CN117186765A - Solid self-lubricating coating and preparation method thereof - Google Patents
Solid self-lubricating coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 77
- 239000007787 solid Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000004642 Polyimide Substances 0.000 claims abstract description 69
- 229920001721 polyimide Polymers 0.000 claims abstract description 69
- 239000006184 cosolvent Substances 0.000 claims abstract description 35
- 239000000945 filler Substances 0.000 claims abstract description 32
- 239000000049 pigment Substances 0.000 claims abstract description 32
- -1 5-amino-o-cresol modified fluorinated graphene Chemical class 0.000 claims abstract description 31
- 239000013530 defoamer Substances 0.000 claims abstract description 21
- UEXCJVNBTNXOEH-UHFFFAOYSA-N Ethynylbenzene Chemical group C#CC1=CC=CC=C1 UEXCJVNBTNXOEH-UHFFFAOYSA-N 0.000 claims description 78
- 239000000203 mixture Substances 0.000 claims description 57
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 48
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 48
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 46
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- 239000002244 precipitate Substances 0.000 claims description 27
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 16
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 16
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- MQAHXEQUBNDFGI-UHFFFAOYSA-N 5-[4-[2-[4-[(1,3-dioxo-2-benzofuran-5-yl)oxy]phenyl]propan-2-yl]phenoxy]-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(OC2=CC=C(C=C2)C(C)(C=2C=CC(OC=3C=C4C(=O)OC(=O)C4=CC=3)=CC=2)C)=C1 MQAHXEQUBNDFGI-UHFFFAOYSA-N 0.000 claims description 15
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- QLOAVXSYZAJECW-UHFFFAOYSA-N methane;molecular fluorine Chemical compound C.FF QLOAVXSYZAJECW-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
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- DBFYESDCPWWCHN-UHFFFAOYSA-N 5-amino-2-methylphenol Chemical compound CC1=CC=C(N)C=C1O DBFYESDCPWWCHN-UHFFFAOYSA-N 0.000 claims description 12
- 239000013067 intermediate product Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000002518 antifoaming agent Substances 0.000 claims description 11
- 238000005507 spraying Methods 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 229920005575 poly(amic acid) Polymers 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 7
- 239000005457 ice water Substances 0.000 claims description 7
- 238000010907 mechanical stirring Methods 0.000 claims description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 229910021389 graphene Inorganic materials 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 238000005238 degreasing Methods 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
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- 238000001291 vacuum drying Methods 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 21
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 7
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 150000003949 imides Chemical class 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000010534 nucleophilic substitution reaction Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 238000004381 surface treatment Methods 0.000 abstract 1
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- 238000012360 testing method Methods 0.000 description 12
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- 239000003795 chemical substances by application Substances 0.000 description 7
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- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 5
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
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Abstract
The application discloses a solid self-lubricating coating and a preparation method thereof, belonging to the technical field of surface treatment; the coating comprises the following components in parts by weight: 40-50 parts of phenylacetylene-terminated polyimide, 5-15 parts of 5-amino-o-cresol modified fluorinated graphene, 5-8 parts of pigment and filler, 4-6 parts of cosolvent and 2-6 parts of defoamer. According to the application, the amino surface is modified on the fluorinated graphene through nucleophilic substitution reaction, so that the fluorinated graphene has good dispersibility, can be uniformly dispersed in a polyimide matrix, and is endowed with hydrogen bond acting force formed between the fluorinated graphene and imide molecules, so that the tensile strength and wear resistance of the coating are improved; the introduction of the amino-containing micromolecular chain segment ensures that the aminated fluorinated graphene is uniformly oriented and dispersed in the coating, and a covalent bond acting interface with good compatibility and thermal stability is constructed, so that the chemical stability of the coating is improved.
Description
Technical Field
The application belongs to the technical field of self-lubricating coating materials, and particularly relates to a solid self-lubricating coating and a preparation method thereof.
Background
Wear failure is a major cause of material and part failure in engineering applications, and the use of advanced lubrication materials and techniques is an effective way to reduce wear.
The oil casing is a special pipe in petroleum exploitation engineering, the casing supports a well wall after well drilling is finished, and the oil pipe conveys crude oil and natural gas to the surface of the earth to finally finish oil and gas exploitation. In the process, the oil pipe and the casing pipe are connected through threaded joints, and the threaded joints are used for connecting the oil pipe and the casing pipe in series to form a pipe column to complete oil and gas exploitation tasks.
Friction can be generated between threads in the process of connecting the oil pipe and the sleeve in series to form a tubular column, and the existing oil sleeve thread coating technology lubricates market demands; at present, common screw thread oil (thread grease) is mainly adopted as lubricating oil, and 19 to 25 percent of inorganic fillers such as lead, zinc, lithium, graphite and the like are added, so that the thread grease can pollute the environment; and developed in places with high environmental requirements such as ocean (North sea, mediterranean sea), brazilian tropical rain forest and the like, and the use of screw thread grease is not allowed; in areas where the use of the thread compound is allowed, if the thread compound is smeared on a drill floor too much, the excessive thread compound can squeeze into the oil casing, pollute the reservoir after falling into the bottom of the well, and affect the quality of produced petroleum.
Thus, there is an urgent need for a process technology that can be applied to the surface of the friction member of an oil casing thread to reduce its frictional wear, giving the oil casing thread effective protection, to solve the above problems and to seek a more viable solution.
Disclosure of Invention
The application aims to provide a solid self-lubricating coating and a preparation method thereof, which are used for meeting the lubricating requirement of oil casing threads; and the problems that the existing thread grease squeezes the oil inlet sleeve, pollutes a reservoir after falling into the bottom of a well and affects the quality of produced petroleum are solved.
The application is realized by the following technical scheme: the solid self-lubricating coating comprises the following components in parts by weight: 40-50 parts of phenylacetylene-terminated polyimide, 5-15 parts of 5-amino-o-cresol modified fluorinated graphene, 5-8 parts of pigment and filler, 4-6 parts of cosolvent and 2-6 parts of defoamer;
the phenylacetylene-terminated polyimide comprises the following components in parts by weight: 4-10 parts of bisphenol A type dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride.
Preparation of phenylacetylene end capped polyimide: adding 4,4' -diaminodiphenyl ether and N, N-dimethylformamide into a reaction vessel with mechanical stirring, fully stirring at room temperature, and slowly adding a uniform mixture of bisphenol A dianhydride and 4-phenylacetylene phthalic anhydride after dissolving; after being uniformly mixed, the reaction vessel is placed in an ice-water bath for reaction for 5 hours; obtaining an intermediate product phenylacetylene end-capped polyamic acid solution; slowly adding triethylamine and acetic anhydride into phenylacetylene end-capped polyamic acid solution according to the mass ratio of 1:1, and placing a reaction container in a water bath at 60 ℃ for reaction for 3 hours; and then pouring the reacted mixture into enough absolute ethyl alcohol to separate out, obtaining light yellow precipitate, washing and filtering the prepared precipitate for multiple times, and then placing the precipitate in a 120 ℃ oven to be dried to constant weight, thus obtaining the phenylacetylene-terminated polyimide.
Preparation of 5-amino-o-cresol modified graphene fluoride: weighing graphite fluoride, adding the graphite fluoride into an ethanol solution of polyvinylpyrrolidone, performing ultrasonic dispersion, and then performing high-speed mechanical shearing and stirring on the solution after ultrasonic dispersion, wherein after stirring is completed; centrifuging the solution, collecting supernatant, filtering to remove excessive polyvinylpyrrolidone, and drying in a vacuum drying oven to obtain black precipitate; grinding and uniformly mixing black precipitate and 5-amino-o-cresol, adding the mixture into a reaction container, and fully reacting under the protection of argon; and adding distilled water into a reaction container, performing suction filtration to obtain a black sample, and repeatedly washing the black sample with distilled water and ethanol solution for multiple times to obtain the 5-amino-o-cresol modified fluorinated graphene.
The preparation method of the solid self-lubricating coating comprises the following steps: weighing 5-amino-o-cresol modified fluorinated graphene and a cosolvent according to a formula, and uniformly mixing the graphene and the cosolvent by utilizing ultrasound to obtain a mixture A; weighing phenylacetylene-terminated polyimide according to a formula, adding pigment and filler into a dispersion tank, and stirring and dispersing uniformly under the stirring condition of the rotating speed of 300-600r/min to obtain a mixture B; and finally, adding the mixture A into the mixture B, adding the defoaming agent, and stirring and dispersing uniformly under the stirring condition of the rotating speed of 800-1200r/min to obtain the solid self-lubricating coating.
The preparation method of the solid self-lubricating coating applied to the oil casing thread comprises the following steps: firstly degreasing the joint of a threaded joint oil pipe, fully spraying a mixed solution of sodium silicate and sulfonate on the threaded joint, reacting for 10min, and wiping off possible scraps and dust on the threaded surface by using absolute ethyl alcohol and absorbent cotton; finally, flushing with plasma water, wiping, and uniformly spraying along the thread surface by using a spray gun, wherein the spraying pressure is 0.5-0.8MPa; the distance between the spray gun nozzle and the threaded surface is 120-150mm, and the thickness of the coating is controlled to be 20-35 mu m; and (3) placing the sprayed sample into an electrothermal blowing drying oven, sintering for 10min at 260 ℃, cooling along with the furnace, and after cooling to normal temperature, preparing the solid self-lubricating coating applied to the oil sleeve threads.
The application has the beneficial effects that:
1. according to the application, the polyimide subjected to end-capping modification is introduced, so that the polyimide is subjected to crosslinking reaction without other auxiliary agents or crosslinking agents, no volatile byproducts escape in the crosslinking reaction process, and the reservoir is not polluted, so that the quality of produced petroleum is not influenced; compared with unmodified polyimide, the polyimide subjected to end capping modification has the advantages that the basic mechanical properties, tensile strength and microhardness are improved, and the polyimide is more difficult to strip by a dual material due to the excellent mechanical properties in the friction process; the increase of the microhardness is beneficial to the damage caused by the resistance load of the material and the reduction of corresponding abrasion deformation;
2. the fluorine atoms in the solid self-lubricating coating are introduced, so that the fluorinated graphene has larger interlayer spacing and weaker interlayer shearing force compared with the original graphene, and therefore, the fluorinated graphene has better lubricating performance compared with the original graphene;
3. according to the application, the amino surface is modified on the fluorinated graphene through nucleophilic substitution reaction, so that the fluorinated graphene has good dispersibility, can be uniformly dispersed in a polyimide matrix, and is endowed with hydrogen bond acting force formed between the fluorinated graphene and imide molecules, so that the tensile strength and wear resistance of the coating are improved; the introduction of the amino-containing micromolecular chain segment ensures that the aminated fluorinated graphene is uniformly oriented and dispersed in the coating, and a covalent bond acting interface with good compatibility and thermal stability is constructed, so that the chemical stability of the coating is improved.
Detailed Description
The present application will be described in further detail with reference to the following examples, for the purpose of making the objects, technical solutions and advantages of the present application more apparent, and the description thereof is merely illustrative of the present application and not intended to be limiting. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the application. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the application described herein without departing from the scope or spirit of the application. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present application. The specification and examples of the present application are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The "parts" indicated in the examples below are parts by weight.
Example 1
The solid self-lubricating coating comprises the following components in parts by weight: 40 parts of phenylacetylene terminated polyimide, 5 parts of 5-amino-o-cresol modified fluorinated graphene, 5 parts of pigment and filler, 4 parts of cosolvent and 2 parts of defoamer;
wherein, the phenylacetylene end capped polyimide comprises the following components in parts by weight: 4 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride;
wherein the pigment and filler is titanium dioxide, and the cosolvent is ethylene glycol;
wherein the defoamer is a mixture of tributyl phosphate and higher alcohols.
Preparation of phenylacetylene end capped polyimide: adding 40g of 4,4' -diaminodiphenyl ether and 80g of N, N-dimethylformamide into a reaction vessel with mechanical stirring, fully stirring at room temperature, and slowly adding a uniform mixture of 16g of bisphenol A dianhydride and 4g of 4-phenylacetylene phthalic anhydride after dissolving; after being uniformly mixed, the reaction vessel is placed in an ice-water bath, the temperature is controlled at 0-5 ℃, and after reaction for 5 hours; obtaining an intermediate product phenylacetylene end-capped polyamic acid solution; measuring the intrinsic viscosity and the number average molecular weight of the intermediate product, wherein the intrinsic viscosity is 0.18, and the number average molecular weight is 3000; then, after uniformly mixing 12g of triethylamine and 12g of acetic anhydride, slowly adding the mixture into phenylacetylene terminated polyamide acid solution, and placing a reaction container in a water bath at 60 ℃ for reaction for 3 hours; and then pouring the reacted mixture into enough absolute ethyl alcohol to precipitate to obtain light yellow precipitate, washing and filtering the light yellow precipitate for multiple times, and then placing the light yellow precipitate in a 120 ℃ oven to be dried to constant weight, thus obtaining the phenylacetylene capped polyimide.
Preparation of 5-amino-o-cresol modified graphene fluoride: weighing 10g of graphite fluoride, adding the graphite fluoride into an ethanol solution of polyvinylpyrrolidone with the solution concentration of 10mg/ml, and performing ultrasonic dispersion for 30min; then carrying out high-speed mechanical shearing stirring on the solution after ultrasonic dispersion, and continuously stirring for 12 hours at the rotating speed of 1500 r/min; after stirring, carrying out 5000r/min centrifugal treatment on the solution for 10min, taking supernatant, carrying out suction filtration to remove excessive polyvinylpyrrolidone, and then placing the obtained solution into a vacuum drying oven for drying at 60 ℃ for 12h to obtain black precipitate; grinding and uniformly mixing black precipitate and 10g of 5-amino-o-cresol, adding the mixture into a reaction container, and reacting for 4 hours at 180 ℃ under the protection of argon; and adding distilled water into a reaction container, performing suction filtration to obtain a black sample, and repeatedly washing the black sample with distilled water and 95% ethanol solution for multiple times to obtain the 5-amino-o-cresol modified fluorinated graphene.
The preparation method of the solid self-lubricating coating comprises the following steps: firstly, weighing 5 parts by weight of 5-amino-o-cresol modified fluorinated graphene and 4 parts by weight of cosolvent according to a formula, placing the mixture in an ultrasonic homogenizer, and uniformly mixing the two by utilizing ultrasonic waves to obtain a mixture A; then, 40 parts by weight of phenylacetylene-terminated polyimide and 5 parts by weight of pigment and filler are weighed according to a formula, added into a dispersion tank, stirred for 45min under the stirring condition of the rotating speed of 300-600r/min, and uniformly stirred and dispersed to obtain a mixture B; and finally, adding the mixture A into the mixture B, adding 2 parts by weight of defoaming agent, stirring for 30min under the stirring condition of the rotating speed of 800-1200r/min, and uniformly stirring and dispersing to obtain the solid self-lubricating coating.
Example 2
The solid self-lubricating coating comprises the following components in parts by weight: 42 parts of phenylacetylene capped polyimide, 8 parts of 5-amino-o-cresol modified fluorinated graphene, 6 parts of pigment and filler, 4 parts of cosolvent and 4 parts of defoamer;
wherein, the phenylacetylene end capped polyimide comprises the following components in parts by weight: 6 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride;
wherein the pigment and filler is hydrophilic silicon dioxide, and the cosolvent is ethylene glycol diethyl ether;
wherein the defoamer is polydimethylsiloxane.
Wherein, the preparation of phenylacetylene end capped polyimide: adding 40g of 4,4' -diaminodiphenyl ether and 80g of N, N-dimethylformamide into a reaction vessel with mechanical stirring, fully stirring at room temperature, and slowly adding a uniform mixture of 24g of bisphenol A dianhydride and 4g of 4-phenylacetylene phthalic anhydride after dissolving; after being uniformly mixed, the reaction vessel is placed in an ice-water bath, the temperature is controlled at 0-5 ℃, and after reaction for 5 hours; obtaining an intermediate product phenylacetylene end-capped polyamic acid solution; measuring the intrinsic viscosity and the number average molecular weight of the intermediate product, wherein the intrinsic viscosity is 0.28, and the number average molecular weight is 5000; then, after uniformly mixing 12g of triethylamine and 12g of acetic anhydride, slowly adding the mixture into phenylacetylene terminated polyamide acid solution, and placing a reaction container in a water bath at 60 ℃ for reaction for 3 hours; then pouring the reacted mixture into enough absolute ethyl alcohol to precipitate to obtain light yellow precipitate, washing and filtering the light yellow precipitate for many times, and then placing the light yellow precipitate in a 120 ℃ oven to be dried to constant weight, thus obtaining the phenylacetylene-terminated polyimide;
in example 2, the preparation method of the 5-amino-o-cresol modified fluorinated graphene and the preparation method of the solid self-lubricating coating are the same as those in example 1.
Example 3
The solid self-lubricating coating comprises the following components in parts by weight: 45 parts of phenylacetylene capped polyimide, 10 parts of 5-amino-o-cresol modified fluorinated graphene, 6 parts of pigment and filler, 5 parts of cosolvent and 4 parts of defoamer;
wherein, the phenylacetylene end capped polyimide comprises the following components in parts by weight: 8 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride;
wherein the pigment and filler is a mixture of titanium dioxide and aluminum oxide, and the cosolvent is ethylene glycol;
wherein the defoamer is tributyl phosphate.
Wherein, the preparation of phenylacetylene end capped polyimide: adding 40g of 4,4' -diaminodiphenyl ether and 80g of N, N-dimethylformamide into a reaction vessel with mechanical stirring, fully stirring at room temperature, and slowly adding a uniform mixture of 32g of bisphenol A dianhydride and 4g of 4-phenylacetylene phthalic anhydride after dissolving; after being uniformly mixed, the reaction vessel is placed in an ice-water bath, the temperature is controlled at 0-5 ℃, and after reaction for 5 hours; obtaining an intermediate product phenylacetylene end-capped polyamic acid solution; measuring the intrinsic viscosity and the number average molecular weight of the intermediate product, wherein the intrinsic viscosity is 0.36, and the number average molecular weight is 8000; then, after uniformly mixing 12g of triethylamine and 12g of acetic anhydride, slowly adding the mixture into phenylacetylene terminated polyamide acid solution, and placing a reaction container in a water bath at 60 ℃ for reaction for 3 hours; then pouring the reacted mixture into enough absolute ethyl alcohol to precipitate to obtain light yellow precipitate, washing and filtering the light yellow precipitate for many times, and then placing the light yellow precipitate in a 120 ℃ oven to be dried to constant weight, thus obtaining the phenylacetylene-terminated polyimide;
in example 3, the preparation method of the 5-amino-o-cresol modified fluorinated graphene and the preparation method of the solid self-lubricating coating are the same as those in example 1.
Example 4
The solid self-lubricating coating comprises the following components in parts by weight: 50 parts of phenylacetylene capped polyimide, 15 parts of 5-amino-o-cresol modified fluorinated graphene, 8 parts of pigment and filler, 6 parts of cosolvent and 6 parts of defoamer;
wherein, the phenylacetylene end capped polyimide comprises the following components in parts by weight: 8 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride;
wherein the pigment and filler is a mixture of titanium dioxide and aluminum oxide, and the cosolvent is ethylene glycol;
wherein the defoamer is tributyl phosphate.
Wherein, the preparation of phenylacetylene end capped polyimide: adding 40g of 4,4' -diaminodiphenyl ether and 80g of N, N-dimethylformamide into a reaction vessel with mechanical stirring, fully stirring at room temperature, and slowly adding a uniform mixture of 32g of bisphenol A dianhydride and 4g of 4-phenylacetylene phthalic anhydride after dissolving; after being uniformly mixed, the reaction vessel is placed in an ice-water bath, the temperature is controlled at 0-5 ℃, and after reaction for 5 hours; obtaining an intermediate product phenylacetylene end-capped polyamic acid solution; measuring the intrinsic viscosity and the number average molecular weight of the intermediate product, wherein the intrinsic viscosity is 0.21, and the number average molecular weight is 10000; then, after uniformly mixing 12g of triethylamine and 12g of acetic anhydride, slowly adding the mixture into phenylacetylene terminated polyamide acid solution, and placing a reaction container in a water bath at 60 ℃ for reaction for 3 hours; then pouring the reacted mixture into enough absolute ethyl alcohol to precipitate to obtain light yellow precipitate, washing and filtering the light yellow precipitate for many times, and then placing the light yellow precipitate in a 120 ℃ oven to be dried to constant weight, thus obtaining the phenylacetylene-terminated polyimide;
in example 4, the preparation method of the 5-amino-o-cresol modified fluorinated graphene and the preparation method of the solid self-lubricating coating are the same as those in example 1.
Example 5
The solid self-lubricating coating comprises the following components in parts by weight: 45 parts of phenylacetylene capped polyimide, 10 parts of 5-amino-o-cresol modified fluorinated graphene, 6 parts of pigment and filler, 5 parts of cosolvent and 4 parts of defoamer;
wherein, the phenylacetylene end capped polyimide comprises the following components in parts by weight: 6 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride;
wherein the pigment and filler is hydrophilic silicon dioxide, and the cosolvent is ethylene glycol diethyl ether;
wherein the defoamer is polydimethylsiloxane.
Wherein, the preparation of phenylacetylene end capped polyimide: adding 40g of 4,4' -diaminodiphenyl ether and 80g of N, N-dimethylformamide into a reaction vessel with mechanical stirring, fully stirring at room temperature, and slowly adding a uniform mixture of 24g of bisphenol A dianhydride and 4g of 4-phenylacetylene phthalic anhydride after dissolving; after being uniformly mixed, the reaction vessel is placed in an ice-water bath, the temperature is controlled at 0-5 ℃, and after reaction for 5 hours; obtaining an intermediate product phenylacetylene end-capped polyamic acid solution; measuring the intrinsic viscosity and the number average molecular weight of the intermediate product, wherein the intrinsic viscosity is 0.28, and the number average molecular weight is 5000; then, after uniformly mixing 12g of triethylamine and 12g of acetic anhydride, slowly adding the mixture into phenylacetylene terminated polyamide acid solution, and placing a reaction container in a water bath at 60 ℃ for reaction for 3 hours; then pouring the reacted mixture into enough absolute ethyl alcohol to precipitate to obtain light yellow precipitate, washing and filtering the light yellow precipitate for many times, and then placing the light yellow precipitate in a 120 ℃ oven to be dried to constant weight, thus obtaining the phenylacetylene-terminated polyimide;
in example 5, the preparation method of the 5-amino-o-cresol modified fluorinated graphene and the preparation method of the solid self-lubricating coating are the same as those in example 1.
Comparative example 1
The solid self-lubricating coating comprises the following components in parts by weight: 42 parts of non-end-capped modified polyimide, 8 parts of 5-amino-o-cresol modified fluorinated graphene, 6 parts of pigment and filler, 4 parts of cosolvent, 4 parts of defoamer and 5 parts of curing agent triglycidyl isocyanurate;
wherein the pigment and filler is hydrophilic silicon dioxide, and the cosolvent is ethylene glycol diethyl ether;
wherein the defoaming agent is polydimethylsiloxane;
wherein, in comparative example 1, the preparation of 5-amino-o-cresol modified graphene fluoride was the same as in example 2;
the preparation method of the solid self-lubricating coating comprises the following steps: firstly, 8 parts by weight of 5-amino-o-cresol modified fluorinated graphene and 4 parts by weight of cosolvent are weighed according to a formula, placed in an ultrasonic homogenizer, and uniformly mixed by utilizing ultrasonic waves to obtain a mixture A; then, weighing 42 parts of non-end-capped modified polyimide and 6 parts by weight of pigment and filler according to a formula, adding into a dispersion tank, stirring for 45min under the stirring condition of the rotating speed of 300-600r/min, and uniformly stirring and dispersing to obtain a mixture B; and finally, adding the mixture A into the mixture B, adding 4 parts by weight of an antifoaming agent and 5 parts by weight of triglycidyl isocyanurate as a curing agent, stirring for 15min under the stirring condition of the rotating speed of 800-1200r/min, and uniformly stirring and dispersing to obtain the solid self-lubricating coating.
Comparative example 2
The solid self-lubricating coating comprises the following components in parts by weight: 45 parts of non-end-capped modified polyimide, 10 parts of 5-amino-o-cresol modified fluorinated graphene, 6 parts of pigment and filler, 5 parts of cosolvent, 4 parts of defoamer and 5 parts of curing agent triglycidyl isocyanurate;
wherein the pigment and filler is a mixture of titanium dioxide and aluminum oxide, and the cosolvent is ethylene glycol;
wherein the defoaming agent is tributyl phosphate;
wherein, in comparative example 2, the preparation of 5-amino-o-cresol modified graphene fluoride was the same as in example 3;
the preparation method of the solid self-lubricating coating comprises the following steps: firstly, weighing 10 parts by weight of 5-amino-o-cresol modified fluorinated graphene and 5 parts by weight of cosolvent according to a formula, placing the mixture in an ultrasonic homogenizer, and uniformly mixing the two by utilizing ultrasonic waves to obtain a mixture A; then, weighing 45 parts of non-end-capped modified polyimide and 6 parts by weight of pigment and filler according to a formula, adding into a dispersion tank, stirring for 45min under the stirring condition of the rotating speed of 300-600r/min, and uniformly stirring and dispersing to obtain a mixture B; and finally, adding the mixture A into the mixture B, adding 4 parts by weight of an antifoaming agent and 5 parts by weight of triglycidyl isocyanurate as a curing agent, stirring for 15min under the stirring condition of the rotating speed of 800-1200r/min, and uniformly stirring and dispersing to obtain the solid self-lubricating coating.
Comparative example 3
The solid self-lubricating coating comprises the following components in parts by weight: 42 parts of phenylacetylene end-capped polyimide, 8 parts of graphite fluoride, 6 parts of pigment and filler, 4 parts of cosolvent and 4 parts of defoamer;
wherein, the phenylacetylene end capped polyimide comprises the following components in parts by weight: 6 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride;
wherein the pigment and filler is hydrophilic silicon dioxide, and the cosolvent is ethylene glycol diethyl ether;
wherein the defoaming agent is polydimethylsiloxane;
in comparative example 3, the phenylacetylene terminated polyimide was prepared, and the preparation method of the solid self-lubricating coating was the same as that of example 2.
Comparative example 4
The solid self-lubricating coating comprises the following components in parts by weight: 42 parts of phenylacetylene end-capped polyimide, 8 parts of graphite fluoride, 4 parts of 5-amino-o-cresol, 6 parts of pigment and filler, 4 parts of cosolvent and 4 parts of defoamer;
wherein, the phenylacetylene end capped polyimide comprises the following components in parts by weight: 6 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride;
wherein the pigment and filler is hydrophilic silicon dioxide, and the cosolvent is ethylene glycol diethyl ether;
wherein the defoamer is polydimethylsiloxane.
The preparation method of the solid self-lubricating coating comprises the following steps: firstly, 8 parts by weight of graphite fluoride, 4 parts by weight of 5-amino-o-cresol and 4 parts by weight of cosolvent are weighed according to a formula, placed in an ultrasonic homogenizer, and uniformly mixed by utilizing ultrasonic waves to obtain a mixture A; then, 40 parts by weight of phenylacetylene-terminated polyimide and 5 parts by weight of pigment and filler are weighed according to a formula, added into a dispersion tank, stirred for 45min under the stirring condition of 300-600r/min, and uniformly stirred and dispersed to obtain a mixture B; finally, adding the mixture A into the mixture B, adding 2 parts by weight of defoaming agent, stirring for 30min under the stirring condition of the rotating speed of 800-1200r/min, and uniformly stirring and dispersing to obtain the solid self-lubricating coating;
wherein the phenylacetylene terminated polyimide of comparative example 4 was prepared in the same manner as in example 2.
Comparative example 5
The solid self-lubricating coating comprises the following components in parts by weight: 42 parts of polyimide, 8 parts of graphite fluoride, 6 parts of pigment and filler, 4 parts of cosolvent, 4 parts of defoamer and 5 parts of curing agent triglycidyl isocyanurate;
wherein the pigment and filler is hydrophilic silicon dioxide, and the cosolvent is ethylene glycol diethyl ether;
wherein the defoaming agent is polydimethylsiloxane;
in comparative example 5, the preparation method of the solid self-lubricating coating layer is: firstly, 8 parts by weight of graphite fluoride and 4 parts by weight of cosolvent are weighed according to a formula, and are placed in an ultrasonic homogenizer, and the graphite fluoride and the cosolvent are uniformly mixed by utilizing ultrasonic waves to obtain a mixture A; then, 42 parts of polyimide and 6 parts of pigment and filler are weighed according to the formula, added into a dispersion tank, stirred for 45min under the stirring condition of the rotating speed of 300-600r/min, and uniformly stirred and dispersed to obtain a mixture B; and finally, adding the mixture A into the mixture B, adding 4 parts by weight of an antifoaming agent and 5 parts by weight of triglycidyl isocyanurate as a curing agent, stirring for 15min under the stirring condition of the rotating speed of 800-1200r/min, and uniformly stirring and dispersing to obtain the solid self-lubricating coating.
Test examples
The solid self-lubricating coating materials prepared in examples 1-5 and comparative examples 1-5 are used for carrying out spraying treatment on the P110 threaded joint oil pipe coupling with the specification of phi 73.02 multiplied by 5.51mm in a spraying manner; and finishing the relevant performance test of the coating;
the preparation method of the solid self-lubricating coating applied to the oil casing thread comprises the following steps: firstly degreasing the joint of a threaded joint oil pipe, fully spraying a mixed solution of sodium silicate and sulfonate on the threaded joint, reacting for 10min, and wiping off possible scraps and dust on the threaded surface by using absolute ethyl alcohol and absorbent cotton; finally, flushing with plasma water, wiping, and uniformly spraying along the thread surface by using a spray gun, wherein the spraying pressure is 0.5-0.8MPa; the distance between the spray gun nozzle and the threaded surface is 120-150mm, and the thickness of the coating is controlled to be 20-35 mu m; and (3) placing the sprayed sample into an electrothermal blowing drying oven, sintering for 10min at 260 ℃, cooling along with the furnace, and after cooling to normal temperature, preparing the solid self-lubricating coating applied to the oil sleeve threads.
Lubrication performance test: in order to simulate the actual working condition, the lubrication performance of the threaded joint oil pipe is tested under the two conditions of low load and high load;
the test conditions of the low-load lubricating performance are as follows: performing friction and wear tests on the oil pipe coupling of the threaded joint of examples 1-5 and comparative examples 1-5 after the preparation of the solid self-lubricating coating applied to the threads of the oil casing by using a small pin disc under the conditions of 120N load, 180rpm and 600s storage time, and calculating the friction coefficient and the wear amount;
the test conditions of the high-load lubricating performance are as follows: performing friction and wear tests on the oil pipe coupling of the threaded joint of examples 1-5 and comparative examples 1-5 after the preparation of the solid self-lubricating coating applied to the threads of the oil casing by using a small pin disc under the conditions of 300N load, 180rpm and 600s storage time, and calculating the friction coefficient and the wear amount;
the abrasion loss and friction coefficient test results of examples 1 to 5 and comparative examples 1 to 5 under low load and high load are shown in Table 1;
TABLE 1
The oil casing coated with the solid self-lubricating coating is repeatedly subjected to the shackle test, the number of times of shackle when the first thread of the oil casing is exposed is recorded, and the test result is shown in Table 2;
TABLE 2
Analysis of coating lubrication performance test results: examples 1 to 5 have excellent lubricating properties, both at low load and at high load; wherein the proportions of examples 1-5 in example 2 have the best lubricating ability; the possible reasons are: in the process of introducing phenylacetylene-terminated polyimide, phenylacetylene phthalic anhydride is added in the polycondensation reaction of the total polyimide precursor to prepare the phenylacetylene-terminated prepolymer with different molecular weights, and when the molecular weight is 5000, the prepared phenylacetylene-terminated polyimide has the best mechanical property tensile strength and microhardness.
The lubricating properties of comparative examples 1, 2 are significantly weaker than examples 1-5, wherein comparative example 1 differs from example 2 in that an equivalent amount of the unblocked modified polyimide is used in comparative example 1, and comparative example 2 also differs from example 3 in that an equivalent amount of the unblocked modified polyimide is also used in comparative example 2; and both comparative examples 1, 2 added additional curing agent;
the possible reason for the lubrication performance of the two to be greatly reduced is as follows: compared with unmodified polyimide, the polyimide with the end-capped modified polyimide has the advantages that the basic mechanical properties, tensile strength and microhardness are improved, and the polyimide is more difficult to strip by a dual material due to the excellent mechanical properties in the friction process; the increase of the microhardness is beneficial to the damage caused by the resistance load of the material and the reduction of corresponding abrasion deformation; thereby giving examples 1-5 more excellent lubricating properties.
Comparative example 3 is different from example 2 in that comparative example 3 does not use 5-amino-o-cresol modified graphene fluoride, but is replaced with an equivalent amount of graphite fluoride; comparative example 4 parts of 5-amino-o-cresol was added on the basis of comparative example 3; both have significantly weaker lubricating properties than example 2; the possible reasons are: unmodified graphite fluoride cannot achieve good dispersion effect in the coating by a physical dispersion means only; in the application, 5-amino-o-cresol and fluorinated graphene undergo nucleophilic substitution reaction in a molten state, and the amino surface is modified on the fluorinated graphene, so that the fluorinated graphene has good dispersibility, can be uniformly dispersed in a polyimide matrix, and hydrogen bond acting force is formed between the fluorinated graphene and imide molecules, so that the tensile strength and wear resistance of the coating are improved; thus, the performance of examples 1-5 is significantly better than that of comparative examples 3 and 4.
Comparative example 5 is a blank, and the lubricating properties of the non-modified polyimide and graphite fluoride are much weaker than those of examples 1-5.
And (3) analyzing the test result of the shackle detection performance: repeated shackle loading and unloading tests the durability of the oil casing in the actual use process, and test results show that: examples 1-5 employing the formulation of the present application all have excellent durability in practical applications; due to the self-lubricating property, the screw thread can be repeatedly pulled up and pulled down for more than 50 times, and the coating still covers the screw thread; has excellent application prospect.
Comprehensive analysis: compared with unmodified polyimide, the polyimide with the end-capped modified polyimide has the advantages that the basic mechanical properties, tensile strength and microhardness are improved, and the polyimide is more difficult to strip by a dual material due to the excellent mechanical properties in the friction process; the increase of the microhardness is beneficial to the damage caused by the resistance load of the material and the reduction of corresponding abrasion deformation; the introduction of fluorine atoms in the solid self-lubricating coating ensures that the fluorinated graphene has larger interlayer spacing and weaker interlayer shearing force compared with the original graphene, so that better lubricating performance is shown; in addition, the amino surface is modified on the fluorinated graphene through nucleophilic substitution reaction, so that the fluorinated graphene has good dispersibility, can be uniformly dispersed in a polyimide matrix, and also endows hydrogen bond acting force between the fluorinated graphene and imide molecules, so that the tensile strength and wear resistance of the coating are improved; the introduction of the amino-containing micromolecular chain segment ensures that the aminated fluorinated graphene is uniformly oriented and dispersed in the coating, and a covalent bond acting interface with good compatibility and thermal stability is constructed, so that the chemical stability of the coating is improved.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the application, and is not meant to limit the scope of the application, but to limit the application to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the application are intended to be included within the scope of the application.
Claims (10)
1. The solid self-lubricating coating comprises the following components in parts by weight: 40-50 parts of phenylacetylene-terminated polyimide, 5-15 parts of 5-amino-o-cresol modified fluorinated graphene, 5-8 parts of pigment and filler, 4-6 parts of cosolvent and 2-6 parts of defoamer.
2. The solid self-lubricating coating according to claim 1, wherein the solid self-lubricating coating comprises the following components in parts by weight: 42 parts of phenylacetylene-terminated polyimide, 8 parts of 5-amino-o-cresol modified fluorinated graphene, 6 parts of pigment and filler, 4 parts of cosolvent and 4 parts of defoamer.
3. The solid self-lubricating coating of claim 1, wherein the phenylacetylene terminated polyimide comprises the following components in parts by weight: 4-10 parts of bisphenol A dianhydride, 1 part of 4-phenylacetylene phthalic anhydride, 10 parts of 4,4' -diaminodiphenyl ether, 20 parts of N, N-dimethylformamide, 3 parts of triethylamine and 3 parts of acetic anhydride.
4. The solid self-lubricating coating of claim 1, wherein the pigment and filler is any one or more of titanium dioxide, alumina, hydrophilic silica.
5. The solid self-lubricating coating according to claim 1, wherein the cosolvent is any one of ethylene glycol and ethylene glycol ethyl ether.
6. The solid self-lubricating coating of claim 1, wherein the defoamer is one or more of polydimethylsiloxane, higher alcohols, and tributyl phosphate.
7. The solid self-lubricating coating of any one of claims 1-6, wherein the phenylacetylene terminated polyimide is prepared by the following steps: adding 4,4' -diaminodiphenyl ether and N, N-dimethylformamide into a reaction vessel with mechanical stirring, fully stirring at room temperature, and slowly adding a uniform mixture of bisphenol A dianhydride and 4-phenylacetylene phthalic anhydride after dissolving; after being uniformly mixed, the reaction vessel is placed in an ice-water bath for reaction for 5 hours; obtaining an intermediate product phenylacetylene end-capped polyamic acid solution; slowly adding triethylamine and acetic anhydride into phenylacetylene end-capped polyamic acid solution according to the mass ratio of 1:1, and placing a reaction container in a water bath at 60 ℃ for reaction for 3 hours; and then pouring the reacted mixture into enough absolute ethyl alcohol to separate out, obtaining light yellow precipitate, washing and filtering the prepared precipitate for multiple times, and then placing the precipitate in a 120 ℃ oven to be dried to constant weight, thus obtaining the phenylacetylene-terminated polyimide.
8. The solid self-lubricating coating according to any one of claims 1 to 6, wherein the preparation method of the 5-amino-o-cresol modified fluorinated graphene comprises the following steps: weighing graphite fluoride, adding the graphite fluoride into an ethanol solution of polyvinylpyrrolidone, performing ultrasonic dispersion, and then performing high-speed mechanical shearing and stirring on the solution after ultrasonic dispersion, wherein after stirring is completed; centrifuging the solution, collecting supernatant, filtering to remove excessive polyvinylpyrrolidone, and drying in a vacuum drying oven to obtain black precipitate; grinding and uniformly mixing black precipitate and 5-amino-o-cresol, adding the mixture into a reaction container, and fully reacting under the protection of argon; and adding distilled water into a reaction container, performing suction filtration to obtain a black sample, and repeatedly washing the black sample with distilled water and ethanol solution for multiple times to obtain the 5-amino-o-cresol modified fluorinated graphene.
9. The method for preparing a solid self-lubricating coating according to any one of claims 1 to 6, wherein the method for preparing a solid self-lubricating coating comprises the steps of: weighing 5-amino-o-cresol modified fluorinated graphene and a cosolvent according to a formula, and uniformly mixing the graphene and the cosolvent by utilizing ultrasound to obtain a mixture A; weighing phenylacetylene-terminated polyimide according to a formula, adding pigment and filler into a dispersion tank, and stirring and dispersing uniformly under the stirring condition of the rotating speed of 300-600r/min to obtain a mixture B; and finally, adding the mixture A into the mixture B, adding the defoaming agent, and stirring and dispersing uniformly under the stirring condition of the rotating speed of 800-1200r/min to obtain the solid self-lubricating coating.
10. Use of a solid self-lubricating coating according to any one of claims 1 to 6 on an oil casing thread, characterized in that the process for the preparation of the solid self-lubricating coating applied to an oil casing thread comprises: firstly degreasing the joint of a threaded joint oil pipe, fully spraying a mixed solution of sodium silicate and sulfonate on the threaded joint, reacting for 10min, and wiping off possible scraps and dust on the threaded surface by using absolute ethyl alcohol and absorbent cotton; finally, flushing with plasma water, wiping, and uniformly spraying along the thread surface by using a spray gun, wherein the spraying pressure is 0.5-0.8MPa; the distance between the spray gun nozzle and the threaded surface is 120-150mm, and the thickness of the coating is controlled to be 20-35 mu m; and (3) placing the sprayed sample into an electrothermal blowing drying oven, sintering for 10min at 260 ℃, cooling along with the furnace, and after cooling to normal temperature, preparing the solid self-lubricating coating applied to the oil sleeve threads.
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