JP6018576B2 - Process for coating threaded tubular component, threaded tubular component and method for manufacturing the same, and threaded tubular connection - Google Patents

Description

  The present invention relates to tubular components used for drilling and working in hydrocarbon wells, and more precisely to the screw ends of the components, where the ends are male or female and the correspondence of another component The connection part can be formed by connecting to the terminal.

  The invention further relates to a process for producing an abrasion resistant film on the tubular component.

  “Used for drilling and working with hydrocarbon wells” refers to a string or maintenance riser (workpiece) for drilling hydrocarbon wells connected to another element of the same or different type Also known as an over riser) or a tube that is substantially tubular in shape, intended to ultimately constitute either a riser or other work string or a casing string or tubing string used in well work Means any element. The invention is further applicable to components used in drill strings such as drill pipes, heavy drill pipes, drill collars and pipe joints known as tool joints and heavy pipe parts.

  Each tubular component includes only one end with a male threaded region and / or one end with a female threaded region, each threadedly engaged with a corresponding end of another component that is an assembly defining a connection. Intended to be connected.

  Taking into account that a threaded tubular component can undergo several assembly-disassembly cycles in the well, the threaded tubular component is connected under a given stress to meet the tightening and sealing requirements imposed by the conditions of use. .

  Depending on the conditions in which the threaded tubular component is used, various types of stress occur, which necessitates the use of a coating on the sensitive part of the component, such as the threaded area, adjacent portion or sealing surface.

  The screwing operation is generally carried out under the weight of a pipe of several meters in length connected by a screw connection, which can be limited by high axial loads, e.g. a slight displacement of the axis of the screw element to be connected, This induces a risk of wear at the threaded area and the metal / metal sealing surface. For this reason, it is necessary to coat the threaded area, the adjacent surface and the metal / metal sealing surface with a lubricant.

  Furthermore, threaded tubular components are assembled in harsh environments after being stored (possibly for several years). For example, offshore with salt spray or on land where sand, dust or other contaminants are present. Therefore, it must be coated against corrosion on cooperating surfaces by screwing (screw area) or interference contact (metal / metal sealing surface). Furthermore, surface treatment against corrosion is also necessary.

US Patent Application Publication No. 4822081 US Reissue Patent Application No. 30467 US Reissue Patent Application No. 34467 International Publication No. 2008/032872

D Kuhlmann-Wilsdorf et al, “Plastic flow between Bridgman anvils under high pressures”, J. Mater. Res., Vol 6, no 12, Dec 1991

  However, using threaded grease of API (American Petroleum Institute) standard RP5A3 does not seem to be a long-term solution from an environmental point of view. This is because the grease containing heavy metal can be discharged from the tubular component and released into the environment or well, resulting in blockage and special cleaning operations. Furthermore, the grease does not sufficiently protect against corrosion and must be applied on the site for each screwing operation.

  In order to overcome the problems that require long-term corrosion resistance and wear resistance and meet environmental advantages, those skilled in the field of threaded connections are lubricants and are protected from corrosion to ensure the tubular components at the factory. Solid dry coatings (ie, not sticky or sticky like grease) have been actively developed.

  In particular, coatings have been developed that are environmentally inert and resistant to abrasion.

  The present invention uses polyaryletherketone to provide high wear resistance, anti-wear properties, high mechanical strength, low friction coefficient, and resistance to extreme hydrocarbon well working conditions. Based on findings obtained dry film. The solution used can be adapted to various grades of metal for the connection of the tubular component.

  The use of the polyaryletherketone and the properties associated with the defined threaded tubular component have not been described or suggested in the prior art.

  More precisely, the present invention relates to a threaded tubular component for drilling or working a hydrocarbon well, said tubular component having an outer circumferential surface or inner circumferential surface at one of its ends depending on whether the screw end is male or female. There is a threaded region made on the surface, and at least a portion of the ends are coated with at least one lubricating dry film comprising at least 65 weight percent polyaryletherketone.

  Any complementary or alternative characteristics are defined below.

  The polyaryletherketone is selected from polyetheretherketone (PEEK), polyetherketone (PEK) and mixtures thereof.

  The lubricated dry film has a structure with a crystallinity of 10% to 35%.

  The lubricated dry film further comprises at least one type 4 solid lubricant in a mass ratio of 10% to 35%.

  The lubricating dry film contains a perfluoroalkoxyethylene copolymer in a mass ratio of 10% to 30%.

  The lubricated dry film is a mechanical reinforcement selected from the following list of pigments: carbon black, mica, wollastonite, nanometer aluminum oxide, nanometer titanium oxide, glass powder, nanodiamond, nanometer WS2 or WS2-fullerene In a mass ratio of 1% to 15%.

  Parts coated with a lubricious dry film are from the group consisting of iron and zinc alloys deposited in advance by sanding, manganese phosphate film treatment, electrolytic deposition of copper or copper-tin-zinc alloy, and injection. A selected surface preparation step is applied.

  The part coated with the lubricious dry film is pre-coated with a semi-crystalline polyetheretherketone primer containing mica pigment.

  The entire thread area is coated with a lubricious dry film.

  The threaded tubular component includes a metal / metal sealing surface, which is coated with a lubricious dry film.

  The invention further relates to a threaded tubular connection comprising a male threaded tubular component and a female threaded tubular component combined with each other, wherein at least one said threaded tubular component is as defined above.

The invention further relates to a process for coating a threaded tubular component for drilling or working in a hydrocarbon well, said tubular component having an outer peripheral surface or one of its ends depending on whether the threaded end is male or female. There is a threaded area made on the inner surface, the process is as follows:
Producing a mixture comprising polyaryletherketone powder in a suspension in water in a proportion of 25% to 35% by weight;
Applying the mixture to the end (1, 2) portion of the threaded tubular component;
Drying the coated end (1,2) part at a temperature of 100 ° C. to 150 ° C. for 5 to 10 minutes;
Heating the coated end (1,2) portion to a temperature of 350 ° C. to 450 ° C. for 5 to 15 minutes at a rate of temperature increase of 10 ° C. to 20 ° C. per minute; and Cooling the coated end (1,2) portion to ambient temperature at a cooling rate of less than 10 ° C. to obtain a structure;
including.

  Any complementary or alternative characteristics are defined below.

  The mixture further comprises a fusing agent having a boiling point of 100 ° C. to 200 ° C. and a rapid evaporation rate in a proportion of 2.5% to 10% by weight.

  The mixture further comprises nonionic wetting and dispersing agents in proportions ranging from 2.5% to 10 weight percent.

  The mixture further comprises at least one Group 4 solid lubricant in a proportion of 3% to 12% by weight.

  The Group 4 solid lubricant is a perfluoroalkoxyethylene copolymer having a mass ratio of 3% to 12%.

  The mixture further comprises a mechanical reinforcement selected from the following list of pigments: carbon black, mica, wollastonite, nanometer aluminum oxide, nanometer titanium oxide, glass powder, nanodiamond, nanometer WS2 or WS2-fullerene. It is included at a mass ratio of 0.5% to 5%.

  The end portion is coated using a pneumatic spray system, the system diameter is 0.7-1.8 mm and the air pressure is 4-6 bar.

  A surface preparation step selected from the group consisting of sanding, manganese phosphate coating, electrolytic deposition of copper or copper-tin-zinc alloy, and particles of iron and zinc alloy deposited by injection; Before applying to said part.

  A surface preparation step consisting of priming a semi-crystalline polyetheretherketone containing mica pigment is performed before applying the mixture to the end portion.

The present invention further provides a process for coating a threaded tubular component for drilling or working in a hydrocarbon well, wherein the tubular component has one of its ends (1, 2) depending on whether the threaded end is male or female. Have threaded areas (3, 4) made on the outer peripheral surface or the inner peripheral surface, the following:
Heating the end (1, 2) portion of the threaded tubular component to a temperature of 360-420 ° C, preferably close to 400 ° C;
Injecting PEK and / or PEEK powder onto said part of the end (1, 2) of said threaded tubular component;
Maintaining the portion of the end (1,2) coated in this way at a temperature of 360 ° C. to 420 ° C., preferably close to 400 ° C. for 1 to 4 minutes; and Cooling the coated end (1,2) portion to ambient temperature at a cooling rate of less than 10 ° C. per minute;
including.

  Advantageously, a step of degreasing the coated part is carried out before heating said part.

  The characteristics and advantages of the present invention will be described in more detail in the following description with reference to the accompanying drawings.

FIG. 4 is a view of the resulting connection that connects two tubular components by assembly. FIG. 3 is a screw curve of two threaded tubular components. FIG. 2 is a diagram of a substrate coated with a lubricious dry film. FIG. 6 is a diagram of a test setup. FIG. 6 is another test setup diagram. A test curve is shown. A test curve is shown.

  The screw connection shown in FIG. 1 includes a first tubular component with a rotating shaft 10 with a male end 1 and a second tubular component with a rotating shaft 10 with a female end 2. The two ends 1 and 2 each end with a radially facing end face with respect to the axis 10 of the screw connection and are each provided with screw regions 3 and 4 which are screwed together and cooperate with each other in the connection of the two components. The screw regions 3 and 4 may be screw types such as trapezoidal and self-locking types. Furthermore, after connecting two screw components by screwing, the metal / metal sealing surfaces 5, 6 intended to come into sealing interference contact with each other are male and female close to the screw regions 3, 4 respectively. Provided on the end. Finally, the male end 1 ends with an end face 7 adjacent to the corresponding surface 8 provided on the female end 2 when the two ends are combined with each other.

  The Applicant has also foreseen other structures in which the adjacent formed by the two contact surfaces 7 and 8 is replaced by a self-locking clamping cooperation of the screw regions 3, 4 (Patent Document 1, (See Patent Document 2 and Patent Document 3).

As can be seen in FIGS. 1 and 3, at least one threaded tubular connection is coated with a lubricious dry film 12 comprising at least 65 weight percent polyaryletherketone throughout the terminal 1 portion of the substrate 11, and The film 12 has a structure with a crystallinity of at least 10%. It will be recalled that crystallinity can be measured by polymer fusion or crystallization enthalpy (ΔΗ ⁰ ). The theoretical fusion enthalpy of fully crystalline polyaryletherketone, especially polyetheretherketone (PEEK), is 122 J / g according to Hay and Coll (Polymer Communications, 1984, 25, 175-178). The presence of at least 10% crystallinity has the advantage of excellent mechanical properties and particularly good shoulder torque resistance. However, it is preferred to keep the crystallinity below 35% and preserve the film properties for surface preparation adhesion and protection against corrosion.

  The polyaryl ether ketone used in the present invention is obtained from an aqueous polyether ether ketone dispersion or an aqueous polyether ketone dispersion. The aqueous dispersions are muscovite and / or black composed of organic or inorganic mechanical reinforcing agents such as aluminum silicate and hydrated potassium or magnesium, gamma crystal structure and amorphous aluminum oxide with a particle size of 20-300 nm. Mica-type mica pigment, titanium dioxide pigment with particle size of 10-100 nm, perfluoroalkoxyethylene copolymer resin (PFA), amorphous carbon black pigment, synthetic graphite powder with diameter less than 5 μm, particle size obtained by detonation Is nanodiamond powder of 4-6 nm, fiber thickness is 1-1.3 μm, C-type glass with diameter D90 <50 μm, WS2 fullerene nanomaterial with particle size of 80-220 nm or particle size D50 = 55 nm WS2 tungsten disulfide Mera pigment may include.

  Polyetheretherketone (abbreviation PEEK) and polyetherketone (abbreviation PEK) are obtained by a nucleophilic substitution type synthetic route. As a result of the polyetherification, a hard semicrystalline polymer having a high melting point is obtained. They fall into the category with the best performance materials in the thermoplastic material group. Their glass transition temperature is 143 ° C. and they are semi-crystalline, so they retain their excellent mechanical properties up to a melting point of 343 ° C .. The quasi-linear and aromatic structures provide PEEK and PEK with excellent long-term thermal stability.

  The molecular structure of polyetheretherketone is as follows:

ポリエーテルケトンの分子構造は以下のとおりである：

The molecular structure of polyetherketone is as follows:

ガラス転移温度が１５７℃、融点が３７４℃で、ポリエーテルケトン（ＰＥＫ）は、ポリエーテルエーテルケトン（ＰＥＥＫ）と比較して、剛性、固体性及び耐薬品性等で同様の利点を全て有しつつ、高温で性能が拡張する。

With a glass transition temperature of 157 ° C and a melting point of 374 ° C, polyether ketone (PEK) has all the same advantages in terms of rigidity, solidity and chemical resistance, etc., compared to polyether ether ketone (PEEK). However, the performance expands at high temperatures.

  The continuous use temperature is 240 ° C., and the load deformation temperature exceeds 300 ° C. for reinforcement grades PEEK and PEK compared to other polymers.

  PEEK has high mechanical properties that hold it up to 250 ° C. for tensile strength and 300 ° C. for bending strength. The mechanical properties are greatly improved by incorporating 10-30% solid lubricants such as graphite, carbon black, fluorinated PTFE type polymers or perfluoroalkoxyethylene (PFA) type resins or glass fibers. The

  PEK retains its mechanical and physical properties at temperatures above 30 ° C. higher than PEEK, while being permanently deformed and adapting to higher loads up to 3 times higher than PEEK at high temperatures.

  PEEK and PEK are particularly resistant to saturated salt solutions, gaseous hydrogen sulfide at 200 ° C., and further resistant to hydrolysis at 200 ° C. under 1.6 MPa, comparable to fluorinated polymers. There is also temperature resistance. Table 1 clearly shows the superior mechanical properties of PEEK and PEK compared to fluorinated polymers (PTFE and PFA).

ＰＥＫ及びＰＥＥＫについて様々な実施が可能であるが、３７０℃〜４２０℃の温度で融解させる変換を含む。堆積は、静電粉末射出、水性分散液の噴霧及び熱射出により実施できる。ＰＥＥＫ及びＰＥＫは腐食に対して融解状態では感受性でない。しかし、分解を触媒してコーティングが酸化に対して耐性の低い、（例えば、１３％のクロムを含むある等級のマルテンサイトステンレス鋼において）銅又はクロムを含有する合金から形成される型に汚染されうる。全体として、融解による変換後、ＰＥＫ及びＰＥＥＫは特に金属があまり研磨されていない場合に金属によく接着する。許容される粗度はドライフィルムの所望の厚さ全体の２０％〜２５％である。接着は、下塗りを接着促進剤として用いて、又は機械的摩耗（サンディング又はショットブラスティング）による表面処理を用いて、クロム酸中での媒染により、若しくは空気あるいはＯ₂タイプの酸化剤さらにＮＨ₃タイプの還元剤でのプラズマ処理により、増大させうる。同時に、ほとんど全ての金属の表面酸化により重合体の接着が低下する傾向がある。支持体の表面エネルギーを変えないため、金属を不活性雰囲気中で又は誘導により加熱しなければならないことが明らかである。最後に、冷却により再結晶が良好に得られ、重合体の内因的特性、例えば耐摩耗性及び耐ひっかき性を保存するために十分遅くなければならない。急速冷却で、当該部分を２００℃で３０分間アニーリングすると依然として再結晶化しうるアモルファスコーティングが生成されるであろう。例えば、４００℃から２５０℃まで１０℃／分の冷却速度、その後３０分〜１時間２５０℃での一定温度段階が続くよう制御された冷却プロセスで結晶化度を高めて、重合体の機械的特性を高め得る。

Various implementations are possible for PEK and PEEK, including transformations that melt at temperatures between 370 ° C and 420 ° C. Deposition can be performed by electrostatic powder injection, aqueous dispersion spraying and thermal injection. PEEK and PEK are not sensitive to corrosion in the molten state. However, catalyzing decomposition, the coating is less resistant to oxidation and is contaminated with molds formed from copper or chromium containing alloys (eg, in certain grades of martensitic stainless steel containing 13% chromium). sell. Overall, after conversion by melting, PEK and PEEK adhere well to the metal, especially when the metal is not very polished. Acceptable roughness is 20% to 25% of the overall desired thickness of the dry film. Adhesion can be achieved by using a primer as an adhesion promoter, or by surface treatment by mechanical abrasion (sanding or shot blasting), by mordanting in chromic acid, or by air or an O ₂ type oxidant and NH ₃ It can be increased by plasma treatment with a type of reducing agent. At the same time, polymer adhesion tends to decrease due to surface oxidation of almost all metals. It is clear that the metal must be heated in an inert atmosphere or by induction in order not to change the surface energy of the support. Finally, good recrystallization is obtained by cooling and must be slow enough to preserve the intrinsic properties of the polymer, such as abrasion resistance and scratch resistance. With rapid cooling, annealing the part at 200 ° C. for 30 minutes will produce an amorphous coating that can still be recrystallized. For example, the crystallinity can be increased by a controlled cooling process from 400 ° C. to 250 ° C. at a cooling rate of 10 ° C./min, followed by a constant temperature step at 250 ° C. for 30 minutes to 1 hour, Can enhance the properties.

  In the first stage, the applicant has to increase at least one solid lubricant, preferably a fluorinated polymer of perfluoroalkoxyethylene copolymer resin type and / or polishing resistance to enhance the wear resistance. It was investigated to obtain a polyaryletherketone coating from an aqueous suspension of polyetheretherketone sold under the name Vicote F800 series from Victrex, which contains at least one inorganic carbon black type solid compound. The physicochemical properties of various aqueous phases of Vicote F800 series suspensions were evaluated in Table 2.

本出願人はさらに、ポリエーテルエーテルケトン粉末の水性懸濁液の組成を正確に測定した。特に、水性懸濁液は、好ましくは２５％〜３５質量パーセントの範囲の、Victrexから商品名Vicote 704で販売される１０μｍの粒子サイズＤ９０のＰＥＥＫ粉末を含んでよいことが示された。

The Applicant has further accurately determined the composition of an aqueous suspension of polyetheretherketone powder. In particular, it has been shown that the aqueous suspension may comprise 10 μm particle size D90 PEEK powder sold by Victrex under the trade name Vicote 704, preferably in the range of 25% to 35% by weight.

  The aqueous suspension further comprises at least one, one, two and four kinds of solid lubricant particles, preferably 3% to 12% by weight of four kinds of solid lubricants from DYNEON having an average particle size of 20 to 30 μm. It may also be included in the form of a perfluoroalkoxyethylene copolymer type fluorinated powder sold under the trade name Hyflon® PFA.

The term “solid lubricant” as used herein is a solid, stable material that can reduce the coefficient of friction when placed between two friction surfaces and reduce wear and damage to the surface. Means an object. The object has different categories depending on the mechanism of action and the structure:
-Class 1: For example, solids whose lubricating properties are attributable to the crystal structure, such as graphite, zinc oxide (ZnO) or boron nitride (BN);
・ Class 2: Solids whose lubricating properties such as molybdenum disulfide MoS ₂ , graphite fluoride, tin sulfide, bismuth sulfide, tungsten disulfide or calcium fluoride are also attributed to the reactive chemical elements in the crystal structure and composition ;
• Class 3: solids whose lubricating properties are due to chemical reactivity, such as certain compounds of the thiosulfate type or Desilube 88® sold by Desilube Technologies Inc;
Class 4: Solids whose lubricating properties such as polytetrafluoroethylene (PTFE) or polyamide are caused by plasticity or viscoplastic behavior under frictional stress;
Can be classified.

The aqueous suspension is a mechanical reinforcing agent, preferably 0.5% to 1% by weight, sold by Evonik under the trade name Printex, with a BET specific surface area of 25 to 300 m ² / g and an average particle size of 1 A carbon black pigment of ˜5 μm may be included.

  Aqueous suspensions promote fusion or film formation by external resin processing of the polymer and change the surface tension of the suspension to promote diffusion, preferably with a rapid evaporation rate and a boiling point of 100 ° C to 200 ° C. An ethylene glycol monobutyl ether type fusing agent at 0 ° C. may be included at 2.5% to 10 weight percent, more preferably 2.5% to 5 weight percent of the suspension.

  Aqueous suspensions improve the wetting of the support and prevent the powder from precipitating out of solution, preferably non-ionic wetting and dispersing agents (of water and ethanol) of the sodium dioctylsulfosuccinate type. The compound of sulfuric acid and aliphatic ester) in the mixture may be comprised between 2.5% and 10% by weight of the suspension, preferably between 2.5% and 5% by weight.

  For a process for depositing a dry film on the distal end 1, 2 portion of a threaded tubular component, Applicants have used a Statice 704 polyetherether by injection using an electrostatic gun and either a dry or wet procedure. It was shown that ketone powder grade can be applied.

  In the first variation, the PEEK powder is applied after preheating the portions 1 and 2 to 400 ° C. Next, maintaining the coating portion at an initial temperature of 360 ° C. to 420 ° C. for 2 minutes, preferably 400 ° C., improves the surface appearance. The operation may be repeated several times to achieve the desired thickness. The powder must be dehydrated at 180 ° C for a minimum of 2 hours.

  In the second variation, the ends 1, 2 are coated with a pneumatic spray of a cold aqueous suspension of Vicote 704 powder (with or without strengthening). In this process, the terminal 1 and 2 portions are completely cleaned and preferably degreased using a solvent, preferably a polar aprotic solvent such as acetone.

  Application can be performed using a pneumatic gun spray system with a gravity feed gun and cup, with the ends 1, 2 being at ambient temperature. The temperature of the mixture is preferably close to ambient temperature, which is preferably in the range of 20 ° C to 30 ° C.

  The diameter of the gun nozzle is preferably 0.7 to 1.8 mm and the minimum air pressure of 4 bar is preferably 4 to 6 bar.

  The coated part is then left for 5-10 minutes at ambient temperature.

  This part is placed in an oven or furnace at a temperature of 120 ° C. for 5-10 minutes. This drying operation can be performed by induction, for example. This portion is then placed in a furnace at either 400 ° C. or lower and subsequently raised to 400 ° C. at a rate in the range of 10 ° C. to 20 ° C./min.

  When the maximum metal temperature is reached, the screw ends 1, 2 are left at that temperature for 5-15 minutes, preferably at least 10 minutes, in order to completely fuse the dry film to form a uniform film.

  The screw end portions 1, 2 are then removed from the furnace and allowed to cool to ambient temperature. The cooling rate for obtaining the semicrystalline structure is preferably slow, i.e. from 1 ° C / min to 200 ° C / min.

  An alternative to electrostatic injection consists of applying Vicote powder by dry heat injection onto the screw ends 1, 2 using a heat gun. In this process, the terminal 1 and 2 portions are completely cleaned and preferably degreased with a solvent, preferably a polar aprotic solvent such as acetone.

  Preheat the part in an oven or furnace at 260 ° C. The polyaryletherketone microparticles are heated to the melting point using a heat gun with vector gas, accelerated, transported to the substrate and Vicote powder applied to the part. This is followed by rapid cooling to ambient temperature in air. The operation may be repeated several times to obtain the desired thickness.

  The thickness of the dry coating is 20 to 70 μm, preferably 30 to 50 μm.

The test has a number of parameters:
-Friction torque at the contacted surface under high Hertz stress (Bridgman test);
-Adhesive strength of the film on the substrate (scratch test, cross-hatch test);
-Wet medium exposure resistance;
・ Immersion resistance in water;
・ High pressure wear resistance (Falex test)
Consists of evaluating.

  The Bridgman test can measure the tribological properties of dry film pigments during screwing operations specific to “premium” connections. More precisely, the shoulder torque resistance value CSB, also known as ToSR (shoulder torque resistance value), is modeled and measured. This torque occurs during the screwing operation specific to the premium connection used in the oil industry and is represented in FIG.

  The curve in FIG. 2 represents the screwing (or tightening) torque as a function of the applied rotational speed. As shown, the “premium” connection screw torque profile is divided into four parts.

  In the first part P1, the male thread of the male thread element (or pin) of the first component of the threaded tubular connection is still the female thread of the corresponding female thread element (or box) of the second component of the same threaded tubular connection. It is not tightened in the radial direction.

  In the second part P2, the geometric interference of the threads of the male and female screw elements increases the radial tightening as the screwing continues (screwing torque is small but increases).

  In the third part P3, the sealing surface at the outer periphery of the end part of the male screw element interferes radially with the corresponding sealing surface of the female screw element, resulting in a metal / metal seal.

  In the fourth part P4, the front end surface of the male screw element is axially adjacent to the annular surface of the adjacent assembly of the female screw element. The fourth portion P4 corresponds to the end stage of assembly.

  The assembly torque CAB corresponding to the end of the third portion P3 and corresponding to the start of the fourth portion P4 is referred to as shoulder torque.

  The assembly torque CP corresponding to the end of the fourth portion P4 is referred to as resin processing torque. When this resin processing torque CP is exceeded, the plasticity of the male assembly adjacent portion (the end portion of the male screw element) and / or the female assembly adjacent portion (the band located behind the annular adjacent surface of the female screw element) is increased. It is thought that it deform | transforms and, thereby, the performance regarding the closeness of the contact between the sealing surfaces by the resin processing of the sealing surface may fall similarly.

  A difference between the values of the resin processing torque CP and the shoulder torque CAB is referred to as a shoulder torque resistance value CSB (CSB = CP−CAB). The threaded tubular connection is optimally tightened at the end of assembly, which ensures the optimum mechanical strength of the threaded connection, not only for tension, but also for accidental disassembly and optimum sealing performance during use.

  In other words, the designer of the screw connection part has a shoulder torque that is lower than the resin processing torque CP (in order to avoid the resin processing of the adjacent part and the disadvantages thereof) for a given type of screw connection part. An optimum assembly torque value higher than (CAB) must be specified. If the assembly is finished with a torque lower than CAB, the correct relative placement of the male and female elements cannot be ensured and an effective interference fit between the sealing surfaces cannot be ensured. In addition, there is a risk of disassembly. The effective value of shoulder torque CAB depends on the diametrical and axial machining tolerances of the male and female screws and the sealing surface (s), so it varies greatly from connection to connection, even for connections of the same type. The optimum assembly torque must be substantially higher than the shoulder torque CAB.

  As a result, the higher the value of the shoulder torque resistance value CSB, the larger the margin for defining the optimized assembly torque, and the more screw connection portions are resistant to working stress.

  The friction test was carried out using a Bridgman type machine. This type of machine is described in particular in Non-Patent Document 1. FIG. 5 shows an outline and an example of functions of the Bridgman machine.

  The machine is: a disc DQ that can be driven to rotate at a selected speed; a first anvil EC1 that is permanently installed on the first side of the disc DQ, preferably a conical first anvil; a first side opposite the first side of the disc DQ Second anvil EC2, preferably conical, installed permanently on two sides; for example, a first EP1 and a second EP2 pressure element such as a piston capable of exerting a selected axial pressure P; one of the first pressure elements EP1 A third anvil EC3, preferably cylindrical, permanently installed on the surface; a fourth anvil EC4, preferably cylindrical, permanently installed on one surface of the second pressure element EP2.

  To test the lubricant composition, the same two materials that make up the screw element are coated with the composition to form a first sample S1 and a second sample S2. Next, the first sample S1 is inserted between the free surfaces of the first EC1 and the third EC3 anvil, and the second sample S2 is inserted between the free surfaces of the second EC2 and the fourth EC4 anvil. Next, the axial pressure P (for example, about 1 GPa) selected by each of the first EP1 and second EP2 pressure elements is applied to rotate the disk DQ at the selected speed, and the assembly torque to which the samples S1 and S2 are attached is measured. To do. In order to simulate the Hertz pressure and relative speed of adjacent surfaces at the end of assembly, axial pressure, rotational speed and rotational angle are selected in the Bridgman test. Apply a predetermined assembly torque to the samples S1 and S2, and whether the samples S1 and S2 are in close contact with a predetermined assembly torque profile, in particular, at least equal to a selected threshold for the selected assembly torque before being worn Several different parameter pairs (assembly torque, rotational speed) can be fixed using the machine to see if the complete rotational speed has been reached.

  In this case, the selected contact pressure was 1 GPa and the rotation speed was 1 rpm. Test samples were formed from 13% Cr containing stainless steel, machined, and then coated with different dry film formulations.

  The scratch test schematically shown in FIG. 4 can measure the adhesion or adhesion of the film on the surface or surface preparation. In a method consisting of shearing and deforming the film with spherical beads with increased load, two main tribological parameters can be measured, the critical load corresponding to the coefficient of friction and the loss of film aggregation.

  The experimental conditions use a spherical indenter formed from 5 mm diameter Inconel 718 and a metal sample formed from zinc or manganese phosphate coating or XC48 carbon steel treated by electrolytic copper-tin-zinc deposition. The parameters were: a load increasing rate from 10 N to 310 N at 15 N / s or a load increasing from 25 N to 750 N at 25 N / s. The bead replacement speed was 2 mm / s for 20 seconds (track length 40 mm). The measured coefficient of friction is considered to be low in the range of μ = 0.05 for a 10N load and μ = 0.09 for a 310N load. It was measured to be 0.07 μ at a load of 310 N on the carbon steel surface. It should be noted that the load and operating conditions for each type of coating test need to be clearly presented.

  The cross-hatch test consists of assessing the resistance of a single or multi-layer coating when it is separated from the substrate when the coating is cross-hatched until the substrate is classified into six categories by classification. The excellent adhesion of the coating to the substrate corresponds to class 0 of ISO standard 2409 (2007), the edges of the incision are perfectly smooth and the four corners of the cross hatch are not cut off. Considering the environment, the cross-hatch test is performed after placing in a wet medium (35 ° C. and 90% RH). Good moisture resistance is characterized by no change in appearance, no bubble formation, no corrosion, no cracks, no scaling corresponding to ISO 4628 classification and no loss of adhesion.

  The corrosion test consists of a salt spray test carried out in a climatic chamber under the following conditions: 50 g / L with a density of 1.029-1.036 at 35 ° C. and 25 ° C. and a pH of 6.5-7.2 at 25 ° C. Was collected at an average rate of 1.5 mL / h.

  The rust-free intact sample then corresponded to ISO standard 9227 ReOs after exposure. The method provides a means to verify that the relative quality of the metal material is maintained with or without a coating that prevents corrosion (metal or organic coating on the metal material).

  The water resistance test consists of subjecting the sample to an accelerated corrosion test according to DIN standard 50017 carried out in a climate chamber. The test consisting of one cycle per day consists of depositing water vapor by condensation for 8 hours at 35 ° C. and 90% relative humidity (RH), and then drying the sample. After 7 cycles, the substrate protected with the coating is investigated to see if it corroded.

Excellent resistance is classified according to ISO standard 4628: no corrosion, no foam formation, no cracks and with or without phosphate coating with zinc (8-20 g / m ² phosphate deposit) or manganese, Alternatively, there is no scaling of chromium or carbon steel plates treated with electrolytic deposition of a ternary copper-tin-zinc alloy with a Ni intermediate layer.

  The underwater immersion test is much more severe than the DIN standard 50017 water resistance test. It consists of testing the water resistance of the coating. Derived from ASTM standard D870-09 for industrial and automotive paints.

  Soaking in water can cause the coating to degrade. Knowledge about how the coating resists immersion in water is useful for predicting service life. Rupture or breakage in an underwater immersion test can occur due to a number of factors, notably the coating itself, contamination of the substrate or poor surface preparation. Therefore, the test is useful for evaluation in a single or complete coating system.

  The test consisted of immersing the sample in demineralized water halfway in an oven at 40 ° C. for 168 hours. Adhesion, foam formation, rust, or blowholes are visually observed, indicating the sensitivity of the coating to water.

For high-pressure wear resistance (also referred to as Falex test), a rotary indenter pressed between two V-shaped blocks shown in FIG. 6 is used. The Falex test is used at particularly high speeds to evaluate anti-wear and excessive pressure characteristics of lubricating fluids according to ASTM standards D2670 and ASTM D3233, but is also used at low speeds to evaluate solid lubricants according to ASTM method D2625. The Falex exam:
Semi-closed contact geometry (to trap the third lubricant);
・ Pressure / speed range in harmony with the connection;
The possibility to perform one-way or alternating tests to model assembly and disassembly operations;
Is adapted to adjust the screw connections used in the operation of hydrocarbon wells.

The test conditions are as follows:
・ Load = 785N;
-Indenter rotation speed = 60 rpm;
-Average metal / metal contact pressure = 560 MPa;
Indenter slide speed = 20 mm / s.

  The purpose of the test is to model and evaluate the durability from the viewpoint of the wear resistance of various films without the need to evaluate the connection. This test means that the performance of various coatings can be compared with the actual test on the connection. The wear criteria is defined using ASTM standard D2625-94 for the measurement of solid lubricant film load, and for a load of 785N, 1130N. This corresponds to a rapid increase in torque as compared to the initial state of the friction coefficient approximately equal to mm and approximately equal to 0.15. In general, wear is observed when the applied load decreases regardless of material and configuration.

  The Applicant has observed the performance, in particular the tribological and rheological performance of various films obtained with aqueous suspensions of polyetheretherketone, especially the fluoroethane type thermosetting films or waxy thermoplastic matrices that are observed. In order to compare with a certain viscoplastic film, it was evaluated.

  The fluoroethane film is composed of an aqueous dispersion of fluoroethylene vinyl ether cured with an aliphatic polyisocyanate curing agent.

  The waxy thermoplastic matrix comprises at least one polyethylene wax and predominantly excess base calcium sulfonate in which the friction modifying pigment is dispersed, as described in patent application WO 2008/139058.

In the first stage, the Applicant has the following specific surface preparation treatment:
-As-machined XC48 carbon steel (XC48AsM);
-Z20C13 stainless steel (13Cr);
-XC48 carbon steel with zinc (PhZn) or manganese (PhMn) phosphate coating treatment;
-The adhesion, coefficient of friction, anti-corrosion protection and immersion in water properties of aqueous suspensions of polyetheretherketone on various substrates with electrolytic copper-tin-zinc deposited (TA) XC48 carbon steel were evaluated.

  Tables 3, 4 and 5 show the adhesion results obtained with each aqueous suspension of Vicote F804, Vicote F805 and Vicote F807Blk on various surface prepared samples by scratch and crosshatch tests according to ISO standard 2409. To summarize.

  It will be recalled that the scratch test specifies high performance materials, preferably thermosetting or thermoplastic adhesion as a function of increasing load. The critical load that determines interfacial rupture and the adhesion of the material are high when the material is resistant and adhesive. If it is below the minimum critical load of 310 N, the increased wear product amount can come into contact and the pressure can be 1.1 GPa, which is the minimum adhesion that is insufficient as wear resistance.

  For a crosshatch test according to ISO standard 2409, which provides a measure of adhesion to the interface after damage due to material scratching, a score of 0 corresponds to excellent adhesion, while a score of 5 is defined as very low adhesion.

試験フィルムは、マンガンのリン酸塩皮膜処理をした炭素鋼を除いて、亜鉛のリン酸塩皮膜処理をした炭素鋼上で、実施された表面調製に関係なく接着力が不十分であった。加えて、ポリエーテルエーテルケトンフィルムは、亜鉛のリン酸塩皮膜処理タイプの表面処理と適合性がほとんどなかった。

The test films had insufficient adhesion on carbon steel with zinc phosphate coating treatment, regardless of the surface preparation performed, except for carbon steel with manganese phosphate coating treatment. In addition, the polyetheretherketone film was hardly compatible with the zinc phosphate film treatment type surface treatment.

  In order to explain the results, the applicant further evaluated the incidence of roughness obtained without the phosphate coating treatment. Since the adhesion mechanism of polyetheretherketone film is mainly physical by mechanical keying, the roughness of the substrate is a decisive factor.

  At the same time, to ensure good adhesion of the film, that is, the roughness Ra (Ra is the arithmetic average of the center line of the roughness width) at a minimum of 4 μm to 6 μm, the roughness Ra of the desired final film thickness To achieve 20% or 25%, it is recommended to sand the substrate by injection. The roughness was measured using a rugosimeter according to ISO standard 1997.

表６は、マンガンのリン酸塩皮膜処理により得られた比較的高い粗度は、接着度が良好であることを示す。表６はまた微弱極性表面調製、例えば３成分銅−スズ−亜鉛の電解堆積は接着を促進しないことも示す。

Table 6 shows that the relatively high roughness obtained by the manganese phosphate coating treatment has good adhesion. Table 6 also shows that weakly polar surface preparations such as ternary copper-tin-zinc electrolytic deposition do not promote adhesion.

  In view of these initial results, Applicants chose only a substrate with inherently low corrosion resistance to determine the corrosion resistance, so that the critical adhesion load for the polyetheretherketone film is 13% chromium greater than 180N. The contained martensitic stainless steel was excluded.

  The thickness of the film produced by the cold air spray was 20 to 45 μm. The degree of rust of Re0 to Re9 was determined according to ISO standard 4528-3. The degree of water bubble formation and peeling from 2S2 (low concentration water bubble formation and small dimensions) to 5S5 (overall water bubble formation and large dimensions) was determined according to ISO standard 4628-2. The results are summarized in Tables 7 and 8.

単層ポリエーテルエーテルケトンフィルムでコーティングされた表面調製の耐食性は、応力下ではフィルムの接着性が低く、凝集の損失が強力であったにもかかわらず、銅−スズ−亜鉛電解堆積を除いては概して不十分であった。結果はさらに、表面調製に関係なく、無機カーボンブラックタイプ化合物を含むVicote F807Blkポリエーテルエーテルケトンフィルムの耐食性はVicote F805と比較して比較的良好であることも示す。最良の結果が電解堆積で得られ、１０００時間後に腐食が５点しかなかった。導電性カーボンブラック補強剤を添加すると、犠牲アノードとして作用すると腐食に対する保護機序が補強されることが観察された。

The corrosion resistance of the surface preparation coated with a single layer polyetheretherketone film, except for the copper-tin-zinc electrolytic deposition, despite the low film adhesion under stress and the strong loss of aggregation Was generally inadequate. The results further show that the corrosion resistance of Vicote F807Blk polyetheretherketone film containing inorganic carbon black type compound is relatively good compared to Vicote F805 regardless of surface preparation. The best results were obtained with electrolytic deposition, with only 5 points of corrosion after 1000 hours. It has been observed that the addition of conductive carbon black reinforcement enhances the protection mechanism against corrosion when acting as a sacrificial anode.

  Finally, Applicants evaluated the average coefficient of friction of films exposed to abrasion by a scratch test over a wide load range of 10N to 750N. The results are summarized in Table 9.

ポリエーテルエーテルケトンフィルムの摩擦係数は表面調製に関係なく０．１３５未満であり、パーフルオロアルコキシエチレンタイプのフッ素化重合体を含むポリエーテルエーテルケトンでは平均接触圧力５００ＭＰａに対して０．０７５に達した。

The coefficient of friction of the polyetheretherketone film is less than 0.135 regardless of the surface preparation, and the polyetheretherketone containing perfluoroalkoxyethylene type fluorinated polymer reaches 0.075 for an average contact pressure of 500 MPa. did.

  The first result shows that the single layer polyetheretherketone film has anti-corrosion performance and sufficient lubricity depending on not only the film composition but also the adhesion of the substrate.

  Next, in a second stage, the applicant developed a means to improve adhesion and anti-corrosion performance. Applicant has sought to replace the sanding when the shape of the part is impossible to coat. In particular, the Applicant investigated without changing the composition of the commercial films considered. In fact, when adhesion promoters or corrosion-inhibiting pigments are added in excess of 10%, PCV (pigment volume concentration) is more than PCV with the minimum binder required to coat powdered materials (pigments and fillers). Resulting in increased porosity and agglomeration loss of films obtained from commercial aqueous suspensions.

  Other alternatives using Vicote 704 polyetheretherketone powder can be envisaged.

  The Applicant has devised enhancing adhesion with an adhesion promoter type primer. Direct adhesion between materials is rare. Direct bonding is not unique but is primarily related to van der Waals interactions, occurs only with very clean and smooth materials (eg mica or silicon), and contacts closely, ie at the atomic scale (nanometers) . That is, this is often not possible when the surface is rough, as opposed to being perfectly suitable for low roughness films.

  Accordingly, Applicants have primarily investigated films that are compatible with the process for obtaining polyetheretherketone films by melting at 400 ° C.

  The primer may be an injection deposit of an alloy of iron and zinc sold under the trade name Dacroforge Z by Dacral, an alternative to zinc phosphate coating treatment, and is a mechanical injection process equivalent to sanding / shot blasting. Then, use is restricted by a hollow body having a short diameter and a low height.

  The primer is preferably a filled polyaryletherketone. In particular, a solution containing a muscovite or biotite type mica pigment in an organic polyetheretherketone binder in a proportion of 25 to 50% by weight is sold under the trade name Vicote F817 by the supplier Victrex.

  The process for applying and melting the primer is the same as the top layer (overcoat) process. In contrast, rapid cooling rates are desirable in order to delay the onset of corrosion pits and reduce the passive retention current density of the material, so as to obtain a low crystal structure that is more insulating.

  The thickness of the undercoat may be 30-40 μm.

  The anti-corrosion and adhesion properties of the primer evaluated using two processes with different cooling kinetics are summarized in Tables 10 and 11, respectively.

Vicote F817下塗りは保護力や接着性は十分であるが潤滑性は十分でない。潤滑特性はポリアリールエーテルケトン上層により提供された。

The Vicote F817 undercoat has sufficient protection and adhesion, but not sufficient lubricity. Lubrication properties were provided by the polyaryl ether ketone upper layer.

  Anti-corrosion, adhesion and double layer friction performance are summarized in Tables 12 and 13. The total film thickness including undercoat and topcoat was 40-70 μm.

平均接触圧力５００ＭＰａ、特に表面調製に関係なくμ＝０．０８５であるVicote F807 Blkフィルムの摩擦係数は十分低く、フルオロエタン又はエポキシド熱硬化性フィルムの摩擦係数に匹敵し、得られる最適組立トルクの肩トルク値を７０％未満にしうるはずである。

The coefficient of friction of Vicote F807 Blk film with an average contact pressure of 500 MPa, in particular μ = 0.085 regardless of surface preparation, is sufficiently low, comparable to that of fluoroethane or epoxide thermosetting films, Shoulder torque values should be less than 70%.

  Overall, the coefficient of friction, adhesion and anti-corrosion protection of the polyetheretherketone film is preferably a polyetheretherketone primer containing a mica pigment filler, more particularly at least one fluorinated heavy which undergoes plastic deformation under stress. A significant improvement is achieved with an overcoat of polyetheretherketone containing coalesced and / or carbon black type mechanical reinforcing pigments.

  Finally, the Applicant evaluated the tribological and rheological behavior of the film by the Bridgman test in order to measure the shoulder torque resistance value. The shoulder torque resistance value obtained with Vicote F807 Blk was equal to 85% of the reference value of API RP5A3 grease on XC48 carbon steel and Z20C13 stainless steel. However, the problem of sample preparation due to the process of manufacturing the film and the small diameter of the sample means that this value cannot be considered an absolute reference. Crystal structure and many potential van der Waals type intermolecular interactions in polyetheretherketone show a tendency for material agglomeration to be strong and high shear strength, ie, substantially higher shoulder torque resistance Will show.

  At the same time, the Applicant evaluated the wear resistance of the film in the Falex test. Test configurations adapted to the joint consisted of a pair of differently prepared V-shaped Vee blocks coated with PEEK film in single or double layers and machined XC48 carbon containing 13% chromium. A steel indenter or a Z20C13 stainless steel indenter may be included.

  The test conditions carried out at a load of 785 N are relatively close to the recorded (100-300 MPa) during screwing at the beginning of shouldering on the screw and bearing surface, with an average pressure during contact of 150 MPa and a pressure rate coefficient (PV ) = 5 MPa. PV = 11.2 MPa. which is close to the proof of the wear rule of thread cutting with load flank at m / s. It corresponds to m / s.

  Applicants investigated Vicote F805 and F807Blk reinforced polyetheretherketone.

  FIG. 6 compares the double layer Vicote F807 / Vicote F807 Blk film despite the ternary electrolytic deposition type surface treatment that is considered anti-wearing compared to the wax-like thermoplastic solution currently in use on the connection. It shows very good durability (see Patent Document 4). Wear as defined by ASTM standard D2625-94 is never obtained, but was obtained after 51 minutes with the HMS3 waxy thermoplastic solution. The constant friction coefficient μ = 0.08 was relatively low, and there was a characteristic that the abrasion was very low.

  In order to determine the following film wear resistance limits, Applicants evaluated film durability and coefficient of friction using the Falex test with increasing loads from 1335N to 4200N. The slide speed was 10 mm / s versus 20 mm / s used previously. The results are shown in FIG.

  As a result, when the average contact pressure was 350 MPa, no abrasion occurred, indicating that the film of the present invention has very high wear resistance. Furthermore, when the pressure increased, the friction coefficient decreased to 0.056-0.078.

  In particular, to confirm the wear resistance and coefficient of friction observed in the laboratory using a Falex and scratch test for a sample of electrolytic copper-tin-zinc deposited carbon steel, Applicants are very sensitive to wear. 7 "29 L80 VAM TOP HT connection part was assembled. The assembly torque was 29900Nm.

  Carbon steel female end 2 is treated with electrolytic deposition, male end 1 is treated with zinc phosphate coating and coated with UV curable acrylic resin as described in patent publication WO 2006/104251 did. Double layer PEEK film was applied to the treatment coupling at a cooling rate of less than 5 ° C / min. Table 14 summarizes the assembly results.

得られた組立結果は、ポリエーテルエーテルケトンフィルム及び特に強化されたポリエーテルエーテルケトンフィルムの顕著な抗摩耗性を裏付ける。

The resulting assembly results support the remarkable anti-wear properties of polyetheretherketone films and particularly reinforced polyetheretherketone films.

したがって、本発明は、炭素鋼表面又は少なくとも１３％のクロムを含む鋼鉄表面に適用する場合、非常に興味深い耐摩耗特性である潤滑剤フィルムを提供する。それにより、２成分銅−スズ又は３成分銅−スズ−亜鉛タイプの電解堆積を用いないですむ。

Thus, the present invention provides a lubricant film that is a very interesting antiwear property when applied to carbon steel surfaces or steel surfaces containing at least 13% chromium. This eliminates the need for electrolytic deposition of the two component copper-tin or ternary copper-tin-zinc type.

Claims (17)

A threaded tubular component for drilling or working in a hydrocarbon well, said tubular component being on the outer peripheral surface or inner peripheral surface at one of its ends (1, 2) depending on whether the screw end is male or female And at least a portion of the ends (1, 2) is coated with at least one lubricating dry film (12) comprising at least 65 weight percent polyaryletherketone ,
The lubricating dry film (12) further comprises at least one Type 4 solid lubricant in a mass ratio of 10% to 35%,
The lubricating dry film (12) is seen containing perfluoro alkoxy ethylene copolymer mass ratio of 10% to 30%,
A threaded tubular component , wherein the lubricated dry film (12) has a crystallinity of 10% to 35% .   The threaded tubular component of claim 1, wherein the polyaryletherketone is selected from polyetheretherketone (PEEK), polyetherketone (PEK), and mixtures thereof. Said lubricated dry film (12) is selected from the following list of pigments: carbon black, mica, wollastonite, nanometer aluminum oxide, nanometer titanium oxide, glass powder, nanodiamond, nanometer WS2 or WS2-fullerene The threaded tubular component according to claim 1 or 2 , comprising a mechanical reinforcing agent in a mass ratio of 1% to 15%. The portion coated with the lubrication dry film (12) is composed of iron and zinc alloy deposited in advance by sanding, manganese phosphate film treatment, electrolytic deposition of copper or copper-tin-zinc alloy and injection. The method for manufacturing a threaded tubular component according to any one of claims 1 to 3 , wherein a surface preparation step selected from the group is applied. The lubricating dry film (12) coated part is, in advance, is primed polyetheretherketone semi-crystalline structure containing mica pigments, screw tubular component according to any one of claims 1 to 3 Manufacturing method. The entire threaded region (3, 4) is coated with the lubricating dry film (12), the manufacturing method of the screw tubular component according to any one of claims 1-5. Comprises a metal / metal sealing surface, the sealing surface is coated with the lubricating dry film (12), the manufacturing method of the screw tubular component according to any one of claims 1-6. A threaded tubular connection comprising a male threaded tubular component and a female threaded tubular component combined with each other, wherein at least one threaded tubular component is a threaded tubular component according to any one of claims 1-3. A threaded tubular connection. A process of coating a threaded tubular component for drilling or working in a hydrocarbon well, said tubular component having an outer peripheral surface or one of its ends (1, 2) depending on whether the threaded end is male or female There are threaded areas (3, 4) made on the inner peripheral surface, and the process is as follows:
Producing a mixture comprising polyaryletherketone powder in a suspension in water in a proportion of 25% to 35% by weight;
Applying the mixture to the end (1, 2) portion of the threaded tubular component;
Drying the coated end (1,2) part at a temperature of 100 ° C. to 150 ° C. for 5 to 10 minutes;
Heating the coated end (1,2) portion to a temperature of 350 ° C. to 450 ° C. for 5 to 15 minutes at a rate of temperature increase of 10 ° C. to 20 ° C. per minute; and Cooling the coated end (1,2) portion to ambient temperature at a cooling rate of less than 10 ° C. to obtain a structure;
Including
The mixture further comprises a fusing agent having a boiling point of 100 ° C. to 200 ° C. and a rapid evaporation rate in a proportion of 2.5% to 10% by weight;
The process wherein the mixture further comprises a non-ionic wetting and dispersing agent in a proportion ranging from 2.5% to 10 weight percent. The process of claim 9 , wherein the mixture further comprises at least one Type 4 solid lubricant in a proportion of 3% to 12 weight percent. The process according to claim 10 , wherein the Group 4 solid lubricant is a perfluoroalkoxyethylene copolymer having a mass ratio of 3% to 12%. The mixture further comprises a mechanical reinforcement selected from the following list of pigments: carbon black, mica, wollastonite, nanometer aluminum oxide, nanometer titanium oxide, glass powder, nanodiamond, nanometer WS2 or WS2-fullerene. The process according to claim 10 , comprising a mass ratio of 0.5% to 5%. Part of the end (1,2) is coated with a pneumatic spray system, the diameter of the system is 0.7～1.8Mm, air pressure is not 4～6Bar, according to claim 9 process. A surface preparation step selected from the group consisting of sanding, manganese phosphate coating, electrolytic deposition of copper or copper-tin-zinc alloy, and particles of iron and zinc alloy deposited by injection; 14. The process according to any one of claims 9 to 13 , wherein the process is performed prior to application to the portion of the. Containing mica pigment, the surface preparation steps consisting in primed polyetheretherketone semi-crystalline structure, the mixture is carried out prior to application to said portion of said distal or more of claims 9 to 13 1 The process described in the section. A process of coating a threaded tubular component for drilling or working in a hydrocarbon well, said tubular component having an outer peripheral surface or one of its ends (1, 2) depending on whether the threaded end is male or female There are threaded areas (3, 4) made on the inner circumference, the following:
Heating the end (1, 2) portion of the threaded tubular component to a temperature of 360-420 ° C, preferably close to 400 ° C;
Injecting PEK and / or PEEK powder onto said part of the end (1, 2) of said threaded tubular component;
Maintaining the coated end (1,2) part at a temperature of 360 ° C. to 420 ° C., preferably close to 400 ° C. for 1 to 4 minutes; and • obtaining a predominantly crystalline structure Cooling the coated end (1,2) portion to ambient temperature at a cooling rate of less than 10 ° C. per minute;
Including
The PEK and / or PEEK powder comprises a fusion agent having a boiling point of 100 ° C. to 200 ° C. and a rapid evaporation rate in a proportion of 2.5% to 10% by mass;
The process wherein the PEK and / or PEEK powder further comprises a non-ionic wetting and dispersing agent in a proportion ranging from 2.5% to 10 weight percent. The process of claim 16 , wherein the step of degreasing the coated portion prior to heating the portion is performed.

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