WO2015141159A1 - 固体潤滑被膜用組成物、その組成物から形成された固体潤滑被膜を備えた管用ねじ継手、及び、その管用ねじ継手の製造方法 - Google Patents
固体潤滑被膜用組成物、その組成物から形成された固体潤滑被膜を備えた管用ねじ継手、及び、その管用ねじ継手の製造方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L15/00—Screw-threaded joints; Forms of screw-threads for such joints
- F16L15/04—Screw-threaded joints; Forms of screw-threads for such joints with additional sealings
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L15/00—Screw-threaded joints; Forms of screw-threads for such joints
- F16L15/08—Screw-threaded joints; Forms of screw-threads for such joints with supplementary elements
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/085—Phosphorus oxides, acids or salts
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
- C10M2201/1033—Clays; Mica; Zeolites used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/105—Silica
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/14—Synthetic waxes, e.g. polythene waxes
- C10M2205/143—Synthetic waxes, e.g. polythene waxes used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an acyloxy radical of saturated carboxylic or carbonic acid
- C10M2209/062—Vinyl esters of saturated carboxylic or carbonic acids, e.g. vinyl acetate
- C10M2209/0625—Vinyl esters of saturated carboxylic or carbonic acids, e.g. vinyl acetate used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/003—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions used as base material
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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
- C10N2010/00—Metal present as such or in compounds
- C10N2010/02—Groups 1 or 11
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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
- C10N2010/00—Metal present as such or in compounds
- C10N2010/06—Groups 3 or 13
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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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
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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
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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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
- C10N2050/08—Solids
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/10—Geothermal energy
Definitions
- the present invention relates to a composition for forming a solid lubricating film used for the surface treatment of a threaded joint for pipes used for connecting steel pipes, particularly oil well pipes, and a threaded joint for pipes including a solid lubricating film formed from the composition. And a method of manufacturing the threaded joint for pipes.
- Oil well pipes such as tubing that allows fluid such as crude oil to flow inside and casings that contain the tubing are used for oil well drilling for extracting crude oil and gas oil.
- Oil country pipes are generally connected (fastened) using threaded joints for pipes.
- the depth of the oil well is conventionally 2000 to 3000 m.
- the depth of deep oil wells in recent offshore oil fields can reach 8000 to 10,000 m.
- the length of each individual well pipe is typically a few dozen meters. For this reason, an enormous number of oil well pipes such as a thousand or more may be connected.
- the threaded joints for pipes for oil well pipes are subjected to loads such as axial tensile force due to the mass of the oil well pipes and the joints themselves, combined pressures such as inner and outer surface pressures, and underground heat in the operating environment. Therefore, the threaded joint for pipes is required to maintain airtightness without being damaged even in such a severe environment.
- a pin constituted by a part called a pin having a male screw and a part called a box having a female screw as described in Patent Document 1 -Box structure is mentioned.
- the pins are formed at both ends of the oil well pipe, and the boxes are formed on the inner surfaces on both sides of a threaded joint part called a coupling.
- Compound grease When tightening threaded joints for oil well pipes, a lubricant called “compound grease” is applied to the contact surface of the threaded joints (ie, threaded parts and unthreaded metal contacted parts) to improve seizure resistance and airtightness. Apply to.
- Compound grease is a viscous liquid lubricant (grease lubricant) containing heavy metal powder.
- An example of compound grease is described in API standard BUL 5A2.
- the surface treatment is, for example, nitriding treatment, various types of plating including zinc-based plating and dispersion plating, or phosphate chemical conversion treatment.
- Compound grease contains a large amount of heavy metal powder such as zinc, lead and copper. Therefore, the influence on the use environment, for example, the influence on the marine environment and the working environment has been pointed out.
- a threaded joint for pipes disclosed in Patent Document 2.
- the dry solid film is formed from a thermosetting resin film such as an acrylic resin or an ultraviolet curable resin film.
- a viscous liquid or semi-solid lubricating coating is sticky, and foreign matter tends to adhere to it. Stickiness is eliminated by forming a dry solid film on a viscous liquid or semi-solid lubricating film. Since the dry solid coating is destroyed when the threaded joint is fastened, it does not hinder the lubricity of the underlying lubricating coating.
- the present applicants proposed a threaded joint in which a thin lubricating film without stickiness is formed on a threaded portion (pin and box).
- the lubricating coating described in Patent Document 3 can be obtained by dispersing solid lubricant particles in a solid matrix exhibiting plastic or viscoplastic rheological behavior (flow characteristics).
- the melting point of the solid matrix is preferably in the range of 80-320 ° C.
- This lubricating coating is formed by spray coating in a molten state (hot melt spray method), thermal spraying using powder, or spray coating of an aqueous emulsion.
- composition used in the hot melt spray process contains, for example, polyethylene as a thermoplastic polymer, waxes (eg, carnauba wax) and metal soaps (eg, zinc stearate) as lubricating components, and calcium sulfonate as a corrosion inhibitor. To do.
- polyethylene as a thermoplastic polymer
- waxes eg, carnauba wax
- metal soaps eg, zinc stearate
- calcium sulfonate as a corrosion inhibitor.
- the present applicants proposed a threaded joint for pipes in which a solid anticorrosion coating is formed on the contact surface of the pin and a solid lubricant coating is provided on the contact surface of the box according to Patent Document 4.
- the solid anticorrosive coating is mainly composed of an ultraviolet curable resin and is preferably transparent.
- the solid lubricating coating is preferably formed by a hot melt method from a composition containing a thermoplastic polymer, wax, metal soap, corrosion inhibitor, water-insoluble liquid resin and solid lubricant, and exhibits plastic or viscoplastic rheological behavior. Have.
- the threaded joints for pipes described in Patent Documents 2 to 4 have sufficient adhesion and lubrication performance of the solid lubricant film in a low temperature / warm environment of about ⁇ 10 ° C. to + 50 ° C., and therefore have sufficient seizure resistance.
- an extremely low temperature environment such as ⁇ 60 ° C. to ⁇ 20 ° C.
- peeling due to lower adhesion of the solid lubricating coating and cracking due to coating embrittlement tend to occur, and seizure resistance becomes insufficient.
- extremely high torque is required.
- the object of the present invention is to suppress the occurrence of rust without using compound grease even when connecting steel pipes, particularly oil well pipes, in a cryogenic environment, and has excellent seizure resistance and airtightness.
- Composition for forming a solid lubricating film used for surface treatment of a pipe threaded joint having a less sticky surface, manufacturing of a threaded pipe joint having a solid lubricating film formed from the composition, and the threaded joint for a pipe Is to provide a method.
- the composition according to this embodiment is a composition for forming a solid lubricating film on a threaded joint for pipes.
- the composition contains a binder, a fluorine-based additive, a solid lubricant, and an antirust additive.
- the binder contains an ethylene vinyl acetate resin, a polyolefin resin, and a wax having a melting point of 110 ° C. or lower.
- the ratio of the mass of the ethylene vinyl acetate resin to the mass of the polyolefin resin is 1.0 to 1.8.
- the ratio of the total mass of the polyolefin resin and the ethylene vinyl acetate resin to the mass of the wax is 0.7 to 1.6.
- Threaded joint for pipes includes a pin and a box.
- Each of the pin and box includes a contact surface that includes portions that contact each other.
- the solid lubricant film is formed on the contact surface of at least one of the pin and the box.
- the method for manufacturing a threaded joint for pipes according to the present embodiment includes a step of forming the solid lubricant film by applying the composition to the contact surface.
- Threaded joints for pipes with a solid lubricant film formed using the above composition suppress the generation of rust and exhibit excellent seizure resistance and airtightness without using compound grease even in extremely low temperature environments. And the surface is not sticky.
- FIG. 1 is a lineblock diagram showing an example of a screw joint for pipes of this embodiment.
- FIG. 2 is a diagram illustrating an example of a tightening portion of a threaded joint for pipes, and is a cross-sectional view illustrating a non-threaded metal contact portion (shoulder portion and seal portion) of a special threaded joint.
- FIG. 3A is a cross-sectional view of the vicinity of the contact surface when the contact surface of the threaded joint for pipes is roughened.
- FIG. 3B is a cross-sectional view of the vicinity of the contact surface in the case where a base treatment film for roughening is formed on the contact surface of the threaded joint for pipes.
- FIG. 1 is a lineblock diagram showing an example of a screw joint for pipes of this embodiment.
- FIG. 2 is a diagram illustrating an example of a tightening portion of a threaded joint for pipes, and is a cross-sectional view illustrating a non-threaded metal contact portion (
- FIG. 4 is a schematic diagram of a shear tensile test for measuring the adhesion strength of a solid lubricating coating.
- FIG. 5 is a flowchart showing a process of a low temperature-outdoor exposure test of a solid lubricating coating.
- FIG. 6 is a diagram showing the relationship between the rotational speed of the threaded joint and the torque.
- FIG. 7 is a schematic diagram of a flat plate sliding test for measuring the friction coefficient.
- FIG. 8 is a diagram showing the relationship between the content of talc in the solid lubricating film and the friction coefficient.
- the inventor of the present application uses not only a low temperature / warm / tropical region where the temperature is about ⁇ 20 ° C. to + 50 ° C., but also a screw joint used in a very cold region where the temperature may be ⁇ 60 ° C. to ⁇ 20 ° C.
- the following findings were obtained as a result of studies to realize a threaded joint that has sufficient seizure resistance, rust prevention, and airtightness, and that does not require extremely high torque when tightening or loosening the threaded joint.
- a binder (binder) of the composition an ethylene vinyl acetate (EVA) resin, a polyolefin resin, and a wax (WAX) having a melting point of 110 ° C. or less are blended in a specific ratio; (2) Formulating a fluorine-based additive at a specific ratio, (3) Further adding solid lubricating powder and rust preventive additive, Thus, even when exposed to extremely low temperatures, the solid lubricating coating can maintain high adhesion.
- EVA ethylene vinyl acetate
- WAX wax
- the threaded joint has sufficient seizure resistance and airtightness, and can suppress an increase in torque required when the threaded joint is fastened or loosened at a low temperature. further, (4) blending talc with a specific particle size in a specific ratio; Thus, torque adjustment at the time of fastening can be facilitated.
- the composition of this embodiment completed based on the above knowledge is a composition for forming a solid lubricant film on the threaded joint for pipes.
- the composition contains a binder, a fluorine-based additive, a solid lubricant and an antirust additive.
- the binder contains an ethylene vinyl acetate resin, a polyolefin resin, and a wax having a melting point of 110 ° C. or lower.
- the ratio of the mass of the ethylene vinyl acetate resin to the mass of the polyolefin resin is 1.0 to 1.8.
- the ratio of the total mass of the polyolefin resin and the ethylene vinyl acetate resin to the mass of the wax is 0.7 to 1.6.
- thermoplastic solid lubricating film having excellent seizure resistance can be formed on the contact surface of the threaded joint for pipes without using compound grease.
- This solid lubricating film hardly deteriorates even in an extremely low temperature environment of ⁇ 60 ° C. to ⁇ 20 ° C. Therefore, excellent seizure resistance, airtightness, and rust prevention properties similar to those when using compound grease are exhibited, and further, an increase in torque required when fastening and loosening a threaded joint can be suppressed.
- the composition comprises 60-80% by weight binder, 8-18% by weight fluorine based additive, 5-15% by weight solid lubricant, and 2-10% by weight rust preventive additive. Containing the agent.
- the above composition may further contain 2 to 15% by mass of talc.
- the difference between the yield torque and the shouldering torque can be increased, and as a result, torque adjustment at the time of fastening can be facilitated.
- the particle diameter of talc in the above composition is, for example, 1 to 12 ⁇ m, and the specific surface area of talc is 4 to 12 m 2 / g.
- Threaded joint for pipes includes a pin and a box. Each of the pin and box includes a contact surface that includes portions that contact each other.
- a solid lubricating film is formed on the contact surface of at least one of the pin and the box.
- the solid lubricant film contains a binder, a fluorine-based additive, a solid lubricant, and an antirust additive.
- the binder contains an ethylene vinyl acetate resin, a polyolefin resin, and a wax having a melting point of 110 ° C. or lower.
- the ratio of the mass of the ethylene vinyl acetate resin to the mass of the polyolefin resin is 1.0 to 1.8.
- the ratio of the total mass of the polyolefin resin and the ethylene vinyl acetate resin to the mass of the wax is 0.7 to 1.6.
- the threaded joint for pipes according to the present embodiment includes the solid lubricant film, it can be used without applying compound grease, and can maintain high adhesion even when exposed to a cryogenic environment. As a result, excellent seizure resistance, airtightness, and rust resistance are exhibited. Therefore, it is particularly useful for oil well drilling in extremely cold regions.
- the solid lubricating coating comprises 60 to 80% by mass of binder, 8 to 18% by mass of a fluorine-based additive, 5 to 15% by mass of solid lubricant, and 2 to 10% by mass. % Rust preventive additive.
- the solid lubricant film may further contain 2 to 15% by mass of talc.
- the difference between the yield torque and the shouldering torque can be increased, and as a result, torque adjustment when fastening the threaded joint Can be made easier.
- the particle size of talc is, for example, 1 to 12 ⁇ m, and the specific surface area of talc is, for example, 4 to 12 m 2 / g.
- the threaded joint for pipes further includes a solid anticorrosive coating containing an ultraviolet curable resin.
- the solid lubricant film is formed on one contact surface of the pin and the box.
- a solid anticorrosion coating is formed on the other contact surface of the pin and the box.
- the thickness of the solid anticorrosion coating is, for example, 5 to 50 ⁇ m.
- the thickness of the solid lubricant film is, for example, 10 to 200 ⁇ m.
- the threaded joint for pipes is used for an oil well pipe.
- the method for manufacturing a threaded joint for pipes of the present embodiment is a method for manufacturing a threaded joint for pipes having a pin and a box.
- Each of the pin and box includes a contact surface that includes portions that contact each other.
- the manufacturing method of the threaded joint for pipes of this embodiment is equipped with the process of apply
- the manufacturing method includes a step of forming the solid lubricant film on one contact surface of the pin and the box.
- the said manufacturing method further includes the process of apply
- the manufacturing method further includes a step of irradiating the composition for a solid anticorrosive film with ultraviolet rays to form the solid anticorrosive film.
- the threaded joint for pipes according to the present embodiment will be described more specifically for the purpose of illustration.
- the threaded joint for pipes of a steel pipe for oil country tubular goods will be described as a preferred embodiment.
- the present invention is not particularly limited to this embodiment, and can be applied to, for example, a threaded joint used for a pipe other than an oil well pipe.
- FIG. 1 is a configuration diagram showing an example of a threaded joint for pipes of the present embodiment.
- the threaded joint for pipes includes a steel pipe 2 and a coupling 8.
- Pins 6 having male threaded portions 4 on the outer surface are formed at both ends of the steel pipe 2.
- a box 12 having an internal thread portion 10 on the inner surface is formed on both sides of the coupling 8.
- a coupling 8 is attached to one end of the steel pipe 2 with a screw in advance.
- a protector for protecting each screw portion is provided on the pin 6 (left side in the illustrated example) of the steel pipe 2 and the box 12 (right side in the illustrated example) of the coupling 8 on which the mating member is not mounted. (Not shown) is installed before shipment.
- the pin 6 is formed on the outer surface of both ends of the steel pipe 2 and the box 12 is formed on the inner surface of the coupling 8, as in the threaded joint for pipes of the coupling system shown in FIG.
- the threaded joint for pipes of this embodiment can be applied to both the coupling method and the integral method.
- FIG. 2 is a cross-sectional view showing an example of a tightening portion of a threaded joint for pipes.
- Seal portions 14 and 16 are formed on the outer peripheral surface near the end surface on the tip side of the male screw of the pin 6 and the inner peripheral surface of the base portion of the female screw of the box 12, respectively.
- Shoulder portions (also called torque shoulders) 18 and 20 are formed on the end surface of the tip of the pin 6 and the innermost surface of the box 12 corresponding to the end surface of the tip of the pin 6, respectively.
- a seal part and a shoulder part comprise the metal contact part (what is called a screwless metal contact part) which does not have a screw in a pipe threaded joint.
- the metal contact portion and the screw portion where the pin 6 and the box 12 are in contact with each other constitute the contact surface of the threaded joint for pipes.
- the shoulder portions 18 and 20 of the pin 6 and the box 12 come into contact with each other. This torque is called shouldering torque.
- the seal portions 14 and 16 of the pin 6 and the box 12 are brought into close contact with each other to form a metal-metal seal, thereby ensuring airtightness of the threaded joint for pipes. Is done. The torque at this time is called fastening torque.
- the metal constituting at least one of the pin 6 and the box 12 starts to undergo plastic deformation.
- This torque is called yield torque.
- the fastening torque is set within a range larger than the shouldering torque and smaller than the yield torque. Therefore, when the difference between the yield torque and the shouldering torque is large, the fastening torque can be easily adjusted.
- the thread portion, the seal portion, and the shoulder portion correspond to the contact surface of the threaded joint.
- These contact surfaces are required to have seizure resistance, airtightness, and corrosion resistance.
- compound grease containing heavy metal powder has been applied to the contact surface.
- the solid lubricant film is typically a resin film containing a solid lubricant.
- the conventional solid lubricating coating has a problem that when it is exposed to an extremely low temperature environment of ⁇ 60 ° C. to ⁇ 20 ° C. even once, the coating itself cracks due to embrittlement deterioration. Furthermore, the conventional solid lubricating coating has a problem that due to the difference in coefficient of thermal expansion from the base material (steel), the adhesiveness is lowered and the coating is easily peeled when returning to near normal temperature.
- FIG. 3A and FIG. 3B are sectional views of the vicinity of the contact surface of the threaded joint for steel pipes of this embodiment.
- the contact surface of at least one of the pin and the box is covered with a solid lubricating film 24 formed by a composition described later on the surface of the steel pipe 22 constituting the member.
- the solid lubricating coating 24 can maintain adhesion even when exposed to an extremely low temperature environment of ⁇ 60 ° C. to ⁇ 20 ° C.
- the solid lubricating coating 24 further imparts lubricity to the threaded joint. For this reason, seizure of the threaded joint can be prevented while preventing increase in torque during fastening and loosening, and airtightness after fastening can be ensured.
- the solid lubricating coating 24 may be included in the coating on the surface of the steel pipe 22.
- it may be formed so as to be in direct contact with the surface of the steel pipe 22.
- it may be contained in a coating film formed on the surface of the steel pipe.
- the solid lubricating coating 24 is preferably disposed on the top surface of the coating on the surface of the steel tube 22.
- the arrangement of the solid lubricant film 24 is not particularly limited.
- a rust preventive agent or a coating agent for preventing wrinkles may be applied to the uppermost surface of the film including the solid lubricant film 24.
- the case where the solid lubricating coating 24 is directly formed on the contact surface of the steel pipe 22 will be described as an example.
- the interface between the solid lubricating coating 24 and the steel pipe 22 is preferably a rough surface.
- This roughening can be achieved by directly roughening the surface of the steel pipe 22 by blasting or pickling as shown in FIG. 3A.
- the roughening is performed by applying a ground treatment coating (for example, a phosphate coating or a porous zinc (alloy) plating coating) 26 having a rough surface to the steel pipe before the lubricating coating 24 is formed. It can also be achieved by forming it on the surface of 22.
- a ground treatment coating for example, a phosphate coating or a porous zinc (alloy) plating coating
- the solid lubricant film 24 is formed by the following method, for example.
- a composition for forming a thermoplastic solid lubricating coating is prepared.
- the composition is melted at a predetermined temperature and applied onto the contact surface by a suitable method such as spraying, brushing, spraying and dipping.
- a suitable method such as spraying, brushing, spraying and dipping.
- the composition is solidified by a known cooling means such as air cooling or standing cooling to form a solid lubricating coating 24.
- the solid lubricant film may be formed on the contact surface of both the pin and the box.
- a solid lubricating film may be formed only on one contact surface of the pin and the box at a place where the pin and the box are fastened at the time of shipment.
- a coating with a shorter dimension than a steel pipe having a longer dimension is easier to apply for base treatment or lubrication film formation. Therefore, it is usually preferable to form a lubricating film on the contact surface of the coupling, that is, the contact surface of the box.
- a solid lubricating film may be formed on the contact surface of both the pin and the box to provide rust prevention as well as lubricity.
- the solid lubricating film may be formed only on the contact surface of one of the pins and the box (for example, the box), and the solid anticorrosion film may be formed on the contact surface of the other (for example, the pin). In either case, seizure resistance, airtightness, and rust prevention can be imparted to the threaded joint.
- the solid anticorrosive film is preferably an ultraviolet curable film.
- the solid anticorrosive film is formed after applying a ground treatment for roughening.
- the solid lubricating coating covers all of the contact surfaces of at least one of the pin and the box.
- the solid lubricating coating may cover only a part of the contact surface (for example, only the seal portion).
- Solid lubricating coating As described above, in this embodiment, a solid lubricant film is formed on the contact surface of at least one of the pin and the box constituting the threaded joint for pipes.
- This solid lubricating coating is required to maintain adhesion even when exposed to extremely low temperatures ( ⁇ 60 ° C. to ⁇ 20 ° C.).
- solid lubricant coatings not only in low, warm and tropical areas (-20 ° C to + 50 ° C) but also in extremely low temperature regions (-60 ° C to -20 ° C) It is required that the tightening torque is not increased to cause high shouldering and the screw loosening torque is not increased, thereby suppressing the occurrence of seizure.
- the solid lubricating coating is further required to prevent rusting during storage. If the adhesion strength (hardness) of the solid lubricant film varies greatly between near normal temperature and a cryogenic environment, the solid lubricant film may crack when the solid lubricant film cracks or returns to near ambient temperature in a cryogenic environment. Peeling occurs. For this reason, the solid lubricating coating is further required to have no significant change in the adhesion strength (hardness) of the solid lubricating coating in the vicinity of room temperature and in a cryogenic environment.
- the composition for forming the solid lubricant film of this embodiment is a base material for the film.
- the composition includes a binder that exhibits high adhesion from room temperature to cryogenic temperature, a fluorine-based additive for adhesion at low temperatures and low friction, and a solid lubricant for preventing seizure, Contains a rust preventive for long-term rust prevention from application to use.
- the binder of this embodiment is composed of an ethylene vinyl acetate resin (EVA), a polyolefin resin (PO), and a wax (W) having a melting point of 110 ° C. or less.
- EVA ethylene vinyl acetate resin
- PO polyolefin resin
- W wax
- the mass ratio of ethylene vinyl acetate resin, polyolefin resin, and wax is as follows. 1.0 ⁇ (EVA / PO) ⁇ 1.8 and 0.7 ⁇ ((EVA + PO) / W) ⁇ 1.6
- the mass ratio is a matter that has been experimentally clarified for the first time in the present invention.
- EVA, PO, and W in the above formulas indicate masses of the ethylene vinyl acetate resin, the polyolefin resin, and the wax, respectively.
- the mass ratio of the ethylene vinyl acetate resin to the polyolefin resin (EVA / PO) is less than 1.0, the adhesion strength of the solid lubricating coating is insufficient at a temperature exceeding ⁇ 20 ° C.
- (EVA / PO) exceeds 1.8, the adhesion strength of the solid lubricating film at an extremely low temperature of ⁇ 20 ° C. or lower is insufficient.
- the lower limit of (EVA / PO) is 1.0 and the upper limit is 1.8.
- the preferable lower limit of (EVA / PO) is 1.05, more preferably 1.1, still more preferably 1.15, and still more preferably 1.2. More preferably, it is 1.35.
- the preferable upper limit of (EVA / PO) is 1.7, more preferably 1.65, and still more preferably 1.6.
- the lower limit of ((EVA + PO) / W) is 0.7, and the upper limit is 1.6.
- a preferable lower limit of ((EVA + PO) / W) is 0.8, more preferably 0.85, and still more preferably 0.9.
- a preferable upper limit of ((EVA + PO) / W) is 1.5, more preferably 1.45, and still more preferably 1.4.
- Polyolefin resin (PO) is a general term for chain hydrocarbons having a double bond at one location. Since the polyolefin resin (PO) is made of a crystalline polymer (polymer), the physical properties change depending on the degree of crystallinity. Examples of this type of resin include polyethylene and polypropylene, and specific examples include HM712 (softening point 120 ° C.) manufactured by Cemedine Co., Ltd.
- Ethylene vinyl acetate resin is a copolymer of ethylene and vinyl acetate. Specific examples include HM224 (softening point 86 ° C.) manufactured by Cemedine Co., Ltd.
- Wax (W) suppresses seizure by reducing friction of the solid lubricant film.
- the wax further adjusts the hardness of the solid lubricating coating and increases the toughness of the solid lubricating coating.
- any of animal, vegetable, mineral and synthetic waxes can be used.
- Usable waxes are, for example, beeswax, spermaceti (above, animal), wood wax, carnauba wax, candelilla wax, rice wax (above, plant), paraffin wax, microcrystalline wax, petrolatum, montan wax, ozokerite Ceresin (above, mineral), oxidized wax, polyethylene wax, Fischer-Tropsch wax, amide wax, hardened castor oil (caster wax) (above, synthetic wax).
- a wax having a melting point of 110 ° C. or lower is used. If the melting point of the wax is 110 ° C. or less, the difference between the adhesion strength of the solid lubricant film at around room temperature and the adhesion strength (hardness) of the solid lubricant film in a cryogenic environment becomes small. Thereby, the crack of a solid lubricating film can be suppressed in a cryogenic environment. Furthermore, peeling of the solid lubricant film when returning to around normal temperature can be suppressed. That is, the adhesion strength (hardness) of the solid lubricant film can be maintained in an appropriate range, and the toughness of the solid lubricant film is further increased.
- the melting point of the wax is preferably 100 ° C.
- the wax is preferably solid at room temperature.
- a preferred lower limit of the melting point of the wax is 40 ° C.
- the content of the binder with respect to the composition is preferably 60 to 80% by mass (hereinafter, the content is described in mass% unless otherwise specified). If the content of the binder is 60% or more, the adhesion of the solid lubricating coating is further increased. If the content of the binder is 80% or less, the lubricity is better maintained.
- the binder it is preferable to use an ethylene vinyl acetate resin or a polyolefin resin having a melting temperature (or softening temperature, the same shall apply hereinafter) of 80 to 320 ° C.
- the molten base (binder) returns to a solid when the temperature is lower than the melting temperature.
- the melting temperature is more preferably in the range of 90 to 200 ° C. If the melting temperature of the ethylene vinyl acetate resin or polyolefin resin as the coating base is too high, it becomes difficult to apply in a molten state as in hot melt application. On the other hand, if the melting temperature of the binder is too low, the solid lubricating film may be softened when the temperature is increased, and the performance may be deteriorated.
- the contact surface of the threaded joint for pipes that forms the lubricating coating may be subjected to a ground treatment by chemical conversion or plating, as will be described later.
- a ground treatment by chemical conversion or plating, as will be described later.
- the film formability and the coatability the viscosity when the solid lubricant film melts, the dispersibility of the solid lubricant, etc.
- the ethylene vinyl acetate resin and the polyolefin resin have a melting point
- a mixture of a plurality of types having different properties such as a softening point and a glass transition point is preferable.
- the ethylene vinyl acetate resin used as a base (binder) is particularly preferably a mixture of two or more ethylene vinyl acetate resins having different melting temperatures in order to suppress rapid softening due to temperature rise.
- the polyolefin resin used as a base (binder) is particularly preferably a mixture of two or more polyolefin resins having different melting temperatures.
- the solid lubricating film of the present embodiment is based on a binder and further contains a fluorine-based additive.
- Fluorine-based additives improve slipperiness during sliding.
- the fluorine-based additive further enhances the toughness of the solid lubricating coating at extremely low temperatures.
- the fluorine-based additive include liquid perfluoropolyether (PFPE) and grease-like fluorinated polymer.
- PFPE liquid perfluoropolyether
- PFPE liquid perfluoropolyether
- a modified perfluoropolyether such as a fluorinated polyether having a molecular weight of 500 to 10,000 can also be used as the fluorine-based additive.
- the preferred content of the fluorine-based additive in the composition is 8 to 18%. If content of a fluorine-type additive is 8% or more, the lubricity and adhesiveness in low temperature will improve more. If content of a fluorine-type additive is 18% or less, the adhesiveness at normal temperature can be maintained more favorably.
- Solid lubricant The solid lubricant film contains various solid lubricants in order to further improve the lubricity.
- the solid lubricant means a powder having lubricity.
- Solid lubricants are roughly classified into the following four types.
- a specific crystal structure that is slippery such as a hexagonal layered crystal structure that exhibits lubricity (for example, graphite, zinc oxide, boron nitride), (2) Those having a lubricity by having a reactive element in addition to the crystal structure (for example, molybdenum disulfide, tungsten disulfide, fluorinated graphite, tin sulfide, bismuth sulfide), (3) Those which exhibit lubricity due to chemical reactivity (for example, certain thiosulfate type compounds), and (4) Those which exhibit lubricity due to plasticity or viscoplastic behavior under frictional stress (for example, poly Tetrafluoroethylene (PTFE) and polyamide).
- lubricity for example, graphite, zinc oxide, boron nitride
- Those having a lubricity by having a reactive element in addition to the crystal structure for example, molybdenum disulfide, tungsten disulfide
- any of the solid lubricants (1) to (4) above can be used.
- a preferred solid lubricant is (1).
- the solid lubricant (1) may be used alone, at least one of the solid lubricants (2) and (4) may be used in combination.
- graphite is a preferred solid lubricant, and from the viewpoint of film formability, earthy graphite is more preferred.
- the solid lubricant content in the solid lubricant film (and in the solid lubricant film composition) is preferably in the range of 5 to 15% by mass.
- the composition for the solid lubricating film may further contain an inorganic powder for adjusting the slidability.
- inorganic powders are, for example, titanium dioxide and bismuth oxide.
- the inorganic powder can be contained in the composition in a total amount of up to 10% by mass.
- the solid lubricating coating according to the present invention actively contains a rust preventive additive in order to ensure rust prevention over a long period of time until it is applied and actually used.
- rust preventive additives include aluminum tripolyphosphate, aluminum phosphite and calcium ion exchanged silica.
- reaction water repellents can also be used.
- the preferable content of the anticorrosive additive in the composition is 2 to 10% by mass.
- the rust preventive additive is contained in an amount of 2% by mass or more, the rust preventive property of the solid lubricating coating is further increased. If the rust preventive additive is contained in an amount of 10% by mass or less, the lubricity and adhesion of the solid lubricating film can be maintained better.
- the composition for a solid lubricant film may further contain talc as a friction modifier.
- Talc is a white or gray inorganic powder made by crushing ore called talc.
- the chemical name of talc is hydrous magnesium silicate and has a chemical composition of Mg 3 Si 4 O 10 (OH) 2 .
- Talc contains about 60% by mass of SiO 2 , about 30% by mass of MgO, and about 4.8% by mass of crystal water.
- Talc has a true specific gravity of 2.7 to 2.8 and a Mohs hardness of 1, which is the lowest among inorganic minerals.
- talc is a chemically stable substance with excellent heat resistance. Therefore, talc can be used as a filler.
- the surface-modified talc in which dispersibility is improved by chemically or physically bonding a treatment material to the talc surface is also included in the talc of this embodiment.
- Talc works to increase the difference between yield torque (at high surface pressure) and shouldering torque (at low surface pressure) when fastening threaded joints.
- the difference between the yield torque and the shouldering torque is large, there is a margin in the range of the fastening torque when fastening the threaded joint.
- This effect is obtained because talc maintains the coefficient of friction at an appropriate level when the contact pressure of the contact sliding surface of the threaded joint is high.
- the content of talc in the composition is 2% by mass or more, this effect can be increased.
- the content is 15% by mass or less, there is little fear of damaging seizure resistance.
- the content of talc is preferably 2 to 15% by mass.
- a more preferable lower limit of the talc content is 3% by mass, and further preferably 5% by mass.
- the upper limit with more preferable talc content is 10 mass%, More preferably, it is 8 mass%.
- the particle diameter of the talc of this embodiment is preferably 1 to 12 ⁇ m. If the particle diameter of talc is 1 ⁇ m or more, the effect of increasing the difference between the yield torque and the shouldering torque can be stably obtained. If the particle diameter of talc is 12 ⁇ m or less, there is little fear that the dispersibility and adhesion in the solid lubricating coating will be reduced.
- the more preferable lower limit of the particle size of talc is 3 ⁇ m, and more preferably 4 ⁇ m.
- a more preferable upper limit of the particle size of talc is 10 ⁇ m, and more preferably 8 ⁇ m.
- the “particle diameter” refers to the median diameter (D50) obtained from the particle size distribution.
- a cumulative particle size distribution is created using a laser diffraction particle size distribution measuring device. And it can obtain
- the specific surface area of the talc according to this embodiment is preferably 4 to 12 m 2 / g.
- the specific surface area of talc is 4 m 2 / g or more, the affinity between talc and the binder in the solid lubricating coating increases. Therefore, talc can be prevented from falling off from the surface of the solid lubricant film during sliding.
- the specific surface area of talc is 12 m 2 / g or less, the effect of increasing the difference between the yield torque and the shouldering torque can be stably obtained.
- the more preferable lower limit of the specific surface area of talc is 6 m 2 / g, and more preferably 7 m 2 / g.
- a more preferable upper limit of the specific surface area of talc is 11 m 2 / g, and more preferably 10 m 2 / g.
- the specific surface area of talc can be determined by, for example, the BET method. Specifically, a gas (for example, nitrogen gas) whose adsorption-occupied area is already known is adsorbed on the surface of talc using a specific surface area automatic measuring device. From the relationship between the gas pressure and the gas adsorption amount, the single molecule adsorption amount is calculated by the BET equation. Furthermore, the specific surface area can be calculated by multiplying the adsorption-occupied area per unit gas molecule.
- a gas for example, nitrogen gas
- composition of the present embodiment may contain a small amount of additive components selected from surfactants, colorants, antioxidants and the like, for example, in a total amount of 5% by mass or less.
- the composition for a solid lubricant film can further contain an extreme pressure agent, a liquid oil agent, etc., as long as it is a very small amount of 2% by mass or less.
- a composition for forming a solid lubricant film (hereinafter, also referred to as a coating composition) for forming the solid lubricant film is provided.
- This coating composition may be a solvent-free composition comprising only the components described above, or may be a solvent-type composition dissolved in a solvent.
- the mass% of each component means mass% when the total mass of all components other than the solvent contained in the composition is 100%.
- the solventless coating composition can be prepared by, for example, blending a solid lubricant or a rust preventive additive into a molten base and kneading.
- a powder mixture in which all components are mixed in powder form can be used as a coating composition.
- the solventless composition has an advantage that a lubricating coating can be formed in a short time and there is no evaporation of the organic solvent that affects the environment.
- Such a solvent-free coating composition can form a solid lubricating film using, for example, a hot melt method.
- the coating composition (containing the above-described base and various powders) is heated to melt the base, and the composition in a low-viscosity fluid state is heated to a constant temperature (usually in a molten state).
- the spray gun is sprayed from a spray gun having a function of maintaining the temperature at the same level as the temperature of the composition.
- the heating temperature of the composition is preferably 10 to 50 ° C. higher than the melting point (melting temperature or softening temperature) of the base (mixture in the case of a mixture).
- the contact surface of at least one of the pin and the box to which the composition is applied is preferably preheated to a temperature higher than the melting point of the base. Thereby, good coverage can be obtained.
- the coating composition is heated and melted in a tank equipped with an appropriate stirring device, and supplied to a spray gun spray head (maintained at a predetermined temperature) via a metering pump by a compressor and sprayed.
- the holding temperature of the tank and the spray head is adjusted according to the melting point of the base in the composition.
- the composition for forming the solid lubricating film is solidified, and the solid lubricating film according to the present embodiment is formed on the contact surface.
- the thickness of the solid lubricant film thus formed is preferably in the range of 10 to 200 ⁇ m, more preferably in the range of 25 to 100 ⁇ m. If the film thickness of the solid lubricating coating is too small, the threaded joint for pipes is insufficient in lubricity, and seizure is likely to occur during tightening or loosening. This solid lubricating coating also has a certain degree of anticorrosion, but if the film thickness is too small, the anticorrosion becomes insufficient and the corrosion resistance of the contact surface decreases.
- the film thickness of the solid lubricating film is not only wasted, but it can affect the environment.
- the film thickness is larger than the Rmax of the base. It is preferable. Otherwise, the base may not be completely covered.
- the film thickness when the base is a rough surface is an average value of the film thickness of the entire film, which can be calculated from the area, mass and density of the film.
- a solid or liquid thin film rust preventive film may be further formed on the upper layer or the lower layer of the film.
- thermoplastic solid lubricating coating When the above-mentioned thermoplastic solid lubricating coating is formed only on the contact surface of one of the pin and box (for example, box) of the threaded joint for pipes, the contact surface of the other (for example, pin) is, for example, only the ground treatment described later. However, preferably, a solid anticorrosive film is formed as the uppermost surface treatment film layer in order to impart rust prevention.
- a protector is often attached to a pin and a box that are not tightened before the pipe threaded joint is actually used.
- Solid anti-corrosion coatings are not destroyed by at least the force applied when the protector is attached, and they do not dissolve even when exposed to condensed water due to the dew point during transportation and storage, and are easy even at high temperatures exceeding 40 ° C. Is required not to soften.
- a solid anticorrosive film is formed from a composition mainly composed of an ultraviolet curable resin, which is known to be capable of forming a high-strength film as a film satisfying such properties.
- an ultraviolet curable resin a known resin composition composed of at least a monomer, an oligomer, and a photopolymerization initiator can be used.
- the components and composition of the ultraviolet curable resin composition as long as it causes a photopolymerization reaction upon irradiation with ultraviolet rays and forms a cured film.
- Examples of the monomer include various (meth) acrylate compounds, N-vinylpyrrolidone, N-vinylcaprolactam, and styrene, in addition to polyvalent (di- or tri- or more) esters of polyhydric alcohol and (meth) acrylic acid.
- Examples of the oligomer include, but are not limited to, epoxy (meth) acrylate, urethane (meth) acrylate, polyester (meth) acrylate, polyether (meth) acrylate, and silicone (meth) acrylate.
- a preferred photopolymerization initiator is a compound having absorption at a wavelength of 260 to 450 nm.
- the photopolymerization initiator include benzoin and derivatives thereof, benzophenone and derivatives thereof, acetophenone and derivatives thereof, Michler ketone, benzyl and derivatives thereof, tetraalkylthiuram monosulfide, and thioxanes.
- Particularly preferred photopolymerization initiators are thiooxanes.
- the solid anticorrosive film formed from the ultraviolet curable resin may contain an additive selected from a lubricant and a rust preventive agent from the viewpoint of the film strength and slipperiness.
- An additive for improving the coating strength is a fibrous filler.
- the fibrous filler is, for example, acicular calcium carbonate such as “Whiscal” manufactured by Maruo Calcium.
- lubricants are metal soaps such as calcium stearate or zinc stearate, polytetrafluoroethylene (PTFE) resin.
- PTFE polytetrafluoroethylene
- One or more kinds of these lubricants can be added in an amount of 0.05 to 0.35 with respect to the ultraviolet curable resin 1 by mass ratio. If it is 0.05 or less, the film strength may be insufficient. On the other hand, if it exceeds 0.35, the viscosity may increase and the coating workability may decrease, and conversely, the film strength may decrease.
- the rust preventive is, for example, aluminum tripolyphosphate or aluminum phosphite.
- the rust preventive can be added up to about 0.10 relative to the ultraviolet curable resin 1 by mass ratio.
- the solid anticorrosion coating may contain a colorant.
- the colorant used can be selected from pigments, dyes and fluorescent materials.
- the fluorescent material may not color the film under visible light, and may color the film at least under ultraviolet light. Therefore, the fluorescent material is included in the colorant in the present invention.
- a commercial item may be used for these colorants, and there is no particular limitation as long as the quality inspection of the solid anticorrosion coating can be performed visually or by image processing. Both organic colorants and inorganic colorants can be used.
- the transparency of the solid anticorrosion film is reduced or lost. If the solid anticorrosion coating becomes opaque, it will be difficult to inspect the underlying pin screw part for damage. Accordingly, when a pigment is used, a pigment having a high brightness such as yellow or white is preferable. From the viewpoint of anticorrosion properties, the finer the particle size of the pigment, the better the average particle size is preferably 5 ⁇ m or less. Since the dye does not greatly reduce the transparency of the solid anticorrosion coating, for example, a strong color dye such as red or blue does not cause any trouble.
- the addition amount of the pigment and the dye is preferably up to 0.05 with respect to the ultraviolet curable resin 1 by mass ratio. If it exceeds 0.05, the anticorrosion property may be lowered. A more preferable mass ratio of the added amount is 0.02 or less.
- Fluorescent material may be any of fluorescent pigments, fluorescent dyes, and phosphors used in fluorescent paints. Fluorescent pigments are roughly classified into inorganic fluorescent pigments and daylight fluorescent pigments. Inorganic fluorescent pigments include, for example, zinc sulfide or zinc cadmium sulfide (containing a metal activator), calcium halide phosphate, rare earth activated strontium chloroapatite, and a mixture of two or more of them may be used. Many. Inorganic fluorescent pigments are excellent in weather resistance and heat resistance.
- daylight fluorescent pigments there are several types of daylight fluorescent pigments, but the mainstream is a synthetic resin solid solution type in which a fluorescent dye is contained in a colorless synthetic resin to form a pigment. Fluorescent dyes themselves can also be used. In addition, various inorganic or organic fluorescent pigments, particularly those of a synthetic resin solid solution type, are used for fluorescent paints and fluorescent printing inks, and these phosphors can be used as fluorescent pigments or fluorescent dyes.
- Solid anticorrosive coatings containing fluorescent pigments or dyes are colorless or colored transparent under visible light, but emit light and color when irradiated with black light or ultraviolet rays, so check for the presence of coatings and uneven coating thickness. be able to. Moreover, since it is transparent under visible light, the substrate under the solid anticorrosion coating can be observed. Therefore, the inspection of the threaded portion of the threaded joint is not hindered by the solid anticorrosion coating.
- the addition amount of these fluorescent materials is preferably up to about 0.05 with respect to the ultraviolet curable resin 1 by mass ratio. If it exceeds 0.05, the anticorrosion property may be lowered. A more preferable mass ratio of the added amount is 0.02 or less.
- a fluorescent material particularly a fluorescent pigment, as the colorant.
- An ultraviolet curable resin layer is formed by applying a composition containing an ultraviolet curable resin as a main component (including a composition made only of an ultraviolet curable resin composition) to the contact surface of a screw joint and then irradiating ultraviolet rays to cure the coating.
- a solid anticorrosive coating consisting of is formed.
- a solid anticorrosive film composed of two or more UV-curable resin layers may be formed by repeating application and UV irradiation.
- the coating strength is further increased, and the solid anticorrosion coating is not destroyed even by a force applied during tightening of the threaded joint, and the corrosion resistance of the threaded joint is further improved.
- the corrosion resistance of the screw joint is better when the solid anti-corrosion coating is not destroyed. Get higher.
- UV light can be irradiated by using a commercially available UV irradiation device having an output wavelength in the 200 to 450 nm region.
- the ultraviolet irradiation source include a high-pressure mercury lamp, an ultrahigh-pressure mercury lamp, a xenon lamp, a carbon arc lamp, a metal halide lamp, and sunlight.
- Those skilled in the art can appropriately set the irradiation time and the irradiation ultraviolet intensity.
- the film thickness of the solid anticorrosive film (the total film thickness in the case of comprising two or more UV curable resin layers) is preferably in the range of 5 to 50 ⁇ m, more preferably in the range of 10 to 40 ⁇ m. Moreover, it is preferable to make it smaller than the film thickness of the solid lubricating film formed in the other member. If the film thickness of the solid anticorrosion coating is too thin, it does not function sufficiently as the anticorrosion coating, and the corrosion resistance of the pipe threaded joint may be insufficient.
- the thickness of the solid anticorrosion coating is larger than 50 ⁇ m, the solid anticorrosion coating may be destroyed by the force when the protector is attached when attaching a protective member such as a highly airtight protector to the pipe end of the oil well pipe. Again, the corrosion resistance of the threaded joint for pipes is insufficient. Moreover, since it becomes a wear powder and is discharged
- the solid anticorrosion film composed mainly of UV-curing resin is a transparent film, the state of the substrate can be observed without removing the film, and the screw part before tightening should be inspected from above the film. Is possible. Therefore, this solid anti-corrosion coating is typically formed on the outer surface of the steel pipe end by forming the threaded portion on the outer surface of the pin and the contact surface of the pin that is more susceptible to damage. It is possible to easily inspect the screw portion for damage while leaving the film.
- a threaded portion and a seal portion which are contact surfaces of a threaded joint for pipes, are formed by cutting including threading, and generally have a surface roughness of about 3 to 5 ⁇ m. If the surface roughness of the contact surface is made larger than this, the adhesion of the film formed thereon can be enhanced, and as a result, performance such as seizure resistance and corrosion resistance can be improved.
- Examples of such a base treatment include a blasting process in which a blasting material such as a spherical shot material or a square grid material is projected, or immersion in a strong acid solution such as sulfuric acid, hydrochloric acid, nitric acid or hydrofluoric acid. Examples include pickling that roughens the skin. These are treatments that can increase the surface roughness of the substrate itself.
- Examples of other base treatments include phosphate chemical treatment, oxalate chemical treatment, chemical treatment such as borate chemical treatment, and metallic plating. These are methods for forming a base film having a large surface roughness and high adhesion on the substrate surface.
- chemical conversion treatment a chemical conversion film having a large surface roughness made of acicular crystals is formed.
- metallic plating plating of copper, iron, alloys thereof, etc. by electroplating method (the surface is slightly rough because the convex part is preferentially plated), zinc or zinc-iron on the iron core Impact-plating of zinc or zinc alloy that projects particles coated with an alloy etc. using centrifugal force or air pressure to form a porous metal film on which zinc or zinc-iron alloy particles are deposited, or in metal And composite metal plating that forms a film in which solid fine particles are dispersed.
- the surface roughness Rmax be 5 to 40 ⁇ m by roughening by the surface treatment.
- Rmax is less than 5 ⁇ m, the adhesion with the film formed thereon may be insufficient.
- Rmax exceeds 40 ⁇ m, the friction becomes high and the coating film cannot withstand the shearing force and compression force when subjected to high surface pressure, and may be easily broken or peeled off.
- Two or more kinds of treatments may be used in combination for the surface treatment for roughening. Different ground treatments may be applied to the pin and the box.
- a ground treatment capable of forming a porous coating is preferable.
- a phosphate treatment using manganese phosphate, zinc phosphate, iron manganese phosphate or zinc calcium phosphate, and formation of a zinc or zinc-iron alloy film by impact plating are preferable as the base treatment.
- a manganese phosphate film is preferable, and from the viewpoint of corrosion resistance, a zinc or zinc-iron alloy film that can be expected to have a sacrificial anticorrosive ability with zinc is preferable.
- the base treatment of the solid lubricating coating is manganese phosphate chemical conversion treatment, and particularly preferable as the base treatment of the solid anticorrosion coating is zinc phosphate chemical conversion treatment and zinc or zinc-iron alloy plating by impact plating. .
- Both the coating formed by phosphating and the coating of zinc or zinc-iron alloy formed by impact plating are porous coatings.
- a solid anticorrosion coating or a solid lubricating coating is formed thereon, the adhesion of the coating is enhanced by the so-called “anchor effect” of the porous coating.
- the solid lubricant film does not easily peel off, the metal-to-metal contact is effectively prevented, and seizure resistance, airtightness, and corrosion resistance are further improved.
- the phosphate treatment can be performed by dipping or spraying according to a conventional method.
- a general acidic phosphate treatment solution for galvanized material can be used.
- a zinc phosphate chemical conversion treatment comprising phosphate ions 1 to 150 g / L, zinc ions 3 to 70 g / L, nitrate ions 1 to 100 g / L, and nickel ions 0 to 30 g / L can be mentioned.
- a manganese phosphate chemical conversion treatment commonly used for threaded joints can also be used.
- the liquid temperature may be from room temperature to 100 ° C., and the processing time may be up to 15 minutes depending on the desired film thickness.
- a surface conditioning aqueous solution containing colloidal titanium can be supplied to the treated surface before the phosphate treatment. After the phosphating treatment, it is preferable to dry after washing with water or hot water.
- Impact plating can be performed by mechanical plating in which the particles and the object to be plated collide in the rotating barrel, or by projection plating in which the particles collide with the object to be plated using a blast device.
- projection plating capable of local plating.
- a projection material composed of particles having the surface of an iron-based core coated with zinc or a zinc alloy (eg, zinc-iron alloy) can be projected onto the contact surface to be coated.
- the content of zinc or zinc alloy in the particles is preferably in the range of 20 to 60% by mass, and the particle size of the particles is preferably in the range of 0.2 to 1.5 mm.
- the thickness of the zinc or zinc alloy layer formed by impact plating is preferably 5 to 40 ⁇ m from both aspects of corrosion resistance and adhesion. If the thickness is less than 5 ⁇ m, sufficient corrosion resistance may not be ensured. On the other hand, if the thickness exceeds 40 ⁇ m, the adhesion with the lubricating coating may be lowered. Similarly, the thickness of the phosphate coating is preferably in the range of 5 to 40 ⁇ m.
- a specific single layer or multi-layer electroplating is effective in enhancing seizure resistance particularly when it is used as a base of a solid lubricant film.
- Examples of such plating include single layer plating with Cu, Sn, or Ni metal, or single layer plating with a Cu—Sn alloy as described in Japanese Patent Application Laid-Open No. 2003-074763, Cu layer and Sn layer, Two-layer plating, and further three-layer plating with Ni, Cu, and Sn layers.
- Cu-Sn alloy plating, Cu plating-Sn plating two-layer plating, and Ni plating-Cu plating-Sn plating three-layer plating are preferable. More preferable are two-layer plating of Cu plating-Sn plating, three-layer plating of Ni strike plating-Cu plating-Sn plating, and alloy plating of Cu-Sn-Zn.
- Such metal or metal alloy plating can be performed according to a method as described in JP-A-2003-074763.
- the lowermost plating film (usually Ni plating) is preferably an extremely thin plating layer having a film thickness of less than 1 ⁇ m, called strike plating.
- the plating film thickness (total film thickness in the case of multilayer plating) is preferably in the range of 5 to 15 ⁇ m.
- the present invention is not limited by the examples.
- the contact surface of the pin is referred to as the pin surface
- the contact surface of the box is referred to as the box surface.
- % and part in an Example are the mass% and the mass part, respectively.
- Thread joint VAM21 (registered trademark) manufactured by Nippon Steel & Sumikin Co., Ltd. (outer diameter: 24.448 cm (9-5 / 8 inch), wall thickness: 1.199 cm (0.472 inch)), steel grade is Carbon steel (C: 0.21%, Si: 0.25%, Mn: 1.1%, P: 0.02%, S: 0.01%, Cu: 0.04%, Ni: 0.06 %, Cr: 0.17%, Mo: 0.04%, balance: iron and impurities) were subjected to a base treatment as follows.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a zinc phosphate chemical treatment solution at 75 to 85 ° C. for 10 minutes to form a 10 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m). did.
- the box surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a manganese phosphate chemical conversion solution at 80 to 95 ° C. for 10 minutes to form a 12 ⁇ m thick manganese phosphate coating (surface roughness 10 ⁇ m). Formed.
- composition for forming a solid lubricating film having the following composition is heated to 120 ° C. in a tank with a stirrer to be in a molten state having a viscosity suitable for coating, while the surface of the pin and the surface of the box treated as described above are also used.
- a solid lubricating film having an average thickness of 30 ⁇ m was formed.
- Table 1 shows the component composition (mass%) of the composition for forming a lubricating coating, the ethylene vinyl acetate resin content relative to the polyolefin resin, for each of Invention Example 1, Invention Examples 2 to 8 and Comparative Examples 1 to 6 described later. It represents the mass ratio (EVA / PO), the ratio ((EVA + PO) / W) of the both resins to the mass of WAX, and the sum (mass%) of the mass ratio of the binder to the entire composition.
- composition of the composition for forming a lubricating coating in Invention Example 1 is as follows. In addition, as above-mentioned, content (%) shows the mass% unless there is particular notice.
- (Binder) ⁇ Ethylene vinyl acetate resin: 21.6% ⁇ Polyolefin resin: 16% Wax (paraffin wax, melting point 69 ° C.): 32.4% (Fluorine-based additive) -PFPE (perfluoropolyether): 10% ⁇ Fluorinated polymer: 4% (Solid lubricant) ⁇ Earth graphite (average particle size 7 ⁇ m): 5% -Fluorinated graphite (CFx): 4% (Anti-rust additive) ⁇ Ca ion exchange silica: 5% ⁇ Aluminum phosphite: 2%
- Example 1 of the present invention repeated tightening and loosening tests (screwing speed 10 rpm, tightening torque 42.8 kN ⁇ m) of the threaded joint for pipes up to 10 times were performed at a low temperature of about ⁇ 40 ° C. Specifically, the periphery of the screw fastening portion was cooled to about ⁇ 40 ° C. with dry ice, and then a tightening / loosening test was performed. As a result, even when cooled to ⁇ 40 ° C., the solid lubricating film did not peel off or crack.
- Example 1 of the present invention showed no rust after 1000 hours.
- tube is known from the past experience.
- shear TEST shear tensile test
- two metal plates (for example, carbon steel) 28 and 30 having a length of 75 mm, a width of 25 mm, and a thickness of 0.8 mm are prepared, and a solid of 50 ⁇ m thickness is provided in a 25 mm ⁇ 25 mm region between the two metal plates.
- a lubricating coating 32 was formed.
- the PTFE sheets 34 and 36 having a thickness of 50 ⁇ m are sandwiched at predetermined positions between the metal plates 28 and 30 as a film thickness setting sheet, and a composition for a solid lubricating film heated to 120 ° C. is applied.
- the two metal plates were pressed (in the vertical direction in FIG. 4) and cooled to form the coating 32.
- Example 1 of the present invention has remarkably high adhesion strength at both temperatures of 25 ° C. and ⁇ 40 ° C. as compared with conventional Comparative Examples 1 and 2 described later.
- the adhesion strength pass line was set to 1500 kPa or more for both 25 ° C. and ⁇ 40 ° C.
- step S1 it is confirmed that there is no peeling or cracking in the solid lubricant film of the threaded joint in the initial state (step S1), and then the threaded joint is attached to the protector. In the attached state, it was exposed to a low temperature of ⁇ 60 ° C.
- step S2 the protector was removed to confirm the state of peeling or cracking
- step S3 a protector was attached to the threaded joint, and again exposed to a low temperature of ⁇ 60 ° C. for 24 hours (step S4). Thereafter, the protector was removed and the state of peeling or cracking was confirmed (step S5). Lastly, it is left outdoors for one year regularly (once a day) while taking a shower of water (step S6), and the solid lubricant film of the threaded joint is deteriorated at low temperature, that is, peeled off by a low temperature-atmosphere temperature cycle. -The state of cracking was investigated (step S7).
- Example 1 of the present invention Even when exposed to a low temperature of ⁇ 60 ° C. for a total of 48 hours, or subjected to a temperature difference between low temperature and ambient temperature, the solid lubricating film cracks, peels and swells even after one year of outdoor exposure. (Floating of the film) did not occur at all.
- Table 2 shows the results of the seizure occurrence, salt spray test, shear tensile test, and low temperature-outdoor exposure test for Inventive Example 1, Inventive Examples 2 to 8, and Comparative Examples 1 to 6, which will be described later. Represents.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- an ultraviolet curable resin film-forming composition 0.05 parts of an aluminum phosphite as a rust preventive agent in a mass ratio to an acrylic resin ultraviolet curable resin paint with respect to 1 part of the resin in the paint. And 0.01 parts of polyethylene wax as a lubricant were applied, and the film was cured by irradiating with ultraviolet rays under the following conditions to form an ultraviolet curable resin film having a thickness of 25 ⁇ m.
- the formed solid anticorrosion film was colorless and transparent, and the male screw part could be inspected with the naked
- UV lamp Air-cooled mercury lamp UV lamp output: 4kW UV wavelength: 260nm
- the box surface was subjected to mechanical grinding finish (surface roughness 3 ⁇ m), then Ni strike plating by electroplating and then Cu—Sn—Zn alloy plating to form a plating film with a total thickness of 8 ⁇ m.
- the lubricating film forming composition having the following composition is heated to 120 ° C. in a tank with a stirrer to form a molten state having a viscosity suitable for application, while the surface of the box treated as described above is also induction-heated.
- the composition for forming a solid lubricant film in a molten state was applied by a spray gun having a spray head with a heat retaining function. After cooling, a solid lubricating film having an average thickness of 50 ⁇ m was formed.
- composition of the lubricating film forming composition in Invention Example 2 is as follows.
- Example 2 repeated tightening and loosening tests of the threaded joint for pipes were conducted in the same manner as Example 1 of the invention. The results are shown in Example 2 of the present invention in Table 2. Excellent effects similar to those of Example 1 of the present invention were confirmed.
- the pin surface is coated with an acrylic resin UV curable resin paint as a composition for forming an UV curable resin film after a mechanical grinding finish (surface roughness 3 ⁇ m) in a mass ratio with respect to 1 part of the resin in the paint.
- an acrylic resin UV curable resin paint as a composition for forming an UV curable resin film after a mechanical grinding finish (surface roughness 3 ⁇ m) in a mass ratio with respect to 1 part of the resin in the paint.
- a 25 ⁇ m UV curable resin film was formed.
- the formed film was colorless and transparent, and the male screw portion could be inspected with the naked eye or a magnifier from above the film.
- UV lamp Air-cooled mercury lamp UV lamp output: 4kW UV wavelength: 260nm
- the box surface was subjected to mechanical grinding finish (surface roughness 3 ⁇ m), then Ni strike plating by electroplating and then Cu—Sn—Zn alloy plating to form a plating film with a total thickness of 8 ⁇ m. Thereafter, the composition for forming a lubricating coating having the following composition is heated to 120 ° C. in a tank with a stirrer to obtain a composition having a viscosity suitable for application and in a molten state, while the above-described composition is used.
- the surface of the box treated as a base was also preheated to 130 ° C.
- composition of the lubricating film forming composition in Invention Example 3 is as follows.
- Example 3 of the present invention repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Example 2 of the present invention in Table 2. Excellent effects similar to those of Examples 1 and 2 of the present invention were confirmed.
- Example 4 Using the same threaded joint for pipes and steel types as in Example 1 of the present invention, the base treatment of Example 2 of the present invention was formed on pins and boxes, and then a lubricating film forming composition having the following composition was 120 ° C. in a tank with a stirrer. To a composition in which the base is in a molten state and has a viscosity suitable for coating, while the surface of the box treated as described above is preheated to 130 ° C. by induction heating and then sprayed with a heat retaining function. The composition for forming a solid lubricant film in a molten state was applied by a spray gun having a head. After cooling, a solid lubricating film with an average thickness of 30 ⁇ m was formed.
- composition of the lubricating film forming composition in Invention Example 4 is as follows.
- Example 4 repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the invention. The results are shown in Inventive Example 4 in Table 2. Excellent effects similar to those of Invention Examples 1 to 3 were confirmed.
- Example 5 Using the same threaded joint for pipes and steel types as in Example 1 of the present invention, the base treatment of Example 2 of the present invention was formed on pins and boxes, and then a lubricating film forming composition having the following composition was 120 ° C. in a tank with a stirrer. To a composition in which the base is in a molten state and has a viscosity suitable for coating, while the surface of the box treated as described above is preheated to 130 ° C. by induction heating and then sprayed with a heat retaining function. The composition for forming a solid lubricant film in a molten state was applied by a spray gun having a head. After cooling, a solid lubricating film with an average thickness of 30 ⁇ m was formed.
- composition of the composition for forming a lubricating coating in Invention Example 5 is as follows.
- Example 5 of the present invention repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Inventive Example 5 in Table 2. Compared to Examples 3 and 4 of the present invention, the sum of the mass proportions of the binder was as low as 70%, and although the adhesion strength in the shear tensile test at 25 ° C was sufficient, the shear tensile test at -40 ° C The adhesion strength of was slightly low. In Example 5 of the present invention, the difference between the adhesion strength near normal temperature and the adhesion strength in a cryogenic environment was increased.
- Example 6 Using the same threaded joint for pipes and steel types as in Example 1 of the present invention, the base treatment of Example 2 of the present invention was formed on pins and boxes, and then a lubricating film forming composition having the following composition was 120 ° C. in a tank with a stirrer. To a composition in which the base is in a molten state and has a viscosity suitable for coating, while the surface of the box treated as described above is preheated to 130 ° C. by induction heating and then sprayed with a heat retaining function. The composition for forming a solid lubricant film in a molten state was applied by a spray gun having a head. After cooling, a solid lubricating film with an average thickness of 30 ⁇ m was formed.
- the composition of the lubricant film forming composition in Invention Example 6 is as follows. (Binder) ⁇ Ethylene vinyl acetate resin: 20.5% ⁇ Polyolefin resin: 19.5% Wax (polyethylene wax, melting point 78 ° C.): 36% (Fluorine-based additive) -PFPE (perfluoropolyether): 8% (Solid lubricant) ⁇ Soil-like graphite (average particle size 7 ⁇ m): 7% (Anti-rust additive) ⁇ Ca ion exchange silica: 3% ⁇ Aluminum phosphite: 4% (Friction modifier) Talc (particle diameter 4.5 ⁇ m, specific surface area 9.5 m 2 / g): 2% The particle size of talc was determined as described above using a laser diffraction particle size distribution analyzer (SALD-2000J, manufactured by Shimadzu Corporation). The specific surface area of talc was determined as described above.
- SALD-2000J laser
- Example 6 of the present invention repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Inventive Example 6 in Table 2. Excellent effects similar to those of Examples 1 to 4 of the present invention were confirmed.
- Example 6 of the present invention the difference between the yield torque and the shouldering torque was further measured as follows.
- a threaded joint sample was prepared and fastened using a suitable torque wrench.
- a torque chart as shown in FIG. 6 was produced by further applying torque after tightening to perform tightening.
- the shouldering torque is a torque value when the shoulder portion comes into contact and the torque change starts to move away from the first linear region (elastic deformation region).
- the yield torque is a torque value when plastic deformation starts. Specifically, it is a torque value that starts after reaching the shouldering torque and starts to move away from the second linear region.
- Example 7 Using the same threaded joint for pipes and steel types as in Example 1 of the present invention, the base treatment of Example 2 of the present invention was formed on pins and boxes, and then a lubricating film forming composition having the following composition was 120 ° C. in a tank with a stirrer. To a composition in which the base is in a molten state and has a viscosity suitable for coating, while the surface of the box treated as described above is preheated to 130 ° C. by induction heating and then sprayed with a heat retaining function. The composition for forming a solid lubricant film in a molten state was applied by a spray gun having a head. After cooling, a solid lubricating film with an average thickness of 30 ⁇ m was formed.
- the composition of the lubricating film forming composition in Invention Example 7 is as follows. (Binder) ⁇ Ethylene vinyl acetate resin: 20.5% ⁇ Polyolefin resin: 19.5% Wax (polyethylene wax, melting point 78 ° C.): 33% (Fluorine-based additive) -PFPE (perfluoropolyether): 8% (Solid lubricant) ⁇ Soil-like graphite (average particle size 7 ⁇ m): 7% (Anti-rust additive) ⁇ Ca ion exchange silica: 3% ⁇ Aluminum phosphite: 4% (Friction modifier) Talc (particle size 3.3 ⁇ m, specific surface area 12.0 m 2 / g): 5% The particle diameter and specific surface area of talc were determined by the same method as in Invention Example 6.
- Example 7 of the present invention repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Inventive Example 7 in Table 2. Excellent effects similar to those of Invention Examples 1 to 4 and Invention Example 6 were confirmed.
- Example 7 of the present invention the difference between the yield torque and the shouldering torque was measured in the same manner as Example 6 of the present invention. The results are shown in Inventive Example 7 in Table 2. When the difference between the yield torque and the shouldering torque in Example 3 of the present invention was set to 100, the difference between the yield torque and the shouldering torque in Example 7 of the present invention was 145, indicating excellent overtorque performance.
- Example 8 Using the same threaded joint for pipes and steel types as in Example 1 of the present invention, the base treatment of Example 2 of the present invention was formed on pins and boxes, and then a lubricating film forming composition having the following composition was 120 ° C. in a tank with a stirrer. To a composition in which the base is in a molten state and has a viscosity suitable for coating, while the surface of the box treated as described above is preheated to 130 ° C. by induction heating and then sprayed with a heat retaining function. The composition for forming a solid lubricant film in a molten state was applied by a spray gun having a head. After cooling, a solid lubricating film with an average thickness of 30 ⁇ m was formed.
- composition of the lubricant film forming composition in Invention Example 8 is as follows. (Binder) ⁇ Ethylene vinyl acetate resin: 20.5% ⁇ Polyolefin resin: 19.5% Wax (polyethylene wax, melting point 78 ° C.): 32% (Fluorine-based additive) -PFPE (perfluoropolyether): 8% (Solid lubricant) ⁇ Soil-like graphite (average particle size 7 ⁇ m): 7% (Anti-rust additive) ⁇ Ca ion exchange silica: 3% ⁇ Aluminum phosphite: 4% (Friction modifier) Talc (particle diameter 8.0 ⁇ m, specific surface area 7.0 m 2 / g): 6% The particle diameter and specific surface area of talc were measured in the same manner as in Example 6 of the present invention.
- Example 8 of the present invention repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Inventive Example 8 in Table 2. Excellent effects similar to those of Invention Examples 1 to 4 and Invention Examples 6 to 7 were confirmed.
- Example 8 of the present invention the difference between the yield torque and the shouldering torque was measured in the same manner as Example 6 of the present invention. The results are shown in Inventive Example 8 in Table 2. When the difference between the yield torque and the shouldering torque in Invention Example 3 was set to 100, the difference between the yield torque and the shouldering torque in Invention Example 8 was 180, indicating excellent overtorque performance.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a zinc phosphate chemical treatment solution at 75 to 85 ° C. for 10 minutes to form a 10 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m). did.
- the box surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a manganese phosphate chemical conversion solution at 80 to 95 ° C. for 10 minutes to form a 12 ⁇ m thick manganese phosphate coating (surface roughness 10 ⁇ m). Formed.
- composition for forming a solid lubricating film having the following composition is heated to 130 ° C. in a tank with a stirrer to form a molten state having a viscosity suitable for application, while the surface of the pin and the surface of the box treated as described above are also included.
- a solid lubricating film having an average thickness of 50 ⁇ m was formed.
- composition of the lubricating film forming composition in Comparative Example 1 As the composition of the lubricating film forming composition in Comparative Example 1, a composition corresponding to “Example” described on page 18 of Patent Document 3 was used.
- Comparative Example 1 repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Comparative Example 1 in Table 2. Although seizure did not occur until the third time, slight seizure occurred on the threaded portion at the fourth time, and the test was carried out until the fifth time. However, the seizure occurred to the extent that it could not be maintained at the sixth time, so the test was terminated.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a zinc phosphate chemical treatment solution at 75 to 85 ° C. for 10 minutes to form a 10 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m). did.
- the box surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a manganese phosphate chemical conversion solution at 80 to 95 ° C. for 10 minutes to form a 12 ⁇ m thick manganese phosphate coating (surface roughness 10 ⁇ m). Formed.
- composition for forming a solid lubricating film having the following composition is heated to 130 ° C. in a tank with a stirrer to form a molten state having a viscosity suitable for application, while the surface of the pin and the surface of the box treated as described above are also included.
- a solid lubricating film having an average thickness of 50 ⁇ m was formed.
- composition of the lubricating film forming composition in Comparative Example 2 As the composition of the lubricating film forming composition in Comparative Example 2, the composition corresponding to “Invention Example 1” described on pages 20 to 21 of Patent Document 4 was used.
- Comparative Example 2 repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as in Example 1 of the present invention. The results are shown in Comparative Example 2 in Table 2. Although seizure did not occur until the 4th time, slight seizure occurred on the screw part at the 5th time, and the test was carried out until the 6th time. However, the test was terminated because seizure occurred that could not be maintained in the seventh time.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- an ultraviolet curable resin film-forming composition 0.05 parts of an aluminum phosphite as a rust preventive agent in a mass ratio to an acrylic resin ultraviolet curable resin paint with respect to 1 part of the resin in the paint. And 0.01 parts of polyethylene wax as a lubricant were applied, and the film was cured by irradiating with ultraviolet rays under the following conditions to form an ultraviolet curable resin film having a thickness of 25 ⁇ m.
- the formed solid anticorrosion film was colorless and transparent, and the male screw part could be inspected with the naked
- UV lamp Air-cooled mercury lamp UV lamp output: 4kW UV wavelength: 260nm
- the box surface was subjected to mechanical grinding finish (surface roughness 3 ⁇ m), then Ni strike plating by electroplating and then Cu—Sn—Zn alloy plating to form a plating film with a total thickness of 8 ⁇ m.
- the lubricating film forming composition having the following composition is heated to 120 ° C. in a tank with a stirrer to form a molten state having a viscosity suitable for application, while the surface of the box treated as described above is also induction-heated.
- the composition for forming a solid lubricant film in a molten state was applied by a spray gun having a spray head with a heat retaining function. After cooling, a solid lubricating film having an average thickness of 35 ⁇ m was formed.
- the composition of the composition for forming a lubricating coating in Comparative Example 3 is as follows. (Binder) ⁇ Ethylene vinyl acetate resin: 13.5% ⁇ Polyolefin resin: 15% Wax (paraffin wax, melting point 69 ° C.): 26.5% (Fluorine-based additive) -PFPE (perfluoropolyether): 10% ⁇ Fluorinated polymer: 4% (Solid lubricant) ⁇ Earth graphite (average particle size 7 ⁇ m): 5% -Fluorinated graphite (CFx): 4% (Anti-rust additive) ⁇ Calcium sulfonate derivative: 15% ⁇ Ca ion exchange silica: 5% ⁇ Aluminum phosphite: 2%
- Comparative Example 3 repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Comparative Example 3 in Table 2. Although seizure did not occur until the 4th time, slight seizure occurred on the screw part at the 5th time, and the test was carried out until the 6th time. However, the test was terminated because seizure occurred that could not be maintained in the seventh time.
- the adhesion strength in the shear tensile test is significantly lower than that of the examples of the present invention, and in particular, the adhesion strength at ⁇ 40 ° C. is extremely low, less than 1000 kPa. Further, in the low temperature-outdoor exposure test, it was observed that peeling (coating floating) occurred in 5 to 10% of the solid lubricating coating after one year of outdoor exposure.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- an ultraviolet curable resin film-forming composition 0.05 parts of an aluminum phosphite as a rust preventive agent in a mass ratio to an acrylic resin ultraviolet curable resin paint with respect to 1 part of the resin in the paint. And 0.01 parts of polyethylene wax as a lubricant were applied, and the film was cured by irradiating with ultraviolet rays under the following conditions to form an ultraviolet curable resin film having a thickness of 25 ⁇ m.
- the formed solid anticorrosion film was colorless and transparent, and the male screw part could be inspected with the naked
- UV lamp Air-cooled mercury lamp UV lamp output: 4kW UV wavelength: 260nm
- the box surface was subjected to mechanical grinding finish (surface roughness 3 ⁇ m), then Ni strike plating by electroplating and then Cu—Sn—Zn alloy plating to form a plating film with a total thickness of 8 ⁇ m.
- the lubricating film forming composition having the following composition is heated to 120 ° C. in a tank with a stirrer to form a molten state having a viscosity suitable for application, while the surface of the box treated as described above is also induction-heated.
- the composition for forming a solid lubricant film in a molten state was applied by a spray gun having a spray head with a heat retaining function. After cooling, a solid lubricating film having an average thickness of 35 ⁇ m was formed.
- the composition of the lubricating film forming composition in Comparative Example 4 is as follows. (Binder) ⁇ Ethylene vinyl acetate resin: 25.5% ⁇ Polyolefin resin: 14% Wax (paraffin wax, melting point 69 ° C.): 31.5% (Fluorine-based additive) -PFPE (perfluoropolyether): 10% ⁇ Fluorinated polymer: 4% (Solid lubricant) ⁇ Earth graphite (average particle size 7 ⁇ m): 5% -Fluorinated graphite (CFx): 4% (Anti-rust additive) ⁇ Ca ion exchange silica: 5% ⁇ Aluminum phosphite: 2%
- Comparative Example 4 repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as in Example 1 of the present invention. The results are shown in Comparative Example 4 in Table 2. Although seizure did not occur until the first time, slight seizure occurred on the threaded portion at the second time. However, the test was terminated because of the occurrence of seizure that could not be maintained in the fourth time.
- Comparative Example 4 the adhesion strength in the shear tensile test is significantly lower than that of the present invention example, and in particular, the adhesion at ⁇ 40 ° C. is low.
- Comparative Example 4 has higher adhesion strength than Comparative Examples 1 to 3, in a low-temperature outdoor exposure test, less than 1% of the solid lubricating film peeled off (floating of the film) occurred after 1 year of outdoor exposure. Stayed in.
- EVA / PO exceeds 1.8
- the seizure resistance during the fastening test decreases. The reason for this is presumed that when EVA / PO exceeds 1.8, the coating becomes hard, the sliding resistance of the coating increases, and the lubricity is impaired.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- an ultraviolet curable resin film-forming composition 0.05 parts of an aluminum phosphite as a rust preventive agent in a mass ratio to an acrylic resin ultraviolet curable resin paint with respect to 1 part of the resin in the paint. And 0.01 parts of polyethylene wax as a lubricant were applied, and the film was cured by irradiating with ultraviolet rays under the following conditions to form an ultraviolet curable resin film having a thickness of 25 ⁇ m.
- the formed solid anticorrosion film was colorless and transparent, and the male screw part could be inspected with the naked
- UV lamp Air-cooled mercury lamp UV lamp output: 4kW UV wavelength: 260nm
- the box surface was subjected to mechanical grinding finish (surface roughness 3 ⁇ m), then Ni strike plating by electroplating and then Cu—Sn—Zn alloy plating to form a plating film with a total thickness of 8 ⁇ m.
- the lubricating film forming composition having the following composition is heated to 120 ° C. in a tank with a stirrer to form a molten state having a viscosity suitable for application, while the surface of the box treated as described above is also induction-heated.
- the composition for forming a solid lubricant film in a molten state was applied by a spray gun having a spray head with a heat retaining function. After cooling, a solid lubricating film having an average thickness of 35 ⁇ m was formed.
- the composition of the lubricating film forming composition in Comparative Example 5 is as follows. (Binder) ⁇ Ethylene vinyl acetate resin: 13.5% ⁇ Polyolefin resin: 10% Wax (paraffin wax, melting point 69 ° C.): 46.5% (Fluorine-based additive) -PFPE (perfluoropolyether): 10% ⁇ Fluorinated polymer: 4% (Solid lubricant) ⁇ Earth graphite (average particle size 7 ⁇ m): 5% -Fluorinated graphite (CFx): 4% (Anti-rust additive) ⁇ Ca ion exchange silica: 5% ⁇ Aluminum phosphite: 2%
- Comparative Example 5 repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as Example 1 of the present invention. The results are shown in Comparative Example 5 in Table 2. Although seizure did not occur until the first time, slight seizure occurred on the screw portion at the second time, and the test was continued after maintenance. However, the test was terminated because there was seizure that could not be maintained at the third time.
- Comparative Example 5 also has a significantly lower adhesion strength in the shear tensile test than that of the present invention, and in particular, adhesion at -40 ° C. is low.
- adhesion at -40 ° C. is low.
- the low temperature-outdoor exposure test slight peeling of the film occurred when the protector was removed at the ambient temperature for 24 hours after exposure to a low temperature of -60 ° C.
- the peeled area increased, and after 1 year of outdoor exposure, it was observed that more than 10% of the solid lubricating film was peeled off (floating of the film). It was.
- the pin surface is mechanically ground (surface roughness 3 ⁇ m) and then immersed in a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- a chemical conversion treatment solution for zinc phosphate at 75 to 85 ° C. for 10 minutes to form a 8 ⁇ m thick zinc phosphate coating (surface roughness 8 ⁇ m).
- an ultraviolet curable resin film-forming composition 0.05 parts of an aluminum phosphite as a rust preventive agent in a mass ratio to an acrylic resin ultraviolet curable resin paint with respect to 1 part of the resin in the paint. And 0.01 parts of polyethylene wax as a lubricant were applied, and the film was cured by irradiating with ultraviolet rays under the following conditions to form an ultraviolet curable resin film having a thickness of 25 ⁇ m.
- the formed solid anticorrosion film was colorless and transparent, and the male screw part could be inspected with the naked
- UV lamp Air-cooled mercury lamp UV lamp output: 4kW UV wavelength: 260nm
- the box surface was subjected to mechanical grinding finish (surface roughness 3 ⁇ m), then Ni strike plating by electroplating and then Cu—Sn—Zn alloy plating to form a plating film with a total thickness of 8 ⁇ m.
- the lubricating film forming composition having the following composition is heated to 120 ° C. in a tank with a stirrer to form a molten state having a viscosity suitable for application, while the surface of the box treated as described above is also induction-heated.
- the composition for forming a solid lubricant film in a molten state was applied by a spray gun having a spray head with a heat retaining function. After cooling, a solid lubricating film having an average thickness of 35 ⁇ m was formed.
- the composition of the composition for forming a lubricating coating in Comparative Example 6 is as follows. (Binder) ⁇ Ethylene vinyl acetate resin: 27% ⁇ Polyolefin resin: 20% ⁇ Wax (paraffin wax, melting point 69 ° C.): 23% (Fluorine-based additive) -PFPE (perfluoropolyether): 10% ⁇ Fluorinated polymer: 4% (Solid lubricant) ⁇ Earth graphite (average particle size 7 ⁇ m): 5% -Fluorinated graphite (CFx): 4% (Anti-rust additive) ⁇ Ca ion exchange silica: 5% ⁇ Aluminum phosphite: 2%
- Comparative Example 6 repeated tightening and loosening tests of the threaded joint for pipes were performed in the same manner as in Example 1 of the present invention. The results are shown in Comparative Example 6 in Table 2. Although seizure did not occur until the second time, slight seizure occurred on the screw portion at the third time, and the test was continued until the fourth time. However, the test was terminated because there was seizure that could not be maintained at the fifth time.
- FIG. 7 is a diagram showing an outline of a flat plate sliding test for measuring a friction coefficient.
- the steel plate 51 was the same 13Cr steel as Example 3 of the present invention, and was a steel plate having a width of 10 mm and a length of 25 mm.
- the steel plate 52 was the same 13Cr steel as Example 3 of the present invention.
- An ultraviolet curable resin film was formed on the surface of the steel plate 52 in the same manner as the pin surface of Example 3 of the present invention.
- Example 6 On the surface of the steel plate 51, similarly to the box surface of Example 3 of the present invention, a Cu—Sn—Zn alloy plating was performed, and then a solid lubricating film 53 was formed.
- the composition of the solid lubricating film 53 was the same as in Example 6 except for the content other than talc, and only the content of talc was varied between 1 and 20%.
- the steel plate 52 was attached to the apparatus so as to be sandwiched between the two steel plates 51 in the vertical direction, and one end of the steel plate 52 was gripped using an appropriate chuck 54. The steel plate 52 was slid in the horizontal direction with pressure P applied in the vertical direction to the flat plate surface of the steel plate.
- the pressure P in the vertical direction against the steel plates 51 and 52 was 17.5 kgf / mm 2 .
- the sliding distance of the steel plate 52 was 50 mm, and the sliding speed was 10 mm / s. After about 10 seconds from the start of sliding, the friction coefficient became constant. The coefficient of friction was measured when about 30 seconds passed after the start of sliding. The results are shown in Table 3.
- FIG. 8 shows the relationship between the content of talc in the solid lubricant film and the friction coefficient.
- the friction coefficient was stable in the vicinity of 0.30 to 0.35.
- the content of talc in the solid lubricating coating is 2 to 15% by mass, it is considered that the friction coefficient can be appropriately maintained even when the surface pressure in the radial direction of the threaded joint is high.
- the content of talc exceeds 15% by mass, the friction coefficient greatly increased. If the friction coefficient is too high, seizure occurs, which is not preferable. Therefore, the content of talc is suitably 15% by mass or less.
- the present invention can also be applied to a threaded joint for pipes used for pipes other than oil well pipe applications described in the same manner as in the examples.
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Abstract
Description
管用ねじ継手に形成された固体潤滑被膜、及び該固体潤滑被膜を形成するための組成物(固体潤滑被膜形成用組成物)において、
(1)該組成物の結合剤(バインダー)として、エチレン酢酸ビニル(EVA)樹脂、ポリオレフィン樹脂及び融点が110℃以下のワックス(WAX)を特定の割合で配合すること、
(2)フッ素系添加剤を特定割合で配合すること、
(3)さらに固体潤滑粉末及び防錆添加剤を添加すること、
により、極低温に曝されても固体潤滑被膜が高い密着性を維持できる。そのため、ねじ継手は十分な耐焼付き性と気密性とを備え、かつ低温下でのねじ継手の締結・緩め時に必要なトルクの増加を抑制できる。さらに、
(4)特定粒子径のタルクを特定割合で配合すること、
により、締結の際のトルク調整を容易にすることができる。
上述のとおり、本実施形態では、管用ねじ継手を構成するピンとボックスの少なくとも一方の接触表面に、固体潤滑被膜を形成する。この固体潤滑被膜には、極低温(-60℃~-20℃)に曝されても密着性を維持することが求められる。固体潤滑被膜にはさらに、ねじ継手による鋼管同士の締結の際において、低・温暖・熱帯地域(-20℃~+50℃)だけでなく、極低温地域(-60℃~-20℃)においても、締結トルクが高くなってハイショルダリングを起こしたり、ねじ緩めトルクが高くなったりするということがなく、それにより焼付きの発生を抑制できることが求められる。固体潤滑被膜にはさらに、保管時の発錆を防止することが求められる。常温付近と、極低温環境とで、固体潤滑被膜の密着強度(硬さ)が大きく変化する場合、極低温環境において固体潤滑被膜に割れが発生したり、常温付近に戻った際に固体潤滑被膜に剥離が発生する。そのため、固体潤滑被膜にはさらに、常温付近と極低温環境とで、固体潤滑被膜の密着強度(硬さ)が大きく変化しないことが求められる。
本実施形態の結合剤は、エチレン酢酸ビニル樹脂(EVA)と、ポリオレフィン樹脂(PO)と、融点が110℃以下のワックス(W)とからなる。常温から極低温に亘って高い被膜密着性を実現するために、エチレン酢酸ビニル樹脂と、ポリオレフィン樹脂と、ワックスとの質量比は、次のとおりである。
1.0≦(EVA/PO)≦1.8、かつ
0.7≦((EVA+PO)/W)≦1.6
上記質量比は、本発明において実験的に初めて明らかにされた事項である。なお、上記式中のEVA、PO及びWは、それぞれ、エチレン酢酸ビニル樹脂、ポリオレフィン樹脂及びワックスの質量を示す。
本実施形態の固体潤滑被膜は、結合剤を基剤とし、さらにフッ素系添加剤を含有する。フッ素系添加剤は、摺動時の滑り性を改善する。フッ素系添加剤はさらに、極低温における固体潤滑被膜の靭性を高める。フッ素系添加剤は例えば、液体系のパーフルオロポリエーテル(PFPE)やグリス状のフッ素化ポリマー等である。PFPE及びフッ素化ポリマーは、前記結合剤への添加のし易さから、フッ素系添加剤を使用することが好ましい。基本骨格が分子量500~10000のフッ素化ポリエーテルなどのパーフルオロポリエーテル変性体なども、フッ素系添加剤として使用できる。
固体潤滑被膜は、その潤滑性をさらに高めるために、各種固体潤滑剤を含有する。固体潤滑剤とは、ここでは潤滑性を有する粉末を意味する。固体潤滑剤は、以下の4種類に大別される。
(1)滑り易い特定の結晶構造、例えば、六方晶層状結晶構造を有することにより潤滑性を示すもの(例えば、黒鉛、酸化亜鉛、窒化硼素)、
(2)結晶構造に加えて反応性元素を有することにより潤滑性を示すもの(例えば、二硫化モリブデン、二硫化タングステン、ふっ素化黒鉛、硫化スズ、硫化ビスマス)、
(3)化学反応性により潤滑性を示すもの(例えば、或る種のチオ硫酸塩型化合物)、及び
(4)摩擦応力下での塑性または粘塑性挙動により潤滑性を示すもの(例えば、ポリテトラフルオロエチレン(PTFE)及びポリアミド)。
上記固体潤滑被膜用の組成物はさらに、摩擦調整剤としてタルクを含有してもよい。タルク(Talc)とは、滑石という鉱石を粉砕して作られる、白色又は灰色の無機粉末である。タルクの化学名は含水珪酸マグネシウムであり、Mg3Si4O10(OH)2の化学組成を持つ。タルクは、SiO2を約60質量%、MgOを約30質量%、及び結晶水を約4.8質量%含有する。タルクの真比重は2.7~2.8、モース硬度は1であり、無機鉱物中最も低い。さらに、タルクは耐熱性に優れ、化学的に安定した物質である。そのため、タルクは、充填材として使用できる。タルク表面に、処理材を化学的もしくは物理的に結合させることで分散性を改善した、表面改質タルクも本実施形態のタルクに含まれる。
本実施形態の組成物は、上記成分以外に、界面活性剤、着色剤、酸化防止剤などから選ばれた少量添加成分を、例えば合計で5質量%以下の量で含有してもよい。固体潤滑被膜用の組成物はさらに、極圧剤、液状油剤なども2質量%以下のごく少量であれば、含有することができる。
上記の熱可塑性固体潤滑被膜を管用ねじ継手のピンとボックスの一方(例えば、ボックス)の接触表面だけに形成した場合、他方(例えば、ピン)の接触表面は、例えば、後述する下地処理のみであってもよいが、好ましくは防錆性を付与するために、固体防食被膜を最上表面処理被膜層として形成する。
管用ねじ継手の接触表面であるねじ部やシール部は、ねじ切りを含む切削加工により形成され、一般にその表面粗さは3~5μm程度である。接触表面の表面粗さをこれより大きくすると、その上に形成される被膜の密着性を高めることができ、結果として耐焼付き性や耐食性といった性能を改善することができる。そのために、ピン及びボックスの少なくとも一方の部材、好ましくは両方の部材の接触表面に、被膜形成に先立って、表面粗さを大きくすることができる下地処理を施すことが好ましい。
新日鐵住金(株)社製の管用ねじ継手VAM21(登録商標)(外径:24.448cm(9-5/8インチ)、肉厚:1.199cm(0.472インチ))、鋼種は炭素鋼(C:0.21%、Si:0.25%、Mn:1.1%、P:0.02%、S:0.01%、Cu:0.04%、Ni:0.06%、Cr:0.17%、Mo:0.04%、残部:鉄及び不純物)のピン表面及びボックス表面に、以下のようにして下地処理を施した。
(結合剤)
・エチレン酢酸ビニル樹脂:21.6%
・ポリオレフィン樹脂:16%
・ワックス(パラフィンワックス、融点69℃):32.4%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:4%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):5%
・フッ化黒鉛(CFx):4%
(防錆添加剤)
・Caイオン交換シリカ:5%
・亜燐酸アルミニウム:2%
本発明例1で使用したものと同じ炭素鋼製の管用ねじ継手のピン表面及びボックス表面に、以下のようにして表面処理を施した。
UVランプ出力:4kW
紫外線波長:260nm
(結合剤)
・エチレン酢酸ビニル樹脂:17%
・ポリオレフィン樹脂:12.2%
・ワックス(パラフィンワックス、融点69℃):36.8%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:7%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):10%
(防錆添加剤)
・Caイオン交換シリカ:5%
・亜燐酸アルミニウム:2%
本発明例1と同じねじ種において、炭素鋼より焼付きが起こり易い13Cr鋼(C:0.19%、Si:0.25%、Mn:0.9%、P:0.02%、S:0.01%、Cu:0.04%、Ni:0.11%、Cr:13%、Mo:0.04%、残部:鉄及び不純物)製の管用ねじ継手(外径:24.448cm(9-5/8インチ)、肉厚:1.105cm(0.435インチ))ピン表面及びボックス表面に、以下のようにして表面処理を施した。
UVランプ出力:4kW
紫外線波長:260nm
(結合剤)
・エチレン酢酸ビニル樹脂:22%
・ポリオレフィン樹脂:21%
・ワックス(パラフィンワックス、融点69℃):31%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:4%
(固体潤滑剤)
・PTFE:10%
(防錆添加剤)
・亜燐酸アルミニウム:2%
本発明例1と同じ管用ねじ継手、鋼種を用いて、本発明例2の下地処理をピン及びボックスに形成した後、下記組成を有する潤滑被膜形成用組成物を撹拌機付きタンク内で120℃に加熱して、塗布に適した粘度を有する、基剤が溶融状態の組成物にし、一方、上記のように下地処理したボックス表面も誘導加熱により130℃に予熱した後、保温機能付きの噴霧ヘッドを有するスプレイガンにより溶融状態の固体潤滑被膜形成用組成物を塗布した。冷却後に、平均厚さ30μmの固体潤滑被膜が形成された。
(結合剤)
・エチレン酢酸ビニル樹脂:26%
・ポリオレフィン樹脂:16%
・ワックス(パラフィンワックス、融点69℃):37%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):9%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):5%
・フッ化黒鉛(CFx):4%
(防錆添加剤)
・亜燐酸アルミニウム:3%
本発明例1と同じ管用ねじ継手、鋼種を用いて、本発明例2の下地処理をピン及びボックスに形成した後、下記組成を有する潤滑被膜形成用組成物を撹拌機付きタンク内で120℃に加熱して、塗布に適した粘度を有する、基剤が溶融状態の組成物にし、一方、上記のように下地処理したボックス表面も誘導加熱により130℃に予熱した後、保温機能付きの噴霧ヘッドを有するスプレイガンにより溶融状態の固体潤滑被膜形成用組成物を塗布した。冷却後に、平均厚さ30μmの固体潤滑被膜が形成された。
(結合剤)
・エチレン酢酸ビニル樹脂:21.6%
・ポリオレフィン樹脂:16%
・ワックス(ポリエチレンワックス、融点110℃):32.4%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:4%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):5%
・フッ化黒鉛(CFx):4%
(防錆添加剤)
・Caイオン交換シリカ:5%
・亜燐酸アルミニウム:2%
本発明例1と同じ管用ねじ継手、鋼種を用いて、本発明例2の下地処理をピン及びボックスに形成した後、下記組成を有する潤滑被膜形成用組成物を撹拌機付きタンク内で120℃に加熱して、塗布に適した粘度を有する、基剤が溶融状態の組成物にし、一方、上記のように下地処理したボックス表面も誘導加熱により130℃に予熱した後、保温機能付きの噴霧ヘッドを有するスプレイガンにより溶融状態の固体潤滑被膜形成用組成物を塗布した。冷却後に、平均厚さ30μmの固体潤滑被膜が形成された。
(結合剤)
・エチレン酢酸ビニル樹脂:20.5%
・ポリオレフィン樹脂:19.5%
・ワックス(ポリエチレンワックス、融点78℃):36%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):8%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):7%
(防錆添加剤)
・Caイオン交換シリカ:3%
・亜燐酸アルミニウム:4%
(摩擦調整剤)
・タルク(粒子径4.5μm、比表面積9.5m2/g):2%
タルクの粒子径はレーザー回折式粒子径分布測定装置(島津製作所製、SALD-2000J)を用いて上述のとおりに求めた。タルクの比表面積は上述のとおりに求めた。
本発明例1と同じ管用ねじ継手、鋼種を用いて、本発明例2の下地処理をピン及びボックスに形成した後、下記組成を有する潤滑被膜形成用組成物を撹拌機付きタンク内で120℃に加熱して、塗布に適した粘度を有する、基剤が溶融状態の組成物にし、一方、上記のように下地処理したボックス表面も誘導加熱により130℃に予熱した後、保温機能付きの噴霧ヘッドを有するスプレイガンにより溶融状態の固体潤滑被膜形成用組成物を塗布した。冷却後に、平均厚さ30μmの固体潤滑被膜が形成された。
(結合剤)
・エチレン酢酸ビニル樹脂:20.5%
・ポリオレフィン樹脂:19.5%
・ワックス(ポリエチレンワックス、融点78℃):33%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):8%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):7%
(防錆添加剤)
・Caイオン交換シリカ:3%
・亜燐酸アルミニウム:4%
(摩擦調整剤)
・タルク(粒子径3.3μm、比表面積12.0m2/g):5%
タルクの粒子径及び比表面積は本発明例6と同様の方法で求めた。
本発明例1と同じ管用ねじ継手、鋼種を用いて、本発明例2の下地処理をピン及びボックスに形成した後、下記組成を有する潤滑被膜形成用組成物を撹拌機付きタンク内で120℃に加熱して、塗布に適した粘度を有する、基剤が溶融状態の組成物にし、一方、上記のように下地処理したボックス表面も誘導加熱により130℃に予熱した後、保温機能付きの噴霧ヘッドを有するスプレイガンにより溶融状態の固体潤滑被膜形成用組成物を塗布した。冷却後に、平均厚さ30μmの固体潤滑被膜が形成された。
(結合剤)
・エチレン酢酸ビニル樹脂:20.5%
・ポリオレフィン樹脂:19.5%
・ワックス(ポリエチレンワックス、融点78℃):32%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):8%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):7%
(防錆添加剤)
・Caイオン交換シリカ:3%
・亜燐酸アルミニウム:4%
(摩擦調整剤)
・タルク(粒子径8.0μm、比表面積7.0m2/g):6%
タルクの粒子径及び比表面積は本発明例6と同様に測定した。
本発明例1で使用したものと同じ炭素鋼製の管用ねじ継手のピン表面及びボックス表面に、以下のようにして表面処理を施した。
本発明例1で使用したものと同じ炭素鋼製の管用ねじ継手のピン表面及びボックス表面に、比較例1と同様に以下のようにして表面処理を施した。
本発明例1で使用したものと同じ炭素鋼製の管用ねじ継手のピン表面及びボックス表面に、本発明例2と同様にして以下のような表面処理を施した。
UVランプ出力:4kW
紫外線波長:260nm
(結合剤)
・エチレン酢酸ビニル樹脂:13.5%
・ポリオレフィン樹脂:15%
・ワックス(パラフィンワックス、融点69℃):26.5%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:4%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):5%
・フッ化黒鉛(CFx):4%
(防錆添加剤)
・スルホン酸カルシウム誘導体:15%
・Caイオン交換シリカ:5%
・亜燐酸アルミニウム:2%
本発明例1で使用したものと同じ炭素鋼製の管用ねじ継手のピン表面及びボックス表面に、本発明例2と同様にして以下のような表面処理を施した。
UVランプ出力:4kW
紫外線波長:260nm
(結合剤)
・エチレン酢酸ビニル樹脂:25.5%
・ポリオレフィン樹脂:14%
・ワックス(パラフィンワックス、融点69℃):31.5%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:4%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):5%
・フッ化黒鉛(CFx):4%
(防錆添加剤)
・Caイオン交換シリカ:5%
・亜燐酸アルミニウム:2%
本発明例1で使用したのと同じ炭素鋼製の管用ねじ継手のピン表面及びボックス表面に、本発明例2と同様にして以下のような表面処理を施した。
UVランプ出力:4kW
紫外線波長:260nm
(結合剤)
・エチレン酢酸ビニル樹脂:13.5%
・ポリオレフィン樹脂:10%
・ワックス(パラフィンワックス、融点69℃):46.5%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:4%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):5%
・フッ化黒鉛(CFx):4%
(防錆添加剤)
・Caイオン交換シリカ:5%
・亜燐酸アルミニウム:2%
本発明例1で使用したものと同じ炭素鋼製の管用ねじ継手のピン表面及びボックス表面に、本発明例2と同様にして以下のような表面処理を施した。
UVランプ出力:4kW
紫外線波長:260nm
(結合剤)
・エチレン酢酸ビニル樹脂:27%
・ポリオレフィン樹脂:20%
・ワックス(パラフィンワックス、融点69℃):23%
(フッ素系添加剤)
・PFPE(パーフルオロポリエーテル):10%
・フッ素化ポリマー:4%
(固体潤滑剤)
・土状黒鉛(平均粒径7μm):5%
・フッ化黒鉛(CFx):4%
(防錆添加剤)
・Caイオン交換シリカ:5%
・亜燐酸アルミニウム:2%
固体潤滑被膜中のタルクの含有量とねじ継手締結時の摩擦係数との関係性を調べるため、平板摺動試験を行った。具体的には、図7に示す装置を用いた。図7は、摩擦係数を測定するための平板摺動試験の概要を示す図である。図7を参照して、鋼板51は、本発明例3と同じ13Cr鋼であり、幅10mm×長さ25mmの鋼板であった。鋼板52は、本発明例3と同じ13Cr鋼であった。鋼板52の表面には、本発明例3のピン表面と同様に、紫外線硬化樹脂被膜を形成した。鋼板51の表面には、本発明例3のボックス表面と同様に、Cu-Sn-Zn合金めっきを施した後に固体潤滑被膜53を形成した。固体潤滑被膜53の組成は、タルク以外の含有量を本発明例6と同様にし、タルクの含有量のみを1~20%の間で変化させた。鋼板52を2枚の鋼板51で垂直方向に挟むように装置に取り付け、鋼板52の一端を適当なチャック54を用いて把持した。鋼板の平板面に対し、垂直方向に圧力Pをかけた状態で、鋼板52を水平方向に摺動させた。鋼板51及び52に対する、垂直方向の圧力Pは17.5kgf/mm2であった。鋼板52の摺動距離は50mm、摺動速度は10mm/sであった。摺動開始後約10秒経過すると摩擦係数が一定となった。摺動開始後約30秒経過した時点で摩擦係数を測定した。結果を表3に示す。
4 雄ねじ部
6 ピン
8 カップリング
10 雌ねじ部
12 ボックス
14、16 シール部
18、20 ショルダー部
22 鋼
24 固体潤滑被膜
26 下地処理膜
Claims (14)
- 管用ねじ継手に固体潤滑被膜を形成するための組成物であって、
結合剤と、
フッ素系添加剤と、
固体潤滑剤と、
防錆添加剤とを含有し、
前記結合剤は、
エチレン酢酸ビニル樹脂と、
ポリオレフィン樹脂と、
融点が110℃以下のワックスとを含有し、
前記ポリオレフィン樹脂の質量に対する前記エチレン酢酸ビニル樹脂の質量の比が1.0~1.8であり、
前記ワックスの質量に対する、前記ポリオレフィン樹脂及び前記エチレン酢酸ビニル樹脂を合わせた質量の比が0.7~1.6であることを特徴とする、組成物。 - 請求項1に記載の組成物であって、
60~80質量%の前記結合剤と、
8~18質量%の前記フッ素系添加剤と、
5~15質量%の前記固体潤滑剤と、
2~10質量%の前記防錆添加剤とを含有することを特徴とする、請求項1に記載の組成物。 - 請求項1又は請求項2に記載の組成物であってさらに、
2~15質量%のタルクを含有することを特徴とする、組成物。 - 請求項3に記載の組成物であって、
前記タルクの粒子径が1~12μmであり、前記タルクの比表面積が4~12m2/gであることを特徴とする、組成物。 - ピンとボックスとを備える管用ねじ継手であって、
前記ピン及び前記ボックスの各々は、互いに接触する部分を含む接触表面を備え、前記管用ねじ継手は、前記ピン及び前記ボックスの少なくとも一方の前記接触表面上に固体潤滑被膜を備え、
前記固体潤滑被膜は、
結合剤と、
フッ素系添加剤と、
固体潤滑剤と、
防錆添加剤とを含有し、
前記結合剤は、
エチレン酢酸ビニル樹脂と、
ポリオレフィン樹脂と、
融点が110℃以下のワックスとを含有し、
前記ポリオレフィン樹脂の質量に対する前記エチレン酢酸ビニル樹脂の質量の比が1.0~1.8であり、
前記ワックスの質量に対する、前記ポリオレフィン樹脂及び前記エチレン酢酸ビニル樹脂を合わせた質量の比が0.7~1.6であることを特徴とする、管用ねじ継手。 - 請求項5に記載の管用ねじ継手であって、
前記固体潤滑被膜は、
60~80質量%の前記結合剤と、
8~18質量%の前記フッ素系添加剤と、
5~15質量%の前記固体潤滑剤と、
2~10質量%の前記防錆添加剤とを含有する、管用ねじ継手。 - 請求項5又は請求項6に記載の管用ねじ継手であって、
前記固体潤滑被膜はさらに、
タルクを2~15質量%含有することを特徴とする、管用ねじ継手。 - 請求項7に記載の管用ねじ継手であって、
前記タルクの粒子径が1~12μmであり、前記タルクの比表面積が4~12m2/gであることを特徴とする、管用ねじ継手。 - 請求項5~請求項8のいずれか1項に記載の管用ねじ継手であってさらに、
紫外線硬化樹脂を含有する固体防食被膜を備え、
前記固体潤滑被膜は、前記ピン及び前記ボックスの一方の前記接触表面に形成され、前記固体防食被膜は、前記ピン及び前記ボックスの他方の前記接触表面上に形成されることを特徴とする、管用ねじ継手。 - 請求項9に記載の管用ねじ継手であって、
前記固体防食被膜の厚みは5~50μmであることを特徴とする、管用ねじ継手。 - 請求項5~請求項10のいずれか1項に記載の管用ねじ継手であって、
前記固体潤滑被膜の厚みが10~200μmであることを特徴とする、管用ねじ継手。 - 請求項5~請求項11のいずれか1項に記載の管用ねじ継手であって、
油井管に使用されることを特徴とする、管用ねじ継手。 - ピンとボックスとを備え、前記ピン及び前記ボックスの各々は、互いに接触する部分を含む接触表面を備え、前記ピン及び前記ボックスの少なくとも一方の前記接触表面上に固体潤滑被膜を備える、管用ねじ継手の製造方法であって、
前記接触表面に請求項1~請求項4のいずれか1項に記載の組成物を前記接触表面上に塗布して前記固体潤滑被膜を形成する工程を備えることを特徴とする、管用ねじ継手の製造方法。 - 請求項13に記載の管用ねじ継手の製造方法であって、
前記固体潤滑被膜を形成する工程では、前記ピン及び前記ボックスの一方の前記接触表面上に前記固体潤滑被膜を形成し、
前記製造方法はさらに、
前記ピン及び前記ボックスの他方の前記接触表面に、前記紫外線硬化樹脂を含む固体防食被膜用の組成物を塗布する工程と、
塗布された前記固体防食被膜用の組成物に紫外線を照射して前記固体防食被膜を形成する工程とを備えることを特徴とする、管用ねじ継手の製造方法。
Priority Applications (10)
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AU2015234169A AU2015234169B2 (en) | 2014-03-20 | 2015-03-03 | Composition for solid lubricating coating, threaded connection for pipe or tube including the solid lubricating coating formed from the composition, and method of producing the threaded connection |
US15/126,015 US10336962B2 (en) | 2014-03-20 | 2015-03-03 | Composition for solid lubricating coating, threaded connection for pipe or tube including the solid lubricating coating formed from the composition, and method of producing the threaded connection |
EP15764227.3A EP3121253B1 (en) | 2014-03-20 | 2015-03-03 | Composition for solid lubricating coating, threaded connection for pipe or tube including the solid lubricating coating formed from the composition, and method of producing the threaded connection |
JP2015516322A JP5998278B2 (ja) | 2014-03-20 | 2015-03-03 | 固体潤滑被膜用組成物、その組成物から形成された固体潤滑被膜を備えた管用ねじ継手、及び、その管用ねじ継手の製造方法 |
CN201580014587.4A CN106103676B (zh) | 2014-03-20 | 2015-03-03 | 固体润滑皮膜用组合物、具备由该组合物形成的固体润滑皮膜的管用螺纹接头、以及该管用螺纹接头的制造方法 |
MX2016012117A MX2016012117A (es) | 2014-03-20 | 2015-03-03 | Composición para recubrimiento de lubricante sólido, conexión roscada para tubería o tubo de conducción, incluyendo el recubrimiento de lubricante sólido formado a partir de la composición y método de producción de la conexión roscada. |
EA201691861A EA035203B1 (ru) | 2014-03-20 | 2015-03-03 | Композиция для твердого смазочного покрытия, резьбовое соединение для трубы или трубопровода трубы, включающее твердое смазочное покрытие, сформированное из композиции, и способ изготовления резьбового соединения |
CA2942246A CA2942246C (en) | 2014-03-20 | 2015-03-03 | Composition for solid lubricating coating, threaded connection for pipe or tube including the solid lubricating coating formed from the composition, and method of producing the threaded connection |
PL15764227T PL3121253T3 (pl) | 2014-03-20 | 2015-03-03 | Kompozycja stałej powłoki smarującej, gwintowanych połączeń rur lub rurek, w tym stałych powłok smarowych wykonanych z kompozycji oraz sposób wytwarzania połączenia gwintowanego |
UAA201610407A UA114695C2 (uk) | 2014-03-20 | 2015-03-03 | Композиція для твердого мастильного покриття, нарізне з'єднання для труби або трубопроводу, яке включає тверде мастильне покриття, сформоване з композиціїї, і спосіб виготовлення нарізного з'єднання |
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US (1) | US10336962B2 (ja) |
EP (1) | EP3121253B1 (ja) |
JP (1) | JP5998278B2 (ja) |
CN (1) | CN106103676B (ja) |
AR (1) | AR100308A1 (ja) |
AU (1) | AU2015234169B2 (ja) |
CA (1) | CA2942246C (ja) |
EA (1) | EA035203B1 (ja) |
MX (1) | MX2016012117A (ja) |
MY (1) | MY180902A (ja) |
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WO2024019019A1 (ja) * | 2022-07-20 | 2024-01-25 | 日本製鉄株式会社 | 油井用金属管 |
CN115572631A (zh) * | 2022-09-29 | 2023-01-06 | 马鞍山拓锐金属表面技术有限公司 | 一种润滑剂组合物及其制备方法 |
Also Published As
Publication number | Publication date |
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UA114695C2 (uk) | 2017-07-10 |
CN106103676A (zh) | 2016-11-09 |
AU2015234169B2 (en) | 2017-03-02 |
JP5998278B2 (ja) | 2016-09-28 |
AU2015234169A1 (en) | 2016-11-03 |
MX2016012117A (es) | 2016-12-09 |
PL3121253T3 (pl) | 2020-03-31 |
CA2942246C (en) | 2018-05-01 |
CA2942246A1 (en) | 2015-09-24 |
EP3121253B1 (en) | 2019-09-04 |
US10336962B2 (en) | 2019-07-02 |
EP3121253A4 (en) | 2017-10-25 |
EP3121253A1 (en) | 2017-01-25 |
MY180902A (en) | 2020-12-11 |
JPWO2015141159A1 (ja) | 2017-04-06 |
EA201691861A1 (ru) | 2017-02-28 |
AR100308A1 (es) | 2016-09-28 |
EA035203B1 (ru) | 2020-05-15 |
CN106103676B (zh) | 2019-10-22 |
US20180201868A1 (en) | 2018-07-19 |
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