CN103221519A - 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
- CN103221519A CN103221519A CN2011800539435A CN201180053943A CN103221519A CN 103221519 A CN103221519 A CN 103221519A CN 2011800539435 A CN2011800539435 A CN 2011800539435A CN 201180053943 A CN201180053943 A CN 201180053943A CN 103221519 A CN103221519 A CN 103221519A
- Authority
- CN
- China
- Prior art keywords
- tubular member
- threaded tubular
- threaded
- coating
- 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.)
- Granted
Links
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Images
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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
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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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- Environmental & Geological Engineering (AREA)
- Metallurgy (AREA)
- Paints Or Removers (AREA)
- Non-Disconnectible Joints And Screw-Threaded Joints (AREA)
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- Perforating, Stamping-Out Or Severing By Means Other Than Cutting (AREA)
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 be used for the tubular member of the probing of oil gas well and/or operation and relate to the thread head of this member more accurately.Described end is public type or parent form, and can be connected to the respective end of another member, forms web member.
The invention still further relates to the method for on this tubular member, producing wear-resistant film.
The member that term " is used for the probing and the operation of oil gas well " is meant that shape is essentially tubulose, plan is connected on another member of same type or in other cases, finally constitute or be used to drill the vertical tube that the tubing string of oil gas well or plan are used to safeguard (being also referred to as the renovation vertical tube) or operate this well, for example the string of casing or the tubing string that use at the operation well of vertical tube or be used for.The present invention also can be applicable to the member that uses, for example drilling rod, heavy drilling rod, the part of drill collar and pipe connection and the heavy pipeline that is called drill pipe sub in drill string.
Each tubular member comprises an end that provides of positive thread district end and/or provide the negative thread district, and each end intends adopting the respective end of another member to be screwed into connection.This assembly has been determined web member.
The threaded tubular member connects under the stress of determining, so that satisfy the fastening and seal request that working conditions is forced, because known in well, can require the threaded tubular member to experience several assemblings (makeup)-open (breakout) circulation.
Use the condition of this threaded tubular member to cause inhomogeneous stress, described stress makes need be in the responsive part of these members, and for example threaded area is used coating on adjoining region or the sealing face.
Usually be screwed into operation under high axial load, for example the weight of the pipeline of the length number rice that connects by threaded connector may localize because of the slightly misaligned at screw member axle to be connected.This induces at the threaded area place and/or the risk of wearing and tearing at metal/metal sealing face place.Owing to this reason, need with lubricator be coated with threaded area, abutment surface and metal/metal sealing face.
In addition, store threaded tubular member (several years sometimes), in disagreeableness environment, assemble then.This is for example in the situation of coastal waters situation with salt fog or the land situation in the presence of sand, dust or other pollutents.Therefore, need to use erosion-resisting from the teeth outwards coating, described surface must be by being screwed into (threaded area) or cooperating by interference contact (metal/metal surface).Also need treat surface to prevent corrosion.
Yet, from environmental point of view, as if use the grease that is screwed into that meets API (American Petroleum Institute) standard RP5A3 not constitute long-term solution, this is because these greases contain heavy metal, can be driven away by tubular member and be discharged in environment or the well, thereby cause stopping up, need special clean operation and stop up.In addition, these greases do not provide competent corrosion prevention, and must apply on the spot for each screw rod attended operation.
In order to overcome the long-term erosion resistance of requirement and wear-resistant problem; and satisfy environmental characteristics; the Primary Actor in threaded connector field has developed the solid drying coating (promptly energetically; be not pasty state and not as the viscosity of grease); described coating is a lubricant; play protection again and prevent the corrosive effect, and can be applied on the tubular member at last in factory.
Especially, developed at environment and be inertia and anti abrasive coating.
The present invention is based on following discovery: use PAEK can obtain lubricated dry film, described film highly abrasion-resistant resistance to wears, and has high physical strength and low frictional coefficient, and the operational condition of anti-extreme oil gas well.Employed solution also can be adapted to the metal of the various grades that the web member of the above tubular member of quoting as proof uses.
Both do not describe in the prior art, and do not have hint in the threaded tubular member of above definition, to use this PAEK and performance thereof yet.
More accurately, the present invention relates to be used for the threaded tubular member of the probing and/or the operation of oil gas well, described tubular member has outside it or the threaded area of making on the interior perimeter surface at one end place, this depends on that thread end is public type or parent form, and at least a portion end is coated with at least a lubricated dry film of the PAEK that contains 65% weight at least in described threaded area.
To have given a definition or complementation or alternate optional feature.
PAEK is selected from polyether-ether-ketone (PEEK), polyetherketone (PEK) and composition thereof.
Should have the structure that the degree of crystallinity scope is 10%-35% by lubricated dry film.
Should lubricate the solid lubricant that dry film further comprises at least a the 4th class, its proportional range is a 10%-35% weight.
Should comprise the perfluoroalkyl ethylene oxy multipolymer by lubricated dry film, its proportional range is a 10%-30% weight.
Should comprise the mechanical toughener that is selected from following pigment by lubricated dry film: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS2 or WS2-soccerballene, its proportional range are 1%-15% weight.
The part that has been coated with lubricated dry film has experienced in advance and has been selected from sand milling, phosphoric acid manganese, the electrolytic deposition of Cu or Cu-Sn-Zn alloy and Fe by jet deposition and the stage of surface preparation in the Zn alloy.
The part that has been coated with lubricated dry film has been coated with the priming paint that has the hemihedral crystal structure and contain the polyether-ether-ketone of pigments, mica in advance.
The lubricated dry film of whole threaded area coating.
The threaded tubular member comprises the metal/metal sealing face, and described sealing face has been coated with lubricated dry film.
The invention still further relates to the threaded tubular web member, described web member comprises public type threaded tubular member and parent form threaded tubular member, and one is assembled in another at least one in wherein said threaded tubular member as defined above.
The invention still further relates to that coating is used to drill or the method for the threaded tubular member of process oil gas well, described tubular member locates to have the threaded area of making on its periphery or interior perimeter surface in one of its end, make on the still interior perimeter surface of its periphery of threaded area and depend on that thread head is public type or parent form, this method comprises the steps:
Production is included in the mixture of the polyaryl ether ketone powder that suspends in the water, and its proportional range is a 25%-35% weight;
Apply described mixture to the end sections of described threaded tubular member;
Dry so end sections of coating lasts 5-10 minute under 100 ℃-150 ℃ temperature range;
Under the temperature rise rate in 10 ℃-20 ℃/minute temperature range, heating is the temperature range of the end sections to 350 ℃-450 ℃ of coating so, lasts 5-15 minute;
Under the rate of cooling less than 10 ℃/min, envrionment temperature is arrived in the cooling so end sections of coating, so that obtain crystalline structure basically.
With complementation or the alternate optional feature given a definition.
This mixture comprises that also the boiling spread with rapid evaporation speed is 100 ℃-200 ℃ a coalescing agent, and its proportional range is a 2.5%-10% weight.
This mixture further comprises non-ionic wetting and dispersion agent, and its proportional range is a 2.5%-10% weight.
This mixture also comprises the solid lubricant of at least a the 4th class, and its proportional range is a 3%-12% weight.
The solid lubricant of the 4th class is the perfluoroalkyl ethylene oxy multipolymer, and its proportional range is a 3%-12% weight.
This mixture also comprises the mechanical toughener that is selected from following pigment: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS
2Or the WS2-soccerballene, its proportional range is a 0.5%-5% weight.
Use pneumatic spraying system, the coating end sections, the diameter range of described system is that 0.7-1.8mm and gas pressure range are 4-6bar.
Apply mixture to the end sections before, be selected from the stage of surface preparation in following: sand milling, phosphoric acid manganese, the electrolytic deposition of Cu or Cu-Sn-Zn alloy and Fe and Zn alloying pellet by jet deposition.
Apply mixture to the end sections before, carry out stage of surface preparation, the priming paint that described stage of surface preparation has the hemihedral crystal structure by generation and contains the polyether-ether-ketone of pigments, mica is formed.
The invention still further relates to and be used to drill or the coating process of the threaded tubular member of process oil gas well, described tubular member locates to have the threaded area of making on its periphery or interior perimeter surface in one of its end, this depends on that thread head is public type or parent form, and this method comprises the steps:
The end sections that heats described threaded tubular member is 360 ℃-420 ℃ a temperature to scope, preferably to the temperature that approaches 400 ℃;
Spray PEK and/or PEEK powder to the end sections of described threaded tubular member;
Through scope is time period of 1-4 minute, and the end sections of keeping coating like this preferably approaches 400 ℃ temperature under 360 ℃-420 ℃ temperature range, last 1-4 minute;
Under the rate of cooling less than 10 ℃/min, envrionment temperature is arrived in the cooling so end sections of coating.
Before the described part of heating, preferably make the step of partially skimmed to be coated.
In the following description, in conjunction with reference to the accompanying drawings, the features and advantages of the present invention have been described in further detail.
Fig. 1 is the synoptic diagram by the web member that obtains by two tubular members of assembling connection;
Fig. 2 is the synoptic diagram of the screw rod junction curve of two threaded tubular members;
Fig. 3 is the synoptic diagram with the substrate of lubricated dry film coating;
Fig. 4 is the synoptic diagram of testing apparatus;
Fig. 5 is the synoptic diagram of another testing apparatus;
Fig. 6 and 7 shows trial curve.
Threaded connector shown in Figure 1 comprises first tubular member with turning axle 10 that provides male end portion 1 and second tubular member with turning axle 10 that provides female end portion 2.Stop in two ends 1 and 2 each comfortable terminal surface, described terminal surface is radial oriented with respect to the axle 10 of threaded connector, and provides threaded area 3 and 4 separately, and described threaded area 3 and 4 cooperation mutually interconnects two members for by being screwed into.Threaded area 3 and 4 can be thread type such as trapezoidal, self-locking.In addition, by be screwed into connect two screw members after, the interference that provides plan relative to each other to enter sealing respectively in the male end portion that approaches threaded area 3,4 and female end portion contacts the metal/ metal sealing face 5,6 of (interfering contact).At last, male end portion 1 stops in terminal surface 7, and the respective surfaces 8 that provides in the female end portion 2 is provided described terminal surface 7, when assemble each other two ends.
The applicant also predicts other structures, wherein under situation of the present invention, is substituted (referring to US4822081, US RE30467 and US RE34467) by two surface in contacts 7 and 8 adjacency that form by the fastening cooperation of the self-locking of threaded area 3,4.
Can find out among Fig. 1 and 3 that on its end 1 part (being called substrate 11), with lubricated dry film 12 at least one threaded tubular web member of coating of the PAEK that contains at least 65% weight, described dry film 12 has the structure of at least 10% degree of crystallinity.To remind, by the fusion 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 crystalline PAEK, polyether-ether-ketone (PEEK) especially, theoretical melting enthalpy becomes 122J/g.The advantage of the degree of crystallinity of existence at least 10% provides good mechanical property, especially good anti-shoulder moment of torsion.Yet, preferably keep degree of crystallinity to be lower than 35%, so that with regard to binding property and surface preparation protection prevent corrosion, the feature of maintenance film.
Can obtain the PAEK of use in the present invention by moisture polyether-ether-ketone dispersion or by moisture polyetherketone dispersion.These aqueous dispersions can comprise organic or inorganic machinery toughener, the for example white mica that constitutes by pure aluminium silicate and hydrated potassium or magnesium and/or the pigments, mica of meroxene, has the amorphous alumina that γ crystalline texture and size range are 20-300nm, size range is the TiO 2 pigment of 10-100nm, perfluoroalkyl ethylene oxy copolymer resin (PFA), the amorphous carbon mineral black, diameter is less than the synthetic graphite powder of 5 μ m, by explosion acquisition and size range is the Nano diamond of 4-6nm, the fiber thickness scope is the C type glass of 1-1.3 μ m and diameter D90＜50 μ m, size range is the WS2 soccerballene nano material 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).Polyethersization causes having dystectic hard hemihedral crystal polymkeric substance.They belong to the material category of the peak performance in the thermoplastic material scope.Therefore their second-order transition temperature is 143 ℃ and because they have the character of hemihedral crystal, keeps their good mechanical propertys until approach the temperature (343 ℃) of its fusing point.Their standard-linearity and aromatic structure provide PEEK and the PEK with good long-term thermal stability.
The molecular structure of polyether-ether-ketone is as described below:
The molecular structure of polyetherketone is as described below:
PEEKs compares with polyether-ether-ketone, adopts 157 ℃ of polyetherketone PEKs with 374 ℃ of fusing points of second-order transition temperature that the performance of extension at high temperature is provided, and has all identical advantage, for example rigidity, hardness and chemical resistant propertiess simultaneously.
With other polymer phase ratios, the continuous use temperature that strengthens the PEEK of grade and PEK is that 240 ℃ and the distortion under load temperature are above 300 ℃.
PEEK has high-caliber mechanical property and is keeping its tensile strength performance and until 300 ℃ of its flexural strength performances of maintenance down up to 250 ℃.By mixing the solid lubricant of 10%-30%, graphite for example, carbon black is fluoridized PTFE base polymer or perfluoroalkyl ethylene oxy (PFA) resinoid or glass fibre, and these mechanical featuress are improved widely.
At high temperature, PEKs provides the wear resistance of maximum 3 times of PEEKs, and taller and bigger under 30 ℃ temperature than those of PEEK, keeps its machinery and physicals, is not having to adapt to higher load under the situation of tension set simultaneously.
Under 200 ℃, PEEKs and PEKs have chemical resistant properties, and especially to saturated salt solution, gaseous hydrogen sulfide has chemical resistant properties, and under 200 ℃, go back hydrolysis under 1.6MPa, and temperature tolerance is suitable with fluorinated polymer.Table 1 clearly illustrates that with fluorinated polymer (PTFE and PFA) compares the mechanical property of PEEK and PEK excellence.
| Performance | PEEK | PEK | PTFE | PFA |
| Fusing point (℃) | 343 | 372 | 327 | 310 |
| Continuous use temperature (℃) | 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 implementations are possible, but involve by being that fusion changes under 370 ℃-420 ℃ the temperature in scope.Can spray by electrostatic powder,, deposit by the spraying aqueous dispersion with by thermojet.Under molten state, PEKs and PEEKs are insensitive to corroding, but their may be by the mold fouling that is formed by the alloy that contains copper or chromium (because of in the Martensite Stainless Steel of some grades, comprising for example 13% chromium), and described mould is with catalyzed degradation and produce the coating of less oxidation-resistance.If in a word, after passing through melting transition, PEKs and PEEKs are adhered on the metal well, particularly the words that it is not polished fully.The roughness that is allowed accounts for the 20%-25% of the total desired thickness of dry film.Can use priming paint as adhesion promotor,, use surface treatment, by mordant dyeing in chromic acid or by with airborne oxygenant or O perhaps by abrasion (sand milling or sandblast cleaning)
2Class or even NH
3The class reductive agent carries out plasma treatment, increases binding property.Meanwhile, nearly all metallic surface tendency to oxidize is in the binding property that reduces polymkeric substance.In inert atmosphere or by the induction, it is necessary that heating of metal proves, so that there is not the surface energy of modified support.At last, must enough cool off lentamente, causing good recrystallization, and keep the proper property of polymkeric substance, for example wear resistance and scratch-proofness.Cooling will produce unbodied coating fast, and described amorphous coating still may be passed through annealing these parts 30 minutes under 200 ℃ and recrystallization.Can be by the process for cooling of control, for example, the rate of cooling that adopts 10 ℃/min then 250 ℃ of constant temperature stages of following 30 minutes-1 hour, thereby by increasing degree of crystallinity, increases the mechanical property of polymkeric substance from 400 ℃ to 250 ℃.
In the fs, the applicant has studied the aqueous dispersion acquisition PAEK coating with the polyether-ether-ketone of Vicote F800 series title sale by Victrex, described aqueous dispersion can contain at least a solid lubricant, the fluorinated polymer of preferred perfluorinated alkoxy vinyl copolymer resin lipid, to strengthen wear resistance and/or at least a inorganic carbon black class solid chemical compound, to strengthen abrasion resistance.Estimated the physical-chemical feature of the Vicote F800 series suspension of various waters in the table 2.
Table 2
The applicant has also accurately measured the composition of the aqueous dispersion of polyether-ether-ketone powder.Especially, having established this aq suspension, can to preferably include scope be that 25%-35% weight is the powder of the PEEK of 10 μ m with trade(brand)name Vicote704 by the granularity D90 that Victrex sells.
This aqueous dispersion also can comprise from least a 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 μ m is fluoridized powder.
Term as used herein " solid lubricant " is meant solid and stable object (body), in case place between two friction surfaces, its coefficient of can reducing friction then, and reduce abrasion and wearing and tearing to the surface.These objects can be divided into the different kind according to its function mechanism and organization definition thereof, that is:
The 1st group: its lubricity is owing to the solid objects of its crystalline texture, graphite for example, zinc oxide (ZnO) or boron nitride (BN);
The 2nd group: its lubricity is owing to the solid objects of the chemical element in its crystalline texture and their compositions, for example molybdenumdisulphide MoS
2, fluorographite, tin sulfide, bismuth sulfide, tungsten disulfide or Calcium Fluoride (Fluorspan);
The 3rd group: its lubricity is owing to its chemically reactive solid objects, some compounds of thiosulfates for example, or the Desilube that is sold by Desilube Technologies Inc
The 4th class: its lubricity is owing to plasticity under frictional stress or viscoplastic solid objects, for example polytetrafluoroethylene (PTFE) or polymeric amide.
This aqueous dispersion can comprise mechanical toughener, and preferable range is that 0.5%-1% weight is 25-300m by Evonik with the BET specific surface area scope that trade(brand)name Printex sells
2/ g and mean particle size range are the charcoal blacks of 1-5 μ m.
This aqueous dispersion can comprise that scope is the 2.5%-10% weight of suspension weight, more preferably scope is the coalescing agent of the glycol monomethyl-butyl ether class of 2.5%-5% weight, it preferably has fast, and vaporator rate and boiling spread are 100 ℃-200 ℃, so that by outside plasticizing polymerization thing entity, promote the coalescent of film or formation, and the surface tension of modified suspension, spread out so that help.
Aqueous dispersion can comprise tensio-active agent, non-ionic wetting and dispersion agent (sulfuric acid in water and alcoholic acid mixture and aliphatic ester compound) with preferred dioctyl sulfo-succinic acid salt, its scope is the 2.5%-10% of suspension weight, with preferable range be 2.5%-5% weight so that improve the wetting of carrier and prevent that powder from avoiding settling from solution.
About the method for deposition dry film on 1,2 part of the end of threaded tubular member, the applicant has established and can use or dry or moistening operation, uses static gun, by spraying, applies Vicote704 polyether-ether-ketone powder level.
In first variant, before applying the PEEK powder, preheating end 1,2 part to 400 ℃.Next, the part of keeping coating is under 360 ℃-420 ℃ the temperature 2 minutes and preferred under 400 ℃ starting temperature in scope, generates the surface of good outward appearance.But repeatable operation for several times, so that produce required thickness.Must under 180 ℃, make minimum 2 hours of powder dehydration.
In 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 is used solvent, preferred polar aprotic solvent, and for example acetone fully cleans 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 approaches envrionment temperature, and described envrionment temperature preferable range is 20 ℃-30 ℃.
The diameter range of rifle mouth is preferably 0.7-1.8mm and minimum gas pressure 4bar, preferably in the 4-6bar scope.
Then, the part with coating leaves standstill at ambient temperature the 5-10 minute time period in the scope.
Under 120 ℃ temperature, this part placed in baking oven or the stove 5-10 minute time period.Can carry out this drying operation by for example induction.
Next, or 400 ℃ down or at a lower temperature, this part is placed in the baking oven, be that the speed of 10 ℃ of-20 ℃/min makes it to be warmed up to 400 ℃ then with scope.
In case reach the maximum temperature of metal, then thread head 1,2 part left standstill under this temperature 5-15 minute and preferably at least 10 minutes, so that allow dry film to fuse and form uniform film fully.
From stove, take out thread head part 1,2 then, and allow to be cooled to envrionment temperature.Rate of cooling is preferably slow, that is scope is l ℃/min-200 ℃/min, so that obtain the hemihedral crystal structure.
The replacement scheme of electrostatic spraying is sprayed by dry heat by using heating gun, applies the Vicote powder and forms on thread head 1,2 part.In this method, preferred end 1,2 part ideally cleans and uses solvent, preferred polar aprotic solvent, for example acetone degreasing.
In baking oven or stove, 260 ℃ of these parts of following preheating.Use has the heating gun of directed gas, allows the polyaryl ether ketone powder to be heated to fusing point, quickens and is transported in the substrate, thereby apply the Vicote powder on this part.This operation is followed by be cooled fast to envrionment temperature in air.But repeatable operation for several times, so that obtain desired thickness.
The thickness range of dry coating is 20-70 μ m, and preferable range is 30-50 μ m.
This test is formed by estimating some parameter values, that is:
Under high Hertz stress, the friction torque (Bridgman test) at the surface in contact place;
Bounding force (scratch test, cross-hatching test) at suprabasil film
Moisture-resistant medium exposure property;
Anti-water retting;
High-pressure anti-wear (Falex adaptive faculty).
The 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, be also referred to as ToSR (anti-shoulder moment of torsion).In to oily industry, in the special screw rod attended operation process of employed senior web member, produce this moment of torsion and be illustrated in Fig. 2.
The curve representation of Fig. 2 be screwed into (or clamping) moment of torsion as the function of the rotating cycle that carries out.Can find out that the torque curve that is screwed into of " senior " web member is divided into four parts.
In the P1 of first part, it is radially airtight that the external screw-thread of the pin members (or male joint) in first member of threaded tubular web member does not still have the internal whorl of the corresponding parent form screw member (or female joint) in second member with identical threaded tubular web member.
In second section P2, it is radially airtight that the geometrical interference of the screw thread in public type and the parent form screw member produces, wherein connect when continuing when screw rod, described radially airtight increase (thereby generate little, but increase be screwed into moment of torsion).
In third part P3, the corresponding sealing face at the sealing face radial interference parent form screw member of the outer circumference of the end sections of public type screw member produces the metal/metal sealing.
In the 4th part P4, the axial adjacency of circular surface of the assembling adjacency of the front side end of public type screw member surface and parent form screw member.The P4 of this first part is corresponding to the end segment of assembling (makeup).
Assembling moment of torsion CAB (it is corresponding to the end of third part P3 and the starting end of the 4th part P4) is called the shoulder moment of torsion.
Assembling moment of torsion CP (it is corresponding to the end of the 4th part P4) is called the plasticizing moment of torsion.Exceed this plasticizing moment of torsion CP, think that then public type assembles adjacency (end sections of public type screw member) and/or the parent form assembling is carried out viscous deformation in abutting connection with (being positioned at the circular abutment surface zone afterwards of parent form screw member), wherein by same plasticizing sealing face, but described viscous deformation deterioration is with regard to the performance of the tightness that contacts between the 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).The threaded tubular web member dispose in the assembling end in the best airtight down, this is the optimal mechanical strength (for example, with regard to drawing force, and riving once in a while in the use just) of threaded connector and the assurance of optimal seal performance.
Therefore the obligated threaded connector definition the best at given type of the planner of threaded connector is assembled torque value, all connections for this class web member, described value must be lower than plasticizing moment of torsion CP (so that avoiding plastifying juncture and the shortcoming that causes) and be higher than shoulder moment of torsion, CAB.Moment of torsion is less than the impossible correct relative positioning that guarantees sun and female element of terminal assembling of CAB, and so effective interference fit between their sealing face.In addition, there is the risk of riving.For the web member of same type, the virtual value of shoulder moment of torsion CAB is very big to another web member fluctuation from a web member, and this is because it depends on the diameter and the axial cutting tolerance of sun and negative thread and sealing face; Best assembling moment of torsion should be significantly higher than shoulder moment of torsion CAB.
As a result, anti-shoulder torque value CSB is high more, then determines the big more and more anti-operational stresses induced of threaded connector in border of the assembling moment of torsion of optimization.
Use the machine of Bridgman type, carry out rub(bing)test.At people's such as D Kuhlmann-Wilsdorf article " Plastic flow between Bridgman anvils under high pressures ", J.Mater.Res., vol6, no12 has especially described the machine of this type in 1991 12 months.Illustrate the sketch plan and the function example of Bridgman machine among Fig. 5.
This machine comprises: disk DQ, and it can select rotation driving under the speed; First platform (anvil) ECl, it is preferably the circular cone type, for good and all is fixed on first of disk DQ; The second platform EC2, it is preferably the circular cone type, for good and all is fixed on relative second of with disk DQ first; The one EP1 and the 2nd EP2 pressure member, piston for example, it can produce the axle pressure P of selection; The 3rd platform EC3, it is preferably cylinder type, for good and all is fixed on the face of the first pressure member EP1; The platform EC4 of Siping City, it is preferably cylinder type, for good and all is fixed on the face of the second pressure member EP2.
For the test lubricant composition, cover and two identical sheet material of formation screw member with described composition, so that form a S1 and the 2nd S2 sample.Next, the first sample S1 is placed between the free surface of an EC1 and the 3rd EC3 platform, and the second sample S2 places between the free surface of the 2nd EC2 and the 4th EC4 platform.Next, selecting rotating-disk DQ under the speed, adopt simultaneously an EP1 and the 2nd EP2 pressure member each, apply the axle pressure P (for example order of magnitude 1GPa) of selection, and measure each sample S1, the assembling moment of torsion that S2 lives through.Select axle pressure in the Bridgman test, speed of rotation and rotation angle are so that simulation is at the Hertz pressure and the relative rate on junction surface, place, assembling end.Use this machine, can fix several different parameters to (assembling moment of torsion, speed of rotation), so that on sample S1 and S2, produce predetermined assembling moment of torsion, with therefore detect these samples S1 and whether S2 closely follows given assembling torque curve, especially whether they can reach whole number of turns before wearing and tearing, and described whole number of turns equal the threshold value selected with respect to selected assembling moment of torsion at least.
Under situation of the present invention, the contact pressure of selection is that 1GPa and speed of rotation are 1rpm.Form sample by the stainless steel that contains 13%Cr, machining is then with different dry film formulation coatings.
Illustrated scratch test allows on surface to be determined or prepare on the surface among Fig. 4 bounding force or binding property.This method is by shearing and adopt the spherical-shaped beads that is increased under the load that deformation of thin membrane is formed, and it also allows to measure two main tribology parameters, that is frictional coefficient and the critical load that is equivalent to occur poly-loss in the film.
The metal sample that experiment condition uses spherical indenter that the Inconel718 by diameter 5mm forms and formed by phosphoric acid salt that passes through zinc or manganese or XC48 carbon steel that electrolysis Cu-Sn-Zn settling was handled.Parameter is: load is increased to 310N from 10N under the load of 15N/s is advanced the speed, and perhaps advancing the speed down in the load of 25N/s, load is increased to 750N from 250N.The rate of displacement of bead is that 2mm/s is through the time period of 20s (course length is 40mm).Think load for 10N, when it in μ=0.05 scope the time, measured frictional coefficient is low and for the load of 310N, μ=0.09.On steel surface, be 0.07 at the load measure μ of 310N.Should be noted that load and the operational condition that clearly to list at each type coating test.
The cross-hatching test is divided into six time-likes by when drawing lattice by cutting to coating up to described substrate, estimates single or multiple lift coating isolating resistance from substrate and forms.Coating must be corresponding to 0 grade of iso standard 2409 (2007) to the excellent adhesion of substrate: preferred otch has smooth edges, the square delamination of no stroke lattice.In order to consider environment, in placing moist medium (35 ℃ and 90%RH) after, carry out the cross-hatching test.Outward appearance does not change, and does not have sand holes, not corrosion, and not be full of cracks does not have fouling corresponding to the grade in the iso standard 4628 with not have fusible loss be the feature of good moisture resistance.
Corrosion test is made up of the neutral salt spray test that carries out under the following conditions in climatic chamber: under 35 ℃, adopting 50g/L25 ℃ of lower density scope is 1.029-1.036, at 25 ℃ of following pH scopes salts solution that is 6.5-7.2, and reclaim with the mean rate of 1.5ml/h.
After exposing, the sample that is kept perfectly that does not get rusty then must be corresponding to the ReO level of iso standard 9227.This method provides to be kept or the check system of the suitable quality of the metallic substance of unshielded coating (metal on metallic substance or organic coating).
Water tolerance test is carried out accelerated corrosion test to sample and is formed by according to the DIN standard 50017 of carrying out in climatic chamber.This test comprises circulation every day, and it allows sample drying to form by following to condensation connate water steam in following condition (35 ℃, following 8 hours of 90% relative humidity (RH)) then.After 7 circulations, test, whether the substrate of observing coated protection corrodes.
Good resistance must be corresponding to the grade of iso standard 4628: with zinc (8-20g/m
2Sedimentary phosphoric acid salt) or the manganese phosphorylation handle or do not handle or be the chromium or the not corrosion of carbon steel sheet of the ternary Cu-Sn-Zn alloy treatment of Ni by the electrolytic deposition middle layer, do not have sand holes, be full of cracks does not have fouling.
Water immersion test than the water tolerance test harshness of DIN standard 50017 many.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.
Dipping can cause the coating deterioration in water.Knowledge about the mode of flooding in the anti-water of coating can be used for expecting its work-ing life.Can be by many factors, the defective in the coating itself especially, the pollution of substrate, perhaps the surface is prepared not enoughly, causes fracture or destruction in water immersion test.Therefore, this test can be used for estimating independent coating or whole coating systems.
This test is by in baking oven, and 168 hours time period of half impregnated sample is formed in softening water under 40 ℃.The visual observation binding property, sand holes, rusty stain, or ventilating pit show the susceptibility of coating to water.
High-pressure anti-wear (being also referred to as the Falex test) uses the rotary press head of describing among Fig. 6 that compresses between two V-shape piece material.Especially under high speed, use the Falex test,, estimate the wear resistance and the extreme pressure property of lubricant fluid, but it also can according to ASTM method D2625, estimate solid lubricant under low speed according to ASTM standard D2670 and ASTM D3233.Transform the Falex test,, be its use to adapt to the threaded connector that in the oil gas well, uses:
The contact geometry shape (to catch the lubricant body of winning the third place) of half-sealing;
Pressure-the speed range that matches with web member;
Carry out folk prescription to or the possibility of alternate test so that the simulation assembling and the generic operation of riving.
Test conditions is as described below:
Load=785N;
Cycle rate=the 60rpm of pressure head;
Average metal/metal contact pressure=560MPa;
Pressure head slip speed=20mm/s.
The purpose of this test is need at various films, with regard to wearability, not simulate and also estimate weather resistance under situation about estimating on the web member.This test be meant can more various coatings performance and actual tests on web member.Use ASTM standard D2625-94 definition wearing and tearing standard, described standard relates to the carrying capacity of measuring solid lubricant film, and corresponding to the order of magnitude be the initial state of 1130N.mm or for the load of 785N, the order of magnitude is that 0.15 frictional coefficient is compared, the increasing rapidly of moment of torsion.Usually, do not consider material and structure, when the load that is applied descends, observe wearing and tearing.
The applicant has estimated the performance of the various films of the aq suspension acquisition of adopting polyether-ether-ketone, tribological property particularly, so as especially relatively they with adopt fluoroethane class thermoset film or have observed those performances of visco-plasticity film of wax shape thermoplastic matrix.
The fluoroethane film is made up of the aqueous dispersion that uses aliphatic polyisocyanate stiffening agent solidified vinyl fluoride Vinyl Ether.
Wax shape thermoplastic matrix comprises at least a 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 fs, the applicant has estimated the aq suspension of polyether-ether-ketone and has been the various suprabasil binding property that specific surface preparation is handled, frictional coefficient, and anticorrosive protection and water retting feature:
The XC48 carbon steel (XC48AsM) of former state machining;
Z20C13 stainless steel (13Cr);
XC48 carbon steel with phosphorylation processing of zinc (PhZn) or manganese (PhMn);
XC48 carbon steel with electrolytic Cu-Sn-Zn settling (TA).
Table 3,4 and 5 have summarized according to iso standard 2409, by scratch test with by the cross-hatching test, Vicote F804, the adhesion results of the aq suspension of Vicote F805 and Vicote F807Blk on the sample of being the different surfaces preparation.
Remind, scratch test characterizes the function as the applied load that increases herein, high performance material, the bounding force of preferred thermoset or thermoplastic material.Critical load is determined the fracture and the therefore bounding force of material at the interface, and when material had resistance and binding property, critical load was higher.The minimum critical load of 310N is lower than described pressure corresponding to the minimal adhesion pressure that can reach 1.1GPa, and the increase and and then the abrasion resistance deficiency of abraded product amount takes place in contact.
For the cross-hatching test (described test is provided at by scratching material, damages interface binding property afterwards and measures) according to iso standard 2409, mark 0 is corresponding to good binding property, and the binding property of the non-constant of mark 5 definition.
| Prepare on the surface | XC48AsM | PhMn | TA |
| Binding property, scratch test (Lc, the N of unit) | 242 | 750 | 400 |
| Binding property, |
0 | 0 | 0 |
The bond properties of table 3:Vicote F804
The bond properties of table 4:Vicote F805
| Prepare on the surface | XC48AsM | 13Cr | PhZn | PhMn | TA |
| Binding property, scratch test (Lc, the N of unit) | 750 | 254 | 50 | 750 | 188 |
| Binding property, |
0 | 0 | 5 | 0 | 0 |
The bond properties of table 5:Vicote F807Blk
The film of being tested has insufficient bounding force, with the surface of on carbon steel, carrying out with phosphorylation zinc prepare irrelevant, exception be 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 applicant has also estimated the incident that does not have the roughness that obtains under the phosphorylation situation.Because the adhesion mechanism of poly (ether ether ketone) film is the physical adhesion by mechanical keying (keying) basically, the roughness of substrate is a deciding factor.
Meanwhile, recommend by spraying the sand milling substrate, so that obtain required final film thickness 20% or 25% roughness Ra (Ra is the arithmetical av with respect to the average line of roughness amplitude), so that guarantee the binding property that film is good, promptly the Ra scope is the minimum value of 4 μ m-6 μ m.According to iso standard 1997, use rugosimeter, measure roughness.
| Prepare on the surface | 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: as the function that prepare on the surface, the roughness of sample
Table 6 has been set forth the high relatively roughness that obtains by phosphorylation manganese bondability preferably is provided.It also shows very slight polar surfaces preparation, and for example electrolytic deposition ternary Cu-Sn-Zn alloy does not help bonding.
In view of these first results, the applicant determines to measure the erosion resistance of the substrate that only has natural low erosion resistance, thereby gets rid of the Martensite Stainless Steel that contains 13% chromium (it to the critical bonding load of poly (ether ether ketone) film greater than 180N).
The thickness range of the film of producing by the pneumatic spraying of low temperature is 20-45 μ m.According to iso standard 4528-3, measure the corrosion degree in ReO and the Re9 scope.According to standard ISO 4628-2, be determined at sand holes and extent of delamination in 2S2 (lower concentration sand holes and little size) and 5S5 (sand holes of generalization (generalized) and the big size) scope.Summarized the result in the table 7 and 8.
Table 7: the erosion resistance that adopts the different surfaces preparation of Vicote F805
Table 7: the erosion resistance that adopts the different surfaces preparation of Vicote F807Blk
The erosion resistance of preparing with the surface of individual layer poly (ether ether ketone) film coating is insufficient in broad terms, exception be the Cu-Sn-Zn electrolytic deposit, although under stress, have poly-loss in low binding property or the intensive.This result also shows, compares with Vicote F805, and the Vicote F807Blk poly (ether ether ketone) film that contains inorganic carbon black compounds has erosion resistance relatively preferably, and prepares irrelevant with the surface.Adopt electrolytic deposit, obtain absolute best result, 5 corrosion pits only after 1000 hours.Observe and add the graphitized carbon black toughener,, strengthen corrosion prevention mechanism by serving as sacrificial anode.
At last, the applicant has estimated in the wide load range between 10N to 750N, by scratch test, carries out the frictional coefficient of abrasive material abrasive film.Summarized the result in the table 9.
Table 9: average friction coefficient, scratch test
The frictional coefficient of poly (ether ether ketone) film prepare to have nothing to do with the surface, and for the polyether-ether-ketone that contains perfluoroalkyl ethylene oxy class fluorinated polymer, the frictional coefficient under the average contact pressure of 500MPa reaches 0.075 less than 0.135.
First result shows that the individual layer poly (ether ether ketone) film is lubricated fully and have corrosion resistance, and this not only depends on the composition of film, and depends on the binding property of substrate.
In subordinate phase, the applicant has developed the result who improves binding property and corrosion resistance then.When this can not the time, the applicant wants to substitute sand milling, this is that the geometrical shape of parts to be coated causes.Especially the applicant has studied the composition that does not change the commercial film of being studied.In fact, PCV when adding proportion can increase PCV (pigment volume concentration (PVC)) and exceeds lucky competent adhesive coated efflorescence material (pigment and filler) greater than 10% adhesion promotor or corrosion inhibition pigment and this are that the porosity and the interior poly-loss of the film that obtained by commercially available aq suspension causes.
Also can predict other replacement schemes of using Vicote704 polyether-ether-ketone powder.
The applicant has studied and has adopted the priming paint with adhesion promotor type, increases binding property.Direct bonding cherishing between the material.Because directly bonding to link to each other with Van der Waals force uniquely basically, but only adopt closely contact, promptly takes place under the very slick material of the extreme cleaning in the distance (nanometer) of atom level (for example, mica or the silicon) situation.Therefore, if surface irregularity, then this usually can not carry out, and on the contrary, it is suitable for having the film of low roughness fully.
Therefore, the applicant has studied basically and has passed through to obtain the compatible film of method of poly (ether ether ketone) film 400 ℃ of following fusions.
Priming paint can be the jet sediment of the alloy of the iron sold by Dacral with trade(brand)name Dacroforge Z and zinc, to substitute phosphorylation zinc, but by mechanical injection, the method for sand milling/sandblast cleaning acquisition priming paint has limited it and has used in the ducted body that has minor diameter and highly lack.
The PAEK that priming paint is preferably filled.Especially the solution that includes the pigments, mica of white mica that part by weight is 25%-50% or meroxene at organic polyether-ether-ketone tackiness agent is sold by supplier Victrex with trade(brand)name Vicote F817.
Apply and the method for fusion priming paint identical with the upper strata.On the contrary, rate of cooling is required fast, so that obtain the less crystalline texture of insulating more, suppresses the initiation of pit and passive (passive) current density of reduction material.
The thickness range of priming paint is 30-40 μ m.
Summarized the anticorrosive and bond properties of the priming paint that uses two kinds of different cooling kinetics methodologys evaluations in the table 10 and 11 respectively.
Table 10: the erosion resistance that adopts the different surfaces preparation of Vicote F817 priming paint
| Prepare on the surface | XC48?asM | TA |
| Binding property, and scratch test (Lc, N) | 350 | 344 |
| Binding property, ISO 2409 | 0 | 0 |
| Average COF (10-310N) | 0.164 | 0.160 |
Bond properties and the frictional coefficient of table 11:Vicote F817
Vicote F817 priming paint is protected fully and has binding property, but the oilness deficiency.PAEK layer by top provides lubricity.
Summarized erosion resistance in the table 12 and 13, binding property and double-deck frictional behaviour.The total thickness that contains the film on priming paint and upper strata (finish paint) is 40-70 μ m.
Table 12: the erosion resistance that prepare on different double-deck surfaces
Table 13: bond properties and double-deck frictional coefficient
Prepare irrelevant with the surface, average contact pressure for 500MPa, frictional coefficient is enough low, especially for the Vicote F807Blk film of μ=0.085 wherein, suitable with fluoroethane or epoxide thermoset film's frictional coefficient, and must allow the shoulder torque value of acquisition less than the 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, have the polyether-ether-ketone priming paint of pigments, mica filler and more specifically be contained under the situation on the polyether-ether-ketone of at least a fluorinated polymer of viscous deformation under the stress and/or the upper strata that carbon black class machinery strengthens pigment preferred the employing.
At last, the tribology behavior of film that the applicant has passed through the Bridgman test evaluation is so that determine anti-shoulder torque value.The anti-shoulder torque value that obtains at Vicote F807Blk equals at 85% of the greasy reference value of API RP5A3 on XC48 carbon steel and Z20C13 stainless steel.Yet the method for film causes being difficult to prepare sample and the little diameter of sample means that this numerical value can not be regarded as absolute reference value owing to produce.
The intramolecular interaction of the crystalline texture in polyether-ether-ketone and many potential Van der Waals force types points to this material intensive cohesion and high shearing resistance and so remarkable higher anti-shoulder torque value of possibility.
Meanwhile, the applicant by the Falex test evaluation wear resistance of film.The test structure that is complementary with web member can be included in has a pair of vee-block material that the different surfaces that adopts the PEEK film coated is prepared in individual layer or the bilayer, the XC48 carbon steel pressure head of V font piece material and former state machining or contain the Z20C13 stainless steel pressure head of 13% chromium.
Use contact pressure and pressure-speed modulus (the PV)=11.2MPa.m/s of the test conditions of 785N load corresponding to average 150MPa, described contact pressure relatively is being screwed into the record (100-300MPa) in the process when being in shoulder at screw thread and load-bearing surface and beginning, described pressure-speed modulus approaches to adopt PV=5MPa.m/s, (load flank) locates at the load flank, in the modulus of the built-in Vertical Mill damage of screw thread law.
The applicant has studied Vicote F805 and F807Blk enhanced polyether-ether-ketone.
During Fig. 6 shows and uses on present web member, compare with wax shape thermoplasticity solution, double-deck Vicote F817/Vicote F807 Blk film is favorable durability very, although surface treatment is regarded as attrition resistant (referring to document WO 2008/032872) with ternary electrolytic deposit class, but never obtain wearing and tearing according to ASTM standard D2625-94 definition, and adopt under the HMS3 wax shape thermoplasticity solution situation, after 51 minutes, obtained described wearing and tearing.Low relatively and constant coefficientoffriction=0.08 shows low-down abrasive wear.
In order to measure the wear resistance limit of following film, the Falex that applicant's working load increases in the 1335N-4200N scope tests, and has estimated the weather resistance and the frictional coefficient of film.Slip speed is 10mm/s, and this is opposite with the 20mm/s that uses before.The result has been shown among Fig. 7.
This result shows, does not occur wearing and tearing and the very high wear resistance of proof film of the present invention for the average contact pressure of 350MPa.When pressure increased, frictional coefficient also reduced and in the 0.056-0.078 scope.
In order to prove at sample, especially have and use Falex and scratch test on the sedimental carbon steel of electrolysis Cu-Sn-Zn, observed wear resistance and frictional coefficient in the laboratory, the applicant " is assembling on the 29#L80VAM TOP HT web member 7 of wear height sensitivity.The assembling moment of torsion is 29900N.m.
Handle the female end portion 2 of carbon steel and announce that by phosphorylation zinc processing male end portion 1 and with patent the curable acrylic resin of describing among the WO2006/104251 of UV is coated with by electrolytic deposit.Under rate of cooling, double-deck PEEK film is applied on the tube stub of handling less than 5 ℃/min.Table 14 has been summarized the assembling result.
Table 14:7 " 29#L80VAM TOP HT-CW UD assembling result's comparison
Gained assembling result proves poly (ether ether ketone) film and the wear-resisting property given prominence to of enhanced poly (ether ether ketone) film especially.
Table 15:7 " the result of 29#L80VAM TOP HT assembling
Therefore, the present invention proposes when being applied to steel surface or contain on the steel surface of 13% chromium lubricant film at least with very interesting wear resistance.It also allow to use need not be good binary Cu-Sn or ternary Cu-Sn-Zn class electrolytic deposit.
Claims (22)
1. one kind is used to drill or the threaded tubular member of process oil gas well, and described tubular member is in its end (1; 2) one of locate to have the threaded area of on its periphery or interior perimeter surface, making (3; 4), threaded area is made on the perimeter surface in its periphery still is and is depended on that thread head is public type or parent form, is characterized in that end (1; 2) at least a portion has been coated with at least a lubricated dry film (12) of the PAEK that contains at least 65% weight.
2. the threaded tubular member of claim 1 is characterized in that PAEK is selected from polyether-ether-ketone (PEEK), polyetherketone (PEK) and composition thereof.
3. claim 1 or 2 threaded tubular member is characterized in that lubricated dry film (12) has the structure that the degree of crystallinity scope is 10%-35%.
4. the threaded tubular member of aforementioned any one claim is characterized in that lubricated dry film (12) comprises that further the part by weight scope is at least a the 4th class solid lubricant of 10%-35%.
5. the threaded tubular member of claim 4 is characterized in that lubricated dry film (12) comprises that the part by weight scope is the perfluoroalkyl ethylene oxy multipolymer of 10%-30%.
6. the threaded tubular member of aforementioned any one claim, it is characterized in that lubricated dry film (12) comprises that the part by weight scope is the mechanical toughener that is selected from following pigment of 1%-15%: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS2 or WS2-soccerballene.
7. the threaded tubular member of aforementioned any one claim, the part that it is characterized in that being coated with lubricated dry film (12) has experienced in advance and has been selected from sand milling, the manganese phosphorylation, electrolytic deposition Cu or Cu-Sn-Zn alloy and by the stage of surface preparation in jet deposition Fe and the Zn alloy.
8. any one threaded tubular member of claim 1-6, the part that it is characterized in that being coated with lubricated dry film (12) are in advance with having the hemihedral crystal structure and containing the polyether-ether-ketone priming paint coating of pigments, mica.
9. the threaded tubular member of aforementioned any one claim is characterized in that whole threaded area (3; 4) be coated with lubricated dry film (12).
10. the threaded tubular member of aforementioned any one claim is characterized in that it comprises the metal/metal sealing face, and described sealing face has been coated with lubricated dry film (12).
11. a threaded tubular web member, it comprises positive thread tubulose member and negative thread tubulose member, and one is assembled in another, it is characterized in that in the described threaded tubular member at least one is defined according to aforementioned any one claim.
12. be used to drill or the coating process of the threaded tubular member of process oil gas well, described tubular member is in its end (1; 2) one of locate to have the threaded area of on its periphery or interior perimeter surface, making (3; 4), make on the still interior perimeter surface of its periphery of threaded area and depend on that thread head is public type or parent form, it is characterized in that this method comprises the steps:
Production is included in the mixture that the part by weight scope that suspends in the water is the polyaryl ether ketone powder of 25%-35%;
Described mixture is applied to the end (1 of described threaded tubular member; 2) on the part;
Dry so end (1 of coating under 100 ℃-150 ℃ temperature range; 2) part is lasted 5-10 minute;
Under 10 ℃-20 ℃/minute temperature rise rate, heating is the end (1 of coating so; 2) part is lasted 5-15 minute to the temperature of 350 ℃ of-450 ℃ of scopes;
Under the rate of cooling less than 10 ℃/min, cooling is the end (1 of coating so; 2) part is to envrionment temperature, so that obtain crystalline structure basically.
13. the coating process of the threaded tubular member of claim 12 is characterized in that this mixture comprises that also the part by weight scope is that have rapid evaporation speed and the boiling spread of 2.5%-10% is 100 ℃-200 ℃ coalescing agent.
14. the coating process of the threaded tubular member of claim 12 or 13 is characterized in that this mixture comprises that further the part by weight scope is the non-ionic wetting and dispersion agent of 2.5%-10%.
15. any one the coating process of threaded tubular member of claim 12-14 is characterized in that this mixture comprises that also the part by weight scope is at least a the 4th class solid lubricant of 3%-12%.
16. the coating process of the threaded tubular member of claim 15 is characterized in that the 4th class solid lubricant is the perfluoroalkyl ethylene oxy multipolymer, its part by weight scope is 3%-12%.
17. the coating process of the threaded tubular member of claim 15, it is characterized in that this mixture comprises that also the part by weight scope is the mechanical toughener that is selected from following pigment of 0.5%-5%: carbon black, mica, wollastonite, nano aluminium oxide, nano-titanium oxide, glass powder, Nano diamond, nanometer WS2 or WS2-soccerballene.
18. the coating process of the threaded tubular member of claim 12 is characterized in that using pneumatic fog system coating end (1; 2) part, the diameter range of described system are that 0.7-1.8mm and air pressure scope are the 4-6 crust.
19. any one the coating process of threaded tubular member of claim 12-18, it is characterized in that applying mixture before the end sections, be selected from following stage of surface preparation: sand milling, the manganese phosphorylation, electrolytic deposition Cu or Cu-Sn-Zn alloy and by jet deposition Fe and Zn alloying pellet.
20. any one the coating process of threaded tubular member of claim 12-18 is characterized in that applying mixture before the end sections, carries out being had the hemihedral crystal structure and being contained the stage of surface preparation that the polyether-ether-ketone priming paint of pigments, mica is formed by production.
21. be used to drill or the coating process of the threaded tubular member of process oil gas well, described tubular member is in its end (1; 2) one of locate to have the threaded area of on its periphery or interior perimeter surface, making (3; 4), make on the still interior perimeter surface of its periphery of threaded area and depend on that thread head is public type or parent form, it is characterized in that this method comprises the steps:
Heat the end (1 of described threaded tubular member; 2) part is 360 ℃-420 ℃ a temperature to scope, preferably approaches 400 ℃ temperature;
Spray PEK and/or PEEK powder end (1 to described threaded tubular member; 2) on the part;
Under 360 ℃-420 ℃ temperature range, preferably in the end (1 of approaching to keep coating like this under 400 ℃ the temperature; 2) part is lasted 1-4 minute;
Under less than 10 ℃/minute rate of cooling, cooling is the end (1 of coating so; 2) part is to envrionment temperature, so that obtain crystalline structure basically.
22. the coating process of the threaded tubular member of claim 21 is characterized in that carrying out before the described part in heating the defatting step of part to be coated.
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 true CN103221519A (en) | 2013-07-24 |
| CN103221519B 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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| 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 |
| US11092266B2 (en) | 2015-02-03 | 2021-08-17 | 925599 Alberta Ltd. | Pipe connector |
| US11339634B2 (en) | 2015-04-10 | 2022-05-24 | 925599 Alberta Ltd. | Pipe connector |
| AU2016244745A1 (en) * | 2015-04-10 | 2017-11-30 | 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 BR BR112013011454-1A patent/BR112013011454B1/en active IP Right Grant
- 2011-11-02 WO PCT/EP2011/005524 patent/WO2012062426A1/en active Application Filing
- 2011-11-02 EP EP11779106.1A patent/EP2638134B1/en active Active
- 2011-11-02 EA EA201370114A patent/EA024642B1/en not_active IP Right Cessation
- 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
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Also Published As
| Publication number | Publication date |
|---|---|
| CA2815723A1 (en) | 2012-05-18 |
| EA024642B1 (en) | 2016-10-31 |
| BR112013011454A2 (en) | 2016-08-09 |
| BR112013011454B1 (en) | 2019-04-24 |
| FR2967199A1 (en) | 2012-05-11 |
| WO2012062426A1 (en) | 2012-05-18 |
| EP2638134B1 (en) | 2019-07-24 |
| AU2011328484A1 (en) | 2013-05-02 |
| AU2011328484B2 (en) | 2015-11-19 |
| AR083823A1 (en) | 2013-03-27 |
| US20130320665A1 (en) | 2013-12-05 |
| EA201370114A1 (en) | 2013-12-30 |
| CN103221519B (en) | 2015-04-15 |
| FR2967199B1 (en) | 2013-11-01 |
| JP2013545946A (en) | 2013-12-26 |
| MX2013005243A (en) | 2013-06-12 |
| UA112064C2 (en) | 2016-07-25 |
| JP6018576B2 (en) | 2016-11-02 |
| EP2638134A1 (en) | 2013-09-18 |
| CA2815723C (en) | 2018-08-21 |
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