US3899364A - Method of pretreating metal surfaces - Google Patents

Method of pretreating metal surfaces Download PDF

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US3899364A
US3899364A US300303A US30030372A US3899364A US 3899364 A US3899364 A US 3899364A US 300303 A US300303 A US 300303A US 30030372 A US30030372 A US 30030372A US 3899364 A US3899364 A US 3899364A
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steel
phosphating agent
oily material
steel surface
percent
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Albert Edward John Evans
Anthony Norbert Aincough
Koen Verschoore
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Greif International Holding BV
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Koninklijke Emballage Industrie Van Leer BV
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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
    • C10M1/00Liquid compositions essentially based on mineral lubricating oils or fatty oils; Their use as lubricants
    • C10M1/08Liquid compositions essentially based on mineral lubricating oils or fatty oils; Their use as lubricants with additives
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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 using aqueous solutions
    • C23C22/06Chemical 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 using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07Chemical 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 using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts thereof
    • C10M2201/081Inorganic acids or salts thereof containing halogen
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts thereof
    • C10M2201/082Inorganic acids or salts thereof containing nitrogen
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts thereof
    • C10M2201/082Inorganic acids or salts thereof containing nitrogen
    • C10M2201/083Inorganic acids or salts thereof containing nitrogen nitrites
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08Inorganic acids or salts thereof
    • C10M2201/084Inorganic acids or salts thereof containing sulfur, selenium or tellurium
    • 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
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085Phosphorus oxides, acids or salts
    • 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
    • C10M2207/28Esters
    • C10M2207/281Esters of (cyclo)aliphatic monocarboxylic 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/282Esters of (cyclo)aliphatic oolycarboxylic 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/283Esters of polyhydroxy compounds
    • 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
    • C10M2207/28Esters
    • C10M2207/286Esters of polymerised unsaturated 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
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/34Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
    • 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
    • C10M2207/40Fatty vegetable or animal oils
    • 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
    • C10M2207/40Fatty vegetable or animal oils
    • C10M2207/402Castor oils
    • 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
    • C10M2207/40Fatty vegetable or animal oils
    • C10M2207/404Fatty vegetable or animal oils obtained from genetically modified species
    • 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
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/20Metal working
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/27Web or sheet containing structurally defined element or component, the element or component having a specified weight per unit area [e.g., gms/sq cm, lbs/sq ft, etc.]
    • Y10T428/273Web or sheet containing structurally defined element or component, the element or component having a specified weight per unit area [e.g., gms/sq cm, lbs/sq ft, etc.] of coating
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/31504Composite [nonstructural laminate]
    • Y10T428/31678Of metal
    • Y10T428/31714Next to natural gum, natural oil, rosin, lac or wax
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/31504Composite [nonstructural laminate]
    • Y10T428/31844Of natural gum, rosin, natural oil or lac

Definitions

  • ABSTRACT A steel surface pre-treated with an oily material and a phosphating agent in which the surface is (a) first coated with up to 50 milligrams phosphating agent per square meter of surface, and then the oily material is coated on the surface; or (b) the phosphating agent and oily material are simultaneously coated on the surface to provide up to 50 milligrams of phosphating agent per square meter of surface and at least 150 milligrams of oily material per meter of surface; or (c) the phosphating agent and oily material are simultaneously coated on the surface to provide up to 150 milligrams of oily material per square meter of surface.
  • the present invention relates to a method of pretreating metal surfaces, by applying a protecting layer thereon, with the object of enhancing the performance of organic coatings and/or preventing early rusting.
  • the metal particularly subjected to said treatment is steel.
  • a serious problem in steel drum production is that the surface of steel coils or sheets received from the steel mills frequently shows contamination, particularly in the form of rust patches, often as speckled rust. Some extra treatments are required to render the steel surface to a condition suitable for coating, without introducing adverse effects, e.g. water-sensitivity. Time and money would be saved if the steel mills were able to deliver steel substantially free from rust and other undesirable contaminants, having a temporary rust resistance, yet remaining a suitable substrate for coating without extra treatments.
  • the steel-drum manufacturer has to de grease the steel surface with organic solvents, such as trichloroethylene, or wash the steel surface with alkaline aqueous solutions, e.g. aqueous solutions of sodium hydroxide, sodium carbonate, alkali metal silicates or condensed phosphate, particularly pyrophosphates, or with acidic aqueous solutions, e.g. aqueous solutions of mono alkali metal phosphate.
  • alkaline aqueous solutions e.g. aqueous solutions of sodium hydroxide, sodium carbonate, alkali metal silicates or condensed phosphate, particularly pyrophosphates
  • acidic aqueous solutions e.g. aqueous solutions of mono alkali metal phosphate.
  • the wearing properties and storage life of metal surfaces may be improved by applying a stabilized solution, paste or emulsion containing orthophosphoric acid and a water insol uble non-drying polar oil or fat in a weight ratio of from
  • U.S. Pat. specification No. 3.525.651 discloses a one step process for applying an aqueous zinc phosphate solution, containing a solid particulate mixture of a fatty lubricant and a water soluble surface active agent. If the material treated has to be subjected to a deforming operation, the coating applied will provide sufficient lubrication, but if it has to be subjected to a severe deforming operation, a lubricant film may be applied to the coated metal surfaces. As would be anticipated and as the applicants have shown, oil films very much lighter than those used for the protection of steel do not as such give adequate protection against atmospheric rusting; phosphate coatings very much lighter than those used as pretreatments for painting also do not give adequate rust protection. But.
  • the term oily material indicates oils that are not water-soluble and small amounts of which easily dissolve in the solvents commonly used in paint or glue systems. These include: mineral oils, vegetable oils, animal oils and other fatty oils, synthetic oils, modified oils and planticizing oils. The selection of the specific material depends on the application.
  • the components may be applied as a mixture of an oily material and a phosphating agent or separately for instance by a treatment of the steel surface with an oily material followed by a further treatment with a phosphating agent.
  • the oily material and the phosphating agent may be applied as an emulsion or as a solution (it is essential that an appreciable amount of water is present during the treatment to facilitate the ionisation of the phosphating agent).
  • the oily material and the phosphating agent are applied as an emulsion.
  • Such as emulsion may be prepared e.g. from dilute phosphoric acid, a surfactant and dioctylsebacate.
  • Dioctylsebacate which is used frequently in the manufacture of tinplate, is the preferred oily material.
  • the preferred phosphating agent is ortho-phosphoric acid, but other phosphoric acids, phosphorus oxy acid or acid phosphating formulations (eventually combined with detergents) are not excluded.
  • the preferred concentration will vary depending on a number of parameters, e.g. substrate, treatment time and temperature, method of application and required performance, but will often be in the range of 0.01 to 1.0% by volume aqueous solution.
  • the amount of phosphate applied per m may be considerably lower than the amount of phosphate generally applied according to prior art.
  • the presently described process preferably produces a phosphate layer of 0.01 50 mg per m It is however not excluded to carry out the process in such a way that phosphate is not measurable or in a way that phosphate layers of greater thickness are obtained.
  • the phosphating agent contains an accelerator, e.g. sodium nitrate, sodium nitrite, sodium chlorate, copper or nickel salts, an improved phosphate layer is formed, whilst the temperature and time required to form said layer are reduced. The same can be achieved if a phosphating accelerator is present on the steel surface to be protected.
  • the preferred accelerator is a combination of sodium nitrite and sodium nitrate.
  • the amount of oily material to be applied is not limited. amounts of 5- mg of oily material per m are preferred. de-
  • an excess of protecting agent eg an aqueous emulsion of the oily material and the phosphating agent.
  • an excess of protecting agent eg an aqueous emulsion of the oily material and the phosphating agent.
  • the usual cleaning treatment given to steel prior to painting may be omitted partially or wholly.
  • the emulsion or solution of the components. as well as both components separately, may be applied to the steel according to various methods. such as rolling, dipping, brushing, spraying.
  • the present process may be used for treating cold reduced steel as well as pickled, hot rolled steel.
  • the treatment may be carried out during any processing step subsequent to annealing (or pickling when necessary) in the manufacture of cold or hot rolled steel.
  • the present process is of particular importance in the manufacture of steel strip, particularly that used in the manufacture of steel drums. Steel treated according to the invention has to be packaged in the usual way.
  • steel stacks and coils are enveloped with a polyethylene paper laminate which, in turn, is enveloped by a steel sheet outer casing, eventually supported by timber battens. thereby preventing the direct impingement of the atmospheric elements.
  • surface conditions are created resulting in (i) a superior degree of rust resistance, (ii) an excellent appearance over a considerable period of time, (iii) enhancement of the performance of subsequently applied organic coatings, and (iv) a favourable degree of lubricity.
  • test methods used in the undermentioned examples ll8 are as follows:
  • I. PAINTABILITY a. General Paint is spray applied to the steel panels I50 X 300mm or 150 X 100mm) which are held vertically in front of a waterfall-type spray booth.
  • a Brillant Green pigmented paint was used in all cases except where otherwise indicated.
  • the spray unit used is a conventional hand spray gun and the paint is applied in a conventional way to a thickness of mm in one coat. A 5 minute flashoff period in a dust free atmosphere is allowed prior to stoving.
  • the specimens are conditioned by exposure to the following environments.
  • a strip of 25mm wide transparent pressure sensitive tape is applied over the indented paint surface and pressed in order that it adheres to the paint.
  • the tape is then snatch-peeled from the paint. removing all non adherent paint film.
  • the resultant strip of tape is then applied to millimetre squared paper for permanent recording of the result and for measurement of area of paint film removed. The measurement is achieved by estimating the diameter of the disc of paint removed. In instances where the disc is not all paint but consists of tiny flakes the area of paint removed is still taken to be the area of the disc.
  • ERICHSEN DRAW - DIN 53156 BS. 3900 Part E4, 1969 (cupping)
  • the method and apparatus are based on BS 390C Part E4, 1969 (cupping) for single depth of indentation with modified interpretation of the results, and include the use of 16, 18 or 20 BO. steel sheet, as steel mill finished or polished, and testing carried out under ambient conditions.
  • RUST RESISTANCE Resistance to rusting is assessed comparatively, results being related to the amount of rust developed according to the system shown in reference table ll (page 12).
  • FIG. 2 is the standard chart for microscopic and. macroscopic examination of corrosion according to Champion (Corrosion Testing Procedures, F. A. Champion, second Edition 1964, pp 203 205).
  • the relationship between descriptive number, standard term and number of rust spots per sq.dm. is given in Table A. The size of individual rust spots observed, was always 8 mm (assessed by the method according to Champion).
  • the coating on the steel panels were as follows:
  • Hot-rolled and oiled steel panels were trichloroethylene degreased and were then dipped into the emulsion for l0 seconds, drained and dried stood vertically for 1 hour at ambient temperature. l56mg/m of dioctyl sebacate were found to be deposited on the steel surface. These steel panels were subjected to the paintability and rust resistance tests detailed above and the following results were obtained:
  • EXAMPLE 1 An emulsion containing 0.25 percent ("/v) epoxidized linseed oil, 0.1 percent ("/v) orthophosphoric acid (90 percent"'/w) and 0.05 percent (WV) Triton X-45 in water was prepared. Cold reduced mild steel panels were dipped in the emulsion for seconds, drained and dried stood vertically for 1 hour at ambient temperatures. 6lmg/m of epoxidised linseed oil were found to be deposited on the steel surface.
  • the emulsion was sprayed onto cold reduced mild steel panels until a uniform liquid level was (a) Paintahilit 'l'richloroethflcne Steel treated Conditions lcst dcgrqascd steel as above Reverse Impact mm remmed 5llmm removed Ambient 7 Erichsen grade 3 grade I Reverse Impact SLA. 40mm removed 1 day water soak Erichsen grade 5/Sl.. ⁇ grade 4 -Continued Cold reduced mild steel panels (centre line average 60 micro inches) were dipped into the emulsion for 10 (a) Paintability seconds, drained and dried stood vertically for 1 hour v at ambient temperature.
  • EXAMPLE l9 Panels were cut from a cold rolled, commercial quality, mild steel plate having a thickness of 1.25 mm.
  • Crodafluid 66938 applied as a thin film from an 21 emulsion containing (1.25% v/v Crodafluid C6938 and 0.0571 v/v Triton X-45
  • Tellus 15 oil applied as a thin film from an emulsion containing 1% v/v Tellus 15 oil and 0.0571 v/v Triton X-45.
  • Crodafluid 06938 and orthophosphoric acid applied according to the invention from an emulsion containing 0.25% v/v Crodafluid 66938, (H /1 v/v orthophosphoric acid (90%) and 0.05% v/v Triton X-45 in water.
  • Tcllus 15 oil and orthophosphoric acid applied according to the invention from an emulsion containing 17! v/v Tellus 15 oil 0.19? v/v orthophosphoric acid (90%) and 0,05% v/v Triton X-45 in water,
  • Orthophosphoric acid treated by dipping in an aqueous solution of 0. 171 v/v orthophosphoric acid 90% Crodafluid @6938 obtained from Croda Chemicals Limited, *Tcllus 15 oil obtained from Shell-Mex and B.P, Limited.
  • Stretch forming lubrication was assessed using Erichsen cupping tests on the 55mm diameter blanks, evaluation being by the depth of draw to failure and the maximum load applied. A large depth of draw and a low maximum load are indicative of efficient lubrication, the ideal being low density polyethylene film. Deep drawing lubrication was assessed using the Erichsen machine with the 33mm cup draw tools and 55mm diameter blanks. The relative lubricity of the various systems was evaluated in terms of the work done in achieving the draw and in terms of the peak drawing load. Low values of work done and peak load are indicative of efficient lubrication the ideal being low density polyethylene film.
  • a steel surface pre-treated to provide superior rust protection, high lubricity and direct paintability without degreasing said surface having a first uniform coating of up to milligrams of phosphating agent per square meter of surface and a second uniform coating of an oily material selected from the group consisting of mineral oils, vegetable oils, animal oils and equivalent synthetic oils, said phosphating agent being coated on said surface from an acidic aqueous solution of said phosphating agent, said second coating being applied subsequent to said first coating.
  • a steel surface pre-treated to provide superior rust protection, high lubricity and direct paintability without degreasing said surface having a uniform coating of up to 50 milligrams of phosphating agent per square meter of surface and at least milligrams of oily material per square meter of surface, said phosphating agent and said oily material being coated on said surface simultaneously, said phosphating agent being coated on said surface from an acidic aqueous solution of said phosphating agent, said oily material being selected from the group consisting of mineral oils, vegetable oils, animal oils and equivalent synthetic oils.
  • a steel surface pre-treated to provide superior rust protection, high lubricity and direct paintability without degreasing said surface being coated with a phosphating agent and up to 150 milligrams of oily material per square meter of surface, said phosphating agent and said oily material being coated on said surface simultaneously, said phosphating agent being coated on said surface from an acidic aqueous solution of said phosphating agent, said oily material being selected from the group consisting of mineral oils, vegetable oils. animal oils and equivalent synthetic oils.
  • I 23 The steel surface of claim 19 in which an acceler ator is used to accelerate the coating of said phosphat ing agent on said surface.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Lubricants (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Paints Or Removers (AREA)
US300303A 1971-10-22 1972-10-24 Method of pretreating metal surfaces Expired - Lifetime US3899364A (en)

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JP (1) JPS5736349B2 (enrdf_load_stackoverflow)
AR (1) AR196092A1 (enrdf_load_stackoverflow)
AU (1) AU476077B2 (enrdf_load_stackoverflow)
BE (1) BE790388A (enrdf_load_stackoverflow)
BR (1) BR7207380D0 (enrdf_load_stackoverflow)
CA (1) CA987208A (enrdf_load_stackoverflow)
CS (3) CS174857B2 (enrdf_load_stackoverflow)
DE (1) DE2251611A1 (enrdf_load_stackoverflow)
ES (1) ES407627A1 (enrdf_load_stackoverflow)
FR (1) FR2156822B1 (enrdf_load_stackoverflow)
GB (1) GB1406114A (enrdf_load_stackoverflow)
HU (1) HU173612B (enrdf_load_stackoverflow)
IT (1) IT975319B (enrdf_load_stackoverflow)
LU (1) LU66337A1 (enrdf_load_stackoverflow)
NL (1) NL7114590A (enrdf_load_stackoverflow)
PL (1) PL83640B1 (enrdf_load_stackoverflow)
SE (1) SE375336B (enrdf_load_stackoverflow)
ZA (1) ZA727277B (enrdf_load_stackoverflow)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4188824A (en) * 1978-06-02 1980-02-19 Youngstown Sheet And Tube Company Coating adherence prospensity testing of metal substrates
US4312922A (en) * 1980-01-11 1982-01-26 Olin Corporation Lubricated cupreous sheet comprising an organophosphonate layer and process therefor
WO1983000415A1 (en) * 1981-07-17 1983-02-03 Western Electric Co Method of preserving the solderability of copper
US5714016A (en) * 1992-09-30 1998-02-03 Sumitomo Electric Industries, Ltd. Gear for wheel speed detection and method of manufacturing the same
EP1350865A3 (de) * 2002-04-05 2004-12-29 ThyssenKrupp Stahl AG Verzinktes und phosphatiertes Blech sowie Verfahren zur Herstellung eines solchen Blechs

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5713629B2 (enrdf_load_stackoverflow) * 1973-07-31 1982-03-18
DE3311738A1 (de) * 1983-03-31 1984-10-04 Metallgesellschaft Ag, 6000 Frankfurt Verfahren zur phosphatierung von metalloberflaechen
DE4129529A1 (de) * 1991-09-05 1993-03-11 Henkel Kgaa Kombiniertes verfahren zur reinigung und zum rostschutz von verschmutzten metalloberflaechen auf basis eisen bzw. stahl
US5540788A (en) * 1995-02-24 1996-07-30 Mdechem, Inc. Method of preparing iron-phosphate conversion surfaces

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3525651A (en) * 1966-12-01 1970-08-25 Kenneth A Smith Coating of metals

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2739915A (en) * 1950-07-20 1956-03-27 Schuster Ludwig Karl Multiple action lubricating composition
US2935432A (en) * 1957-04-02 1960-05-03 Reilly Whiteman Walton Company Metal treatment

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3525651A (en) * 1966-12-01 1970-08-25 Kenneth A Smith Coating of metals

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4188824A (en) * 1978-06-02 1980-02-19 Youngstown Sheet And Tube Company Coating adherence prospensity testing of metal substrates
US4312922A (en) * 1980-01-11 1982-01-26 Olin Corporation Lubricated cupreous sheet comprising an organophosphonate layer and process therefor
WO1983000415A1 (en) * 1981-07-17 1983-02-03 Western Electric Co Method of preserving the solderability of copper
US4373656A (en) * 1981-07-17 1983-02-15 Western Electric Company, Inc. Method of preserving the solderability of copper
US5714016A (en) * 1992-09-30 1998-02-03 Sumitomo Electric Industries, Ltd. Gear for wheel speed detection and method of manufacturing the same
EP1350865A3 (de) * 2002-04-05 2004-12-29 ThyssenKrupp Stahl AG Verzinktes und phosphatiertes Blech sowie Verfahren zur Herstellung eines solchen Blechs

Also Published As

Publication number Publication date
LU66337A1 (enrdf_load_stackoverflow) 1973-01-23
ES407627A1 (es) 1976-01-16
BR7207380D0 (pt) 1973-08-21
FR2156822A1 (enrdf_load_stackoverflow) 1973-06-01
CS174894B2 (enrdf_load_stackoverflow) 1977-04-29
CS174857B2 (enrdf_load_stackoverflow) 1977-04-29
SE375336B (enrdf_load_stackoverflow) 1975-04-14
AU476077B2 (en) 1976-09-09
CA987208A (en) 1976-04-13
FR2156822B1 (enrdf_load_stackoverflow) 1976-08-20
NL7114590A (enrdf_load_stackoverflow) 1973-04-25
JPS4850954A (enrdf_load_stackoverflow) 1973-07-18
BE790388A (nl) 1973-04-20
GB1406114A (en) 1975-09-17
IT975319B (it) 1974-07-20
AU4782772A (en) 1974-04-26
PL83640B1 (enrdf_load_stackoverflow) 1975-12-31
HU173612B (hu) 1979-06-28
DE2251611A1 (de) 1973-04-26
CS174895B2 (enrdf_load_stackoverflow) 1977-04-29
ZA727277B (en) 1973-10-31
AR196092A1 (es) 1973-11-30
JPS5736349B2 (enrdf_load_stackoverflow) 1982-08-03

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