1.00, 0.0020:1.00, 0.0050:1.00, 0.0075:1.00, 0.0100:1.00, 0.0110:1.00, 0.0120:1.00, 0.0130:1.00, 0.0135:1.00, 0.0140:1.00, 0.0145:1.00, 0.0150:1.00, 0.0155:1.00, 0.0158:1.00, or 0.0162:1.00 and independently preferably is not more than, with increasing preference in the order given, 0.50:1.00,
- the treated material usually has inadequate corrosion resistance and is often subject to blackening, while if the ratio of hexavalent chromium to acrylate is too large, the treatment composition may become unstable, will definitely generate higher pollution and/or pollution abatement costs if used in the large majority of jurisdictions where chromium is considered polluting, and will decrease the likelihood of achieving a transparent coating as is usually desired.
- a working treatment composition according to the invention preferably has a pH value that is at least, with increasing preference in the order given, 3.0, 4.0, 5.0, 5.5, 6.0, 6.5, 7.0, or 7.5 and independently preferably is not more than, with increasing preference in the order given, 1 1 , 10.5, 10.0, 9.6, 9.2, 9.0, 8.8, 8.6, or 8.4. If the pH is too high or too low, the composition is likely to be unstable, because of precipitation and/or coagulation of at least part of its constituents.
- an alka- linizing agent will usually be required as optional component (D) in order to achieve a pH value of 8.4 or more when that is desired.
- Any alkaline material may be used, but volatile ones such as ammonia and amines, for example, monoethylamine, diethylamine, triethyl- amine, and the like, and alkanolamines such as monoethanolamine, diethanolamine, and triethanolamine are preferred. At least for economy, simple ammonia, usually added as a concentrated solution in water, is most preferred.
- a fluorinated surfactant more preferably a fluorinated anionic surfactant, most preferably a fluorinated alkyl carboxylate salt surfactant in which at least 80 % of the carboxylate groups have at least 8 carbon atoms, is preferred.
- the concentration of fluorinated surfactant in a working composition according to the invention preferably is at least, with increasing preference in the order given, 0.0010, 0.0020, 0.0030, 0.0040, 0.0050, 0.0060, or 0.0070 % of the total composition and independently preferably is not more than, with increasing preference in the order given, 0.080, 0.060, 0.050, 0.040, 0.030, 0.020, 0.015, 0.010, 0.0090, or 0.0080 % of the total composition.
- a surfactant may also be needed in some instances for abatement of foaming, particularly if preferred amounts and types of component (G) as described below are present in the working composition.
- any antifoam agent used preferably is a non-ionic surfactant and more preferably is selected from the group consisting of poly(oxyalkylene) polymers, ethoxylates of organic substances containing at least one phenol moiety per molecule, and organosiloxane polymers.
- composition according to the invention may be preferred to reduce spontaneous, at least temporary adhesion between a surface treated according to the invention and another surface, optionally also treated according to the invention, which contacts the surface treated according to the invention.
- This phenomenon often called “blocking", is particularly troublesome when surfaces treated according to the invention are wound into a coil that is later unwound before use.
- the compression inherent in winding favors at least temporary adhesion between the surfac- es. If such adhesion occurs, unwinding can cause transfer of coating from one portion of the treated surface to some other surface, thereby producing unsatisfactory coating uniformity.
- blocking can be prevented by including in a composition according to the invention at least one of the following types of surfactants: a silicone and/or ethoxylated silicone polymer in an amount having a ratio to the total solids content of the composition that is at least, with increasing preference in the order given, 0.0010:1.00, 0.0020:1 .00, 0.0030:1.00, 0.0040:1.00, 0.0050:1.00, 0.0080:1.00, 0.010:1.00, 0.015:1.00, 0.020:1.00, 0.023:1.00, or
- 0.025:1.0 and independently, at least for economy preferably is not more than, with increasing preference in the order given, 1.0:1.00, 0.80:1.00, 0.60:1.00, 0.50:1.00, 0.45:1.00, 0.40:1.00, 0.35:1.00, 0.30:1.00, 0.25:1.00, 0.20:1.00, 0.15:1.00, 0.12:1.00, 0.10:1.00, or 0.075:1.00; and - a fluorinated organic surfactant, preferably an anionic surfactant, in an amount having a ratio to the total solids content of the composition that is at least, with increasing preference in the order given, 0.0002:1.00, 0.0004:1.00, 0.0006:1.00, 0.0008:1.00, 0.0010:1.00, 0.0012:1.00, 0.0014:1.00, or 0.0016:1.0 and independently, at least for economy, preferably is not more than, with increasing preference in the order given, 0.010:1 .00, 0.0075
- the fluorinated surfactants have the property that they do not substantially reduce the static frictional properties of the surfaces coated according to the invention, so that the undesired "telescoping" of a coil of substrate treated according to the invention is less likely to occur.
- Silicone polymers are more consistent in preventing blocking but do cause reduced static frictional properties of the surfaces coated with them. A choice between these two types of blocking prevention may be made on this basis.
- Optional component (G) of organic solvent may not be needed and when not needed is preferably omitted for economy and avoidance of pollution problems and/or pollution abatement expense. There are at least three reasons, however, why organic solvents may be needed in a composition according to this invention in some instances.
- desired constituents of components (A) and/or (B) may require the presence of organic solvent as an aid in practical preparation of a composition according to the invention.
- the amount of organic solvent added for this purpose is preferably kept to the minimum required.
- an organic solvent may be useful in removing contaminants from the substrate simultaneously with forming the desired protective coating according to the invention, but ordinarily better results will be achieved if the substrate is conventionally cleaned before any contact with a composition according to this invention.
- component (G) may be needed to avoid cracking of the coating formed in a process according to the invention. Component (G) is unlikely to be needed for this reason if the glass transition temperature of component (A) is not more than 17 °C and is likely to be needed if the glass transition temperature of component (A) is more than 30 °C.
- this component is preferably selected from the group consisting of: esters with a structure that can be made by completely esterifying orthophosphor- ic acid or sulfuric acid with at least one monoalcohol, which may include halogen atoms and/or ether oxygen atoms in its molecules; and glycols, polyglycols, and the ethers and esters of glycols and polyglycols, i.e., molecules that conform to the general chemical formula (I):
- each of R 1 and R 4 which may be the same or different, represents one of a hydrogen moiety, a monovalent hydrocarbon, halohydrocarbon, or halocarbon moiety, and a monovalent acyl or halo-substituted acyl moiety; each of R 2 and R 3 , which may be the same or different, represents a divalent hydrocarbon, halohydrocarbon, or halocarbon moiety; n represents zero or a positive integer; and the R 3 moiety in any one of the n (OR 3 ) moieties may be the same as or different from the R 3 moiety in any other distinct one of these (OR 3 ) moieties.
- component (G) when present to minimize cracking of the coating is selected from molecules that conform to general formula (I) as given above, and more preferably, independently for each preference stated, the molecules selected conform to general formula (I) when:
- R 1 represents a hydrogen atom and R 4 represents an alkyl moiety having a number of carbon atoms that is at least, with increasing preference in the order given, 2, 3, or 4 and independently preferably is not more than, with increasing preference in the order given, 10, 8, 6, 5, or 4; - each of R 2 and R 3 has at least 3 carbon atoms and independently preferably has not more than, with increasing preference in the order given, 10, 8, 6, 5, 4, or 3 carbon atoms; n is not more than, with increasing preference in the order given, 4, 3, 2, or 1.
- component (G) when present to minimize cracking of coatings formed with it comprises, preferably consists essentially of, or more preferably consists of, two distinct subcomponents as follows: subcomponent (G.1 ) is selected from molecules that preferably have not more than, with increasing preference in the order given, 9, 8, or 7 carbon atoms each; and - subcomponent (G.2) is selected from molecules that have at least 10 carbon atoms each and independently preferably have not more than, with increasing preference in the order given, 15, 14, 13, 12, 11 , or 10 carbon atoms each.
- the mass of (.1 ) present has a ratio to the mass of (.2) present that is at least, with increasing preference in the order given, 1.0:1.00, 2.0:1.00, 3.0:1.00,
- component (G) when present in a composition according to the invention to minimize crack formation, it preferably has the property that at least, with increasing preference in the order given, 50, 60, 70, 80, 90,
- the amount of component (G) present in a wet coating formed in a process according to the invention is volatilized and therefore not present in the dry coating eventually formed by the process.
- the temperature at which a composition according to the invention is to be used is not known, preferably at least, with increasing preference in the order given, 50, 60, 70, 80, 90, 95, or 99 % of the amount of component (G) present in a wet layer of a working composition with a thickness of 1.0 millimeter will be volatilized from said wet layer by heating the layer at 121 °C for at least 60 seconds.
- component (G) when component (G) is present in a composition according to the invention to minimize cracking of coatings formed with the composition, preferably at least part of it is emulsified into the composition rather than dissolved in it. (The occurrence of emulsification may normally be detected by a cloudy rather than a transparent appearance of the composition when it is mixed.)
- component (G) preferably consists of solvent(s) that have a solubility in water at 25 °C that is not greater than, with increasing preference in the order given, 15, 13, 11 , 9.0, 8.0, 7.5, 7.3, 7.1 , 6.9, 6.7, or 6.5 grams of solvent per 100 grams of water; and independently at least, with increasing preference in the order given, 1.0, 2.0, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0,
- the concentration of component (G) in a working composition according to the invention in which component (G) is present preferably is at least, with increasing preference in the order given, 0.5, 1.0, 1.5, 2.0, 2.5,
- the resistance to leaching of a chromium con- taining protective coating can be increased by converting part of the initially added hexavalent chromium to trivalent chromium (or, of course, by otherwise supplying trivalent chromium to the composition and correspondingly reducing the content of hexavalent chromium)
- no trivalent chromium is needed for this purpose in a working composition according to the invention, and if not needed is preferably omitted
- it is advantageous for some chromium to be converted to a trivalent form during drying of the working composition into place on the substrate surface to be treated This result may be achieved by using a working composition that contains an organic material that is not readily effective as a reducing agent for hexavalent chromium under the conditions of concentrations and storage and/or use temperature for the working composition, but that is effective as such a reducing agent at
- a reducing agent that does not cause any deterioration in the protective quality of the coatings formed.
- the major reaction product from most of these reducing agents is carbon dioxide that escapes as a gas from the liquid composition before the liquid composition dries.
- preferred component (G) selected from molecules conforming to general formula (I) as described above is present, no other material is normally needed for component (H).
- it is preferred for such a composition to include at least one of various alcohols, glycols, sugars, starch, and like organic materials that are suitable for this purpose, as known to those skilled in the art.
- propylene glycol has been found to be the most preferred of these latent reducing additives to a composition according to the invention to be used under normal commercial operating conditions
- the mass of propylene glycol present in the composition preferably has a ratio to total mass of chromium present in the same composition that is at least, with increasing preference in the order given, 0.30:1.00, 0.50:1.00, 0.70:1.00, 0.90:1.00,
- Optional component (J) of solid filler is generally preferably omitted, because it tends to limit the ready extensibility of the coating formed and therefore to reduce the likelihood that this coating will remain in place during alterations of the shape of the metal substrate.
- a filler can substantially reduce the cost of the treatment and sometimes may be preferred for that reason.
- Numerous finely divided solids such as clays, colloidal silica and silicates, crushed limestone, and the like are known in the art and may be employed in such instances.
- Optional colorant component (K) has no technical effect on the invention, but may be preferred in some instances for aesthetic reasons. Ordinarily, the dried coating formed will have sufficient color to be readily visible, but if exceptionally thin layers and/or exceptionally low fractions of chromium are used, a colorant may be preferred to furnish visual assurance of the presence of the coating. When a coloring is desired, numerous suitable dyes and pigments to achieve such a result are known to those skilled in the art.
- a liquid surface treatment composition according to the invention may be coated onto the substrate by any effective method, such as dipping, spraying, brushing, roll coating, or using an air knife or an electrostatic coating technique, preferably after removing any grease or other soil from the surface of the substrate, to form a liquid coating over the substrate to be treated according to the invention. The coating may be formed on all surfaces of the substrate or on selected portions of the surface only, depending on the positioning of the liquid film from which the dry film is formed.
- the non-volatile contents of the coating are dried into place on the substrate surface to be treated, preferably without any intermediate rinsing.
- any particular polymer or mixture used for component (A) will ordinarily have a "minimum film forming temperature" that the coating must reach while some water still remains in it, in order to assure that a continuous film will be formed.
- the drying operation of a process according to this invention preferably achieves this minimum film forming temperature for component (A) of the liquid film actually being dried.
- the drying may be accomplished simply by exposure to the ambient natural atmosphere at less than 100 % relative humidity.
- drying preferably is accompanied by heating, for example in an oven, with a hot forced air drier, an infrared heater, or an induction heating device to convert the liquid film into an adherent dry coating over the surface of the substrate to be protected.
- a hot forced air drier for example in an oven
- an infrared heater for example, a hot forced air drier
- an induction heating device to convert the liquid film into an adherent dry coating over the surface of the substrate to be protected.
- even air temperatures well above the minimum film forming temperature may not succeed in achieving continuous, crack- free coatings, presumably because too much water evaporates before the polymer content of liquid coating reaches its minimum film forming temperature.
- the temperature of heating should be raised until cracking or other discontinuities in the film do not occur, or an organic solvent component should be added to the working composition to minimize cracking as described above. If there is substantially no air flow rate with respect to the liquid film, a peak metal temperature of 43 °C is sufficient to assure continuous coatings from the preferred compositions according to the invention as described herein, even if they do not contain an organic solvent component to minimize cracking, but with strongly forced air, peak metal temperatures as high as 350 °C may be needed. Under specific process conditions, a suitable drying temperature that assures achieving at least the minimum film forming temperature for the acrylate polymer component in a liquid film composition according to the invention, along with otherwise satisfactory results, can be determined by minimal experimentation.
- a suitable drying temperature will depend on such factors as: whether heat is supplied by radiation, by transfer from a heat transfer fluid such as air, or by other methods or combinations of methods; the direction with respect to the liquid coating from which heat is primarily supplied; and the relative velocity between the liquid coating and the heat transfer fluids if any are used.
- the peak substrate metal temperature reached during drying of a liquid coating to convert it into a solid coating according to this invention is a critical factor in the stabilization of the chromium content of the dried composition against leaching during later contact of the solid coating with water.
- a peak metal temperature of at least 65 °C is preferred over any lower temperature, and under many conditions of drying with some compositions according to the invention even substantially higher temperatures than this are required to minimize leaching.
- a high peak metal temperature requires a large energy input in the drying process. This requires a substantial cost for energy to supply the large energy input required.
- the necessary energy input to achieve such a high peak metal temperature may not be available from the equipment in place where a process according to the invention is desired. Still further, high peak metal temperatures may result in deterioration of other corrosion protective qualities of the coatings formed, even though chromium leaching is reduced.
- the peak metal temperature achieved during drying preferably is at least, with increasing preference in the order given, 43, 48, 53, 58, 63, 68, 73, 78, 83, 88, 93, 98, 103, 108, 1 13, 1 17, or 121 °C and independently
- 5 preferably is not more than, with increasing preference in the order given, 205, 195, 185,
- the amount of coating formed per unit area of the substrate coated may conveniently be determined by o measuring only the chromium content of the coating formed by means of an X-ray emission spectrometer; the total solids content of the coating may then be calculated from the known ratio of the chromium content to the total mass of the coating.
- the mass of chromium per unit area of the substrate coated preferably is at least, with s increasing preference in the order given, 1.0, 3.0, 5.0, 7.0, 8.0, 9.0, 9.5, 10.0, 10.5, 11.0,
- mg/m 2 11.4, or 11.7 milligrams per square meter
- mg/m 2 11.7 milligrams per square meter
- the fraction of chromium in the coating differs widely from 1 %, these values should be adjusted correspondingly to o result in approximately the same total film masses per unit area.
- the coefficient of sliding friction of a sliding contactor of stainless steel against a surface treated according to the invention preferably is not more than, with increasing preference in the order given, 0.270, 0.265, 0.260, 0.255, 0.250, 0.245, 0.240, 0.235, or 0.230. If the coefficient of sliding friction is more than 0.270, fairly frequent cracking 5 and/or flaking of the protective coating applied is likely to result during forming operations that result in corners with a radius of curvature of 1 millimeter or less, and such corners are not particularly unusual in the forming operations to which materials treated according to this invention are subjected. The probability of any such undesirable cracking and/or flaking during forming operations in normal commercial practice has been found 0 to decrease as the coeffcient of sliding friction decreases from 0.270, and when it was
- the coefficient of sliding friction produced in a process according to this invention preferably is at least, with increasing preference in the order given, 0.020, 0.050, 0.080, 0.10, 0.12, 0.14, 0.16, or 0.18.
- the coefficient of sliding friction of a surface may conveniently be measured on a draw bench equipped to record continuously as a function of time the force required to draw a standard weighted contactor at a constant speed across the surface. Such measurements show that a high initial force is required to cause the weighted contactor to begin to move, while a slightly fluctuating but (usually) substantially lower force is sufficient to keep the contactor moving after it has begun to do so. The average value of this latter force, divided by the force measured in the same units of the contactor against the surface across which it is being drawn, yields as a quotient the coefficient of sliding friction.
- the coefficient of static friction of a coating according to this invention may advantageously be considerably higher in value than the coefficient of sliding friction, in order to reduce the incidence and severity of the possible difficulties already noted above that can occur with a very slippery surface for the final substrates treated according to this invention.
- the coefficient of static friction may conveniently be measured by resting a weighted contactor near one end of an initially horizontal but inclinable plane having a surface for which the coefficient of static friction is to be determined, and then gradually increasing the inclination of the plane until the weighted contactor begins to slip. The tangent of the angle to the horizontal that the inclined plane makes when the contactor just begins to slip is the coefficient of static friction.
- the coefficient of static friction against a dry surface produced by a treatment according to this invention preferably is at least, with increasing preference in the order given, 0.30, 0.40, 0.50, 0.60, 0.70, 0.80, 0.90, or 1.00.
- N4 NeocrylTM A640
- JN Joncryl 1532 (supplied by S. C. Johnson; 51 % solids acrylic- styrene copolymer with a glass transition temperature of 14 °C)
- AL ArolonTM 870-W-51 (supplied by Reichhold) Mixed Latexes:
- AX UnithoxTM D-300 (commercially supplied by Petrolite Corp.; 23.5 % solids dispersion in water of molecules of ethoxylated straight chain primary alcohols averaging about 50 carbon atoms each in the alcohol portion and about 50 % of their mass in each of the alcohol portion and the ethoxylate portion)
- AQ AquaslipTM 671 (commercially supplied by Langer & Co.; 40 % solids; polyethylene wax emulsion)
- ME MichemTM Emulsion 39235 (commercially supplied by Michelman Inc.; 35
- AZ JonwaxTM 26 (commercially supplied by Johnson Polymer Div. of S. C.
- S1 81.0 % deionized (hereinafter usually abbreviated as "Dl") water + 10.0 % Chromic Acid + 9.0 % NH4OH (containing 29.7 % NH 3 )
- S1A 90 % water + 10 % chromic acid
- composition 1A Composition 1A partially reduced (with an organic material that leaves no substantial residue in the composition) so that its chromium content is 70 % Cr(VI) and 30 % Cr(lll) MBINED COMPONENTS (A) AND AT LEAST PART OF (C):
- Z8 ZonylTM 8952 anionic surfactant
- ZJ ZonylTM FSJ anionic surfactant (40 % active, same fluorosurfactant as "ZP" with additional unfluorinated surfactant not otherwise specified.
- B3 BYKTM 333 (at least 97 % active)
- B5 BYKTM 375
- T1 Tego GlideTM 100
- T4 Tego GlideTM 410
- compositions, drying conditions, coating weights, and leaching results are shown in Table 1 below for coatings on test panels of commercially supplied steel coated on both sides with an alloy of 55 % aluminum with the balance predominantly zinc. Unless
- drying is in a convection oven with natural air as the heat transfer fluid; the dried samples are allowed to age for at least four days between drying and leach testing; the leaching test is for 15 seconds under rapidly running municipal water at 26 to 32 °C; the amount of chromium is measured before and
- one or more small squares of temperature sensitive paper with a particular indicator temperature were attached directly to a sample of the substrate material that had been coated with a composition to be tested, and several such samples were exposed for different intervals in a particular oven at a perticular temperature, until conditions for attaining at least the desired peak metal temperature were determined, at least one sample to be measured for leaching is then exposed to the conditions so determined, usually without any temperature sensitive paper on the substrate on which actual leaching is measured
- one or more squares of temperature sensitive paper are placed directly on the same substrate on which the leaching value is later measured, on either a coated or an uncoated portion of the substrate sample, so that the blackening of the temperature sensitive paper can be observed either during its actual drying or afterward
- the use of temperature sensitive paper accordingly measures directly only a minimum peak metal temperature, but by advance testing as described above, or by the use of temperature sensitive paper squares with different indicator temperatures on a single coated substrate, it is possible reasonably to assure that the actual peak metal temperature is not further above the minimum than the intervals between temperature sensitive papers with different indicator temperatures, about 6 °C.
- results are shown in Table 2 below These results indicated that the minimum film forming temperature of the polymer in the latex used is between 28 and 38 °C, consistent with the report of the manufacturer of the latex that the minimum film forming temperature is 35 °C. However, even with a contact heater far above that temperature, the coating can be made discontinuous by too high an air flow over its outer surface during drying.
- SPECIFIC EXAMPLE 3 WITH AN ORGANIC SOLVENT COMPONENT ADDED TO MINIMIZE CRACKING
- a precursor solvent and wetting promoting surfactant component for this Example was made by mixing 881 parts of DOWANOLTM PnB, a commercial product of Dow Chemical that is reported by its supplier to be predominantly the mono- ⁇ -butyl ether of propylene glycol, 1 16 parts of DOWANOLTM DpnB, a commercial product of Dow Chemical that is reported by its supplier to be predominantly the mono-n-butyl ether of "dipropylene glycol" (i.e., HO-C 3 H 6 -O-C 3 H 6 -O-C 4 H 9 ), and 3 parts of FLUORADTM FC 129, a commercial product of 3M that is reported by its supplier to be a 49.5 to 53.45 % solution in 2-butoxyethanol of potassium salts of fluorine-substituted carboxylic acids having from 4 to 8 carbon atoms per molecule, with about
- a precursor concentrate for components (A) and (B) was prepared by adding to 834 parts of "A7" latex, with vigorous stirring, first 5 parts of a 20 % solution of CrO 3 in deionized water and then 161 parts of "AZ" wax dispersion.
- a separate precursor concentrate for component (C) was prepared by adding to 810 parts of deionized water, with vigorous stirring, first 100 parts of solid CrO 3 and then 90 parts of 29.9 % solution of ammonia in water.
- the final working composition for this example was then prepared by adding to 74 parts of the precursor concentrate for components (A) and (B), with vigorous stirring, the following materials in the order shown: 0.2 parts of FOAM BANTM MS-30 antifoam agent, a commercial product of Ultra Additives, Inc., Paterson, New Jersey, that is reported by its supplier to consist of polyoxyalkylene polymers, ethoxylated aromatic compounds, and organosiloxane polymers, with further compositional information proprietary; 166 parts of deionized water; 50 parts of the precursor solvent and wetting promoting surfactant component described in the second preceding paragraph above; and 40 parts of the precursor concentrate for component (C) described in the paragraph next above.
- FOAM BANTM MS-30 antifoam agent a commercial product of Ultra Additives, Inc., Paterson, New Jersey, that is reported by its supplier to consist of polyoxyalkylene polymers, ethoxylated aromatic compounds, and organosiloxane polymers, with further compositional information proprietary
- This working composition is applied to galvanized steel coils and dried thereon at a temperature of about 121 °C in a high speed commercial treating facility to provide a crack-free corrosion-protective coating over the galvanized surface.
- SPECIFIC EXAMPLE GROUP 4 WITH BLOCKING EVALUATIONS
- a stock solution without any of component (E) was made with the following contents: 61 % of JoncrylTM 1532, 16 % of JonwaxTM 26; 0.65 % of Cr0 3 ; 0.58 % of concentrated ammonium hydroxide; water as the balance.
- To this stock solution was added 1 % of each of the anti-blocking agents shown in Table 4.
- the resulting composition was coated with a drawdown bar to a uniform thickness on GalvalumeTM substrates and baked for 23 seconds at 232 °C to achieve a peak metal temperature of 121 °C. This produced a coating with 1 1 - 22 milligrams of chromium per square meter of coated surface.
- Example single package concentrates according to the invention with antiblocking additives included are shown in Table 4.
- the balance not shown to 100 % in each concentrate in Table 4 is deionized water.
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- Life Sciences & Earth Sciences (AREA)
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- Wood Science & Technology (AREA)
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Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP00916098A EP1165857A4 (en) | 1999-03-04 | 2000-03-03 | Composition and process for treating metal surfaces |
AU37257/00A AU779227B2 (en) | 1999-03-04 | 2000-03-03 | Composition and process for treating metal surfaces |
US09/914,056 US6899770B1 (en) | 1999-03-04 | 2000-03-03 | Composition and process for treating metal surfaces |
CA2363081A CA2363081C (en) | 1999-03-04 | 2000-03-03 | Composition and process for treating metal surfaces |
Applications Claiming Priority (6)
Application Number | Priority Date | Filing Date | Title |
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US12281099P | 1999-03-04 | 1999-03-04 | |
US60/122,810 | 1999-03-04 | ||
US14793299P | 1999-08-09 | 1999-08-09 | |
US60/147,932 | 1999-08-09 | ||
US15817199P | 1999-10-07 | 1999-10-07 | |
US60/158,171 | 1999-10-07 |
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WO2000052226A1 true WO2000052226A1 (en) | 2000-09-08 |
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PCT/US2000/005766 WO2000052226A1 (en) | 1999-03-04 | 2000-03-03 | Composition and process for treating metal surfaces |
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EP (1) | EP1165857A4 (en) |
AU (1) | AU779227B2 (en) |
CA (1) | CA2363081C (en) |
WO (1) | WO2000052226A1 (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6797407B2 (en) | 2000-12-21 | 2004-09-28 | The Furukawa Electric Co., Ltd. | Metallic plate material for electric/electronic instrument and electric/electronic instrument using same |
WO2005059067A1 (en) * | 2003-12-12 | 2005-06-30 | Motor Works Llc | Lubricant including polyether- or polyester modified polydialkylsiloxane |
WO2006028536A1 (en) * | 2004-09-03 | 2006-03-16 | Motor Works Llc | Engine part coating created from polysiloxane and coating method |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4637840A (en) * | 1984-03-21 | 1987-01-20 | Nihon Parkerizing Co., Ltd. | Coated aluminum-zinc alloy plated sheet steel |
US5378291A (en) * | 1990-01-23 | 1995-01-03 | Nihon Parkerizing Co., Ltd. | Coating composition for metal |
US5456953A (en) * | 1993-02-26 | 1995-10-10 | Armco Steel Company, L.P. | Method for coating bake hardenable steel with a water based chromium bearing organic resin |
US5624978A (en) * | 1987-05-11 | 1997-04-29 | Morton International, Inc. | Conductive, internally lubricated barrier coating for metal |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5859095A (en) * | 1987-05-11 | 1999-01-12 | Morton International, Inc. | Epoxy corrosion-inhibiting coating composition |
WO1992007924A1 (en) * | 1990-11-02 | 1992-05-14 | Smith Noel S | Composition and method for treating metal |
US5252363A (en) * | 1992-06-29 | 1993-10-12 | Morton International, Inc. | Method to produce universally paintable passivated galvanized steel |
JP3256339B2 (en) * | 1993-07-27 | 2002-02-12 | 川崎製鉄株式会社 | Black steel sheet excellent in workability and weldability and method for producing the same |
WO2000035595A1 (en) * | 1998-12-11 | 2000-06-22 | Henkel Corporation | Composition and process for treating metal surfaces |
-
2000
- 2000-03-03 AU AU37257/00A patent/AU779227B2/en not_active Ceased
- 2000-03-03 WO PCT/US2000/005766 patent/WO2000052226A1/en active IP Right Grant
- 2000-03-03 CA CA2363081A patent/CA2363081C/en not_active Expired - Lifetime
- 2000-03-03 EP EP00916098A patent/EP1165857A4/en not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4637840A (en) * | 1984-03-21 | 1987-01-20 | Nihon Parkerizing Co., Ltd. | Coated aluminum-zinc alloy plated sheet steel |
US5624978A (en) * | 1987-05-11 | 1997-04-29 | Morton International, Inc. | Conductive, internally lubricated barrier coating for metal |
US5378291A (en) * | 1990-01-23 | 1995-01-03 | Nihon Parkerizing Co., Ltd. | Coating composition for metal |
US5456953A (en) * | 1993-02-26 | 1995-10-10 | Armco Steel Company, L.P. | Method for coating bake hardenable steel with a water based chromium bearing organic resin |
Non-Patent Citations (1)
Title |
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See also references of EP1165857A4 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6797407B2 (en) | 2000-12-21 | 2004-09-28 | The Furukawa Electric Co., Ltd. | Metallic plate material for electric/electronic instrument and electric/electronic instrument using same |
SG113400A1 (en) * | 2000-12-21 | 2005-08-29 | Furukawa Sky Aluminum Corp | Metallic plate material for electric/electronic instrument and electric/electronic instrument using the same |
WO2005059067A1 (en) * | 2003-12-12 | 2005-06-30 | Motor Works Llc | Lubricant including polyether- or polyester modified polydialkylsiloxane |
WO2006028536A1 (en) * | 2004-09-03 | 2006-03-16 | Motor Works Llc | Engine part coating created from polysiloxane and coating method |
Also Published As
Publication number | Publication date |
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EP1165857A1 (en) | 2002-01-02 |
CA2363081A1 (en) | 2000-09-08 |
CA2363081C (en) | 2010-09-28 |
AU3725700A (en) | 2000-09-21 |
AU779227B2 (en) | 2005-01-13 |
EP1165857A4 (en) | 2003-08-13 |
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