US3661622A - Method of improving resistance to corrosion of metal surfaces and resultant article - Google Patents

Method of improving resistance to corrosion of metal surfaces and resultant article Download PDF

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US3661622A
US3661622A US20038A US3661622DA US3661622A US 3661622 A US3661622 A US 3661622A US 20038 A US20038 A US 20038A US 3661622D A US3661622D A US 3661622DA US 3661622 A US3661622 A US 3661622A
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polymer
composition
parts
molecular weight
percent
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Lynn C Rogers
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ConocoPhillips Co
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Continental Oil Co
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
    • 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—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy
    • 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
    • C10N2070/00—Specific manufacturing methods for lubricant compositions
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31511—Of epoxy ether
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
    • Y10T428/31573—Next to addition polymer of ethylenically unsaturated monomer
    • Y10T428/31576—Ester monomer type [polyvinylacetate, etc.]
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
    • Y10T428/31573—Next to addition polymer of ethylenically unsaturated monomer
    • Y10T428/31587—Hydrocarbon polymer [polyethylene, polybutadiene, etc.]
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31678—Of metal
    • Y10T428/31714—Next to natural gum, natural oil, rosin, lac or wax
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31786—Of polyester [e.g., alkyd, etc.]
    • Y10T428/31797—Next to addition polymer from unsaturated monomers
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31801—Of wax or waxy material
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31844—Of natural gum, rosin, natural oil or lac
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31855—Of addition polymer from unsaturated monomers
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31855—Of addition polymer from unsaturated monomers
    • Y10T428/31859—Next to an aldehyde or ketone condensation product

Definitions

  • a composition comprising (1 a major amount (e.g. at least 75 weight percent) of a thixotropic, grease-like composition consisting essentially of a non-volatile diluent, an oil-soluble dispersing agent and an alkaline earth metal carbonate and (2) a minor amount (e. g. 0.1 to 25 weight percent) of a polymer, and
  • step (b) applying to the coated metal surface a conventional paint.
  • An important feature is the use of the composition described in step (a) as a primer coating.
  • the composition of my invention comprises (1) a major amount of a thixotropic, grease-like composition and a minor amount (e.g. 0.1 to 25 weight percent) of a polymer having certain characteristics.
  • the use of such a composition as a primer results in a film which is harder, tougher and less tacky than the use of the composition of application Ser. No. 729,875.
  • U.S. Pat. No. 3,384,586 teaches the addition of a thixotropic, grease-like composition to a polymer. More specifically, this patent teaches a composition comprising a major amount of a polymer and a minor amount of the thixotropic, greaselike composition.
  • U.S. Pat. No. 3,372,l l4 teaches that gelled materials useful as a lubricant additive in greases are prepared by contacting (A) a fluid mineral oil solution of a carbonated, basic complex of an alkaline earth metal and an organic carboxylic or sulfonic acid, salt thereof, or carboxylic ester containing at least 12 aliphatic carbon atoms, the complex being characterized by a metal ratio of at least 4:5, with (B) oxygen at a temperature of about 150 C. to about 300 C.
  • the patent further teaches that in some instances the product is a grease and that small compatible hydrocarbon resins can be added to the product.
  • compositions taught therein can be used as a primer for conventional paints.
  • the present invention concerns a method of improving resistance to corrosion of metal surfaces wherein the method comprises:
  • a. applying to the metal surface a composition comprising (1) a major amount (at least 75 weight percent) of a thixotropic, grease-like composition consisting essentially of a nonvolatile diluent, an oil-soluble dispersing agent and an alkaline earth metal carbonate and (2) a minor amount (0.1 to 25 weight percent) of a polymer, which, preferably, has the following properties:
  • the composition applied in step (a) should be substantially free of volatile solvents before applying the paint in step (b).
  • the present invention concerns a metal article having improved resistance to corrosion, said metal article having the exterior surface coated with the composition, described in the foregoing, as the primer coat and a conventional paint as the external coat.
  • the present invention concerns the use of the composition, described in the foregoing, as a primer coating when used in conjunction with conventional paints on any of the surfaces normally coated by conventional paints.
  • composition used in my invention comprises a major amount of a thixotropic, grease-like composition and a minor amount of a polymer having certain properties.
  • the thixotropic, grease-like composition consists essentially of the following materials in the amounts stated:
  • the thixotropic, grease-like composition has the following properties:
  • the first method is called simply a two-step method.
  • a colloidal dispersion of alkaline earth metal carbonate is formed first.
  • the dispersion is then treated, preferably, with a small amount of water in the presence of a small amount of alcohol.
  • the second method is called simply a one-step method.
  • an admixture is formed of oil-soluble dispersing agent, nonvolatile diluent, alkaline earth metal compound, alcohol, and water. After treating the admixture with CO the volatile materials are removed by distillation.
  • the two-step method will be described in detail first.
  • the charge (or starting) material for this method of preparing the thixotropic, grease-like composition is a colloidal dispersion of an alkaline earth metal carbonate in a suitable l diluent and having an acetic base number of at least 50.
  • alkaline earth metal refers only to those of this group which are more commonly available, namely, magnesium, calcium, strontium and barium. Of these, calcium and barium are more suitable, with calcium being preferred.
  • alkaline earth metal carbonate While we have used the term alkaline earth metal carbonate it may be well to mention that, although carbonate is the predominant anion, traces of other anions, e.g. hydroxide, oxide, and alkoxide, can be present. This is due to the fact that many processes of preparing dispersions of alkaline earth metal carbonates prepare the carbonate by carbonation of an alkaline earth metal hydroxide, oxide or alkoxide.
  • colloidal dispersions which are used as a starting material consist essentially of a nonvolatile diluent, an oilsoluble dispersing agent, and an alkaline earth metal carbonate. These materials are present in the following range:
  • the colloidal dispersions may contain minor amounts of the alcohol which is employed in manufacturing the colloidal dispersion, and of the metalcontaining intermediate which may be employed in manufacturing the colloidal dispersion.
  • nonvolatile diluents are suitable in the colloidal dispersions used as the starting material.
  • the principal requisite desired in the nonvolatile diluent is that it will act as a solvent for the dispersing agent which is used.
  • nonvolatile diluents which can be used include mineral lubricating oils obtained by any of the conventional refining procedures; liquid synthetic lubricating oils, vegetable oils,
  • oils such as corn oil, cotton seed oil, and castor oil; animal oils, such as lard oil and sperm oil; and waxes, such as the petroleum waxes.
  • waxes the microcrystalline waxes are preferred.
  • the mineral lubricating oils are preferred.
  • the colloidal dispersion is a solid at room temperature.
  • oil-soluble dispersing agents are suitable in the colloidal dispersions which are used in preparing the product used in my invention.
  • suitable dispersing agents include oil-soluble sulfonic acids, carboxylic acids, and the metal salts thereof.
  • the preferred dispersing agents for preparing the grease-like product used in my invention are the oil-soluble sulfonic acids and metal sulfonates.
  • metal refers to those metals which are conventionally used to prepare the metal sulfonates of commerce. This includes metal sulfonates wherein the metal is sodium, potassium, magnesium, calcium, and barium. The more suitable sulfonates are those wherein the metal is calcium or barium.
  • the metal of the metal sulfonate is the same as the metal of the basic metal compound.
  • oil-soluble sulfonates refers to those sulfonates wherein the hydrocarbon portion of the molecule has a molecular weight in the range of about 300 to about 1,000. Preferably, this molecular weight is in the range of about 370 to about 700.
  • These oil-soluble sulfonates can be either synthetic sulfonates or the so-called mahogany or natural sulfonates. The term mahogany sulfonates is believed to be well understood, since it is amply described in the literature.
  • synthetic sulfonates refers to those sulfonates which are derived from sulfonation feedstocks which are prepared synthetically.
  • the synthetic sulfonates include alkyl sulfonates and alkaryl sulfonates.
  • the alkaryl radical can be derived from benzene, toluene, ethyl benzene, xylene isomers, or naphthalene.
  • the alkyl groups are branched chain.
  • the amount of sulfonate derived from branched chain alkaryls is at least 60 percent by weight.
  • post-dodecylbenzene sulfonate An example of an oil soluble alkaryl sulfonate (a synthetic sulfonate) which has been particularly useful in preparing colloidal dispersions is the material known as post-dodecylbenzene sulfonate.
  • Postdodecylbenzene is a bottoms product of the manufacture of dodecylbenzene.
  • the alkyl groups of postdodecylbenzene are branched chain.
  • Postdodecylbenzene consists of monoalkylbenzenes and dialkylbenzenes in the approximate mole ratio of 2:3 and has typical properties as follows:
  • dimer alkylate has branched-chain alkyl groups as does postdodecylbenzene. Briefly described, dimer alkylate is prepared by the following steps:
  • the dimerization step uses a Friedel-Crafts alkylation sludge as the catalyst. This process and the resulting product are described in U.S. Pat. No. 3,410,925.
  • NAB Bottoms are predominantly di-n-alkaryl, wherein the alkyl groups contain from eight to 18 carbon atoms. They distinguish primarily from the preceding sulfonation feedstocks in that they are straight-chain and contain a large amount of di-substituted material.
  • the process of preparing these materials and the resulting product are described in application Ser. No. 521,794 filed Jan. 20, 1966, now abandoned, and having the same assignee as the present application.
  • Another process of preparing a di-n-alkaryl product is described in application Ser. No. 529,284, filed Feb. 23, 1966, now abandoned and having the same assignee as the present application.
  • sulfonates which can be used in the colloidal dispersion employed as a starting material include, for example, monoand poly-wax substituted naphthalene sulfonates, dinonyl naphthalene sulfonates, diphenyl ether sulfonates, naphthalene disulfide sulfonates, diphenyl amine sulfonates, dicetyl thianthrene sulfonates, dilauryl betanaphthol sulfonates, dicapryl nitro-naphthalene sulfonates, unsaturated paraffin wax sulfonates, hydroxy substituted paraffin wax sulfonates, tetramylene sulfonates, monoand poly-chloro-substituted paraffin wax sulfonates, nitrosoparaffin wax sulfonates; cyclo-aliphatic sulfonates,
  • the metal salts of the preceding sulfonates can be formed in situ during preparation of the colloidal dispersion by neutralization of the corresponding sulfonic acid.
  • Suitable carboxylicacids which can be used in preparing the colloidal dispersion used as a starting material include naphthenic acids, such as the substituted cyclopentane monocarboxylic acids, the substituted cyclohexane monocarboxylic acids and the substituted aliphatic polycyclic monocarboxylic acids containing at least carbon atoms.
  • naphthenic acids such as the substituted cyclopentane monocarboxylic acids, the substituted cyclohexane monocarboxylic acids and the substituted aliphatic polycyclic monocarboxylic acids containing at least carbon atoms.
  • Specific examples include cetyl cyclohexane carboxylic acids, dioctyl cyclopentane carboxylic acids, dilauryl decahydronaphthalene and stearyloctahydro indene carboxylic acids and the like and oil-soluble salts thereof.
  • Suitable oilsoluble fatty acids are those containing at least eight
  • fatty acids which are liquids at ambient temperatures down to about 15 C.
  • Specific examples include 2-ethyl hexanoic acid, pelargonic acid, oleic acid, palmitoleic acid, linoleic acid and ricinoleic acid.
  • the metal salts of the preceding carboxylic acids can be formed in situ during preparation of the colloidal dispersion by neutralization of the corresponding carboxylic acid.
  • the thixotropic grease-like composition used to prepare the composition of my invention can be prepared by treating the colloidal dispersion with a small amount of water in the presence of a small amount of an alcohol.
  • the amount of water which is used should be at least about 3 percent, preferably about 7 percent, by weight, based on the colloidal dispersion.
  • the amount of water should not be above 12 percent, and usually not above 20 percent, by weight, based on the colloidal dispersion. (Larger amounts can be used conceivably, but no advantage results therefrom.
  • the amount of alcohol which is used is in the range of about 0.5 to about 10 percent, preferably from about 1 to about 5 percent, by weight, based on the colloidal dispersion. These aforementioned amounts of alcohol include the residual alcohol present in the colloidal dispersion which runs from about 0.5 percent to about 3 percent by weight, usually.
  • alcohols can be used in the conversion of the colloidal dispersion to the thixotropic, grease-like composition used in my invention.
  • suitable alcohols include the C,-C alkanols, the monoether alcohols of ethylene glycol containing up to eight carbon atoms, and the monoether alcohols of diethylene glycols containing up to eight carbon atoms.
  • the alcohols Preferably, the alcohols have boiling points of at least about that of water.
  • suitable alcohols include methanol, ethanol, propanol, isobutanol, pentanol, hexanol, octanol, decanol, Z-methoxy ethanol, and 2- ethoxy ethanol. Of these isobutanol and 2-methoxy ethanol are preferred.
  • modification reaction is meant the change from a fluid, clear colloidal dispersion to a viscous, tacky material.
  • Suitable and preferred nonvolatile diluent, dispersing agent and alkaline earth metal are the same as described previously in connection with the two-step method.
  • an alkaline earth metal carbonate which is formed in situ, is used in the process.
  • an admixture is prepared of alkaline earth metal basic compound, selected from the group consisting of oxides, hydroxides. and alcoholates. dispersing agent, nonvolatile diluent. and alcohol.
  • the admixture is then treated with CO to form the carbonate.
  • the alkaline earth metal carbonate is formed by adding an alcoholic slurry ofthe alkaline earth metal basic compound to an admixture of the other materials. The total admixture is then treated with CO to form the carbonate.
  • Suitable alcohols for use in the one-step process include C,-C alkanols, the monoether alcohols of ethylene glycol containing up to eight carbon atoms, and the monoether alcohols of diethylene glycol containing up to eight carbon atoms.
  • suitable alcohols include methanol, ethanol, propanol, isobutanol, pentanol, hexanol, octanol, decanol, 2-methoxy ethanol, and 2-ethoxy ethanol.
  • the preferred alcohols are the C,-C alkanols, with the C,-C alkanols being more preferred.
  • the oil soluble dispersing agent (whether pre-formed, or formed in situ), nonvolatile diluent and alcohol-alkaline earth metal basic compound slurry are intimately admixed preparatory to carbonation.
  • the water component of the mixture may be added at any time prior to the final controlled heating step, and may be added at different times in two or more increments, if desired. The same is true of any alcohol which is added in addition to that introduced with the slurry. In the case of the water, however, it is preferred to add the entire amount of water at the outset and prior to carbonation since thicker products appear to be yielded when this procedure is followed.
  • the carbon dioxide required may be introduced into the mixture by blowing or bubbling the gas through the mixture. or by immersing dry ice in the mixture.
  • the reaction is exothermic and its progress can be followed by observation of the change in temperature of the reaction mixture. it is preferred that the temperature be retained below about 50 C during carbonation.
  • the mixture which then contains the oil-soluble dispersing agent, the nonvolatile carrier material, and the alkaline earth metal carbonate resulting from carbonation is subjected to a controlled heating step.
  • a controlled heating step Between the carbonation procedure and the heating step, water and/or alcohol may be added to the mixture in order to bring the total content of these two components in the mixture up to that which has been hereinbefore described as the operative requirements in this respect.
  • the heating step with which the one-step method is concluded is quite important, and the manner in which it is conducted determines whether the desired high consistency-low penetration grease-like compositions are yielded, or whether a fluid dispersion of the general type described in U.S. Pat. Nos. 2,956,0l 8 and 2,861,95l to Carlyle and also in U.S. Pat. Nos. 3,l50,088 and 3,027,325 to McMillen are formed.
  • the heating will remove substantially all of the alcohol and water which are not consumed in the grease producing reaction, and any very light hydrocarbon solvents, such as hexane, which are incorporated in the mixture in order to facilitate the carbonation of the alkaline earth metal base compound.
  • the second function of the heating is to supply the heat of reaction which is necessary to effect the conversion of the mixture to a high consistency grease-like composition.
  • the minimum operative quantity of water is present in the mixture at the inception of the final heating step (that is, 0.25 mole of water per mole of overbasing alkaline earth metal present)
  • the time within which the mixture must be maintained between 50 C and 100 C is at least 4.5 hours. This time period decreases in a fairly regular uniform fashion as the amount of water present in the mixture with respect to the amount of alkaline earth metal present increases.
  • t 0.75 +1.7 X (2.5 -m) where t equals the time in hours within which the mixture must be retained in the temperature range of between 50 C and 100 C, and m is the number of moles of water present in the mixture per mole of alkaline earth metal present in the mixture in an overbasing capacity.
  • the formation of the desired grease-like product is clearly evidenced by the marked and rapid change in the observable physical properties of the mixture. The most striking change, perhaps, is in the viscosity of the mixture, which increases rapidly as the conversion to grease-like product occurs.
  • the grease-like product is tacky and opaque and is macroscopically homogeneous. It is highly basic in terms of its acetic base number. (This term is well-known in the art, being described in US. Pat. No. 3,150,088.)
  • polymer as used herein includes certain copolymers which meet the specified requirements. Suitable polymers for use in our invention have the following properties:
  • a high solubility in predominantly aliphatic hydrocarbon solvents such as hexane, n-decane, Stoddard solvent, kerosene and petroleum lubricating oils.
  • Polymers meeting the above-listed description are often termed atactic or amorphous.
  • suitable types of polymers include low molecular weight or low density polyethylene, amorphous polypropylene, polyisobutylene, polyterpenes; copolymers of the foregoing with vinyl monomers, such as vinyl chloride, and vinyl esters, such as vinyl acetate; polyacrylic acids, and polymethacrylic acids.
  • Suitable polymers include the followmg:
  • amorphous polypropylenes amorphous polypropylenes, polyolefins, ethylene-isobutyl acrylate copolymers and ethylene-vinyl acetate copolymers.
  • Preferred polymers are the polyterpenes, amorphous polypropylenes, low molecular weight polyethylenes, and ethylene-vinyl acetate copolymers.
  • composition used in my invention can be applied as is to the metal surface, usually, by means of a brush.
  • the composition is diluted in a volatile solvent for application to the surface.
  • a volatile solvent provides a more uniform film on the metal surface and enables the use of a spray. The latter can reduce substantially the cost of applying the composition.
  • volatile solvent used is not a salient fea ture of my invention, and it is believed those skilled in the art, without undue experimentation, can readily ascertain suitable solvents.
  • suitable solvents include volatile hydrocarbon solvents, such as Stoddard solvent, kerosene, petroleum naphtha and the like. Also, certain nonflammable chlorohydrocarbons are suitable. For reasons of safety, it is preferable to use solvents having a flash point of at least F and even higher.
  • the amount of solvent is dependent on the particular method of application. Usually, a suitable amount of solvent is in the range of from about 40 to about 90 percent by weight. Preferably, it is from about 50 to about 80 percent by weight.
  • composition of my invention can be used as a primer on any type of metal surface which is to be coated with a conventional paint.
  • a conventional paint Preferably it is used on metals which are subject to severe corrosion, such as ferrous metals.
  • a particular advantage of the composition used in my invention is that the metal surface requires little or no preparation prior to application. Many primers require that the surface be meticulously clean (e.g. by chemical cleaning or sandblasting to white metal) prior to application.
  • the composition, used in my invention when applied to rusted surfaces result in a satisfactory film. Usually, the surface is treated moderately, e.g. by scraping or brushing sufficiently to remove loose scale prior to application of the grease-like composition.
  • compositions which are applied can be readily determined by those skilled in the art. A thicker film usually provides better protection but, obviously, is more expensive. A film having a thickness of about 2.5 mils has been found to be optimum with respect to both performance and economics.
  • the composition should be substantially solvent-free before applying the conventional paint. Usually, the composition is solvent-free in 18-72 hours.
  • Suitable Paints A variety of conventional paints have been found to be satisfactorily applied over the composition used in my invention. Examples of suitable generic-type paints include the following:
  • a primary advantage of the use of the composition as a primer is that the metal surface requires little, or no, preparation prior to being coated with the composition.
  • composition as a primer provides an improved resistance to corrosion of metal surfaces.
  • composition as a primer permits an increase in the thickness of a single-coat film, particularly with alkyd paints.
  • composition as a primer results in a film which is harder, tougher and less tacky than the use of the composition of application Ser. No. 729,875 as a primer.
  • EXAMPLE 1 This example illustrates the reduction in tackiness of the polymer-thixotropic, grease-like composition as compared to the thixotropic, grease-like composition alone.
  • the thixotropic grease-like composition was prepared using the one-step" method described hereinbefore.
  • the sulfonic acid solution employed contained 27 percent (by wt.) mixed sulfonic acids, 60 percent (by wt.) n-hexane and 13 percent (by wt.) nonvolatile mineral oil (pale oil).
  • the mixed sulfonic acids contained 70 percent (by wt.) oil-soluble sulfonic acids derived from dimer alkylate and 30 percent (by wt.) oil-soluble sulfonic acids derived from NAB" Bottoms. Both dimer alkylate" and NAB" Bottoms have been described in the foregoing.
  • the carbonated admixture was then heated to reflux temperature (67 C) and maintained at this temperature for 15 minutes.
  • the carbonated admixture was cooled to about 55 C, whereupon parts water were added over a 15-minute period.
  • the resulting admixture was heated to reflux temperature and maintained at this temperature for 15 minutes.
  • the admixture was then heated slowly to a temperature of 160 C. to remove the lower boiling solvents.
  • the final product had the following composition:
  • EXAMPLE 2 This example illustrates the improved mechanical performance of a conventional paint over the composition of my invention as compared to the composition of application Ser. No. 729,875.
  • Example B the thixotropic, grease-like composition of Example 1 similar to A but containing less nonvolatile diluent oil C Composition B plus 3 percent Eponlene C-l6 D Composition B plus 5 percent Eastobond M-5W (amorphous polypropylene) Films of the compositions were cast on 4 in. X 8 in. mild steel Q panels. The coated panels were painted over with a conventional white alkyd enamel. It was noted that the coatings from compositions C and D accepted the paint top coat more readily and covered more smoothly than did the coatings from compositions A and B. The alkyd enamel top coat was dry in 24 hours over all the compositions.
  • Adhesion was evaluated by a scotch tape test. in this test a grid 34 in. X V4 in. was cut through the coating down to bare metal. The grid consisted of 7 lines /2. in. apart intersected at right angles by another 7 lines at Ya in. spacing. A 34. in. wide strip of "Scotch magic transparent tape was placed over the grid and pressed firmly in place with a finger. Then the tape was lifted, quickly and smoothly. The number of squares, out of the total of 36, in which the coating separated from the metal and adhered to the tape was counted. A lower value in this test indicates improved results.
  • the abrasion resistance was measured by determining the amount of force that must be applied to 1 square inch of No. l00 grit sandpaper being pulled over the surface of the coating before bare metal is revealed. In this test a higher value indicutes improved results.
  • the thixotropic, grease-like composition was prepared using the two-step" method.
  • the colloidal dispersion of calcium carbonate used as a starting material had the following composition:
  • the resulting product was a thixotropic, grease-like composition having an ASTM penetration of 133 at 77 F.
  • composition A parts 78.4 Stoddard solvent 53.4*( *This composition is typical of U.S. Pat. No.
  • Composition B parts 61.4 Stoddard solvent 38.6*(*This composition is comparative to US. Pat. No.
  • composition C parts 105.5 Stoddard solvent grease-like composition 90 polyterpene resin (Wing Tack" l0 TGC Composition D parts 60.9 Stoddard solvent i0 polyterpene resin (Wing Tack 95) 90 TGC Composition E parts 61.7 Stoddard solvent 38.3 TGC
  • Table III The viscosity characteristics of the above-described compositions are shown in Table III.
  • n 2:11:5 2: 3 gx's D) have a much higher viscosity than do blends containing a S have z s z in the 5 e an small amount of thixotropic, grease-like composition (A and o om e g C) 15 To a one-liter flask were added:
  • brittle slightly tacky i. from about 2 to about 80 parts nonvolatile diluent P t tacky selected from the group consisting of mineral all! Adhesion Poor Good very very Good lubricating oils, synthetic lubricating oils, and Poor Good petroleum waxes,
  • oil-soluble dispersing agent is a sulfonic acid, or a metal salt thereof.
  • polymer is selected from the group consisting of polyterpenes, amorphous polypropylenes, low molecular weight polyethylenes, and ethylene-vinyl acetate copolymers.
  • the conventional paint is selected from the group consisting of two-component amine cured epoxy, two-component urethane, alkyd enamel, phenolic enamel, acrylic water emulsion, and vinyl.
  • a method of improving resistance to corrosion of metal surfaces comprising:
  • nonvolatile diluent selected from the group consisting of mineral lubricating oils, synthetic lubricating oils and petroleum waxes,
  • said grease-like composition being characterized further in that it has an acetic base number of at least 50, does not flow at 210 F, and has a dropping point of at least 480 F,
  • polymer from about 0.2 to about 10 parts polymer, said polymer being characterized as having a crystallinity of less than 50 percent, a molecular weight in the range of from about 3,000 to about 1 million and a high solubility in predominantly aliphatic hydrocarbon solvents,
  • polymer is selected from the group consisting of polyterpenes, amorphous polypropylenes, low molecular weight polyethylenes, and ethylene-vinyl acetate copolymers.
  • the conventional paint is selected from the group consisting of two-component amine cured epoxy, two-component urethane, alkyd enamel, phenolic enamel, acrylic water emulsion, and vinyl.
  • a method of coating a substrate which comprises:
  • nonvolatile diluent selected from the group consisting of mineral lubricating oils, synthetic lubricating oils, and petroleum waxes,
  • polymer from about 0.1 to about 25 parts polymer, said polymer being characterized as having a crystallinity of less than 50 percent, a molecular weight in the range of from about 3,000 to about 1 million and a high solubility in predominantly aliphatic hydrocarbon solvents,
  • a metal article one surface of which has been coated with a primer composition and a conventional paint adhered to said primer, said primer composition comprising in parts by weight:
  • nonvolatile diluent selected from the group consisting of mineral lubricating oils, synthetic lubricating oils, and petroleum waxes,
  • composition being characterized further in that it has an acetic base number of at least 50, does not flow at 210 F, and has a dropping point of at least 480 F,
  • polymer from about 0.1 to about 25 parts polymer, said polymer being characterized as having a crystallinity of less than 50 percent, a molecular weight in the range of from about 3,000 to about 1 million and a high solubility in predominantly aliphatic hydrocarbon solvents.

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  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Lubricants (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
US20038A 1970-03-16 1970-03-16 Method of improving resistance to corrosion of metal surfaces and resultant article Expired - Lifetime US3661622A (en)

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BE (1) BE777671Q (OSRAM)
CA (1) CA938176A (OSRAM)
DE (1) DE2061177C3 (OSRAM)
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FR (1) FR2084619A5 (OSRAM)
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US3922437A (en) * 1972-10-19 1975-11-25 Japan National Railway Steel material for use in the prestressed concrete
US4495225A (en) * 1984-03-21 1985-01-22 Economics Laboratory, Inc. Method and composition for the prevention or inhibition of corrosion
US4675215A (en) * 1985-09-27 1987-06-23 Economics Laboratory, Inc. Method and composition for the inhibition of corrosion
US4718942A (en) * 1985-08-08 1988-01-12 Witco Corporation Thixotropic overbased alkaline earth metal inorganic-organic compositions containing alkoxylated oxidized petrolatums
US4728578A (en) * 1986-08-13 1988-03-01 The Lubrizol Corporation Compositions containing basic metal salts and/or non-Newtonian colloidal disperse systems and vinyl aromatic containing polymers
US4729791A (en) * 1985-02-25 1988-03-08 Witco Corporation Corrosion-inhibiting coating compositions for metals
US4749412A (en) * 1985-09-27 1988-06-07 Drew Chemical Corporation Method and composition for the inhibition of corrosion
US4954545A (en) * 1987-07-27 1990-09-04 Phillips Petroleum Company Process for cleaning polymer processing equipment
EP0413859A1 (en) * 1988-08-18 1991-02-27 Exxon Chemical Patents Inc. Metal protecting compositions
EP0414967A1 (en) * 1989-08-21 1991-03-06 Exxon Chemical Patents Inc. Coating compositions
US5244957A (en) * 1989-08-17 1993-09-14 Exxon Chemical Patents Inc. Metal protecting compositions
US6126999A (en) * 1998-04-13 2000-10-03 Tomasino; Randolf R. Urethane-acrylic rubber coating and method of forming a vehicle bed liner
US20030224198A1 (en) * 2002-01-11 2003-12-04 Nissan Technical Center North America, Inc. Reusable masking device for sprayable bed liner
US6677281B2 (en) * 2001-04-20 2004-01-13 Exxonmobil Research And Engineering Company Synergistic combination of metallic and ashless rust inhibitors to yield improved rust protection and demulsibility in dispersant-containing lubricants
US20060025317A1 (en) * 2004-07-29 2006-02-02 Olson William D Overbased calcium salicylate greases
US20070157916A1 (en) * 2006-01-11 2007-07-12 Mancini Ralph J Archery bow having improved design to absorb shock and reduce vibration
US20100132241A1 (en) * 2008-05-19 2010-06-03 Mancini Ralph J Method for accurizing a firearm
WO2013066952A1 (en) 2011-10-31 2013-05-10 Nch Corporation Calcium carbonate based calcium sulfonate grease composition and method of manufacture
US9458406B2 (en) 2011-10-31 2016-10-04 Nch Corporation Calcium hydroxyapatite based sulfonate grease compositions and method of manufacture
WO2017120000A1 (en) 2016-01-07 2017-07-13 Nch Corporation Manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents
WO2017200924A1 (en) 2016-05-18 2017-11-23 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
WO2017200927A1 (en) 2016-05-18 2017-11-23 Nch Corporation Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid
US9976101B2 (en) 2011-10-31 2018-05-22 Nch Corporation Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents
US9976102B2 (en) 2011-10-31 2018-05-22 Nch Corporation Composition and method of manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents
US10087391B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent
US10392577B2 (en) 2016-05-18 2019-08-27 Nch Corporation Composition and method of manufacturing overbased sulfonate modified lithium carboxylate grease
US10519393B2 (en) 2016-05-18 2019-12-31 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
WO2020106553A1 (en) 2018-11-20 2020-05-28 Nch Corporation Composition and method of manufacturing sulfonate-based greases using a glycerol derivative
US11661563B2 (en) 2020-02-11 2023-05-30 Nch Corporation Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases
WO2024047447A1 (en) 2022-09-01 2024-03-07 The Lubrizol Corporation Gelling agent for calcium sulfonate greases
WO2024175811A1 (de) 2023-05-23 2024-08-29 Klueber Lubrication München Gmbh & Co. Kg Schmierfett
EP4467632A1 (de) 2023-05-23 2024-11-27 Klueber Lubrication München GmbH & Co. KG Schmierfett
DE102023113449A1 (de) 2023-05-23 2024-11-28 Klüber Lubrication München GmbH & Co. KG Schmierfett

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US4443577A (en) * 1982-05-12 1984-04-17 The Lubrizol Corporation One-component moisture curable urethane coating system
DE3365584D1 (en) * 1982-05-12 1986-10-02 Lubrizol Corp Two-component urethane coating system

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US2834691A (en) * 1956-10-09 1958-05-13 Gen Electric Process for preparing a metal surface for coating and product thereof
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US3372114A (en) * 1965-02-25 1968-03-05 Lubrizol Corp Process for preparing thickened mineral oil compositions
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US2758981A (en) * 1952-10-29 1956-08-14 Exxon Research Engineering Co Corrosion preventive composition
US2834691A (en) * 1956-10-09 1958-05-13 Gen Electric Process for preparing a metal surface for coating and product thereof
US3084066A (en) * 1959-11-03 1963-04-02 Russell P Dunmire Coated metal article and method of producing
US3242079A (en) * 1962-04-06 1966-03-22 Lubrizol Corp Basic metal-containing thickened oil compositions
US3372114A (en) * 1965-02-25 1968-03-05 Lubrizol Corp Process for preparing thickened mineral oil compositions
US3384586A (en) * 1966-03-17 1968-05-21 Lubrizol Corp Resinous compositions

Cited By (53)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3922437A (en) * 1972-10-19 1975-11-25 Japan National Railway Steel material for use in the prestressed concrete
US4495225A (en) * 1984-03-21 1985-01-22 Economics Laboratory, Inc. Method and composition for the prevention or inhibition of corrosion
US4729791A (en) * 1985-02-25 1988-03-08 Witco Corporation Corrosion-inhibiting coating compositions for metals
US4718942A (en) * 1985-08-08 1988-01-12 Witco Corporation Thixotropic overbased alkaline earth metal inorganic-organic compositions containing alkoxylated oxidized petrolatums
US4749412A (en) * 1985-09-27 1988-06-07 Drew Chemical Corporation Method and composition for the inhibition of corrosion
US4675215A (en) * 1985-09-27 1987-06-23 Economics Laboratory, Inc. Method and composition for the inhibition of corrosion
US4728578A (en) * 1986-08-13 1988-03-01 The Lubrizol Corporation Compositions containing basic metal salts and/or non-Newtonian colloidal disperse systems and vinyl aromatic containing polymers
US4954545A (en) * 1987-07-27 1990-09-04 Phillips Petroleum Company Process for cleaning polymer processing equipment
EP0413859A1 (en) * 1988-08-18 1991-02-27 Exxon Chemical Patents Inc. Metal protecting compositions
US5244957A (en) * 1989-08-17 1993-09-14 Exxon Chemical Patents Inc. Metal protecting compositions
EP0414967A1 (en) * 1989-08-21 1991-03-06 Exxon Chemical Patents Inc. Coating compositions
US6126999A (en) * 1998-04-13 2000-10-03 Tomasino; Randolf R. Urethane-acrylic rubber coating and method of forming a vehicle bed liner
US6677281B2 (en) * 2001-04-20 2004-01-13 Exxonmobil Research And Engineering Company Synergistic combination of metallic and ashless rust inhibitors to yield improved rust protection and demulsibility in dispersant-containing lubricants
US20030224198A1 (en) * 2002-01-11 2003-12-04 Nissan Technical Center North America, Inc. Reusable masking device for sprayable bed liner
US20070200383A1 (en) * 2002-01-11 2007-08-30 Nissan Technical Center North America, Inc. Reusable masking device for sprayable bed liner
US7504133B2 (en) 2002-01-11 2009-03-17 Nissan Technical Center North America, Inc. Method of manufacturing a truck bed liner with a reusable masking device
US20060025317A1 (en) * 2004-07-29 2006-02-02 Olson William D Overbased calcium salicylate greases
US7407920B2 (en) 2004-07-29 2008-08-05 Crompton Corporation Overbased calcium salicylate greases
US20070157916A1 (en) * 2006-01-11 2007-07-12 Mancini Ralph J Archery bow having improved design to absorb shock and reduce vibration
US20080216804A1 (en) * 2006-01-11 2008-09-11 Mancini Ralph J Archery bow having improved design to absorb shock reduce vibration
US7438070B2 (en) 2006-01-11 2008-10-21 Mancini Ralph J Archery bow having improved design to absorb shock and reduce vibration
US20090014239A1 (en) * 2006-01-11 2009-01-15 Mancini Ralph J Archery bow having improved design to absorb shock and reduce vibration
US7708000B2 (en) 2006-01-11 2010-05-04 Mancini Ralph J Archery bow having improved design to absorb shock reduce vibration
US20100108048A1 (en) * 2006-01-11 2010-05-06 Mancini Ralph J Archery bow having improved design to absorb shock and reduce vibration
US20100132241A1 (en) * 2008-05-19 2010-06-03 Mancini Ralph J Method for accurizing a firearm
WO2013066955A1 (en) 2011-10-31 2013-05-10 Nch Corporation Calcium hydroxyapatite based calcium sulfonate grease compositions and method of manufacture
US10316266B2 (en) 2011-10-31 2019-06-11 Nch Corporation Calcium hydroxyapatite based calcium sulfonate grease compositions and method of manufacture
US9273265B2 (en) 2011-10-31 2016-03-01 Nch Corporation Calcium carbonate based sulfonate grease compositions and method of manufacture
US9458406B2 (en) 2011-10-31 2016-10-04 Nch Corporation Calcium hydroxyapatite based sulfonate grease compositions and method of manufacture
US11072756B2 (en) 2011-10-31 2021-07-27 Nch Corporation Calcium hydroxyapatite based calcium sulfonate grease compositions and method of manufacture
WO2013066952A1 (en) 2011-10-31 2013-05-10 Nch Corporation Calcium carbonate based calcium sulfonate grease composition and method of manufacture
US9976101B2 (en) 2011-10-31 2018-05-22 Nch Corporation Method of manufacturing calcium sulfonate greases using delayed addition of non-aqueous converting agents
US9976102B2 (en) 2011-10-31 2018-05-22 Nch Corporation Composition and method of manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents
WO2017120000A1 (en) 2016-01-07 2017-07-13 Nch Corporation Manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents
US10392577B2 (en) 2016-05-18 2019-08-27 Nch Corporation Composition and method of manufacturing overbased sulfonate modified lithium carboxylate grease
EP3957709A1 (en) 2016-05-18 2022-02-23 NCH Corporation Method of manufacturing calcium magnesium sulfonate greases
US10087391B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent
US10087387B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
WO2017200927A1 (en) 2016-05-18 2017-11-23 Nch Corporation Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid
US10519393B2 (en) 2016-05-18 2019-12-31 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US12031100B2 (en) 2016-05-18 2024-07-09 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
WO2017200924A1 (en) 2016-05-18 2017-11-23 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US11168277B2 (en) 2016-05-18 2021-11-09 Nch Corporation Composition and method of manufacturing calcium magnesium sulfonate greases
US10087388B2 (en) 2016-05-18 2018-10-02 Nch Corporation Composition and method of manufacturing calcium sulfonate and calcium magnesium sulfonate greases using a delay after addition of facilitating acid
WO2020106553A1 (en) 2018-11-20 2020-05-28 Nch Corporation Composition and method of manufacturing sulfonate-based greases using a glycerol derivative
US12331261B2 (en) 2018-11-20 2025-06-17 Nch Corporation Composition and method of manufacturing sulfonate-based greases using a glycerol derivative
US11661563B2 (en) 2020-02-11 2023-05-30 Nch Corporation Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases
US12146114B2 (en) 2020-02-11 2024-11-19 Nch Corporation Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases
WO2024047447A1 (en) 2022-09-01 2024-03-07 The Lubrizol Corporation Gelling agent for calcium sulfonate greases
WO2024175811A1 (de) 2023-05-23 2024-08-29 Klueber Lubrication München Gmbh & Co. Kg Schmierfett
EP4467632A1 (de) 2023-05-23 2024-11-27 Klueber Lubrication München GmbH & Co. KG Schmierfett
WO2024240605A1 (de) 2023-05-23 2024-11-28 Klueber Lubrication München Gmbh & Co. Kg Schmierfett
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Also Published As

Publication number Publication date
ES387042A2 (es) 1973-11-16
DE2061177A1 (de) 1971-10-07
GB1271629A (en) 1972-04-19
FR2084619A5 (OSRAM) 1971-12-17
DE2061177B2 (de) 1980-07-17
BE777671Q (fr) 1972-05-02
CA938176A (en) 1973-12-11
DE2061177C3 (de) 1981-03-12

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