WO2022255167A1 - 固体潤滑被膜形成用の薬剤、油井管、油井管ねじ継手、及び油井管の製造方法 - Google Patents

固体潤滑被膜形成用の薬剤、油井管、油井管ねじ継手、及び油井管の製造方法 Download PDF

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Publication number
WO2022255167A1
WO2022255167A1 PCT/JP2022/021279 JP2022021279W WO2022255167A1 WO 2022255167 A1 WO2022255167 A1 WO 2022255167A1 JP 2022021279 W JP2022021279 W JP 2022021279W WO 2022255167 A1 WO2022255167 A1 WO 2022255167A1
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WO
WIPO (PCT)
Prior art keywords
solid
lubricating coating
graphite
film
solid lubricant
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2022/021279
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
康英 石黒
城吾 後藤
崇司 古賀
孝将 川井
誠二 尾▲崎▼
秀雄 佐藤
幸子 藤本
浩一 正田
聡 大久保
亮太 小林
良太 久保
孝太 豊澤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JFE Steel Corp
Toyo Drilube Co Ltd
Original Assignee
JFE Steel Corp
Toyo Drilube Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JFE Steel Corp, Toyo Drilube Co Ltd filed Critical JFE Steel Corp
Priority to US18/564,142 priority Critical patent/US12312552B2/en
Priority to CN202280038745.XA priority patent/CN117413040B/zh
Priority to JP2022550248A priority patent/JP7241249B1/ja
Priority to MX2023014265A priority patent/MX2023014265A/es
Priority to BR112023024971A priority patent/BR112023024971A2/pt
Priority to EP22815917.4A priority patent/EP4332202A4/en
Publication of WO2022255167A1 publication Critical patent/WO2022255167A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/04—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a macromolecular organic compound
    • 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
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/02—Carbon; Graphite
    • 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
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
    • 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
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/20—Lubricating compositions characterised by the base-material being a macromolecular compound containing oxygen
    • C10M107/30—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M107/32—Condensation polymers of aldehydes or ketones; Polyesters; Polyethers
    • 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
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/38—Lubricating compositions characterised by the base-material being a macromolecular compound containing halogen
    • 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
    • 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
    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • 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
    • F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
    • F16B33/00—Features common to bolt and nut
    • F16B33/06—Surface treatment of parts furnished with screw-thread, e.g. for preventing seizure or fretting
    • 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
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C10M2201/0413—Carbon; Graphite; Carbon black used as base material
    • 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
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • 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
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C10M2201/0663—Molybdenum sulfide used as base material
    • 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
    • C10M2201/087—Boron oxides, acids or salts
    • C10M2201/0873—Boron oxides, acids or salts used as base material
    • 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
    • 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
    • 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
    • C10M2201/12—Glass
    • C10M2201/123—Glass used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/1003—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/101—Condensation polymers of aldehydes or ketones and phenols, e.g. Also polyoxyalkylene ether derivatives thereof
    • C10M2209/1013—Condensation polymers of aldehydes or ketones and phenols, e.g. Also polyoxyalkylene ether derivatives thereof used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/1033—Polyethers, i.e. containing di- or higher polyoxyalkylene groups used as base material
    • 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
    • C10M2213/06—Perfluoro polymers
    • 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
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • 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
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • C10M2213/0623—Polytetrafluoroethylene [PTFE] used as base material
    • 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
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • 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
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/063—Fibrous forms
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/241—Manufacturing joint-less pipes
    • 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
    • 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
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/08—Solids
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B17/00—Drilling rods or pipes; Flexible drill strings; Kellies; Drill collars; Sucker rods; Cables; Casings; Tubings
    • E21B17/02—Couplings; joints
    • E21B17/04—Couplings; joints between rod or the like and bit or between rod and rod or the like
    • E21B17/042—Threaded
    • 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
    • F16L15/001—Screw-threaded joints; Forms of screw-threads for such joints with conical threads
    • 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

Definitions

  • the present disclosure is a technology related to lubrication and corrosion resistance of oil country tubular goods threaded joints.
  • the present disclosure relates to an oil country tubular good and an oil country tubular good threaded joint in which a solid lubricating coating is formed on the fastening surface (including the metal seal surface) of the threaded portion instead of a wet lubricating compound.
  • the fastening surface which is the surface of the threaded portion, includes the metal sealing surface.
  • the solid lubricating coating means a coating composed of a binder resin as a matrix component, a solid lubricant dispersed and distributed in the binder resin, and additives added as necessary.
  • the present disclosure intends to provide corrosion resistance while improving lubrication by a solid lubricating coating that achieves lubrication of oil country tubular goods threads.
  • lubricity and “high lubricity” mean, in a broad sense, the phenomenon of low friction and slipperiness.
  • high lubricity means that the number of tightening and untightening operations (also referred to as the number of tightening and untightening operations) can be a specified number of times or more.
  • seizure resistance of threaded joints for oil country tubular goods is described in the API 5C5 standard.
  • the API 5C5 standard requires the casing size to allow up to 3 tightenings. Also, the tubing size is required to be able to tighten up to 10 times.
  • tube which has an internal thread may be generically described as a box. That is, coupling is also described as a kind of box.
  • lubrication of the threads has conventionally been accomplished by applying a ring to the fastening surface (sealing surface) (hereinafter also referred to simply as the "fastening surface") of the threaded portion of at least one of the male thread side and female thread side parts.
  • a film is formed by surface treatment using an acid Mn chemical conversion treatment film or electroplating using Cu or the like. After that, a lubricating compound containing Pb, Zn, etc. is applied on the film for lubrication.
  • the fastening surface including the coating is called the fastening surface.
  • a solid lubricating coating is composed of a lubricant component responsible for lubrication and a solid film as a matrix component that retains the lubricant component in the film.
  • a solid film means that it is a non-viscous film and not a liquid film, and it also means that the film itself completes lubrication during screw tightening and untightening.
  • Conventional Mn phosphate films and Cu electroplating films are themselves solid films. However, it is not included in the solid lubricating coating because it assumes lubrication by applying a grease-like compound. In the present disclosure, lubrication is achieved as a solid film, and an organic resin film is assumed as the solid film. Therefore, in the description below, the solid film is also described as a binder resin.
  • the present disclosure uses graphite as the main component of the solid lubricant and PEEK resin as the main component of the binder resin.
  • PEEK resin As the main component of the binder resin.
  • the PEEK resin is controlled within an appropriate range in consideration of special lubrication conditions (severe lubrication conditions such as large loads and unbalanced loads) such as oil country tubular goods threaded joints. .
  • Patent Documents 1 to 6 are available as similar techniques.
  • Patent Documents 1 to 3 are inventions relating to solid lubricating coatings for oil country tubular goods screws.
  • Patent Documents 1 to 3 exemplify graphite as an example of a substance that can be considered as a solid lubricant.
  • Patent Document 3 also describes that graphite is the best candidate material for solid lubricants.
  • Patent document 4 is not an invention of an oil country tubular good screw.
  • Patent Document 4 describes graphite as one of the constituent elements in lubricating the bearing portion.
  • Patent Document 5 relates to water-based agents, and graphite is exemplified as a solid lubricant.
  • graphite has the advantage that the lubrication condition does not change even at high temperatures, and that the lubrication does not change even at high loads.
  • graphite even in the form of fine powder, does not explode but only burns. For this reason, graphite is also widely used to lubricate plugs and billets in the drilling process for manufacturing seamless steel pipes, and is widely understood as a stable lubricant.
  • PEEK resin (simply referred to as PEEK) is a thermoplastic resin that is stable even at high temperatures and is known as a hard plastic.
  • PEEK is an acronym for Poly Ether Ether Ketone.
  • PEEK is a very hard material.
  • PEEK is commercially available in which glass fiber is added to increase strength and rigidity, and in which PTFE, graphite, carbon fiber, etc. are added and mixed to increase lubrication. there is Incidentally, the PEEK resin is sold alone in the form of pellets.
  • Patent Document 6 exemplifies PEEK resin in which PTFE is dispersed.
  • Patent Documents 1 to 3 Although graphite is exemplified, the content of graphite is not specified. That is, it is presumed that the descriptions of Patent Documents 1 to 3 are not particularly conscious of the content, as they include all to no content in the solid lubricant.
  • the PEEK resin described in Patent Document 6 has a Knoop hardness of Hk80. US Pat. No. 6,200,000 is the case of a special PEEK resin that is extremely soft.
  • the standard hardness of PEEK resin is Rockwell hardness: R120
  • Knoop hardness is HK963
  • Patent Document 6 is an example using a heterogeneous PEEK resin, which is inappropriate as the PEEK resin assumed by the present disclosure.
  • the lubrication of oil country tubular goods threads which is the object of the present disclosure, is in a special sliding situation. That is, at the site (actual well), a pin having an actual length of about 8 m or more and less than 15 m is tightened and unfastened with respect to the box set below. At this time, although the pin is tightened and undone using power tongs while being lifted by a crane, the entire load of the pin can be applied to the box screw. This is referred to herein as lubrication under heavy load conditions.
  • the pin is not necessarily tightened and unscrewed in an ideal state. That is, when tightening, the pin screw is either inserted into the box screw or is set in a slightly hand-tightened state. However, the pin is not set upright and stationary with respect to the box screw. Also, the pin is not set in a state in which it stands straight (without bending) while being tilted in an oblique direction. That is, while the lower part of the pin was constrained by the box screw, the upper end side, that is, the tip side opposite to the tightening side, was slightly bent according to the elastic modulus (Young's modulus) of the material and the actual pin length. become a state.
  • the elastic modulus Young's modulus
  • the pin when viewed from below, the pin looks like it is bent while being set straight in the box. From that state, the pin is tightened and untightened, so that the box screw and the pin screw are uniformly and symmetrically loaded and never tightened and untightened. As a result, a portion of the thread surface is in a state where tightening and untightening is performed in a state where it is strongly hit locally (lubrication under an unbalanced load state). In addition, the location of strong local contact also changes according to tightening and loosening.
  • the compound follows the movement when tightening and untightening. Therefore, even if the lubrication conditions fluctuate to some extent, the lubricant (lubricating compound) functions to favorably converge tightening and loosening. Therefore, in the evaluation test (also called laboratory test) of tightening and unfastening of threaded joints in lubrication technology that uses a grease-like compound, evaluation using a short pin, rather than relying on evaluation using a full-size pin, It is possible to grasp the lubrication status of
  • the solid lubricating coating is inevitably scraped off to some extent in the oil country tubular goods lubricating technology using the solid lubricating coating.
  • secondary formations derived from the scraped solid lubricating coating do not always move in conjunction with tightening and loosening. This is what happens in real wells and is very different from lubrication using wet lubricating compounds.
  • the secondary product consisting of the shavings of the solid lubricating film clogs and seizes, or the secondary product is pressed against the fastening surface again, resulting in a lubricating film-like failure. It is not possible to simulate a situation such as maintaining an effect. That is, the conventional evaluation simply using a short pin inevitably results in a lenient evaluation of the solid lubricating coating. Then, when determining the physical property parameters of the solid lubricating coating, there is a problem that even a region that should not be acceptable is erroneously evaluated as a suitable range.
  • the clogged material becomes powdery and clogs the thread gap, causing seizure at the thread portion.
  • burn-in tends to occur after the second time.
  • the present inventor believes that when the solid lubricant is composed of 100% graphite, a tape-shaped secondary product derived from graphite is strongly formed, which clogs screw gaps and is the main cause of seizure. I got some insight.
  • the solid lubricating coating must be a film that can withstand a large load applied as an unbalanced load.
  • a film that can be uprooted or a film that is mostly destroyed and lost cannot be dealt with.
  • oil country tubular goods are mostly used with a length of Range-3 or Range-2 according to the API-5CT standard.
  • the former standard is often used at a length of about 12 to 16 m.
  • an oil well pipe with a length of about 12 m (about 40 feet) has a dead weight of about 1 t with an outer diameter of 9-5/8′′. For this reason, if a 9-5/8" outer diameter oil country tubular good is used, the situation is so severe that about 3 tons are applied to the box side.
  • solid lubricants composed of 100% graphite cannot be applied, and it is necessary to reconsider solid lubricants and optimize the composition of solid lubricants.
  • binder resin In addition to lubricating oil well pipe threads, it is also necessary to consider corrosion resistance. Oil country tubular goods materials are sometimes stored in yards for about one to two years in the long term, so they need to have a membrane that can withstand corrosion even in rainy conditions.
  • the present invention has been made in view of the above points, and is capable of providing a solid lubricating coating capable of imparting good lubricity and corrosion resistance to oil country tubular goods screws even when graphite is used as a solid lubricant. It is intended to
  • the present disclosure is a solid lubricating coating and a drug, in which the main component of the solid lubricant is graphite and the main component of the binder resin is PEEK resin. Then, an appropriate range that can achieve both stable lubrication and corrosion resistance is clarified under severe conditions such as tightening and loosening of an oil country tubular goods threaded joint, where a large load and an unbalanced load are applied. As a result, the present disclosure ensures lubricity that can withstand actual tightening and loosening of a well, and at the same time achieves both corrosion resistance.
  • the present inventors investigated the range of conditions for improvement and found the optimum range of graphite, the optimum range of binder resin, and the optimum ratio, including the mixing ratio thereof.
  • seizure frequently occurs only in the case of "simple use of graphite" as described in past literature.
  • Stable lubrication cannot be achieved simply by adding graphite.
  • PEEK PEEK as the main component of the binder resin.
  • a black tape-like secondary product is strongly formed based on graphite, it clogs the screw gap and directly leads to seizure. For this reason, the inventors have found that it is necessary to select graphite by selecting the type, blending ratio, and particle size of graphite to eliminate the range of graphite that causes seizure.
  • binder resin is also important. Regarding the lubrication of the oil country tubular good threads, as described above, until the threads are sufficiently meshed, they are exposed to severe conditions in which a large load or an unbalanced load is applied. At that time, the solid lubricating coating cannot be said to have zero damage, and is likely to peel off from the hardness and the contact surface.
  • the black tape-shaped secondary product is peeled off during tightening and loosening, and appears in the thread gap. Since this is derived from graphite and binder resin, the above graphite regulation and binder resin are also regulated to reduce black tape-like secondary products, and graphite and binder resin are peeled off. Even if it is, instead of making it into a black tape, consider making it powder-like or a small lump that moves in conjunction with tightening and loosening to block specific locations and prevent seizure. I have come to the knowledge that there is a need.
  • One aspect of the present invention is a chemical agent for forming a solid lubricating coating on a threaded portion of an oil country tubular good, wherein two or more types of solid lubricants are dispersed in a binder resin, and two or more types of solid lubricants are dispersed in a binder resin.
  • graphite is contained in an amount of 50% or more and 90% or less of the total weight of the solid lubricant, and the graphite is scaly in shape and has an average particle size of 10.0 ⁇ m or less.
  • solid lubricants among solid lubricants include BN (boron nitride), mica (mica), talc, MCA (melamine cyanurate), MoS 2 (molybdenum disulfide), PTFE (polytetrafluoroethylene), PFA (perfluoroalkoxyalkane; tetrafluoroethylene/perfluoroalkoxyethylene copolymer resin), FEP (perfluoroethylene propene copolymer; tetrafluoroethylene/hexafluoropropylene copolymer) solid lubrication made of one or more materials
  • the main component of the binder resin is a PEEK resin having an average particle size of 20 ⁇ m or less, and the PEEK resin is contained in an amount of 70% or more of the total weight of the binder resin.
  • An aspect of the present invention is an oil country tubular good in which a lubricating coating having a solid lubricating coating is formed with a threaded portion, wherein the solid lubricating coating comprises a solid lubricant dispersed in a binder resin;
  • the solid lubricating coating comprises a solid lubricant dispersed in a binder resin;
  • graphite is contained in an amount of 50% or more and 90% or less of the total weight of the solid lubricant, the graphite has a scale-like shape and an average particle size of 10.0 ⁇ m or less
  • Other solid lubricants among the above two or more types of solid lubricants include BN (boron nitride), mica (mica), talc, MCA (melamine cyanurate), MoS 2 (molybdenum disulfide), PTFE (polytetra fluoroethylene), PFA (perfluoroalkoxyalkane; tetrafluoroethylene/perflu
  • the gist is that the binder resin contains a solid lubricant made of a material, and the binder resin is mainly composed of a PEEK resin having an average particle size of 20 ⁇ m or less, and contains the PEEK resin in an amount of 70% or more of the total weight of the binder resin.
  • the aspect of the present invention even if graphite is used as a solid lubricant, it is possible to provide a solid lubricating coating capable of imparting good lubricity and corrosion resistance to the threaded portion of an oil country tubular good.
  • a solid lubricating coating capable of imparting good lubricity and corrosion resistance to the threaded portion of an oil country tubular good.
  • the actual well-equivalent condition means that there are many situations where the weight of the pin is applied to the box from above, the load is applied diagonally due to the deviation of the axis, and the load is applied locally rather than uniformly. and other conditions.
  • FIG. 1 is a diagram showing an oil country tubular good and an oil country tubular good threaded joint;
  • FIG. It is a diagram (a) of a tightening chart in an actual well and a diagram (b) showing the initial set position at that time.
  • It is a diagram (a) of a tightening chart in a conventional laboratory test and a diagram (b) showing an initial set position at that time.
  • weight tongue test shows the installation example of the weight in a new laboratory test (weight tongue test).
  • FIG. 2(a) shows an example of tightening occurring in an actual well.
  • Fig. 2(a) is a torque-turn chart (tightening chart) when a tightening test was conducted under the condition that a 40-foot ( ⁇ 12m) actual length pin was used to simulate an actual well. .
  • tightening is often started in a situation where the threads are not sufficiently engaged.
  • FIG. 2(a) the initial setting position is changed from the state where the pin screw is exposed from the box screw at the start of initial tightening, as shown in FIG. , is an example of starting tightening.
  • FIG. 2(a) is a chart when the pin is tightened with vertical tongs while being suspended by a crane that suspends the entire length of the pin from above the rig.
  • FIG. 2(a) can be regarded as a situation that often occurs in an actual well.
  • the torque should not stand in principle. is.
  • the spike-like torque tends to rise irregularly and frequently. This suggests that the pin screw is in irregular and localized contact with the box screw as it rotates. This is the situation that occurs in tightening in actual wells.
  • it means that destruction and peeling of the solid lubricating coating cannot be avoided to some extent depending on the design and optimization of the solid lubricating coating.
  • the state in FIG. 2(a) is not the worst state intentionally created, but is a normal torque-turn chart for a sample with a solid lubricating coating.
  • FIG. 3(a) is a torque-turn chart when using the same solid lubricating coating as in FIG. 2 and tightening with vertical power tongs.
  • a pin having the same outer diameter, thickness, and thread type as those in FIG. 2 is used, but a short pin having a length of about 1 m is used as the pin.
  • FIG. 3(a) is a tightening chart (torque turn chart) when tightening is started from a state in which the screws are sufficiently meshed. That is, as shown in FIG. 3(b), it is a tightening chart (torque turn chart) in the case where the pin threads are exposed at about 1 to 3 threads at the start of the initial tightening.
  • FIG. 3(a) The conditions in FIG. 3(a) are often used in conventional laboratory tests for tightening, and are examples of manual tightening until the screws are engaged. It should be noted that in FIG. 3(a), the unit of the horizontal axis is different from that in FIG. 2(a). In Fig. 3(a), since the tightening by the tongs is started from the state where the screws are hand-tightened to the meshed state, the spike-like torque seen in Fig. 2(a) is not seen. . As can be seen from FIG. 3, in the conventional laboratory test, in phase 1, the solid lubricating coating is not broken, and tightening occurs from the area where the two surfaces of the screw begin to come into contact.
  • FIG. 4 shows FIGS. 2(a) and 3(a) in a state that facilitates comparison.
  • 4A is an example of FIG. 2
  • FIG. 4B is an example of FIG.
  • the ideal solid lubricating coating should be such that the solid lubricating coating is not destroyed in the region (x) in FIG. 4(a). , to minimize concerns about breakage and delamination.
  • spikes may stand to some extent (a situation in which the solid lubricating coating is damaged), secondary products derived from the broken or peeled solid lubricating coating will not clog the screw gap during the tightening and loosening process.
  • it should be designed to adhere well to the threads and assist in lubrication.
  • the large-diameter oil country tubular goods screw generally has a higher tightening torque value and more play between the box screw and the pin screw. For this reason, it is inevitable that the solid lubricating coating will be destroyed and peeled off to some extent before the screws are fully meshed. In addition, at the beginning of the test, when the pin screw is set to the box screw, it is difficult to handle due to the heavy weight, and it often happens that the pin screw accidentally hits the box screw. This also causes the solid lubricating coating to break and peel off. In the present embodiment, the tightening and loosening conditions of an actual well are considered.
  • the present embodiment relates to a coating structure formed on a fastening surface of an oil country tubular goods screw actually used for oil/gas, and a threaded joint having the coating structure as a lubricating coating.
  • This embodiment is characterized by a lubricating coating provided with a solid lubricating coating formed on the fastening surface of a threaded joint, and the thread structure itself of the threaded joint is not particularly limited.
  • a known or novel thread structure may be adopted for the thread structure of the threaded joint.
  • An oil country tubular good is composed of, for example, a box 2 such as a coupling and a pin 1 as shown in FIG.
  • an oil well pipe threaded joint consists of a box 2 such as a coupling having a female thread 2a and a pin 1 having a male thread 1a.
  • a lubricating coating comprising a solid lubricating coating is formed on the contact surface (fastening surface 10) of the threaded portion of at least one of the box 2 and the pin 1.
  • the agent for forming a solid lubricating coating in this embodiment will be described below.
  • the drug of this embodiment is composed of a binder resin as a matrix component and two or more solid lubricants dispersed therein.
  • graphite is included as one of the two or more types of solid lubricants in an amount of 50% or more and 90% or less of the total weight of the solid lubricant.
  • the graphite has a scale-like shape and an average particle size of 10.0 ⁇ m or less.
  • the scale-like shape means that it is preferable that the crystallinity is the best and the graphite purity is high.
  • solid lubricants made of one or more materials selected from the following first group solid lubricant materials and second group solid lubricant materials containing agents.
  • PTFE polytetrafluoroethylene
  • PFA perfluoroalkoxyalkane; tetrafluoroethylene/perfluoroalkoxyethylene copolymer resin
  • FEP perfluoroethylene propene copolymer; tetrafluoroethylene-hexafluoropropylene copolymer
  • the solid lubricant material of the first group and the solid lubricant material of the second group differ in lubrication mechanism.
  • the solid lubricant materials of the first group are lubricants in the form of two-dimensional layered compounds bound together by intermolecular forces in the Z direction. to achieve lubrication.
  • the solid lubricant material of the second group is a lubricant in which strongly formed molecules with a one-dimensional straight chain structure are bound to each other by intermolecular force, and when a force is applied in the lubricating direction, Lubrication is achieved by linear structural units sliding against each other.
  • the reason for mixing the materials selected from the first group of solid lubricant materials and the second group of solid lubricant materials is as follows.
  • a lubricant is assembled only from graphite
  • a secondary "black tape-shaped secondary product” is produced, which is a combination of scraped graphite and scraped PEEK resin. make. And this may cause it to form too strongly.
  • the "black tape-like secondary product” will clog the clearances of the thread and cause seizure.
  • the incorporation of this secondary product is reduced, and the risk of seizure is reduced while maintaining high lubrication.
  • the average particle size of the other solid lubricant is preferably in the range of 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the binder resin is mainly composed of PEEK resin having an average particle size of 20 ⁇ m or less, and contains 70% or more of the total weight of the binder resin.
  • the total weight of the solid lubricant is preferably 0.1 to 2 times the total weight of the binder resin.
  • the content of graphite as a solid lubricant is preferably 20% or more and 50% or less of the sum of the total weight of the solid lubricant and the total weight of the binder resin.
  • the drug contains a solvent that does not remain in the coating and adjusts the liquid viscosity.
  • the weight ratio of the solvent is preferably 30% to 80% with respect to the sum of the total weight of the solid lubricant and the total weight of the binder resin.
  • a lubricating coating comprising a solid lubricating coating is formed on the fastening surface of the threaded portion of at least one of the box and the pin.
  • the solid lubricating coating is composed of a solid lubricant dispersed in a binder resin as a matrix component.
  • graphite is included as one of the two or more types of solid lubricants in an amount of 50% or more and 90% or less of the total weight of the solid lubricant.
  • the graphite has a scale-like shape and an average particle size of 10.0 ⁇ m or less.
  • the scale-like shape means that it is preferable that the crystallinity is the best and the graphite purity is high.
  • a solid lubricant made of one or more materials selected from the solid lubricant materials of the first group and the solid lubricant materials of the second group containing agents is included as another solid lubricant.
  • the average particle size of the other solid lubricant is preferably in the range of 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the binder resin is mainly composed of PEEK resin having an average particle size of 20 ⁇ m or less, and contains 70% or more of the total weight of the binder resin.
  • the total weight of the solid lubricant is preferably 0.1 to 2 times the total weight of the binder resin.
  • the content of graphite as a solid lubricant is preferably 20% or more and 50% or less of the sum of the total weight of the solid lubricant and the total weight of the binder resin.
  • the solid lubricating coating includes, for example, the threads of the threaded portion and is formed up to an area adjacent thereto.
  • the solid lubricating coating preferably has a pencil hardness of 3H or more.
  • the solid lubricating coating preferably has a film thickness of, for example, 10 ⁇ m or more and 150 ⁇ m or less.
  • the lubricating coating may have a base layer 10B between the fastening surface of the threaded portion and the solid lubricating coating 10A (see FIG. 7).
  • the underlying layer 10B is made of, for example, an electroplating film or a chemical conversion treatment film. If the box and pin are made of stainless steel, Ni-based alloy, or Ti alloy, the lubricating coating may have a base layer 10B between the fastening surface of the threaded portion and the solid lubricating coating.
  • the underlying layer 10B is made of, for example, an electroplating film.
  • a lubricating coating comprising a solid lubricating coating is formed on the fastening surface of the threaded portion of one of the box and the pin, and the fastening surface of the threaded portion of the other of the box and the pin is formed.
  • the oil well pipe threaded joint may have a structure in which a film softer than the solid lubricating film is formed.
  • Soft films are also preferably solid lubricating coatings.
  • graphite since graphite has a strong plate-like structure due to its physical structure, graphite tends to be connected to each other to form a tape.
  • the organic resin that constitutes the binder resin acts like a kind of glue, and there is a high tendency to form a strong and thick black tape that completely fills the threads and roots. Therefore, the solid lubricating coating is inevitably scraped off to some extent during tightening and unfastening of the screw.
  • These exfoliated materials (residues) form secondary products in the form of black tapes as described above.
  • the stacking in layers is weak because it is at the level of intermolecular force, and it moves in a slippery direction due to the load applied during tightening and untightening. It won't be destroyed much. Therefore, the black tape-shaped secondary product only increases in thickness, and does not have the mobility to move in conjunction with tightening and unfastening. Also, in practice, the tightening and untightening of screws cannot be performed homogeneously and is not symmetrical. At the initial stage of tightening and the final stage of tightening, most of the tightening is carried out eccentrically to some extent.
  • ⁇ Main component of solid lubricant> two or more types of solid lubricants are used while the main component is graphite. That is, as one of the two or more types of solid lubricants, graphite is included in an amount of 50% or more and 90% or less of the total weight of the solid lubricant. The graphite has a scale-like shape and an average particle size of 10.0 ⁇ m or less. Furthermore, as another solid lubricant among the two or more types of solid lubricants, a solid lubricant made of one or more materials selected from the solid lubricant materials of the first group and the solid lubricant materials of the second group containing agents.
  • graphite which is said to be a highly lubricating substance, is used to improve the lubricating field of oil country tubular goods screws and its application field.
  • each solid The upper and lower limits of the lubricant were set. Also, the upper and lower limits of each solid lubricant were set from the standpoint of dividing and cutting instead of a rigid tape.
  • the reason why the upper limit is set to 90% is that if the upper limit is exceeded, tape-like secondary products derived from graphite are likely to clog the screw gaps and seize.
  • the important point in the present disclosure is to make the properties of the tape-shaped secondary product derived from graphite fragile while using graphite as the main component of the solid lubricant. Also, it is to prevent a thick and strong tape-like thing from being produced. It is an important point in lubrication improvement when graphite is used as the main component of a solid lubricant to produce a tape-shaped secondary product that is divided as short as possible or in a powder state. becomes.
  • one of the features of the present disclosure is to mix graphite with another type of solid lubricant to form a solid lubricating coating.
  • solid lubricants other than graphite even if layered solid lubricants such as MoS 2 , BN, etc. are mixed as subcomponents, the properties of the strong (long) tape-shaped secondary product can be changed, and the tape-shaped length can be changed. can be shortened or powdered. As a result, the gap between the pin screw and the box screw can be prevented from being clogged with secondary products derived from graphite and seizing.
  • a solid lubricant of a type other than a layered solid lubricant, such as PTFE as another type of solid lubricant, the properties of the secondary product can be made powdery or fragile tape-like. can.
  • scale-like graphite is selected as the type of graphite.
  • Earthy graphite, natural graphite-based graphite such as expanded graphite, and artificial graphite were not selected.
  • the reason for choosing the scaly shape is that graphitization is the most advanced, that is, the network of carbon with a two-dimensional layer structure and the layers are linked by intermolecular force, so it is advantageous for lubrication.
  • Graphite having a grain size of 0.1 to 10.0 ⁇ m was selected. This is because if the size exceeds 10 ⁇ m, the graphite itself is too large to make effective use of the lubrication of graphite, and this itself becomes a source of seizure.
  • the main component of the solid lubricant in the solid lubricating coating is graphite, which accounts for 50% or more and 90% or less of the solid lubricant, and the main component of the binder resin is PEEK resin.
  • the solid lubricant is defined as solid lubricant in a broad sense, including additives other than the binder resin component.
  • the secondarily mixed solid lubricant component is a solid lubricant made of one or more materials selected from the first group of solid lubricant materials and the second group of solid lubricant materials.
  • graphite has a strong structure on two-dimensional planes and is in a state in which they are weakly bonded in layers by intermolecular forces. Lubrication is maintained by sliding like a pile of playing cards. When graphite is used at random, it often creates a "black tape-like secondary product" that clogs screw gaps and causes seizure. It should be avoided through graphite optimization and PEEK resin optimization. From such a point of view, it is preferable to select secondary components along the main structure of the present disclosure.
  • the secondarily mixed solid lubricating component causes long molecular chains to slide in the direction in which force is applied to each other.
  • Mechanism lubrication additives are preferred.
  • PTFE as the secondarily mixed solid lubricating component. Preferred conditions at this time are defined, and an average particle diameter of 0.1 to 5 ⁇ m is defined as good. If the thickness exceeds 5 ⁇ m, the PTFE itself becomes entangled and the effect of improving lubrication is small.
  • the lubricating effect of PTFE is submerged when graphite is contained as a secondary component in the main component as in this case, and it does not appear to exhibit particularly excellent lubrication.
  • Other secondarily mixed solid lubricating components for example, preferably have an average particle size of 0.1 to 5 ⁇ m.
  • PFA and FEP are also examples that follow the same mechanism. These have a structure in which side chains are attached to the molecular structure of PTFE, and achieve lubricity based on the sliding of the molecular chains. However, since PTFE has one step of superior characteristics due to the presence of side chains, it was selected as a suitable range.
  • the solid lubricating component that is secondarily mixed can be selected from the viewpoint of improving lubrication by hardening the film quality. Additions, including glass fiber powder and carbon fiber powder, are also intended to be included in this disclosure.
  • the binder resin consists of one kind or two or more kinds of resin components.
  • the binder resin of the present embodiment is mainly composed of PEEK resin having an average particle size of 20 ⁇ m or less.
  • the PEEK resin is contained in an amount of 70% or more and 100% or less of the total weight of the binder resin.
  • the main cause of seizure is the solid resin coating component (solid lubricant + It is a "black tape-shaped secondary product" formed secondarily based on the binder resin component).
  • PEEK resin is defined as 70% or more of the total weight of the binder resin is to harden the solid lubricating coating itself in oil country tubular goods screw lubrication. That is, it is intended to reduce the amount of graphite scraped off from the film and reduce the amount of graphite and binder resin components that are the source of the "black tape-like secondary product".
  • a hard coating is preferable because it reduces the amount of peeling and scraping.
  • PEEK resin polyether ether ketone
  • hard resins examples include polyetherimide (PEI), polyphenylene sulfide (PPS), polyamideimide (PAI), polybenzimidazole (PBI), and phenolic resin (PF).
  • PEI polyetherimide
  • PPS polyphenylene sulfide
  • PAI polyamideimide
  • PBI polybenzimidazole
  • PF phenolic resin
  • polyetherimide has poor abrasion resistance because it is an amorphous resin. Therefore, the solid lubricating coating tends to be scraped off during the process of tightening and unfastening the screw.
  • Polyphenylene sulfide has poor toughness, is not convenient to use depending on the operating temperature, and promotes seizure.
  • PAI polyamide-imide
  • PAI polyamide-imide
  • PBI polybenzimidazole
  • PBI is too hard and unsuitable for lubricating applications per se. In the oil and gas sector, there is a constant concern that S containing, e.g.
  • PPS polyphenylene sulfide
  • Heat generation is unavoidable to some extent in oil country tubular good thread lubrication.
  • Phenol resin (PF) has a heat resistance temperature of about 150° C., so it is poor in heat resistance.
  • the PEEK resin accounts for 70% or more of the main component, there is no particular problem in using these as a secondary mixture.
  • the particle size of the PEEK resin must be 20 ⁇ m or less. This is because, similarly to graphite, if the particle size of the PEEK resin is too large, it itself becomes a source of seizure. When the oil country tubular good screw is tightened and loosened, a large load is applied and the threads are slid in an environment where the threads are in close contact with each other. Both the binder resin and the solid lubricant are crushed and do not retain their original size. However, an initial size of 20 ⁇ m is likely to contribute to image sticking. Therefore, the maximum size of the average particle size of the PEEK resin is defined as 20 ⁇ m or less.
  • the content weight of the solid lubricant should be 0.1 times or more and 2 times or less the weight of the binder resin.
  • the weight fraction of graphite is set to 20% or more and 50% or less. This regulation was also established to minimize the above-mentioned "black tape-like secondary product" and to effectively utilize the solid lubricating effect of graphite.
  • the reason why the graphite-based solid lubricant is blended so that the weight of the total solid lubricant is 0.1 to 2.0 times the weight of the binder resin is as follows.
  • the reason why the lower limit is set to 0.1 times is that if it is less than that, the "black tape-like secondary product" is less likely to occur and it is in a range where there is no problem, but the solid lubricant itself is small and the lubrication effect is not maintained.
  • the reason why the upper limit is set to 2.0 is that if it is exceeded, "black tape-like secondary products" are generated more than necessary, and seizure frequently occurs.
  • PEEK resin and graphite are water repellent.
  • corrosion resistance is provided on the premise that the oil country tubular goods screw with the protector attached may be exposed to the outdoors for about 1 to 2 years and left until it is used. They are often requested products. Therefore, it is also intended to maintain anti-corrosion properties due to the water repellency of the PEEK resin and graphite when secondary components are included.
  • the hard film can reduce minute cracks, it is possible to maintain lubricity and achieve anti-corrosion properties.
  • the agent contains a solvent to adjust the dryness and liquid viscosity without remaining in the film.
  • the component weight ratio of the solvent is preferably 30 to 80% with respect to the sum of the solid lubricant component weight and the binder resin component weight.
  • Components constituting the solid lubricating coating are prepared in a state of being dissolved in a solvent. The chemical is applied, and the solvent is volatilized, baked, or dried by irradiation with far infrared rays, ultraviolet rays, or the like to form a film.
  • the solvent component weight ratio is 30-80% with respect to the sum of the solid lubricant component weight and the binder resin component weight.
  • the solvent material is not particularly limited. It may be a polar solvent or a non-polar solvent.
  • the PEEK resin needs to be baked at a temperature exceeding 350° C., these solvents must volatilize/evaporate up to that temperature range.
  • the reason why the solvent component is less than 80% is that the graphite tends to float in the solvent when the liquid viscosity is adjusted. Another reason is to prevent the graphite from biasing toward the surface when a solid lubricating coating is formed. Therefore, the upper limit is defined as 80%.
  • the reason why the lower limit is 30% is to avoid that if it is less than 30%, the liquid viscosity of the medicine is high and it cannot be applied well.
  • polar solvents examples include DMF (N,N-dimethylformamide), NMP (N-methyl-2-pyrrolidone), DMSO (dimethylsulfoxide), methanol and ethanol.
  • nonpolar solvents examples include n-hexane, toluene, xylene, dioxane, THF (tetrahydrofuran), and the like.
  • organic solvents examples include ketone-based solvents such as MEK (methyl ethyl ketone) and MIBK (methyl isobutyl ketone), ester-based solvents such as ethyl acetate and butyl acetate, and alcohol-based solvents such as methanol, ethanol, and IPA (isopropyl alcohol).
  • ketone-based solvents such as MEK (methyl ethyl ketone) and MIBK (methyl isobutyl ketone)
  • ester-based solvents such as ethyl acetate and butyl acetate
  • alcohol-based solvents such as methanol, ethanol, and IPA (isopropyl alcohol).
  • the solid lubricating coating is utilized as a film that achieves both lubricity and corrosion resistance.
  • the idea and assembly of the present disclosure are based on achieving lubrication of the solid lubricating coating of the oil country tubular goods screw. As shown in FIGS. 2 to 4, the solid lubricating coating is damaged during tightening and untightening of the oil country tubular goods threads, particularly at the beginning of tightening and at the final stage of untightening, due to backlash until the threads engage with each other.
  • the formed film preferably has a pencil hardness of 3H or more, and a film thickness of 10 ⁇ m or more and 150 ⁇ m or less. There is no upper limit for the hardness of the film, and the harder the better. When the film is hard, the "black tape-like secondary product" that often appears can be reduced. If the film has a pencil hardness of 3H or higher, the effect is high, and as a result, the number of times of tightening and unfastening exceeds the target level.
  • the PEEK resin alone has a pencil hardness of about 3H to 5H, the addition of a solid lubricating component should not lower the hardness.
  • glass fiber or carbon fiber may be added to positively increase the hardness of the PEEK resin.
  • the film thickness it is necessary to form a film with a minimum film thickness of 10 ⁇ m in order to maintain lubricity and corrosion resistance.
  • the upper limit of the film thickness differs depending on the type and design of the OCTG threads, and the gaps between the box threads and the pin threads. For this reason, although it is difficult to generalize, the upper limit is set to 150 ⁇ m. Since many oil country tubular goods screws are designed with an upper limit of 100 ⁇ m to 150 ⁇ m for the gap between threads, 150 ⁇ m is defined as the upper limit. More preferably, the film thickness is 10 to 50 ⁇ m.
  • the gap between the peaks and valleys of the male and female threads may be 100 to 150 ⁇ m as described above.
  • the clearance between the male threads, the stubbing flanks of the female threads, and the clearance between the load flanks change during tightening and loosening.
  • the film thickness is preferably in the range of 10 ⁇ m to 50 ⁇ m.
  • the pencil hardness of the solid lubricating coating mentioned above shall be measured by the method specified in JIS K 5600-5-4 (1999).
  • the JIS standard clearly states that this standard is a translation of the "ISO/DIS 15184, Paints and varnishes - Determination of film hardness by pencil test” standard.
  • the pencil hardness test method itself was evaluated based on the JIS standards.
  • the reason why the film hardness was evaluated in terms of pencil hardness is the evaluation of "scratching" with a pencil. This is because the film hardness evaluation method is caused by "scratching", which is similar to the peeling behavior of the solid lubricating coating on the male and female threads of oil country tubular goods.
  • the film hardness measurement method, Rockwell, Vickers, Shore, and Knoop caused by indentation which may be used in coating films, etc., has a thin coating film and is affected by the substrate, so pencil hardness is used in this disclosure. .
  • the metallic material or the oil country tubular good is carbon steel or low alloy steel
  • an underlying layer composed of an electroplating film or a chemical conversion treatment film exists between the metallic material or the oil country tubular good and the solid lubricating coating.
  • the metal material or the oil well pipe is stainless steel material, Ni-based alloy, or Ti alloy
  • an electroplating film exists as a base layer. This is for enhancing the adhesion of the solid lubricating coating.
  • ⁇ Method for producing solid lubricating coating> It is possible to apply a desired thickness at once and to form a film by baking or the like. However, preferably, it is the method of dividing into several times and forming a film. Furthermore, it is preferable to do the following instead of performing main baking each time a film is formed. That is, the film thickness of the solid lubricating coating to be formed at one time is set to 50 ⁇ m or less, and the film formation is repeated multiple times, with a provisional drying step interposed every time or about once every two times between film formations. Then, a film having a thickness of 50 ⁇ m or less is deposited. Then, in the final film formation, temporary drying is stopped and drying is performed in the main drying process.
  • the main drying step baking, infrared irradiation, ultraviolet irradiation, drying means such as hot air, or means such as leaving in the air or natural drying is employed. It is preferable to adjust the final total film thickness of the solid lubricating coating to be 10 to 150 ⁇ m.
  • a film is formed by using a chemical obtained by dissolving a solid lubricant mainly composed of graphite and a binder resin mainly composed of PEEK resin in a solvent.
  • the drug of the present embodiment contains more film components than the solvent and is highly viscous. Therefore, when a film is formed to the desired thickness at one time, surface tension along the OCTG thread structure causes the liquid to be pulled at the corners of the threads, resulting in a lesser thickness. Liquid tends to accumulate at the corners. Therefore, it is better to divide into several times, and to carry out film-forming and baking. However, when the main firing is repeated several times, the adhesion between the films tends to be weak and the layers tend to separate easily. For this reason, calcination is performed in a state in which some of the components of the solvent are blown off. Then, the process of coating and pre-baking is repeated.
  • the pre-drying step refers to drying that only evaporates a portion (eg, 30% to 70%) of the solvent. Moreover, from the viewpoint of anticorrosiveness, it is more difficult to form a pinhole through the entire film when the film is formed multiple times, and this is also advantageous.
  • the solid lubricating coating of this embodiment is used by forming the solid lubricating coating on either or both of the coupling side (female thread side) and the pin side (male thread side) in the oil country tubular goods screw.
  • the solid lubricating coating of this embodiment is formed on either the coupling side (female thread side) or the pin side (male thread side), and the other fastening surface has a different type of solid lubricating coating from the solid lubricating coating.
  • a softer film is formed and used.
  • the hardness of the separate soft film formed on the side on which the solid lubricating coating of the present embodiment is not formed is 4B or less in pencil hardness. The latter is a way to improve the lubricating properties even further.
  • the lubricating properties will be further improved by making one of the films softer than the film of the present disclosure and making them face each other.
  • the soft coating deforms itself when a spike-like torque is applied during tightening and untightening (Phase 1: area (x) in Fig. 4) with rattling until the screws are engaged. , can be expected to reduce the surface pressure.
  • the hard coating of the present disclosure which is mainly composed of graphite and PEEK, can be expected to provide high lubrication throughout the tightening and loosening of screws.
  • the following film may be used for a soft film having a pencil hardness of 4B or less.
  • the soft film is the solid lubricating coating.
  • the soft membrane does not cover grease-like compounds or similar liquid, semi-solid, or viscoelastic membranes. In other words, the present disclosure excludes soft membranes that may come off when touched.
  • a soft film having a pencil hardness of 4B or less meaning 4B, 5B, 6B, .
  • the soft membrane may consist of a dry alkaline soap layer (top layer of Bonderube membrane) or the like.
  • the soft film When the soft film is made of a resin film, it can be made of any kind of resin, such as epoxy resin, acrylate resin, polyester resin, polyether resin, polycarbonate resin, fluorine resin, water-based acrylic resin, and the like.
  • resin such as epoxy resin, acrylate resin, polyester resin, polyether resin, polycarbonate resin, fluorine resin, water-based acrylic resin, and the like.
  • it is necessary to widen the distance between the cross-linking points so that these resins do not become hard, and to design the film so that it does not have three-dimensional complex cross-linking points. good to do
  • a simple crosslinked structure can provide a softer film than a film having three-dimensionally complex crosslinked points.
  • the flexible film it is preferable to select monomers with a small number of functional groups and a small number of epoxy groups for each of the monomers constituting the flexible film. That is, it is preferable to select one having a large functional group equivalent and epoxy equivalent.
  • the epoxy equivalent is a numerical value obtained by dividing the molecular weight of each monomer by the number of functional groups in the monomer that contribute to the cross-linking reaction. That is, it is synonymous with reducing cross-linking points.
  • the lower limit of the hardness of the soft film is not specified, it is defined as the lower limit for measuring up to 6B in the pencil hardness standard. do. However, excluding liquid, semi-solid and viscoelastic properties, the lower limit may be 8B in terms of pencil hardness as long as the level of the film is recognized as a solid lubricating film. That is, when pencils of 7B to 10B are used for measurement, the pencil hardness is out of the standard, but about 8B can be defined as the lower limit.
  • This embodiment defines each material from the viewpoint of realizing lubricating properties that can withstand the environment that may occur in an actual well. Moreover, when specifying the upper and lower limits, confirmation (testing) was carried out under conditions that conformed to the tightening and loosening conditions in actual wells, and these were determined. In the method using horizontal and vertical power tongs using short pins, as in normal laboratory tests, the tightening and unfastening conditions do not conform to the actual well conditions, and in the case of a solid lubricating film, the evaluation is loose. becomes a condition. For this reason, it is meaningless to explain the upper and lower limits of each material by evaluating them in a normal laboratory test.
  • a test was performed with the apparatus configuration shown in FIG. 5 based on the above new laboratory test conditions.
  • we will basically evaluate under conditions that can be realized, such as a large load during tightening and an unbalanced load during tightening and untightening. For example, in the case of a process in which screws are tightened by applying a large load equivalent to that of an actual size pin, rattling until the screws engage with each other is taken into consideration. Also, in the case of the process of loosening the screws, the fact that the screws are disengaged from each other and cause rattling is reflected.
  • the new lab test uses the vertical power tongs 4. Also, a short pin 1 is employed as a test pin. However, a load can be applied to the upper part of the pin 1 by the weight 3 and the load can be removed. The thread of the short pin 1 and the thread of the box 2 are tightened by the pin threaded portion 1a and the box threaded portion 2a. At that time, in order to simulate a situation in which the threads do not mesh, the initial temporary tightening position is set so that the pin thread 1a is exposed from the box 2 to half the total number of threads. (See FIG. 2(b)). This is one of the causes of rattling. Start tightening from that state.
  • a weight 3 When tightening, a weight 3 is attached to the end of the pin 1 opposite to the tightening screw of the box 2 .
  • the weight of the weight 3 is a load corresponding to one to three actual size pins, which is calculated based on the pin's outer diameter and wall thickness. 9-5/8"53.5# is about 1t load (2,200Lb) per one, and about 3 tons (6,600Lb) if three are connected.
  • the weight 3 illustrated in FIG. 5 consists of a weight main body 3A and an insertion rod 13 as shown in FIG.
  • the insertion rod 13 is welded to the lower surface of the weight body 3A and arranged at an axially symmetrical position with respect to the weight 3.
  • the weight is attached to the pin by loosely inserting the insertion rod 13 into the pin 1.
  • ⁇ Reference numeral 1c denotes an inner diameter surface of the pin 1.
  • the insertion rod 13 and the pin 1 are previously provided with holes 1d and 13a through which the pin 1 and the insertion rod 13 are inserted when the weight 3 is attached as described above. Then, as shown in FIG. 6, the weight 3 and the pin 1 are integrated by inserting the through rod 12 into the holes 1d and 13a.
  • a swivel-type hook 11 is welded to the axial center position of the upper part of the weight 3, and the weight 3 is hung from a hanging device 20 on the ceiling via a hanging chain 21. - ⁇ As a result, by adjusting how the weight is lifted by the suspension device 20, the magnitude of the load of the weight on the pin can be adjusted.
  • the secondary product is a product of components derived from the solid lubricating coating that is released into the screw gap due to unavoidable flaking or the like.
  • the upper and lower limits of the parameters relating to the solid lubricating coating can be defined in accordance with the actual well conditions.
  • the components and others are specified in order to realize lubricating properties that can withstand the environment that may occur in an actual well. Moreover, when specifying the upper and lower limits, they were determined by confirming conditions that conformed to the tightening and loosening conditions in actual wells.
  • PEEK resin which has hardly been used in combination with graphite, was selected.
  • PEEK resin which has hardly been used in combination with graphite.
  • the present embodiment achieves high lubrication.
  • high lubrication can be achieved by eliminating seizure or lubrication instability that was conventionally unavoidable when graphite was selected as a solid lubricant component. become.
  • corrosion resistance can also be achieved in this embodiment.
  • the application may be expanded to metal materials in addition to the lubrication of oil country tubular goods threads.
  • not only membranes, but also drugs for making membranes are targeted.
  • the present disclosure can also take the following configurations.
  • solid lubricants include BN (boron nitride), mica (mica), talc, MCA (melamine cyanurate), MoS2 (molybdenum disulfide), PTFE (polytetrafluoroethylene), PFA (perfluoroalkoxyalkane tetrafluoroethylene/perfluoroalkoxyethylene copolymer resin), FEP (perfluoroethylene propene copolymer; tetrafluoroethylene/hexafluoropropylene copolymer), including a solid lubricant made of one or more materials selected from the above
  • the binder resin contains PEEK resin having an average particle size of 20 ⁇ m or less as a main component, and contains 70% or more of the total weight of the binder resin.
  • the total weight of the solid lubricant is 0.1 to 2 times the total weight of the binder resin, and the content of graphite as the solid lubricant is the total weight of the solid lubricant. It is 20% or more and 50% or less of the total weight of the binder resin.
  • a solvent is contained, and the weight ratio of the solvent is 30% or more and 80% or less with respect to the total weight of the total weight of the solid lubricant and the total weight of the binder resin.
  • At least PTFE is included as the other solid lubricant, and the average particle size of the PTFE is in the range of 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the solid lubricating coating is formed by dispersing a solid lubricant in a binder resin, and as one of the two or more types of solid lubricants, graphite is added in an amount of 50% or more of the total weight of the solid lubricant and 90 % or less, the graphite has a scale-like shape and an average particle size of 10.0 ⁇ m or less, and further, as another solid lubricant among the two or more types of solid lubricants, BN (boron nitride) , mica (mica), talc, MCA (melamine cyanurate), MoS 2 (molybdenum disulfide), PTFE (polytetrafluoroethylene), PFA (perfluoroalkoxyalkane; tetrafluoroethylene/perfluoroalkoxyethylene copolymer resin ), a solid lubricant made of one or more materials selected from FEP (perfluoroethylene propene copolymer;
  • the total weight of the solid lubricant is 0.1 to 2 times the total weight of the binder resin, and the content of graphite as the solid lubricant is the total weight of the solid lubricant. It is 20% or more and 50% or less of the total weight of the binder resin.
  • At least PTFE is included as the other solid lubricant, and the average particle size of the PTFE is in the range of 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the solid lubricating coating includes the threads of the threaded portion and is formed up to a region adjacent thereto. (9) The solid lubricating coating has a pencil hardness of 3H or more. (10) The thickness of the solid lubricating coating is 10 ⁇ m or more and 150 ⁇ m or less.
  • the material of the oil country tubular good is carbon steel or low-alloy steel, and the lubricating coating has an underlayer between the fastening surface of the threaded portion and the solid lubricating coating, and the underlayer comprises: It consists of an electroplating film or a chemical conversion treatment film.
  • the material of the oil country tubular good is a stainless steel material, a Ni-based alloy, or a Ti alloy, and the lubricating coating has a base layer between the fastening surface of the threaded portion and the solid lubricating coating, The underlying layer is made of an electroplated film.
  • a threaded joint for oil country tubular goods in which a box having a female thread and a pin having a male thread are connected, wherein at least one of the box and the pin is an oil country tubular good having the lubricating coating of the present disclosure.
  • An oil well pipe threaded joint made of pipes.
  • a lubricating coating comprising the solid lubricating coating is formed on the fastening surface of the threaded portion of one of the box and the pin, and the threaded portion of the other of the box and the pin is fastened.
  • a film softer than the solid lubricating coating is formed on the surface.
  • the soft film has a film hardness of 4B or less in pencil hardness.
  • the film forming step of applying the chemical described above to form a solid lubricating coating having a film thickness of 50 ⁇ m or less is replaced by a temporary drying step.
  • the total film thickness of the solid lubricating coating is adjusted to 10 ⁇ m or more and 150 ⁇ m or less by drying means, leaving in the atmosphere, or natural drying means.
  • Judgment criteria are as follows.
  • the casing size was judged to be acceptable if tightening and untightening were performed 3 times or more, and that if it was possible to tighten and untighten 5 times, it was considered superior.
  • a tubing size of 5 times or more was judged as acceptable, and a tubing size of 10 times or more was evaluated as excellent.
  • the regulation of the casing size is in line with the regulation of ISO13679. Tubing, on the other hand, was considered acceptable from 5 times or more, which is lower than the ISO 13679 specification.
  • weights based on the condition that multiple connected loads were applied, heavy weights with good sharpness were adopted in units of MKS, such as 1 ton, 1.5 ton, 2 ton, and 3 ton. Then, the weight was attached to the top of the pin screw (see FIG. 5). The initial tightening position is tightened only to the point where half of the total number of pin threads is exposed to the box screw, that is, the threads do not mesh with each other (the position where the threads are half exposed). carried out. That is, this example was carried out using the apparatus shown in FIGS.
  • Example 1 describes lubrication property evaluation using weight tongs. Tables 1 to 6 describe the conditions and evaluation results of each example.
  • a solid lubricating film is also called a coating film.
  • the graphite was used as the main component of the solid lubricant, and the graphite used was scale-like (flake-like grade) with an average particle size of 5 ⁇ m or 10 ⁇ m.
  • the binder resin used was PEEK resin having an average particle size of ⁇ 1 ⁇ m. Then, the film thickness of the solid lubricating coating was formed to be 50 ⁇ m.
  • No. 2-4 and 10 are examples of graphite content in the preferred range. In both cases, the number of tightening and unfastening times exceeded the acceptance criteria.
  • No. 2 to 4 and 10 are cases where the graphite content is not 100%, used in a mixed state with other solid lubricants, and the required amount of graphite is 50% or more. As a result, it seems that high lubrication and a state in which "black tape-like secondary products" are difficult to clog were achieved.
  • No. 11 is an example with 40% graphite content, which is less than the scope of this disclosure.
  • No. No. 11 is an example in which the lubricity of graphite was not fully utilized and seizure occurred due to insufficient lubricity.
  • No. 4 to 6 are cases in which PTFE was used as a secondary solid lubricant and the particle size of the PTFE was changed. No. From 4 to 6, both when the PTFE grain size is 10 ⁇ m and when it is 5 ⁇ m, the number of times of tightening and unfastening is within the acceptable range. However, when the thickness is 10 ⁇ m, compared with 5 ⁇ m, there is a tendency that the lubricity is beginning to decline slightly. That is, it can be seen that a PTFE particle size of up to 5 ⁇ m is preferable.
  • No. 4, 8 and 9 are comparative examples of graphite shapes and grades.
  • No. No. 7 is obtained by adding glass fiber in addition to PTFE as another additive of the solid lubricant.
  • No. 7 is a case where the addition of glass fiber made the film quality hard (pencil hardness: 7H), and in particular, the number of times of tightening and unfastening was not a problem, but rather improved.
  • No. 12-20 are steel grade: carbon steel sour resistant material C110, the thread size is 9-5/8"53.5# and the threads were implemented using JFELION TM .
  • a weight of 3 tons was used as the weight for the weight tong test described above, and evaluation was performed under conditions assuming that three actual long pins are connected.
  • On the coupling side a base layer and a solid lubricating coating were formed in this order on the fastening surface as the lubricating coating.
  • the base layer was a Mn phosphate chemical conversion treatment layer.
  • the solid lubricating coating on the coupling side graphite was used as the main component of the solid lubricant, scaly (flaky grade) was selected as the graphite, and BN was used as the secondary solid lubricating component.
  • the main component of the binder resin is a PEEK resin.
  • the fastening surface on the pin side was formed with a solid lubricating coating composed of metal soap (calcium stearate) dispersed in fluororesin as a binder resin on the shot-blasted surface.
  • No. 12 to 20 look at the average particle size of graphite, the particle size of PEEK resin, and the possibility of secondary resin components mixed with PEEK resin.
  • No. 13 and 16 are examples in which the average particle size of graphite is 20 ⁇ m and 25 ⁇ m, respectively, and are cases exceeding the upper limit of 10 ⁇ m of the present disclosure.
  • No. 13 and 16 are cases where the number of times of tightening and unfastening is less than acceptable.
  • No. In Nos. 13 and 16 "a black tape-like secondary product" was likely to appear, and seizure occurred. In addition, the damage due to seizure was accumulated and seizure occurred early.
  • No. 14 to 17 are examinations of the conditions under which secondary resin components are mixed into the PEEK resin. No. 14 to 17, if the PEEK resin content is 70% or more, for example, even if the solid lubricating coating is composed of a composite resin coating containing epoxy resin, PEKK resin, PAEK resin, etc., other If the specified items are within the target specified range, it can be seen that the number of times of tightening and unfastening is acceptable.
  • No. No. 15 is a comparative example, which is an example of conditions in which 60% of PEEK resin and 40% of PE resin (polypropylene) and PE resin (polyethylene) are mixed. No. In 15, the PEEK resin content was below specification and a soft resin was added. For this reason, No. In No. 15, the pencil hardness of the solid lubricating coating was also lower than specified, and the number of tightening and unfastening times fell below the acceptable level.
  • No. No. 17 is also a case reinforced with carbon fiber, and is a case in which the number of times of tightening and unfastening is even better.
  • No. 17 it is presumed that the hardened film quality reduced the peeling of the solid lubricating coating itself, and as a result, reduced the amount of "black tape-like secondary product".
  • No. No. 19 is a comparative example in which the average particle size of the PEEK resin is 25 ⁇ m, which exceeds the scope of the present disclosure. No. 19, the number of times of tightening and unfastening is less than the acceptance criteria. No. 19 shows that lubrication also deteriorates when the particle size of the PEEK resin is too large.
  • No. No. 20 is an example in which the graphite weight is 25%, which is below the lower limit of 50% of the present disclosure, and graphite is not the main component of the solid lubricant.
  • No. No. 20 seems to have less "black tape-like secondary product" due to less graphite. Moreover, even without it, it is burned.
  • Examples 21-29 are steel grade: carbon steel material Q125, screw size is 5.5"23#, and the screw was performed by JFELION TM . Evaluation was made under conditions assuming a situation in which a 1-ton one was used and a little less than three actual length pins were connected.
  • a base layer and a solid lubricating coating were formed in this order on the fastening surface as the lubricating coating.
  • the base layer was a Mn phosphate chemical conversion treatment layer.
  • graphite was selected as the main component
  • scaly graphite (flake-like grade) was selected
  • PTFE was selected as the secondary solid lubricating component.
  • the main component of the binder resin is a PEEK resin.
  • a solid lubricating coating was applied to the shot-blasted surface using fluororesin as a binder resin and PMSQ (polymethyl silsesquioxane) as a solid lubricant.
  • No. Cases 21 to 27 are for examining the film thickness of the solid lubricating coating.
  • No. 21 to 27 it was found that excellent number of times of tightening and undoing was exhibited within the film thickness range of 10 ⁇ m to 150 ⁇ m.
  • No. 21 to 27 it was found that lubrication (number of times of tightening and unfastening) was particularly excellent when the film thickness was in the range of 10 to 75 ⁇ m. Also, No.
  • No. Example 28 is an example in which the solid lubricating coating on the pin side and the solid lubricating coating on the coupling side are exchanged.
  • No. No. 29 is an example in which a solid lubricating coating mainly composed of a combination of graphite and PEEK resin is formed on both the pin side and the coupling side.
  • No. No. 29 has the number of times of tightening and unfastening. Compared to No. 24 and 28, it is slightly degraded, but it sufficiently shows the pass judgment value.
  • No. 30 to 34 are steel grade: carbon steel material Q125, screw size is 9-5/8"47#, and screws are made by JFELION TM .
  • Nos. 30 to 34 are weights It was used as a 3 ton, and was evaluated in a new laboratory test under the conditions assuming the connection of three actual length pins.
  • a base layer and a solid lubricating coating were formed in this order on the fastening surface as the lubricating coating.
  • the base layer was a Mn phosphate chemical conversion treatment layer.
  • the main component of the solid lubricant was used as the main component of the solid lubricant, scaly (flaky grade) was selected as the shape of the graphite, and PTFE was selected as the secondary solid lubricating component.
  • the main component of the binder resin is a PEEK resin. This is an example of forming a solid lubricating coating on the fastening surface of the pin, the binder resin being water-based acrylic resin and the solid lubricant being aluminum powder, on the shot blasted surface.
  • No. 35-36 relate to the application to stainless steel materials.
  • No. No. 35 is also an example in which glass fiber is added to increase film hardness.
  • the embodiments described above are examples using oil country tubular goods screws. In lubrication, it is not only the lubrication behavior that starts when the two objects to be rubbed come into contact with each other, but also the lubricating film is severely lubricated, including peeling and partial breakage, depending on the material to be rubbed, when the screws are not meshed. An example of conditions is shown.
  • the present disclosure can also be applied to lubrication that starts when two objects to be rubbed contact each other, and as long as this lubricating film structure is used, it can be applied to materials other than oil country tubular goods screw materials and application fields without limitation. is.
  • Example 2 evaluates the anticorrosion property by a salt spray test. Among the cases shown in Tables 1 to 6, No. Constructions 3, 10, and 22 were evaluated with salt spray. These cases are for carbon steel-based OCTG thread conditions. In Example 2, a new solid lubricating coating was formed on a new coupling sample for this salt spray test.
  • an SPCC ordinary thin steel sheet/cold-rolled annealed sheet of general mild steel
  • a thickness of 0.8 mm was also used.
  • both ends of the coupling screw were tightened and loosened once with a protector.
  • a salt spray test was carried out for the case where the protector was attached as it was and the case where the protector was attached again (corresponding to the second tightening), and it was evaluated after arranging them side by side for a predetermined time (meaning that they could not stand up).
  • the outer side of the coupling material was covered with imide tape for protection. Detailed conditions are as follows.
  • Spraying conditions JIS K 5600-7-1 Salt water concentration: 5 ⁇ 0.5 wt% Temperature: 35°C Humidity: 98-99% Amount of spray: 1-2ml/hr/80cm 2 pH: 6.5-7.2 Time: 24 hours
  • the SPCC plate was cut into a size of 75 mm x 150 mm as a sample, and No. 2 was marked on the surface.
  • the same film as 3 was formed. That is, after the Mn phosphate treatment, a chemical agent was applied and baked to form a solid lubricating coating. Also, two samples were prepared and one side was protected with an imide tape. Furthermore, the back side (test object side) to which the overall protective film was adhered was also sampled with an imide tape adhered 1 mm from the edge. One of the two was cross-cut with a cutter knife (No. A), and the other was used as a sample as it was (No. B).
  • No. 3-10, and 22 after tightening once with a protector, tightening it back, tightening it again, attaching a protector, and spraying salt water (No. 3-2, 10-2, 22-2), After tightening and untightening once, the samples (Nos. 3-3, 10-3, and 22-3) which were directly sprayed with salt water were evaluated.
  • No. 3-4 is an example in which the salt spray test is performed as it is without tightening and untightening with the protector.
  • Comparative example No. A is SPCC thin steel plate No. This is an example in which the solid lubricating coating of No. 3 is formed, cross-cut, and the coating is scratched so that the scratches reach the substrate. Comparative example No. In A, rust was observed at the cross-cut portion. On the other hand, the film itself, which was not cross-cut, had excellent corrosion resistance and no corrosion was observed. No. 3-2 to 3-4, No. 10-2 to 10-3, No. All of 22-2 to 22-3 remained sound and no corrosion was confirmed. This indicates that the solid lubricating coating of the present disclosure is also excellent in corrosion resistance.
  • Graphite itself and PEEK resin itself are water repellent and have excellent corrosion resistance.
  • the solid lubricating coating is hard enough not to be broken under conditions such as tightening and untightening the proctator. For this reason, even minute cracks were not formed, so it is considered that such corrosion resistance is exhibited.
  • the point is that the No. 1 cross-cut was made on the membrane with a cutter knife.
  • Condition A is an impossibly too severe condition for a solid lubricating film, and shows that the film is not destroyed even at the level of tightening and untightening with a protector. At the same time, it has been found that good corrosion resistance is exhibited if a solid lubricating coating of this composition is formed.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Emergency Medicine (AREA)
  • Health & Medical Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)
  • Non-Disconnectible Joints And Screw-Threaded Joints (AREA)
  • Paints Or Removers (AREA)
PCT/JP2022/021279 2021-05-31 2022-05-24 固体潤滑被膜形成用の薬剤、油井管、油井管ねじ継手、及び油井管の製造方法 Ceased WO2022255167A1 (ja)

Priority Applications (6)

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US18/564,142 US12312552B2 (en) 2021-05-31 2022-05-24 Agent for forming solid lubricating coating film, oil country tubular goods, threaded joint for oil country tubular goods, and method for manufacturing oil country tubular goods
CN202280038745.XA CN117413040B (zh) 2021-05-31 2022-05-24 固体润滑被膜形成用试剂、油井管、油井管螺纹接头和油井管的制造方法
JP2022550248A JP7241249B1 (ja) 2021-05-31 2022-05-24 固体潤滑被膜形成用の薬剤、油井管、油井管ねじ継手、及び油井管の製造方法
MX2023014265A MX2023014265A (es) 2021-05-31 2022-05-24 Agente para la formacion de una pelicula solida de recubrimiento lubricante, articulos tubulares para la industria petrolera, union roscada para articulos tubulares para la industria petrolera y metodo para la fabricacion de articulos tubulares para la industria petrolera.
BR112023024971A BR112023024971A2 (pt) 2021-05-31 2022-05-24 Agente para formação de filme de revestimento lubrificante sólido, produtos tubulares para campos petrolíferos, junta roscada para produtos tubulares para campos petrolíferos, e método para fabricação de produtos tubulares para campos petrolíferos
EP22815917.4A EP4332202A4 (en) 2021-05-31 2022-05-24 Chemical substance for forming solid lubricant coating film, oil well pipe, screw-threaded joint for oil well pipes, and method for manufacturing oil well pipe

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JP2021091462 2021-05-31
JP2021-091462 2021-05-31

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CN117413040A (zh) 2024-01-16
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