CN103221519B - Process for coating a threaded tubular component, threaded tubular component and resulting connection - Google Patents
Process for coating a threaded tubular component, threaded tubular component and resulting connection Download PDFInfo
- Publication number
- CN103221519B CN103221519B CN201180053943.5A CN201180053943A CN103221519B CN 103221519 B CN103221519 B CN 103221519B CN 201180053943 A CN201180053943 A CN 201180053943A CN 103221519 B CN103221519 B CN 103221519B
- Authority
- CN
- China
- Prior art keywords
- tubular component
- threaded tubular
- threaded
- coated
- dry film
- 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.)
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Classifications
-
- 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
-
- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/003—Threaded pieces, e.g. bolts or nuts
-
- 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
- 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
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- 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
-
- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/04—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/04—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen
- C10M2213/043—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/06—Groups 3 or 13
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/08—Groups 4 or 14
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/08—Solids
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- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2080/00—Special pretreatment of the material to be lubricated, e.g. phosphatising or chromatising of a metal
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Abstract
The invention concerns a threaded tubular component for drilling or working hydrocarbon wells, said tubular component having at one of its ends (1; 2) a threaded zone (3; 4) produced on its outer or inner peripheral surface depending on whether the threaded end is male or female in type, in which at least a portion of the end (1; 2) is coated with at least one lubricating dry film (12) comprising at least 65% by weight of a polyaryletherketone. The invention also concerns a process for depositing said film (12).
Description
The present invention relates to the tubular member of probing for Oil/gas Well and/or operation, and relate to the thread head of this component more accurately.Described end is male or parent form, and can be connected to the respective end of another component, forms web member.
The invention still further relates to the method for producing wear resisting films on this tubular member.
The component of term " probing and operation for Oil/gas Well " refers to that shape is essentially tubulose, on another component intending being connected to identical type or in other cases, final formation or for the tubing string of drilling Oil/gas Well or intend for safeguarding (also referred to as renovation vertical tube) or operating the vertical tube of this well, such as vertical tube or for the string of casing that uses in operating well or tubing string.The present invention also can be applicable to the component used in drill string, such as drilling rod, heavy drilling rod, drill collar, the part be connected with pipeline and be called the heavy pipeline of drill pipe sub.
Each tubular member comprises the end providing positive thread district and/or the end providing negative thread district, and each end intends adopting the respective end of another component to be screwed into connection.This assembly determines web member.
Threaded tubular component connects under the stress determined, to meet the fastening and seal request that working conditions forces, since it is known in well, can require that threaded tubular component experiences several assembling (makeup)-open (breakout) circulation.
Use the condition of this threaded tubular component to cause inhomogeneous stress, described stress makes to need the non-sensitive part at these components, and such as threaded area, adjoining region or sealing face use coating.
Usually carry out being screwed into operation under high axial load, such as, weight by the pipeline of the length number rice of threaded connector connection may localize because of the slightly misaligned at screw member axle to be connected.This induction is in threaded area place and/or the risk in the wearing and tearing of metal/metal sealing face place.Due to this reason, need with lubricator to be coated with threaded area, abutment surface and metal/metal sealing face.
In addition, store threaded tubular component (sometimes several years), then assemble in disagreeableness environment.This is such as in the situation with the coastal waters situation of salt fog or the land situation under sand, dust or other pollutents exist.Therefore, need to be used in erosion-resisting coating on the surface, described surface must cooperate by being screwed into (threaded area) or contacting (metal/metal surface) by interfering.Treat surface is also needed to prevent corrosion.
But, from the angle of environment, seeming the grease that is screwed into that use meets API (American Petroleum Institute) standard RP5A3 does not form long-term solution, this is because these greases contain heavy metal, can be driven away by tubular member and be discharged in environment or well, thus cause blocking, and blocking needs special clean operation.In addition, these greases do not provide sufficient corrosion prevention, and must apply on the spot for each screw rod attended operation.
In order to overcome requirement Long-term Anti corrodibility and wear-resistant problem; and meet environmental characteristics; (namely the Primary Actor in threaded connector field develops solid drying coating energetically; not not pasty state and there is no the viscosity as grease); described coating is lubricant; play again the effect that protection prevents from corroding, and finally can be applied on tubular member in factory.
Especially, develop and be inertia and anti abrasive coating for environment.
The present invention is based on following discovery: use PAEK can obtain lubrication dry film, described film highly abrasion-resistant, resistance to wears, and has high physical strength, and low frictional coefficient, and the operational condition of resistance to extreme Oil/gas Well.The solution used also can be adapted to the metal of the various grades of the web member of the above tubular member quoted as proof.
Both do not describe in the prior art, also do not imply and use this PAEK and performance thereof in threaded tubular component defined above.
More accurately, the present invention relates to the threaded tubular component of probing for Oil/gas Well and/or operation, described tubular member has the threaded area that or inner peripheral surface outer at it are made at its one end place, this depends on that thread end is male or parent form, the end at least one lubrication dry film coating of the PAEK containing at least 65% weight at least partially in described threaded area.
Below define or optional feature that is complementary or that substitute.
PAEK is selected from polyether-ether-ketone (PEEK), polyetherketone (PEK) and composition thereof.
This lubrication dry film has the structure that crystallinity range is 10%-35%.
This lubrication dry film comprises the solid lubricant of at least one the 4th class further, and its proportional range is 10%-35% weight.
This lubrication dry film comprises perfluoroalkyl ethylene oxy multipolymer, and its proportional range is 10%-30% weight.
This lubrication dry film comprises the mechanical toughener being selected from following pigment: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS2 or WS2-soccerballene, and its proportional range is 1%-15% weight.
The part being coated with lubrication dry film experienced by advance and is selected from sand milling, phosphoric acid manganese, the electrolytic deposition of Cu or Cu-Sn-Zn alloy, and by the stage of surface preparation in Fe and the Zn alloy of jet deposition.
The part being coated with lubrication dry film is coated with in advance has half crystal structure and the priming paint containing the polyether-ether-ketone of pigments, mica.
Whole threaded area coating lubrication dry film.
Threaded tubular component comprises metal/metal sealing face, and described sealing face is coated with lubrication dry film.
The invention still further relates to threaded tubular connection, described web member comprises male threaded tubular component and parent form threaded tubular component, one be assembled in another in wherein said threaded tubular component at least one as defined above.
The invention still further relates to coating for drilling or the method for threaded tubular component of process oil gas well, described tubular member has the threaded area of making on its periphery or inner peripheral surface at one of its end place, its periphery, threaded area or inner peripheral surface are made and depends on that thread head is male or parent form, the method comprises the steps:
Produce the mixture being included in the polyarylether ketone powder suspended in water, its proportional range is 25%-35% weight;
Apply described mixture on the end sections of described threaded tubular component;
The end sections of dry so coating under the temperature range of 100 DEG C-150 DEG C, lasts 5-10 minute;
Under temperature rise rate in the temperature range of 10 DEG C-20 DEG C/min, the end sections that heating is so coated with, to the temperature range of 350 DEG C-450 DEG C, lasts 5-15 minute;
Under the rate of cooling being less than 10 DEG C/min, cool the end sections be coated with like this to envrionment temperature, to obtain the structure of crystallization substantially.
Below define complementation or alternative optional feature.
This mixture also comprises the coalescing agent that the boiling spread with rapid evaporation rate is 100 DEG C-200 DEG C, and its proportional range is 2.5%-10% weight.
This mixture comprises non-ionic wetting and dispersion agent further, and its proportional range is 2.5%-10% weight.
This mixture also comprises the solid lubricant of at least one the 4th class, and its proportional range is 3%-12% weight.
The solid lubricant of the 4th class is perfluoroalkyl ethylene oxy multipolymer, and its proportional range is 3%-12% weight.
This mixture also comprises the mechanical toughener being selected from following pigment: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS
2or WS2-soccerballene, its proportional range is 0.5%-5% weight.
Use pneumatic spraying system, coating end sections, the diameter range of described system is 0.7-1.8mm, and gas pressure range is 4-6bar.
Before on applying mixture to end sections, carry out being selected from following in stage of surface preparation: sand milling, phosphoric acid manganese, the electrolytic deposition of Cu or Cu-Sn-Zn alloy, and by Fe and the Zn alloying pellet of jet deposition.
Before on applying mixture to end sections, carry out stage of surface preparation, described stage of surface preparation has half crystal structure by generation and the priming paint containing the polyether-ether-ketone of pigments, mica forms.
The invention still further relates to for drilling or the coating process of threaded tubular component of process oil gas well, described tubular member has the threaded area of making on its periphery or inner peripheral surface at one of its end place, this depends on that thread head is male or parent form, and the method comprises the steps:
The end sections heating described threaded tubular component is the temperature of 360 DEG C-420 DEG C to scope, preferably arrives the temperature close to 400 DEG C;
Spray PEK and/or PEEK powder on the end sections of described threaded tubular component;
Through the time period that scope is 1-4 minute, the end sections maintaining so coating, under the temperature range of 360 DEG C-420 DEG C, preferably close to the temperature of 400 DEG C, lasts 1-4 minute;
Under the rate of cooling being less than 10 DEG C/min, the end sections that cooling is so coated with is to envrionment temperature.
Before the described part of heating, preferably carry out the step making partially skimmed to be coated.
In the following description, in conjunction with reference to accompanying drawing, described in more detail the features and advantages of the present invention.
Fig. 1 is by the schematic diagram of the web member obtained by assembly connection two tubular members;
Fig. 2 is the schematic diagram of the screw rod junction curve of two threaded tubular components;
Fig. 3 is the schematic diagram of the substrate with the coating of lubrication dry film;
Fig. 4 is the schematic diagram of testing apparatus;
Fig. 5 is the schematic diagram of another testing apparatus;
Fig. 6 and 7 shows trial curve.
Threaded connector shown in Fig. 1 comprises first tubular member with turning axle 10 providing male end portion 1, and provides second tubular member with turning axle 10 in female end portion 2.Stop in two each comfortable terminal surfaces in end 1 and 2, described terminal surface is radial oriented relative to the axle 10 of threaded connector, and provides threaded area 3 and 4 separately, and described threaded area 3 and 4 mutually cooperation, for by being screwed into, is interconnected two components.Threaded area 3 and 4 can be the thread type such as trapezoidal, self-locking.In addition, by after being screwed into connection two screw members, the metal/metal sealing face 5,6 of (interfering contact) is being contacted close to the interference that male end portion and the female end portion of threaded area 3,4 provide plan relative to each other to enter sealing respectively.Finally, male end portion 1 stops in terminal surface 7, and described terminal surface 7 abuts against the respective surfaces 8 that female end portion 2 provides, when two ends are assembled each other.
Applicant also predicts other structures, and wherein in the present case, what formed by two surface in contacts 7 and 8 is adjoined by the fastening cooperation of self-locking of threaded area 3,4 alternative (see US4822081, US RE30467 and US RE34467).
Can find out in Fig. 1 and 3, in its end 1 part (being called substrate 11), be coated with at least one threaded tubular connection with the lubrication dry film 12 of the PAEK containing at least 65% weight, described dry film 12 has the structure of at least 10% degree of crystallinity.To remind, by melting or crystallization enthalpy change (the Δ Η of polymkeric substance herein
0), measure degree of crystallinity.According to Hay and Coll (Polymer Communications, 1984,25,175-178), for complete holocrystalline PAEK, especially polyether-ether-ketone (PEEK), theoretical melting enthalpy becomes 122J/g.The advantage that there is the degree of crystallinity of at least 10% is to provide excellent mechanical property, especially good anti-shoulder moment of torsion.But, preferably keep degree of crystallinity lower than 35%, to prevent from, with regard to corrosion, keeping the feature of film with regard to binding property and surface preparation protection.
By moisture polyether-ether-ketone dispersion or the PAEK used in the present invention can be obtained by moisture polyetherketone dispersion.These aqueous dispersions can comprise organic or inorganic machinery toughener, the white mica be such as made up of pure aluminium silicate and hydrated potassium or magnesium and/or the pigments, mica of meroxene, there is γ crystalline texture and size range is the amorphous alumina of 20-300nm, size range is the TiO 2 pigment of 10-100nm, perfluoroalkyl ethylene oxy copolymer resin (PFA), amorphous carbon mineral black, the synthetic graphite powder that diameter is less than 5 μm, by explosion obtain and size range is the Nano diamond of 4-6nm, fiber thickness scope is 1-1.3 μm and the C type glass of diameter D90<50 μm, size range is the WS2 fullerene nanomaterial of 80-220nm, or the WS2 tungsten disulfide layered pigments of granularity D50=55nm.
By the synthesis path of nucleophilic substitution type, obtain polyether-ether-ketone (it is abbreviated as PEEK), and polyetherketone (it is abbreviated as PEK).Polyethers causes having dystectic hard semi-crystalline polymer.They belong to the material category of the peak performance within the scope of thermoplastic material.Their second-order transition temperature is 143 DEG C, and because they have the character of hemihedral crystal, and the mechanical property therefore keeping them excellent is until close to the temperature (343 DEG C) of its fusing point.Their standard-linear and aromatic structure provide PEEK and PEK with excellent long-term thermal stability.
The molecular structure of polyether-ether-ketone is as described below:
The molecular structure of polyetherketone is as described below:
Compared with polyether-ether-ketone PEEKs, adopt the polyetherketone PEKs of second-order transition temperature 157 DEG C and fusing point 374 DEG C at high temperature to provide the performance of extension, there is all identical advantage, such as rigidity, hardness and chemical resistant properties simultaneously.
With other polymer phase ratios, the continuous use temperature of PEEK and PEK strengthening grade is 240 DEG C, and deforms more than 300 DEG C under load temperature.
PEEK has high-caliber mechanical property and at 250 DEG C, is keeping its tensile strength performance and until 300 DEG C of its flexural strength performances of maintenance.By mixing the solid lubricant of 10%-30%, such as graphite, carbon black, fluoridize PTFE base polymer or perfluoroalkyl ethylene oxy (PFA) resinoid or glass fibre, these mechanical featuress are improved widely.
At high temperature, PEKs provides the wear resistance of maximum 3 times of PEEKs, and taller and bigger at the temperature of 30 DEG C than those of PEEK, keep its machinery and physicals, adapting to higher load simultaneously when not having tension set.
At 200 DEG C, PEEKs and PEKs has chemical resistant properties, and especially to saturated salt solution, gaseous hydrogen sulfide has chemical resistant properties, and at 200 DEG C, under 1.6MPa, goes back hydrolysis, and temperature tolerance is suitable with fluorinated polymer.Table 1 clearly illustrates that to be compared with fluorinated polymer (PTFE with PFA), the mechanical property of PEEK and PEK excellence.
| Performance | PEEK | PEK | PTFE | PFA |
| Fusing point (DEG C) | 343 | 372 | 327 | 310 |
| Continuous use temperature (DEG C) | 260 | 280 | 260 | 260 |
| Tensile strength (MPa) | 100 | 100 | 14-35 | 28-31 |
| Tensile modulus (GPa) | 3.5 | 3.5 | 0.55 | 0.78 |
| Modulus in flexure (GPa) | 4 | 4 | 0.45 | 0.67 |
| Hardness (Shore D) | D85 | D85 | D50-D55 | D60-D64 |
| Compressive strength (MPa) | 118 | 118 | - | 12 |
| Density | 1.3 | 1.3 | 2.1-2.2 | 2.1-2.2 |
Table 1
For PEKs and PEEKs, various implementation is possible, but under involving the temperature by scope being 370 DEG C-420 DEG C, melting changes.Spray by electrostatic powder, by spraying aqueous dispersion, and by thermojet, deposit.In the molten state, PEKs and PEEKs is insensitive to corrosion, but they may by the mold fouling (because in the Martensite Stainless Steel of some grades, comprise such as 13% chromium) formed by the alloy containing copper or chromium, described mould is by catalyzed degradation and produce the coating of less oxidation-resistance.In a word, after passing through melting transition, PEKs and PEEKs is adhered on metal well, if particularly it is not by the words of polishing fully.The roughness allowed accounts for the 20%-25% of the total desired thickness of dry film.Priming paint can be used as adhesion promotor, or by abrasion (sand milling or sandblast cleaning), use surface treatment, by mordant dyeing in chromic acid or by the oxygenant in use air or O
2class or even NH
3class reductive agent carries out plasma treatment, increases binding property.Meanwhile, nearly all metallic surface tendency to oxidize is in the binding property reducing polymkeric substance.In inert atmosphere or by induction, heating of metal proves necessary, not have the surface energy of modified support.Finally, sufficiently cool lentamente, to cause good recrystallization, and keep the proper property of polymkeric substance, such as wear resistance and scratch-proofness.Quick cooling will produce unbodied coating, and described amorphous coating still can by annealing these parts 30 minutes and recrystallization at 200 DEG C.Can, by the process for cooling controlled, such as, adopt the rate of cooling of 10 DEG C/min from 400 DEG C to 250 DEG C, then constant temperature stage of 30 minutes-1 hour at 250 DEG C, thus by increasing degree of crystallinity, increase the mechanical property of polymkeric substance.
In the first phase, the aqueous dispersion that applicants studied the polyether-ether-ketone sold with Vicote F800 series name by Victrex obtains PAEK coating, described aqueous dispersion can contain at least one solid lubricant, the fluorinated polymer of preferred perfluorinated alkoxy vinyl copolymer resin lipid, to strengthen wear resistance and/or at least one inorganic carbon black class solid chemical compound, to strengthen abrasion resistance.The physical-chemical characteristics of the Vicote F800 series suspension of various aqueous phase is have rated in table 2.
Table 2
Applicant also accurately determines the composition of the aqueous dispersion of polyether-ether-ketone powder.Especially, establish this aq suspension can to preferably include scope be 25%-35% weight is the powder of the PEEK of 10 μm with the granularity D90 that trade(brand)name Vicote704 is sold by Victrex.
This aqueous dispersion also can comprise from least one solid lubricant particle in the 1st, 2 and 4 group and preferred 3%-12% weight range with trade(brand)name
the mean particle size range that PFA is sold by DYNEON is the solid lubricant from the 4th class that the perfluoroalkyl ethylene oxy copolymer analog of 20-30 μm fluoridizes powder.
Term as used herein " solid lubricant " refers to solid and stable object (body), once be placed between two friction surfaces, then it can reduce frictional coefficient, and reduces abrasion and the wearing and tearing of effects on surface.These objects can be divided into the different kind according to its mechanism and organization definition thereof, that is:
1st group: its lubricity such as, owing to the solid objects of its crystalline texture, graphite, zinc oxide (ZnO) or boron nitride (BN);
2nd group: the solid objects of the chemical element during its lubricity forms owing to its crystalline texture and their, such as molybdenumdisulphide MoS
2, fluorographite, tin sulfide, bismuth sulfide, tungsten disulfide or Calcium Fluoride (Fluorspan);
3rd group: its lubricity owing to its chemically reactive solid objects, some compounds of such as thiosulfates, or by Desilube Technologies Inc sell Desilube
4th class: its lubricity owing to the plasticity under frictional stress or viscoplastic solid objects, such as tetrafluoroethylene (PTFE) or polymeric amide.
This aqueous dispersion can comprise mechanical toughener, and the preferable range BET specific surface area scope that to be 0.5%-1% weight sold with trade(brand)name Printex by Evonik is for 25-300m
2/ g and mean particle size range are the charcoal blacks of 1-5 μm.
This aqueous dispersion can comprise the 2.5%-10% weight that scope is suspension weight, more preferably scope is the coalescing agent of the ethylene glycol list-butyl ether class of 2.5%-5% weight, it preferably has vaporator rate and boiling spread is fast 100 DEG C-200 DEG C, so that by outside plasticizing polymerization thing entity, promote the coalescent of film or formed, and the surface tension of modified suspension, to contribute to spreading out.
Aqueous dispersion can comprise tensio-active agent, with the non-ionic wetting of preferred dioctyl sulfosuccinate class and dispersion agent (sulfuric acid in the mixture of water and ethanol and aliphatic ester compound), its scope is the 2.5%-10% of suspension weight, be 2.5%-5% weight with preferable range, to improve soaking and preventing powder from avoiding settling from solution of carrier.
About the method for end 1, the 2 deposited on portions dry film at threaded tubular component, applicant establishes and can use or dry or moistening operation, uses static gun, by spraying, applies Vicote704 polyether-ether-ketone powder level.
In the first variant, before applying PEEK powder, preheating end 1,2 part is to 400 DEG C.Next, the part maintaining coating is at the temperature of 360 DEG C-420 DEG C 2 minutes in scope, and preferred under the starting temperature of 400 DEG C, generates good appearance.Can repeatable operation for several times so that the thickness needed for producing.Powder must be made at 180 DEG C minimum 2 hours to dewater.
In the second variant, by the cold aq suspension (it can or can not strengthen) of pneumatic spraying Vicote704 powder, coating end 1,2 part.For this method, preferred end 1,2 part uses solvent, preferred polar aprotic solvent, such as acetone fully clean and degreasing.
Can use the air gun system with gravity feed rifle and cup, apply, its medial end portions 1,2 part at ambient temperature.The temperature of preferred mixture is close to envrionment temperature, and described envrionment temperature preferable range is 20 DEG C-30 DEG C.
The diameter range of rifle mouth is preferably 0.7-1.8mm, and minimum gas pressure 4bar, preferably within the scope of 4-6bar.
Then, the part of coating is left standstill the time period at ambient temperature within the scope of 5-10 minute.
At the temperature of 120 DEG C, this part is placed in the time period of in baking oven or stove 5-10 minute.By such as responding to, carry out this drying operation.
Next, or 400 DEG C at or at a lower temperature, be placed in baking oven by this part, the speed being then 10 DEG C-20 DEG C/min with scope makes it to be warmed up to 400 DEG C.
Once reach the maximum temperature of metal, then thread head 1,2 parts leave standstill 5-15 minute at this temperature, and preferably at least 10 minutes, to allow dry film to fuse completely and to form uniform film.
Then from stove, take out threaded end portions 1,2, and allow to be cooled to envrionment temperature.Rate of cooling is preferably slow, that is scope be l DEG C/min-200 DEG C/min, to obtain half crystal structure.
The replacement scheme of electrostatic spraying, by using heating gun, is sprayed by dry heat, applies Vicote powder to thread head 1,2 parts form.In this process, preferred end 1,2 part ideally cleans and uses solvent, preferred polar aprotic solvent, such as acetone degreasing.
In baking oven or stove, this part of preheating at 260 DEG C.Use the heating gun with directed gas, allow polyarylether ketone powder to be heated to fusing point, accelerate and be transported in substrate, thus apply Vicote powder in this part.This operation is followed by being cooled fast to envrionment temperature in atmosphere.Can repeatable operation for several times, to obtain desired thickness.
The thickness range of dry coating is 20-70 μm, and preferable range is 30-50 μm.
This test forms by evaluating some parameter values, that is:
Under high Hertz stress, at the friction torque (Bridgman test) at surface in contact place;
At the bounding force (scratch test, crosscut adhesion test) of suprabasil film
Moisture-resistant medium exposed property;
Water resistant is immersion;
High-pressure anti-wear (Falex adaptive faculty).
Bridgman test can be determined in the special screw rod attended operation process of " senior " web member, the tribology feature of dry film pigment.More accurately, simulate and measure anti-shoulder moment of torsion (torque on shoulder resistance) CSB, also referred to as ToSR (anti-shoulder moment of torsion).In the screw rod attended operation process that the senior web member used in oily industry is special, produce this moment of torsion and be illustrated in Fig. 2.
The curve representation of Fig. 2 as the rotating cycle carried out function be screwed into (or clamping) moment of torsion.Can find out, the torque curve that is screwed into of " senior " web member is divided into four parts.
In first part P1, the external screw-thread of the pin members (or male joint) in the first component of threaded tubular connection does not still have airtight with the internal whorl radial direction of the corresponding parent form screw member (or female joint) in the second component of identical threaded tubular connection.
In second section P2, the geometrical interference of the screw thread in male and parent form screw member produces radial airtight, wherein when screw rod connect continue time, the airtight increase of described radial direction (thus generate little, but increase be screwed into moment of torsion).
In Part III P3, at the corresponding sealing face of the sealing face radial interference parent form screw member of the outer circumference of the end sections of male screw member, produce metal/metal sealing.
In Part IV P4, the circular surface that the front side end surface of male screw member is adjacent with the assembling of parent form screw member is axially adjacent.This first part P4 corresponds to the end segment of assembling (makeup).
Assembling moment of torsion CAB (it corresponds to the end of Part III P3 and the starting end of Part IV P4) is called shoulder moment of torsion.
Assembling moment of torsion CP (it corresponds to the end of Part IV P4) is called plasticizing moment of torsion.Exceed this plasticizing moment of torsion CP, then think that viscous deformation is carried out in male assembling adjacent (end sections of male screw member) and/or parent form assembling adjacent (being positioned at the region after the circular abutment surface of parent form screw member), wherein by plastifying sealing face equally, described viscous deformation can the deteriorated performance with regard to the tightness of the Contact of sealing face.
The difference of plasticizing moment of torsion CP and shoulder moment of torsion CAB value is called anti-shoulder moment of torsion CSB (CSB=CP-CAB).Threaded tubular connection assembling end be placed in best airtight under, this is the optimal mechanical strength (such as, with regard to drawing force, and riving once in a while just in use) of threaded connector and the guarantee of optimal seal performance.
Therefore the obligated definition of the threaded connector for given type of the planner of threaded connector best assembling torque value, for all connections of this kind of web member, described value must lower than plasticizing moment of torsion CP (avoiding the shortcoming plastifying juncture and cause) and higher than shoulder moment of torsion, CAB.The terminal assembling that moment of torsion is less than CAB can not ensure correct relative positioning that is positive and female element, and the effective interference fit therefore between their sealing face.In addition, there is the risk of riving.For the web member of identical type, the virtual value of shoulder moment of torsion CAB fluctuates very large from a web member to another web member, this is because it depends on the diameter of sun and negative thread and sealing face and axially cuts tolerance; Best assembling moment of torsion should be significantly higher than shoulder moment of torsion CAB.
As a result, anti-shoulder torque value CSB is higher, then determine that the border of the assembling moment of torsion optimized is larger, and the anti-operational stresses induced of more threaded connector.
Use the machine of Bridgman type, carry out rub(bing)test.At the article " Plastic flow between Bridgmananvils under high pressures " of the people such as DKuhlmann-Wilsdorf, J.Mater.Res., vol6, no12, particularly depict the machine of this type in 1991 12 months.Sketch plan and the function example of Bridgman machine is illustrated in Fig. 5.
This machine comprises: disk DQ, and it can select rotary actuation under speed; First platform (anvil) ECl, it is preferably cone type, is for good and all fixed on the first surface of disk DQ; Second platform EC2, it is preferably cone type, is for good and all fixed on second relative with the first surface of disk DQ; One EP1 and the 2nd EP2 pressure member, such as piston, it can produce the axle pressure P of selection; 3rd platform EC3, it is preferably cylinder type, is for good and all fixed on a face of the first pressure member EP1; 4th platform EC4, it is preferably cylinder type, is for good and all fixed on a face of the second pressure member EP2.
In order to test lubricant composition, cover two sheet material identical with forming screw member, to form a S1 and the 2nd S2 sample with described composition.Next, between the free surface the first sample S1 being placed in an EC1 and the 3rd EC3 platform, and the second sample S2 is placed between the free surface of the 2nd EC2 and the 4th EC4 platform.Next, rotating-disk DQ under selection speed, adopt simultaneously an EP1 and the 2nd EP2 pressure member each, apply the axle pressure P (such as order of magnitude 1GPa) selected, and measure each sample S1, the assembling moment of torsion that S2 lives through.Axle pressure is selected, speed of rotation and rotation angle, so that the Hertz pressure of simulating on assembling junction surface, end and relative rate in Bridgman test.Use this machine, several different parameter can be fixed to (assembling moment of torsion, speed of rotation), to produce predetermined assembling moment of torsion on sample S1 and S2, therefore detect these samples S1 and S2 and whether closely follow given assembling torque curve, especially before wearing and tearing, whether they can reach whole number of turns, and described whole number of turns at least equals the threshold value selected relative to selected assembling moment of torsion.
In the present case, the contact pressure of selection is 1GPa, and speed of rotation is 1rpm.Sample is formed, machining, then with different dry film formulation coating by the stainless steel containing 13%Cr.
The bounding force that in Fig. 4, illustrated scratch test permission prepares on surface to be determined or surface or binding property.The method suffers the spherical-shaped beads increased under load that deformation of thin membrane is formed by shearing and adopting, the tribology parameters that it also allows mensuration two main, that is frictional coefficient and be equivalent to the critical load occurring film cohesion loss.
Experiment condition uses the spherical indenter that formed by the Inconel718 of diameter 5mm and by the metal sample formed by the phosphoric acid salt of zinc or manganese or the XC48 carbon steel of electrolysis Cu-Sn-Zn settling process.Parameter is: be increased to 310N in the load of 15N/s lower load of advancing the speed from 10N, or is increased to 750N in the load of 25N/s lower load of advancing the speed from 250N.The rate of displacement of bead is the time period (course length be 40mm) of 2mm/s through 20s.Think that when it is in the scope of μ=0.05, measured frictional coefficient is low for the load of 10N, and for the load of 310N, μ=0.09.On steel surface, the load measure μ for 310N is 0.07.It should be noted that and need clearly to list for the load the test of each type coating and operational condition.
Crosscut adhesion test, by when by carrying out cutting drawing lattice to coating, until when described substrate is divided into six classes, evaluates the resistance composition that single or multiple lift coating is separated from substrate.Coating must correspond to 0 grade of iso standard 2409 (2007) to the excellent adhesion of substrate: preferably otch has smooth edge, without the square delamination of stroke lattice.In order to consider environment, after being placed in moist medium (35 DEG C and 90%RH), carry out crosscut adhesion test.Outward appearance does not change, and does not have sand holes, not corrosion, not be full of cracks, does not have fouling to correspond to grade in iso standard 4628, and does not have fusible loss to be the feature of good moisture resistance.
Corrosion test is made up of the neutral salt spray test carried out under the following conditions in climatic chamber: at 35 DEG C, 50g/L25 DEG C of lower density scope is adopted to be 1.029-1.036, at 25 DEG C, pH scope is the salts solution of 6.5-7.2, and reclaims with the mean rate of 1.5ml/h.
After exposure, then the complete sample of the maintenance of not getting rusty must correspond to the ReO level of iso standard 9227.The method provides maintenance to have or the check system of the suitable quality of the metallic substance of unshielded coating (metal on the metal material or organic coating).
Water tolerance test, by according to the DIN standard 50017 of carrying out in climatic chamber, carries out accelerated corrosion test composition to sample.This test comprises circulation every day one, and it passes through condensation connate water steam by under following condition (35 DEG C, lower 8 hours of 90% relative humidity (RH)), then allows sample drying composition.After 7 circulations, test, whether the substrate observing coated protection corrodes.
Excellent resistance must correspond to the grade of iso standard 4628: with zinc (8-20g/m
2the phosphoric acid salt of deposition) or manganese phosphatizing treatment or do not process or the chromium of the ternary Cu-Sn-Zn alloy treatment that by electrolytic deposition middle layer is Ni or carbon steel sheet do not corrode, do not have sand holes, be full of cracks, does not have fouling.
Water immersion test is much harsher than the water tolerance test of DIN standard 50017.It is made up of the water tolerance of testing coating.It derives from ASTM standard D870-09, and this standard relates to industry and motor vehicle paint.
In water, dipping can cause coating degradations.Knowledge about the mode of flooding in coating water resistant can be used for expecting its work-ing life.Can by many factors, the defect especially in coating itself, the pollution of substrate, or surface prepares not enough, causes the fracture in water immersion test or destruction.Therefore, this test can be used for evaluating independent coating or whole coating systems.
This test is by baking oven, and at 40 DEG C, in softening water, the half impregnated sample time period of 168 hours formed.Visual Observations Observations binding property, sand holes, rusty stain, or ventilating pit, show the susceptibility of coating to water.
High-pressure anti-wear (also referred to as Falex test) uses the rotary press head compressed between two V-shape block material described in Fig. 6.Especially use at high speeds Falex test, according to ASTM standard D2670 and ASTM D3233, evaluate wear resistance and the extreme pressure property of lubricant fluid, but it also under the low speed, according to ASTM method D2625, can evaluate solid lubricant.Transformation Falex test, to adapt to the threaded connector used in Oil/gas Well, is that it uses:
Half-contact geometry the shape (to catch lubricant body of winning the third place) closed;
Pressure-the speed range matched with web member;
Carry out the possibility of one direction or alternate test, so that simulate assemble and generic operation of riving.
Test conditions is as described below:
Load=785N;
Cycle rate=the 60rpm of pressure head;
Average metal/metallic contact pressure=560MPa;
Pressure head gliding cable structure=20mm/s.
The object of this test is, when not needing to evaluate on web member, for various film, with regard to wearability, simulating and evaluating weather resistance.This test refers to can the performance of more various coating and the actual tests on web member.ASTM standard D2625-94 is used to define wearing and tearing standard, described standard relates to the carrying capacity measuring solid lubricant film, and to correspond to be the initial state of 1130N.mm or the load for 785N with the order of magnitude, the order of magnitude be 0.15 frictional coefficient compare, increasing rapidly of moment of torsion.Usually, do not consider materials and structures, when applied load declines, observe wearing and tearing.
Applicant have rated the performance of the various films adopting the aq suspension of polyether-ether-ketone to obtain, particularly tribological property, especially to compare they and those performances adopting fluoroethane class thermoset film or the visco-plasticity film with wax-like thermoplastic matrix to observe.
Fluoroethane film is made up of the aqueous dispersion of the vinyl fluoride Vinyl Ether using aliphatic polyisocyanate stiffening agent to solidify.
Wax-like thermoplastic matrix comprises at least one polyethylene wax, and mainly overbasic calcium sulphonate, and wherein friction modified colo(u)rant dispersion is in described overbasic calcium sulphonate, described in patent WO2008/139058.
In the first phase, the aq suspension that applicant have rated polyether-ether-ketone by the various suprabasil binding property being specific surface and preparing process, frictional coefficient, anticorrosive protection and water retting feature:
The XC48 carbon steel (XC48AsM) of former state machining;
Z20C13 stainless steel (13Cr);
There is the XC48 carbon steel of the phosphatizing treatment of zinc (PhZn) or manganese (PhMn);
There is the XC48 carbon steel of the Cu-Sn-Zn settling (TA) of electrolysis.
Table 3,4 and 5 outline according to iso standard 2409, and by scratch test with by crosscut adhesion test, the aq suspension of Vicote F804, Vicote F805 and Vicote F807Blk is by the adhesion results be on sample that different surfaces prepares.
Remind, scratch test characterizes the function as the applied load increased, high performance material, the bounding force of preferred thermoset or thermoplastic material herein.Critical load determines the fracture of interface and the bounding force of therefore material, and when material has resistance and binding property, critical load is higher.The minimum critical load of 310N corresponds to the minimal adhesion pressure that can reach 1.1GPa, lower than described pressure, the increase of abraded product amount occurs in contact, and and then abrasion resistance deficiency.
For the crosscut adhesion test (described test is provided in by torn material, and the binding property damaged after interface is measured) according to iso standard 2409, mark 0 corresponds to excellent binding property, and marks the binding property of the non-constant of 5 definition.
| Surface prepares | XC48AsM | PhMn | TA |
| Binding property, scratch test (Lc, unit N) | 242 | 750 | 400 |
| Binding property, ISO2409 | 0 | 0 | 0 |
The bond properties of table 3:Vicote F804
The bond properties of table 4:Vicote F805
| Surface prepares | XC48AsM | 13Cr | PhZn | PhMn | TA |
| Binding property, scratch test (Lc, unit N) | 750 | 254 | 50 | 750 | 188 |
| Binding property, ISO2409 | 0 | 0 | 5 | 0 | 0 |
The bond properties of table 5:Vicote F807Blk
The film tested has not enough bounding force, prepares to have nothing to do with the surface of carrying out on the carbon steel with phosphorylation zinc, exception be the carbon steel with phosphorylation manganese.In addition, poly (ether ether ketone) film prepares to have very little consistency to phosphorylation zinc class surface.
In order to explain these results, the event of the roughness that applicant obtains under also been evaluated and not having Phosphorylation status.Adhesion mechanism due to poly (ether ether ketone) film is the physical adhesion by mechanical keying (keying) substantially, and the roughness of substrate is deciding factor.
Meanwhile, recommend by spraying sand milling substrate, so that the roughness Ra (Ra is the arithmetical av of the average line relative to roughness amplitude) of the final film thickness 20% or 25% needed for obtaining, to guarantee the binding property that film is good, namely Ra scope is the minimum value of 4 μm-6 μm.According to iso standard 1997, use rugosimeter, measure roughness.
| Surface prepares | XC48AsM | 13Cr | PhZn | PhMn | TA |
| Ra(μm) | 0.9±0.05 | 0.09 | 0.8±0.05 | 1.6±0.1 | 1±0.2 |
| Rz(μm) | 4.8±0.2 | 0.9±0.1 | 5.1±0.3 | 11.1±1.0 | 8±1.4 |
Table 6: the function prepared as surface, the roughness of sample
Table 6 has been set forth the relatively high roughness obtained by phosphorylation manganese and is provided good bondability.It also shows that very slight polar surfaces prepares, and such as electrolytic deposition ternary Cu-Sn-Zn alloy does not contribute to bonding.
In view of these the first results, applicant determines to measure the erosion resistance of the substrate only with natural low erosion resistance, thus gets rid of the Martensite Stainless Steel (it is greater than 180N to the critical bonding load of poly (ether ether ketone) film) containing 13% chromium.
The thickness range of the film produced by the pneumatic spraying of low temperature is 20-45 μm.According to iso standard 4528-3, measure the corrosion degree within the scope of ReO and Re9.According to standard ISO 4628-2, be determined at the sand holes in 2S2 (lower concentration sand holes and little size) and 5S5 (sand holes of generalization (generalized) and large size) scope and extent of delamination.Result is outlined in table 7 and 8.
Table 7: adopt the erosion resistance that the different surfaces of Vicote F805 prepares
Table 7: adopt the erosion resistance that the different surfaces of Vicote F807Blk prepares
With individual layer poly (ether ether ketone) film coating surface prepare erosion resistance be not enough in broad terms, exception be Cu-Sn-Zn electrolytic deposit, although have low binding property or strong cohesion loss under stress.This result also shows, compared with Vicote F805, the Vicote F807Blk poly (ether ether ketone) film containing inorganic carbon black compounds has erosion resistance relatively preferably, and prepares irrelevant with surface.Adopt electrolytic deposit, obtain absolute best result, only 5 corrosion pits after 1000 hours.Observing and add graphitized carbon black toughener, by serving as sacrificial anode, strengthening corrosion prevention mechanism.
Finally, applicant have rated in the wide load range between 10N to 750N, by scratch test, carries out the frictional coefficient of the film of abrasive wear.Result is outlined in table 9.
Table 9: average friction coefficient, scratch test
The frictional coefficient of poly (ether ether ketone) film is less than 0.135, prepare irrelevant, and for the polyether-ether-ketone containing perfluoroalkyl ethylene oxy class fluorinated polymer, the frictional coefficient under the average contact pressure of 500MPa reaches 0.075 with surface.
First result shows that individual layer poly (ether ether ketone) film lubricates fully and has corrosion resistance, and this not only depends on the composition of film, and depends on the binding property of substrate.
In subordinate phase, then applicant develops the result improving binding property and corrosion resistance.When this can not time, applicant wants alternative sand milling, and this is that the geometrical shape of parts to be coated causes.Especially applicants studied the composition not changing studied commercial film.In fact, adding proportion be greater than 10% adhesion promotor or corrosion inhibitive pigments can increase PCV when PCV (pigment volume concentration (PVC)) exceeds just sufficient adhesive coated efflorescence material (pigment and filler), and this is that the porosity of the film obtained by commercially available aq suspension and cohesion loss cause.
Also other replacement schemes using Vicote704 polyether-ether-ketone powder can be predicted.
Applicants studied the priming paint adopting and there is adhesion promotor type, increase binding property.Direct bonding between material is rare.Because directly bonding there is no and is connected with Van der Waals force uniquely, but only adopt close contact, occur in material (such as, mica or the silicon) situation of the extreme clean unusual light namely in the distance (nanometer) of atom level.Therefore, if surface irregularity, then this usually can not carry out, and on the contrary, it is suitable for the film with low roughness completely.
Therefore, applicant substantially have studied and passes through melting at 400 DEG C, obtains the film that the method for poly (ether ether ketone) film is compatible.
Priming paint can be the jet sediment of the alloy of iron and the zinc sold by Dacral with trade(brand)name Dacroforge Z, with alternative phosphorylation zinc, but by mechanical injection, sand milling/method of sandblast cleaning acquisition priming paint limits it to be had minor diameter and is using in highly short ducted body.
The PAEK that priming paint is preferably filled.Especially including part by weight at organic polyether-ether-ketone tackiness agent is that the solution of the white mica of 25%-50% or the pigments, mica of meroxene is sold by supplier Victrex with trade(brand)name Vicote F817.
The method applying also melting priming paint is identical with upper strata.On the contrary, rate of cooling is required fast, to obtain the less crystalline texture that more insulate, suppresses the initiation of pit and reduces passive (passive) current density of material.
The thickness range of priming paint is 30-40 μm.
Anticorrosive and the bond properties of the priming paint of use two kinds of different cooling powers method evaluations is outlined respectively in table 10 and 11.
Table 10: adopt the erosion resistance that the different surfaces of Vicote F817 priming paint prepares
| Surface prepares | XC48 asM | TA |
| Binding property, scratch test (Lc, N) | 350 | 344 |
| Binding property, ISO 2409 | 0 | 0 |
| Average COF (10-310N) | 0.164 | 0.160 |
The bond properties of table 11:Vicote F817 and frictional coefficient
Vicote F817 priming paint is protected fully and is had binding property, but oilness is not enough.Lubricity is provided by the PAEK layer on top.
Erosion resistance is outlined, binding property and double-deck frictional behaviour in table 12 and 13.Total thickness containing the film of priming paint and upper strata (finish paint) is 40-70 μm.
Table 12: the erosion resistance that different double layer surface prepares
Table 13: bond properties and double-deck frictional coefficient
Prepare irrelevant with surface, for the average contact pressure of 500MPa, frictional coefficient is enough low, especially for the Vicote F807Blk film of wherein μ=0.085, suitable with the frictional coefficient of fluoroethane or epoxide thermoset film, and must allow to obtain the shoulder torque value being less than best assembling moment of torsion 70%.
In a word, the frictional coefficient of poly (ether ether ketone) film, binding property and anticorrosive protection are significantly improved, preferably adopting the polyether-ether-ketone priming paint with pigments, mica filler, and when more specifically strengthening the upper strata of pigment containing the polyether-ether-ketone of at least one fluorinated polymer of viscous deformation under stress and/or carbon black class machinery.
Finally, applicant passes through the tribology behavior of film of Bridgman test evaluation, to determine anti-shoulder torque value.The anti-shoulder torque value obtained for Vicote F807Blk equals 85% of the reference value for the API RP5A3 grease on XC48 carbon steel and Z20C13 stainless steel.But, cause being difficult to preparing sample and the little diameter of sample means that this numerical value can not be regarded as absolute reference value owing to producing the method for film.
The intramolecular interaction of the crystalline texture in polyether-ether-ketone and many potential Van der Waals force types points to the strong cohesion of this material, and high shearing resistance, and anti-shoulder torque value that therefore may be significantly higher.
Meanwhile, applicant passes through the Falex test evaluation wear resistance of film.The test structure matched with web member can be included in individual layer or bilayer a pair vee-block material having and adopt the different surfaces of PEEK film coated to prepare, the XC48 carbon steel pressure head of V-shaped block material and former state machining or the Z20C13 stainless steel pressure head containing 13% chromium.
The test conditions of 785N load is used to correspond to contact pressure and pressure-speed modulus (the PV)=11.2MPa.m/s of average 150MPa, described contact pressure is relatively being screwed into the record in process (100-300MPa) close to being in when shoulder starts at screw thread and load-bearing surface, described pressure-speed modulus is close to employing PV=5MPa.m/s, at load flank (load flank) place, damage the modulus of law at the built-in Vertical Mill of screw thread.
Applicants studied the polyether-ether-ketone that Vicote F805 and F807Blk strengthens.
During Fig. 6 shows and uses on current web member, compared with wax-like thermoplasticity solution, the weather resistance that double-deck Vicote F817/Vicote F807 Blk film is very good, although be regarded as wear-resisting (see document WO2008/032872) with the surface treatment of ternary electrolytic deposit class, but never obtain the wearing and tearing defined according to ASTM standard D2625-94, and under adopting the wax-like thermoplasticity solution conditions of HMS3, after 51 minutes, obtain described wearing and tearing.Relatively low and constant coefficientoffrictionμ=0.08 shows low-down abrasive wear.
In order to measure the wear resistance limit of following film, the Falex test that applicant's working load increases within the scope of 1335N-4200N, have rated weather resistance and the frictional coefficient of film.Gliding cable structure is 10mm/s, and this is contrary with the 20mm/s used before.Result has been shown in Fig. 7.
This result shows, for 350MPa average contact pressure there are not wearing and tearing, and prove the very high wear resistance of film of the present invention.When the pressure was increased, frictional coefficient also reduces and within the scope of 0.056-0.078.
In order to prove at sample, especially have on the sedimental carbon steel of electrolysis Cu-Sn-Zn and use Falex and scratch test, the wear resistance observed in the lab and frictional coefficient, applicant " 29#L80VAM TOP HT web member assembles in 7 to wear height sensitivity.Assembling moment of torsion is 29900N.m.
By the female end portion 2 of electrolytic deposit process carbon steel, with by phosphorylation zinc process male end portion 1 also with the acrylic resin coating that the UV described in patent disclosure WO2006/104251 is curable.Under the rate of cooling being less than 5 DEG C/min, double-deck PEEK film is applied on the tube stub processed.Table 14 outlines assembling result.
" 29#L80VAM TOP HT-CW UD assembles the comparison of result to table 14:7
Gained assembling result proves the wear-resisting property that poly (ether ether ketone) film and the poly (ether ether ketone) film especially strengthened are given prominence to.
Table 15:7 " the result that 29#L80VAM TOP HT assembles
Therefore, the present invention proposes when be applied to steel surface or containing at least 13% chromium steel on the surface time, there is the lubricant film of very interesting wear resistance.It also allow use need not be good binary Cu-Sn or ternary Cu-Sn-Zn class electrolytic deposit.
Claims (19)
1., for drilling or the threaded tubular component of process oil gas well, described tubular member is in its end (1; 2) one of place has the threaded area (3 of making on its periphery or inner peripheral surface; 4), threaded area is made and is depended on that thread head is male or parent form, end (1 on its periphery or inner peripheral surface; 2) at least one lubrication dry film (12) be coated with at least partially containing the PAEK of at least 65% weight, it is characterized in that lubrication dry film (12) has the structure that crystallinity range is 10%-35%, and comprise at least one the 4th class solid lubricant that part by weight scope is 10%-35% further, described 4th class solid lubricant be its lubricity owing to the plasticity under frictional stress or viscoplastic solid, wherein said threaded area at least partly by lubrication dry film be coated with.
2. the threaded tubular component of claim 1, is characterized in that PAEK is selected from polyether-ether-ketone, polyetherketone and composition thereof.
3. the threaded tubular component of claim 1, is characterized in that lubrication dry film (12) comprises the perfluoroalkyl ethylene oxy multipolymer that part by weight scope is 10%-30%.
4. the threaded tubular component of claim 1, it is characterized in that lubrication dry film (12) comprises the mechanical toughener being selected from following pigment that part by weight scope is 1%-15%: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS2 or WS2-soccerballene.
5. the threaded tubular component of claim 1, the part that it is characterized in that being coated with lubrication dry film (12) experienced by advance and is selected from sand milling, manganese phosphorylation, electrolytic deposition Cu or Cu-Sn-Zn alloy, and by the stage of surface preparation in jet deposition Fe and Zn alloy.
6. the threaded tubular component of claim 1, the part that it is characterized in that being coated with lubrication dry film (12) is in advance with having hemihedral crystal structure and polyether-ether-ketone priming paint containing pigments, mica is coated with.
7. the threaded tubular component of claim 1, is characterized in that whole threaded area (3; 4) lubrication dry film (12) is coated with.
8. the threaded tubular component of claim 1, is characterized in that it comprises metal/metal sealing face, and described sealing face is coated with lubrication dry film (12).
9. a threaded tubular connection, it comprises male threaded tubular component and box tubular component, and one is assembled in another, and at least one that it is characterized in that in described threaded tubular component defined according to any one claim aforementioned.
10., for drilling or the coating process of threaded tubular component of process oil gas well, described tubular member is in its end (1; 2) one of place has the threaded area (3 of making on its periphery or inner peripheral surface; 4), threaded area is made and is depended on that thread head is male or parent form on its periphery or inner peripheral surface, it is characterized in that the method comprises the steps:
Produce and be included in the mixture that the part by weight scope suspended in water is the polyarylether ketone powder of 25%-35%, described mixture also comprises at least one the 4th class solid lubricant that part by weight scope is 3%-12%, and described 4th class solid lubricant is that its lubricity is owing to the plasticity under frictional stress or viscoplastic solid;
Described mixture is applied to the end (1 of described threaded tubular component; 2) in part;
The end (1 of dry so coating under the temperature range of 100 DEG C-150 DEG C; 2) part, lasts 5-10 minute;
Under the temperature rise rate of 10 DEG C-20 DEG C/min, the end (1 that heating is so coated with; 2) part is to the temperature of 350 DEG C of-450 DEG C of scopes, lasts 5-15 minute;
Under the rate of cooling being less than 10 DEG C/min, the end (1 that cooling is so coated with; 2) part is to envrionment temperature, to obtain the structure of crystallization substantially.
The coating process of the threaded tubular component of 11. claims 10, it is characterized in that this mixture also comprise part by weight scope be 2.5%-10% there is rapid evaporation rate and boiling spread is the coalescing agent of 100 DEG C-200 DEG C.
The coating process of the threaded tubular component of 12. claims 10 or 11, is characterized in that this mixture comprises the non-ionic wetting and dispersion agent that part by weight scope is 2.5%-10% further.
The coating process of the threaded tubular component of 13. claims 10, it is characterized in that the 4th class solid lubricant is perfluoroalkyl ethylene oxy multipolymer, its part by weight scope is 3%-12%.
The coating process of the threaded tubular component of 14. claims 10, it is characterized in that this mixture also comprises the mechanical toughener being selected from following pigment that part by weight scope is 0.5%-5%: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS2 or WS2-soccerballene.
The coating process of the threaded tubular component of 15. claims 10, is characterized in that using pneumatic fog system to be coated with end (1; 2) part, the diameter range of described system is 0.7-1.8mm and air pressure range is 4-6 bar.
The coating process of the threaded tubular component of 16. claims 10 or 11, it is characterized in that, before applying mixture to end sections, carrying out being selected from following stage of surface preparation: sand milling, manganese phosphorylation, electrolytic deposition Cu or Cu-Sn-Zn alloy, and by jet deposition Fe and Zn alloying pellet.
The coating process of the threaded tubular component of 17. claims 10 or 11, is characterized in that before applying mixture to end sections, carries out having half crystal structure and the stage of surface preparation formed containing the polyether-ether-ketone priming paint of pigments, mica by producing.
18. for drilling or the coating process of threaded tubular component of process oil gas well, and described tubular member is in its end (1; 2) one of place has the threaded area (3 of making on its periphery or inner peripheral surface; 4), threaded area is made and is depended on that thread head is male or parent form on its periphery or inner peripheral surface, it is characterized in that the method comprises the steps:
Heat the end (1 of described threaded tubular component; 2) part is the temperature of 360 DEG C-420 DEG C to scope;
Spray the end (1 of PEK and/or PEEK powder to described threaded tubular component; 2) in part;
Under the temperature range of 360 DEG C-420 DEG C, maintain the end (1 of so coating; 2) part, lasts 1-4 minute;
Be less than under the rate of cooling of 10 DEG C/min, the end (1 that cooling is so coated with; 2) part is to envrionment temperature, to obtain the structure of crystallization substantially.
The coating process of the threaded tubular component of 19. claims 18, is characterized in that the defatting step carrying out part to be coated before the described part of heating.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR10/04399 | 2010-11-10 | ||
| FR1004399A FR2967199B1 (en) | 2010-11-10 | 2010-11-10 | METHOD FOR COATING A THREADED TUBULAR COMPONENT, THREADED TUBULAR COMPONENT AND RESULTING SEAL |
| PCT/EP2011/005524 WO2012062426A1 (en) | 2010-11-10 | 2011-11-02 | Process for coating a threaded tubular component, threaded tubular component and resulting connection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103221519A CN103221519A (en) | 2013-07-24 |
| CN103221519B true CN103221519B (en) | 2015-04-15 |
Family
ID=44245076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201180053943.5A Active CN103221519B (en) | 2010-11-10 | 2011-11-02 | Process for coating a threaded tubular component, threaded tubular component and resulting connection |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US20130320665A1 (en) |
| EP (1) | EP2638134B1 (en) |
| JP (1) | JP6018576B2 (en) |
| CN (1) | CN103221519B (en) |
| AR (1) | AR083823A1 (en) |
| AU (1) | AU2011328484B2 (en) |
| BR (1) | BR112013011454B1 (en) |
| CA (1) | CA2815723C (en) |
| EA (1) | EA024642B1 (en) |
| FR (1) | FR2967199B1 (en) |
| MX (1) | MX2013005243A (en) |
| UA (1) | UA112064C2 (en) |
| WO (1) | WO2012062426A1 (en) |
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| EP2150740B2 (en) | 2007-04-13 | 2017-10-18 | Vallourec Oil And Gas France | Tubular threaded member with dry protection coating |
| FR2981395B1 (en) | 2011-10-14 | 2016-04-01 | Vallourec Mannesmann Oil & Gas | TUBULAR THREADED COMPONENT AND RESULTING SEAL |
| FR2985297B1 (en) | 2011-12-29 | 2016-04-01 | Vallourec Mannesmann Oil & Gas | TUBULAR THREADED COMPONENT AND METHOD FOR COATING SUCH TUBULAR THREADED COMPONENT |
| JP6428101B2 (en) * | 2014-09-26 | 2018-11-28 | 住友電気工業株式会社 | Optical fiber core and optical fiber ribbon |
| CA2920030A1 (en) | 2015-02-03 | 2016-08-03 | 925599 Alberta Ltd. | Reinforced pipe connector |
| MX2017012976A (en) * | 2015-04-10 | 2018-06-06 | 925599 Alberta Ltd | Pipe connector. |
| US11339634B2 (en) | 2015-04-10 | 2022-05-24 | 925599 Alberta Ltd. | Pipe connector |
| BR112018007949B1 (en) * | 2015-11-30 | 2022-04-05 | Halliburton Energy Services, Inc | Oilfield tool, method and system for oilfield operations. |
| EP3192853B1 (en) * | 2016-01-15 | 2023-04-26 | Sikemia | Method for treating a surface in order to obtain a hydrophobic and/or oleophobic coating |
| RU2626390C1 (en) * | 2016-09-19 | 2017-07-26 | Акционерное общество "Обнинское научно-производственное предприятие "Технология" им. А.Г. Ромашина" | Method for determining nature of dielectrics' conduction |
| AR117811A1 (en) * | 2019-01-16 | 2021-08-25 | Nippon Steel Corp | THREADED CONNECTION FOR PIPES OR PIPES, AND METHOD FOR PRODUCING A THREADED CONNECTION FOR PIPES OR PIPES |
| US20200378194A1 (en) * | 2019-05-28 | 2020-12-03 | Saudi Arabian Oil Company | Casing With External Thread and Methods of Manufacture |
| JP7336311B2 (en) * | 2019-08-21 | 2023-08-31 | 信越ポリマー株式会社 | dummy wafer |
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- 2011-11-02 US US13/884,717 patent/US20130320665A1/en not_active Abandoned
- 2011-11-02 MX MX2013005243A patent/MX2013005243A/en active IP Right Grant
- 2011-11-02 JP JP2013538092A patent/JP6018576B2/en active Active
- 2011-11-02 BR BR112013011454-1A patent/BR112013011454B1/en active IP Right Grant
- 2011-11-02 EP EP11779106.1A patent/EP2638134B1/en active Active
- 2011-11-02 CN CN201180053943.5A patent/CN103221519B/en active Active
- 2011-11-02 AU AU2011328484A patent/AU2011328484B2/en not_active Ceased
- 2011-11-02 CA CA2815723A patent/CA2815723C/en active Active
- 2011-11-02 EA EA201370114A patent/EA024642B1/en not_active IP Right Cessation
- 2011-11-02 WO PCT/EP2011/005524 patent/WO2012062426A1/en active Application Filing
- 2011-11-09 AR ARP110104195A patent/AR083823A1/en active IP Right Grant
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Also Published As
| Publication number | Publication date |
|---|---|
| EP2638134A1 (en) | 2013-09-18 |
| UA112064C2 (en) | 2016-07-25 |
| AU2011328484A1 (en) | 2013-05-02 |
| JP6018576B2 (en) | 2016-11-02 |
| EA024642B1 (en) | 2016-10-31 |
| MX2013005243A (en) | 2013-06-12 |
| WO2012062426A1 (en) | 2012-05-18 |
| CA2815723C (en) | 2018-08-21 |
| FR2967199B1 (en) | 2013-11-01 |
| EP2638134B1 (en) | 2019-07-24 |
| US20130320665A1 (en) | 2013-12-05 |
| AR083823A1 (en) | 2013-03-27 |
| FR2967199A1 (en) | 2012-05-11 |
| BR112013011454B1 (en) | 2019-04-24 |
| AU2011328484B2 (en) | 2015-11-19 |
| BR112013011454A2 (en) | 2016-08-09 |
| JP2013545946A (en) | 2013-12-26 |
| CA2815723A1 (en) | 2012-05-18 |
| EA201370114A1 (en) | 2013-12-30 |
| CN103221519A (en) | 2013-07-24 |
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