CN117660076A - Composite multi-soap-based bearing grease resistant to 260 ℃ high temperature and extreme pressure and preparation method thereof - Google Patents
Composite multi-soap-based bearing grease resistant to 260 ℃ high temperature and extreme pressure and preparation method thereof Download PDFInfo
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- CN117660076A CN117660076A CN202311441163.9A CN202311441163A CN117660076A CN 117660076 A CN117660076 A CN 117660076A CN 202311441163 A CN202311441163 A CN 202311441163A CN 117660076 A CN117660076 A CN 117660076A
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- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 239000004519 grease Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000344 soap Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000007670 refining Methods 0.000 claims description 44
- 239000002585 base Substances 0.000 claims description 34
- 239000002562 thickening agent Substances 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 30
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000654 additive Substances 0.000 claims description 22
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 22
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- -1 alkyl naphthalene Chemical compound 0.000 claims description 20
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- 230000000996 additive effect Effects 0.000 claims description 18
- 229910052791 calcium Inorganic materials 0.000 claims description 18
- 239000011575 calcium Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 239000000440 bentonite Substances 0.000 claims description 14
- 229910000278 bentonite Inorganic materials 0.000 claims description 14
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 14
- 229920013639 polyalphaolefin Polymers 0.000 claims description 14
- 229940114072 12-hydroxystearic acid Drugs 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 239000012429 reaction media Substances 0.000 claims description 12
- 150000002148 esters Chemical class 0.000 claims description 11
- 159000000007 calcium salts Chemical class 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 238000007872 degassing Methods 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052582 BN Inorganic materials 0.000 claims description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- ALRFTTOJSPMYSY-UHFFFAOYSA-N tin disulfide Chemical compound S=[Sn]=S ALRFTTOJSPMYSY-UHFFFAOYSA-N 0.000 claims description 9
- 239000005069 Extreme pressure additive Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 239000007866 anti-wear additive Substances 0.000 claims description 8
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 8
- 239000000920 calcium hydroxide Substances 0.000 claims description 8
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 8
- 238000005260 corrosion Methods 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 8
- 229920001059 synthetic polymer Polymers 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 6
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000010702 perfluoropolyether Substances 0.000 claims description 6
- 229920005862 polyol Polymers 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 125000003354 benzotriazolyl group Chemical class N1N=NC2=C1C=CC=C2* 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 238000012858 packaging process Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 150000004867 thiadiazoles Chemical class 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 230000001050 lubricating effect Effects 0.000 abstract description 31
- 238000005553 drilling Methods 0.000 abstract description 7
- 238000005065 mining Methods 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 4
- 238000005461 lubrication Methods 0.000 abstract description 4
- 239000011707 mineral Substances 0.000 abstract description 4
- 239000003208 petroleum Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 description 18
- 238000000227 grinding Methods 0.000 description 14
- 230000035515 penetration Effects 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002199 base oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
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- Lubricants (AREA)
Abstract
The invention discloses a composite multi-soap-based anti-extreme pressure bearing grease with 260 ℃ high temperature resistance and a preparation method thereof. The lubricating grease has good oxidation resistance and bearing capacity, can meet the lubricating requirement of an ultra-deep well exploration tool at a high temperature of 200-260 ℃, and can also meet the effective lubrication of a sealed mining drill bit bearing. The method is suitable for the mixed drill bit and the roller bit in the fields of petroleum geological drilling, mineral geological development and the like, and has great significance for improving the service temperature and the bit pressure of the drill bit bearing.
Description
Technical Field
The invention relates to lubricating grease for hybrid drill bits and roller cone drill bits in the technical fields of petroleum geological exploration drilling, mineral geological development and the like. More specifically, the invention relates to a composite multi-soap base bearing grease with 260 ℃ high temperature resistance and extreme pressure resistance and a preparation method thereof.
Background
High-temperature oil and gas resources such as deep shale oil and gas, a myriameter well and the like are explored, the bottom hole temperature can reach 200-260 ℃, the rotation speed of the hybrid bit bearing is high, and 20-60% higher than that of the tricone bit bearing; the drilling pressure of the mining drill bit is doubled compared with that of the drill bit for oil in mineral geological development, the drilling pressure of the mining drill bit can reach about 50 tons, and the working temperature of the bearing is high under the conditions of high drilling pressure and high rotating speed, so that the high-temperature high-pressure resistant performance of the bearing lubricating grease is required.
The patent ZL201611055286.9 ultrahigh temperature resistant composite multi-soap base self-repairing bearing grease adopts composite synthetic base fluid, boron nitride, light calcium carbonate and other inert extreme pressure additives, so that the grease has good high temperature resistance, the product performance is kept unchanged under the environment of up to 200 ℃, and the drill bit bearing failure caused by performance degradation of the grease under the high temperature condition is avoided.
The ultra-high temperature resistant lubricating grease developed for the patent ZL201611055286.9 is subjected to high temperature resistance test. The method for measuring the extreme pressure performance of the lubricating grease is SH/T0202 (four-ball method), the sintering load of the ZL201611055286.9 patent product is 400KG under the high temperature condition of 260 ℃, and the heavy load abrasion test is 500KG-900rpm-600s is failed, so that the high temperature of 260 ℃ has obvious influence on the performance of the lubricating grease, the extreme pressure abrasion resistance of the product is obviously reduced, and the high temperature and high pressure resistant requirements of the ultra-high temperature hybrid drill bit and the sealed mining roller bit aimed by the method cannot be met. The technical problem in the field of the current lubricating materials is how to ensure that the performances of the lubricating grease for the bearings of the hybrid drill bit and the roller bit are not reduced and the lubricating grease for the bearings of the hybrid drill bit and the roller bit has higher temperature resistance and pressure resistance.
Disclosure of Invention
The invention aims to provide a composite multi-soap-base bearing grease with 260 ℃ high temperature resistance and extreme pressure resistance and a preparation method thereof, which not only can meet the high temperature, extreme pressure and wear-resistant lubrication requirements of a hybrid drill bit and a sealed mining roller bit bearing, but also can be used in an environment with the temperature of 200-260 ℃ and avoid the failure of the bit bearing caused by the reduction of the bearing capacity of the grease under the conditions of high temperature and high pressure.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a composite multi-soap base bearing grease resistant to high temperature of 260 ℃ and extreme pressure, comprising a composite base fluid, a composite calcium soap thickener, a high temperature antioxidant and corrosion resistant additive, an extreme pressure additive, an inert extreme pressure antiwear additive, a self-repairing additive and a structure improver, wherein the components are mixed and formulated according to weight percent:
wherein the composite base solution comprises, by weight, 150-25 parts of synthetic polymer poly alpha-olefin PAO, 20-25 parts of synthetic polymer poly alpha-olefin PAO, 40-50 parts of synthetic polymer poly alpha-olefin PAO, 1-25 parts of alkyl naphthalene, 0-25 parts of synthetic perfluoropolyether, 5-50 parts of synthetic polyol ester, 1-25 parts of synthetic metaphenylene ester and 1-25 parts of synthetic ester polymer; the composite base liquid is added with a synthetic ester polymer, which is high-viscosity synthetic ester, carboxylic acid derivative, and has excellent high temperature resistance, and the working temperature can reach 300 ℃;
the extreme pressure additive comprises 1-25 parts by weight of tin disulfide and 1-25 parts by weight of bismuth oxide;
the inert extreme pressure antiwear additive comprises, by weight, 1-25 parts of polarized graphite, 1-25 parts of tungsten disulfide, 1-25 parts of boron nitride, 0-25 parts of lanthanum oxide, 0-25 parts of neodymium oxide and 0-25 parts of nano calcium carbonate.
Preferably, the inert extreme pressure antiwear additive comprises 1-3 parts by weight of lanthanum oxide and 2.8-5.6 parts by weight of neodymium oxide.
Preferably, the extreme pressure additive is in a micron level, wherein the passing rate of 325 mesh particle diameters of tin disulfide and bismuth oxide is 90%, and the average particle diameter is 3-15 mu m; the inert extreme pressure antiwear agent is of a micron level, wherein the purity of lanthanum oxide and neodymium oxide is 99% (m/m), and the average particle size is 3-15 mu m; the polarized graphite is in micron level, the average grain diameter is 3-15 mu m, and the purity is 99% (m/m); the boron nitride is in micron level, the average grain diameter is 5-30 mu m, and the purity is 99% (m/m); the average grain diameter of the nano calcium carbonate is 20-30 nm, and the purity is 60-70% (m/m).
Preferably, the composite calcium soap thickener comprises 1 to 25 parts of composite calcium-based thickener and 1 to 25 parts of organic bentonite thickener by weight;
the composite calcium-based thickening agent is prepared by reacting and compounding calcium hydroxide with C8 acid, 12-hydroxystearic acid and C2 acid calcium salt, wherein the content of each component comprises 1-15 parts by weight of calcium hydroxide, 0-25 parts by weight of C8 acid, 1-25 parts by weight of 12-hydroxystearic acid and 1-25 parts by weight of C2 acid calcium salt; the calcium salt of C2 acid is micron-sized, the average grain diameter is 3-10 mu m, and the purity is 99% (m/m);
the organic bentonite thickener is prepared by reacting organic bentonite with one or more of water, alcohol and acetone, wherein the content of each component comprises 1-25 parts by weight of organic bentonite, 0-5 parts by weight of water, 0-5 parts by weight of alcohol and 0-5 parts by weight of acetone, and the total amount of water, alcohol and acetone is not less than 1 part and not more than 10 parts by weight.
Preferably, the high-temperature antioxidant and corrosion-resistant additive comprises a high-temperature antioxidant additive and an anti-corrosion metal passivating agent, wherein the high-temperature antioxidant additive is selected from 0-5 parts of one or more of phenol type, amine type or phenol amine type antioxidant additives; the anticorrosive metal passivating agent is one or more selected from benzotriazole derivative, thiadiazole derivative and other metal passivating agents in 0-5 parts.
Preferably, the self-repairing additive comprises 1-10 parts by weight of one or more of nano-scale copper, silver and zinc metal powder fillers, 0-5 parts by weight of magnesium oxide and 0-5 parts by weight of titanium dioxide.
Preferably, the structure improver is glycerol.
The invention also provides a preparation method of the composite multi-soap base bearing grease with 260 ℃ high temperature resistance and extreme pressure resistance, which comprises the following steps:
step one, preparing part of composite base solution serving as a reaction medium in a first refining kettle and a second refining kettle respectively;
step two, preparing a composite calcium-based thickening agent in a composite base solution of a reaction medium in a first refining kettle;
thirdly, preparing the organobentonite thickener in the composite base liquid of the reaction medium in a second refining kettle;
fourthly, compounding the organic bentonite thickener and the composite calcium-based thickener in a blending kettle;
and fifthly, adding and homogenizing the other additives in a blending kettle, blending, degassing and packaging.
Preferably, in the first step, the preparation process of the reaction medium composite base solution comprises the following steps: sequentially adding synthetic polymers of poly alpha-olefin PAO150, PAO20, PAO40, alkyl naphthalene and synthetic perfluoropolyether into a first refining kettle according to a proportion, dispersing, heating and preparing into uniform medium for standby; sequentially adding synthetic polyol ester, synthetic ester polymer and synthetic partial phenyl ester into a second refining kettle according to the formula proportion, dispersing, heating and preparing into uniform medium for later use;
in the second step, the preparation process of the composite calcium-based thickener comprises the following steps: adding calcium hydroxide into a reaction medium composite base solution in a first refining kettle, dispersing by a high-speed dispersing machine for not less than 40min, heating to 60 ℃, adding C8 acid, dispersing by the high-speed dispersing machine for not less than 20min, then adding 12-hydroxystearic acid, dispersing by the high-speed dispersing machine for not less than 20min, adding C2 acid calcium salt for composite refining, heating to 100 ℃ for reaction and dehydration, heating to 120 ℃, sampling and measuring the free acid-base content of a basic soap sample, regulating and controlling the free alkali content to 0.01-0.05 NaOH (m/m) by using 12-hydroxystearic acid, thickening, adding glycerol when heating to 160 ℃, continuously heating to the maximum refining temperature of 200-220 ℃, and keeping constant temperature for 20min;
in the third step, the preparation process of the organobentonite thickener comprises the following steps: adding organic bentonite into a reaction medium composite base solution in a second refining kettle, dispersing for at least 30min by a high-speed dispersing machine, heating to 50 ℃, adding one or more of water, alcohol and acetone, reacting for 30min, heating to 100 ℃, circularly stirring, removing alcohol and acetone for at least 60min, and standing by after preparation is completed;
in the fourth step, the preparation process of the composite calcium soap thickener comprises the following steps: transferring the composite calcium-based thickener prepared in the first refining kettle and the organobentonite thickener prepared in the second refining kettle to a blending kettle, compositing for 60min at 120-160 ℃ in the blending kettle, and cooling to below 100 ℃;
in the fifth step, the additive adding and homogenizing, blending, degassing and packaging processes are as follows: stirring, circulating and preserving heat of the cooled basic grease in a blending kettle, sequentially adding tin disulfide powder, bismuth oxide, tungsten disulfide, polarized graphite, boron nitride, lanthanum oxide, neodymium oxide and nano calcium carbonate, stirring and circulating for 60min, adding a high-temperature antioxidant and corrosion-resistant additive, then adding a self-repairing additive, fully and circularly dispersing, and finally homogenizing, shearing and degassing to obtain a finished product.
The above-mentioned homogenization, shearing, tempering and degassing are specifically referred to as: homogenizing: a technological mode of treating the lubricating grease by a homogenizer under the pressure condition of 15-20 Mpa; shearing: a technological mode of treating the lubricating grease by a static shearing machine under the pressure condition of 0.6-0.8 Mpa; blending: stirring and circularly treating the lubricating grease in a production kettle; degassing: the opening degree of the submarine valve of the production kettle is adjusted to enable the lubricating grease passing through the submarine valve to be in a negative pressure state, and the air in the lubricating grease is removed by utilizing the negative pressure.
The invention at least comprises the following beneficial effects:
1. the invention relates to a composite multi-soap-based high temperature resistant extreme pressure bearing grease with 260 ℃ resistance and a preparation method thereof on the basis of the extension and continuation of the patent of ZL200510120518.X, ZL201210033794.2 and ZL201611055286.9, in particular to the patent of ZL201611055286.9 ultra-high temperature resistant composite multi-soap-based self-repairing bearing grease. The lubricating grease has excellent high temperature resistance, high pressure resistance, extreme pressure wear resistance, good oxidation resistance and bearing capacity, thereby effectively meeting the application range of high temperature resistance and high bit pressure resistance of a bit bearing, being particularly suitable for being used in a hybrid bit bearing and a mining sealing roller bit in the field of petroleum geological drilling, not only meeting the lubrication requirements of high temperature, extreme pressure and wear resistance of the hybrid bit bearing of an ultra-deep well high temperature exploration tool at 200-260 ℃, but also meeting the effective lubrication of the bearing under the high bit pressure of the sealing mining roller bit. The method is suitable for the mixed drill bit and the roller bit in the fields of petroleum geological drilling, mineral geological development and the like, and has great significance for improving the service temperature and the bit pressure of the drill bit bearing.
2. The invention effectively improves the high-temperature extreme pressure wear resistance of the drill bit bearing grease. The working cone penetration of the product is not higher than 340mm 1/10, the working cone penetration of 6 ten thousand times is not higher than 370mm l/10, the drop point is not lower than 330 ℃, the extreme pressure sintering load is higher than 800KG, the comprehensive wear index is higher than 160, the scratch resistance is higher than 100lbf, and the high-temperature evaporation loss at 200 ℃ is not higher than 5%; high temperature wear resistance experiment: baking at 260 deg.C for 20min, wherein the diameter of the grinding mark of the sintered powder is not more than 2.0mm,500KG-900rpm-600s, and the diameter of the grinding mark is not more than 2.1mm.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description. It will be apparent that the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
The embodiment of the application provides a composite multi-soap-based bearing grease with 260 ℃ high temperature resistance and extreme pressure resistance and a preparation method thereof, which can solve the problem of insufficient bearing capacity of the bearing grease for a drill bit at the temperature of 200-260 ℃.
The preparation method is used for further improving the high temperature resistance of the lubricating grease, optimizing the formulas of the base liquid and the additive in the original patent ZL201611055286.9, and improving the preparation process, wherein on one hand, a refining kettle is added to avoid the influence of the additive on refining, and on the other hand, a high-speed dispersing machine is used for dispersing part of the thickening agent at a high speed, so that the high-temperature extreme pressure wear resistance and the stability of the lubricating grease are greatly improved.
The invention has the technical characteristics that: on the basis of ZL201611055286.9 patent, the high-temperature extreme pressure wear resistance of the lubricating grease is greatly improved by optimizing the formulas of the base fluid and the additive; the adopted composite synthetic base solution consists of several synthetic base oils with excellent high-temperature performance and supplementary performance, wherein synthetic ester polymer is newly introduced, and the high-temperature stability and lubricity of the lubricating grease product are improved; the adopted inert extreme pressure antiwear additive is still tungsten disulfide, polarized graphite and the like as the same as the ZL201611055286.9 patent, and is more different in that lanthanum oxide and neodymium oxide are adopted as the inert extreme pressure antiwear additive and tin disulfide is adopted as the extreme pressure additive in order to improve the high-temperature extreme pressure antiwear performance of the lubricating grease; and fourthly, the process is optimized, on one hand, a refining kettle is added to avoid the influence of additive residue on the refining effect of the composite thickener, and on the other hand, high-speed dispersing equipment is added to ensure that the stability and structural stability of the product are more excellent, and the high-temperature resistance of the product is greatly and positively improved.
Example 1
The lubricating grease is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
respectively adding 10 parts of PAO150 into a first refining kettle according to the measurement, uniformly and sequentially adding 7 parts of PAO20, 6 parts of PAO40, 4 parts of alkyl naphthalene and 6 parts of synthetic perfluoropolyether in a stirring state, uniformly mixing, heating and stirring the first refining kettle to 60 ℃, adding 2 parts of calcium hydroxide powder, circularly dispersing by a high-speed dispersing machine for not less than 40min, then adding 1 part of octanoic acid for not less than 20min, then adding 2 parts of 12-hydroxystearic acid for not less than 20min, reacting for 20min, then adding 3 parts of C2 calcium salt powder for not less than 30min, heating to 100 ℃, dehydrating by reaction, measuring the free alkali content by using a basic soap sample in the measured solution, regulating the free alkali content to 0.01-0.05 NAOH% (m/m) by using a proper amount of 12-hydroxystearic acid, continuously heating to 160 ℃, continuously heating to the maximum refining temperature of 200-220 ℃ for 20min, and standing for later use.
Respectively adding 7 parts of synthetic polyol ester into a second refining kettle according to the measurement, uniformly adding 7 parts of synthetic partial phenyl ester, 5 parts of synthetic ester polymer and 6 parts of PAO40 into the second refining kettle under the stirring state, uniformly mixing, adding 7 parts of organic bentonite, dispersing by a high-speed dispersing agent for not less than 30min, heating the second refining kettle to 50 ℃, adding 2 parts of alcohol, reacting for 30min, continuously heating to 100 ℃, stirring, circularly dispersing, removing alcohol for not less than 60min, and finishing preparation for later use;
transferring the materials in the first refining kettle and the second refining kettle to a blending kettle by a pump, reacting for 45min at 120-160 ℃, and stirring, circulating and cooling to below 100 ℃;
sequentially adding 5 parts of tin disulfide, 1 part of bismuth oxide, 5 parts of polarized graphite powder, 6 parts of tungsten disulfide powder, 2 parts of lanthanum oxide, 6 parts of boron nitride powder and 2 parts of nano calcium carbonate powder, stirring and circulating for 120min, adding 0.5 part of titanium dioxide and 1.5 parts of nano metallic silver paste, then adding 0.5 part of diphenylamine antioxidant additive and 0.5 part of alkyl thiadiazole metal passivator, stirring for 45min in a circulating way, and homogenizing, shearing, degassing and packaging the finished product.
The grease produced by the above procedure has 60 working cone penetration degrees of 321mm 1/10, a dropping point of 340 ℃, a sintering load of more than 800KG, an OK value of 103lbf, a comprehensive wear value of 169, an extreme pressure sintering load of 800KG at 260 ℃, and a high-temperature evaporation loss of 3.3% at 200 ℃, and the high-temperature wear-resisting experiment: at 260 ℃, the diameter of the 620KG sintering grinding mark is 1.81mm,500KG-900rpm-600s, and the diameter of the grinding mark is 1.76mm.
Example 2
The lubricating grease is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps: the preparation method is the same as in example 1.
The lubricating grease produced by the process has 60 working cone penetration degrees of 328mm 1/10, a dropping point of 338 ℃, a sintering load of more than 800KG, an OK value of 107lbf, a comprehensive wear value of 172, an extreme pressure sintering load of 800KG at 260 ℃ and a high-temperature evaporation loss of 3.5% at 200 ℃, and is subjected to high-temperature wear-resisting experiments: at 260 ℃, the diameter of the 620KG sintered grinding mark is 1.72mm,500KG-900rpm-600s, and the diameter of the grinding mark is 1.87mm.
Example 3
The lubricating grease is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps: the preparation method is the same as in example 1.
The lubricating grease produced by the process has 60 working cone penetration degrees of 326mm 1/10, a dropping point of 334 ℃, a sintering load of more than 800KG, an OK value of 106lbf, a comprehensive wear value of 167, an extreme pressure sintering load of 800KG under the condition of 260 ℃, and a high-temperature evaporation loss of 3.2% at 200 ℃, and is subjected to a high-temperature wear-resistant experiment: at 260 ℃, the diameter of the 620KG sintering grinding mark is 1.91mm,500KG-900rpm-600s, and the diameter of the grinding mark is 1.67mm.
Example 4
The lubricating grease is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
adding 7 parts of PAO150 into a first refining kettle according to the measurement, uniformly and sequentially adding 4 parts of PAO20, 5 parts of alkyl naphthalene and 8 parts of synthetic perfluoropolyether under the stirring state, uniformly mixing, heating the stirring refining kettle to 60 ℃, adding 3 parts of calcium hydroxide powder, circularly dispersing by a high-speed dispersing machine for not less than 40min, then adding 2 parts of octanoic acid for not less than 20min, then adding 2 parts of 12-hydroxystearic acid for not less than 20min, reacting for 20min, then adding 7 parts of C2 calcium salt powder for not less than 30min, heating to 100 ℃, dehydrating to 120 ℃, measuring the content of free alkali by using a basic soap sample in a measured solution, adjusting the content of the free alkali to 0.01-0.05 NAOH% (m/m) by using a proper amount of 12-hydroxystearic acid, continuously heating to 160 ℃, continuously heating to the maximum refining temperature of 200-220 ℃, and keeping the temperature for 20min for standby.
Adding 6 parts of synthetic polyol ester into a second refining kettle 2 according to the measurement, uniformly adding 5 parts of synthetic partial phenyl ester, 8 parts of synthetic ester polymer and 10 parts of PAO40 into the second refining kettle under the stirring state, uniformly mixing, adding 5 parts of organic bentonite, dispersing by a high-speed dispersing agent for not less than 30min, heating the second refining kettle to 50 ℃, adding 3 parts of alcohol, reacting for 30min, continuously heating to 100 ℃, stirring, circularly dispersing, removing alcohol for not less than 60min, and preparing for later use;
transferring the materials in the first refining kettle and the second refining kettle to a blending kettle by a pump, reacting for 45min at 120-160 ℃, and stirring, circulating and cooling to below 100 ℃;
sequentially adding 4 parts of tin disulfide, 4 parts of polarized graphite powder, 5 parts of tungsten disulfide powder, 4 parts of neodymium oxide, 6 parts of boron nitride powder and 0.5 part of nano calcium carbonate powder, stirring and circulating for 120min, adding 1 part of titanium dioxide and 0.5 part of nano metallic silver paste, then adding 0.5 part of diphenylamine antioxidant additive and 0.5 part of alkyl thiadiazole metal passivator, stirring for 45min in a circulating way, homogenizing in a circulating way, shearing, degassing and packaging to obtain a finished product.
The grease produced by the above procedure has 60 working cone penetration degrees of 323mm 1/10, a dropping point of 358 ℃, a sintering load of more than 800KG, an OK value of 101lbf, a comprehensive wear value of 177, an extreme pressure sintering load of 800KG at 260 ℃, and a high-temperature evaporation loss of 1.95% at 200 ℃, and the high-temperature wear resistance test: at 260 ℃, the diameter of the 620KG sintered grinding mark is 1.73mm,500KG-900rpm-600s, and the diameter of the grinding mark is 1.91mm.
Example 5
The lubricating grease is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps: the preparation method is the same as in example 4.
The lubricating grease produced by the process has 60 working cone penetration degrees of 330mm 1/10, a dropping point of 346 ℃, a sintering load of more than 800KG, a 0K value of 101Ibf, a comprehensive wear value of 175, an extreme pressure sintering load of 800KG at 260 ℃ and a high-temperature evaporation loss of 1.89% at 200 ℃, and is subjected to a high-temperature wear-resistant experiment: baking at 260 deg.C, sintering grinding mark diameter of 620Kg 1.69mm,500Kg-900rpm-600s, grinding mark diameter 2.19mm.
Example 6
The lubricating grease is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps: the preparation method is the same as in example 4.
The lubricating grease produced by the process has 60 working cone penetration degrees of 328mm 1/10, a dropping point of 352 ℃, a sintering load of more than 800KG, a 0K value of 101Ibf, a comprehensive wear value of 176, an extreme pressure sintering load of 800KG under the condition of 260 ℃, and high-temperature evaporation loss of 1.91% at 200 ℃, and the high-temperature wear resistance test: baking at 260 deg.C, sintering grinding mark diameter of 620Kg of 1.87mm,500Kg-900rpm-600s, grinding mark diameter of 1.81mm.
Examples 1, 2 and 3, the proportion of other additives is fixed, and only the adding proportion of lanthanum oxide serving as an inert extreme pressure wear-resistant agent is adjusted, so that the influence on the extreme pressure wear-resistant performance is achieved; examples 4, 5 and 6, the proportion of other additives is fixed, and only the adding proportion of the inert extreme pressure wear-resistant agent neodymium oxide is adjusted, so that the influence on the extreme pressure wear resistance is achieved.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use for which the invention is suited, and further modifications may be readily made by one skilled in the art, and the invention is therefore not to be limited to the particular details and examples shown and described herein, without departing from the general concepts defined by the claims and the equivalents thereof.
Claims (9)
1. The composite multi-soap-based 260 ℃ high temperature resistant extreme pressure bearing grease is characterized by comprising a composite base fluid, a composite calcium soap thickener, a high temperature antioxidant corrosion resistant additive, an extreme pressure additive, an inert extreme pressure antiwear additive, a self-repairing additive and a structure improver which are mixed and prepared, wherein the contents of the components are as follows by weight:
wherein the composite base solution comprises, by weight, 150-25 parts of synthetic polymer poly alpha-olefin PAO, 20-25 parts of synthetic polymer poly alpha-olefin PAO, 40-50 parts of synthetic polymer poly alpha-olefin PAO, 1-25 parts of alkyl naphthalene, 0-25 parts of synthetic perfluoropolyether, 5-50 parts of synthetic polyol ester, 1-25 parts of synthetic metaphenylene ester and 1-25 parts of synthetic ester polymer;
the extreme pressure additive comprises 1-25 parts by weight of tin disulfide and 1-25 parts by weight of bismuth oxide;
the inert extreme pressure antiwear additive comprises, by weight, 1-25 parts of polarized graphite, 1-25 parts of tungsten disulfide, 1-25 parts of boron nitride, 0-25 parts of lanthanum oxide, 0-25 parts of neodymium oxide and 0-25 parts of nano calcium carbonate.
2. The composite multi-soap base 260 ℃ high temperature extreme pressure resistant bearing grease according to claim 1, wherein the inert extreme pressure antiwear additive comprises 1-3 parts by weight of lanthanum oxide and 2.8-5.6 parts by weight of neodymium oxide.
3. The composite multi-soap base high temperature 260 ℃ resistant extreme pressure bearing grease according to claim 1, wherein the extreme pressure additive is in micron order, wherein the passing rate of 325 mesh particle size of tin disulfide and bismuth oxide is 90%, and the average particle size is 3-15 μm; the inert extreme pressure antiwear agent is of a micron level, wherein the purity of lanthanum oxide and neodymium oxide is 99% (m/m), and the average particle size is 3-15 mu m; the polarized graphite is in micron level, the average grain diameter is 3-15 mu m, and the purity is 99% (m/m); the boron nitride is in micron level, the average grain diameter is 5-30 mu m, and the purity is 99% (m/m); the average grain diameter of the nano calcium carbonate is 20-30 nm, and the purity is 60-70% (m/m).
4. The composite multi-soap-based anti-extreme pressure bearing grease with 260 ℃ high temperature resistance according to claim 1, wherein the composite calcium soap thickener comprises 1-25 parts of composite calcium-based thickener and 1-25 parts of organic bentonite thickener by weight;
the composite calcium-based thickening agent is prepared by reacting and compounding calcium hydroxide with C8 acid, 12-hydroxystearic acid and C2 acid calcium salt, wherein the content of each component comprises 1-15 parts by weight of calcium hydroxide, 0-25 parts by weight of C8 acid, 1-25 parts by weight of 12-hydroxystearic acid and 1-25 parts by weight of C2 acid calcium salt; the calcium salt of C2 acid is micron-sized, the average grain diameter is 3-10 mu m, and the purity is 99% (m/m);
the organic bentonite thickener is prepared by reacting organic bentonite with one or more of water, alcohol and acetone, wherein the content of each component comprises 1-25 parts by weight of organic bentonite, 0-5 parts by weight of water, 0-5 parts by weight of alcohol and 0-5 parts by weight of acetone, and the total amount of water, alcohol and acetone is not less than 1 part and not more than 10 parts by weight.
5. The composite multi-soap-based 260 ℃ high temperature extreme pressure resistant bearing grease according to claim 1, wherein the high temperature antioxidant and corrosion resistant additive comprises a high temperature antioxidant additive and an anti-corrosion metal passivating agent, wherein the high temperature antioxidant additive is selected from 0-5 parts of one or more of phenol type, amine type or phenol amine type antioxidant additives; the anticorrosive metal passivating agent is one or more selected from benzotriazole derivative, thiadiazole derivative and other metal passivating agents in 0-5 parts.
6. The composite multi-soap base 260 ℃ high temperature resistant extreme pressure resistant bearing grease according to claim 1, wherein the self-repairing additive comprises 1-10 parts by weight of one or more of nano-scale copper, silver and zinc metal powder fillers, 0-5 parts by weight of magnesium oxide and 0-5 parts by weight of titanium dioxide.
7. The composite multi-soap base 260 ℃ high temperature extreme pressure resistant bearing grease according to claim 1, wherein the structure improver is glycerol.
8. A method for preparing the composite multi-soap base 260 ℃ high temperature resistant extreme pressure resistant bearing grease according to any one of claims 1 to 7, comprising the following steps:
step one, preparing part of composite base solution serving as a reaction medium in a first refining kettle and a second refining kettle respectively;
step two, preparing a composite calcium-based thickening agent in a composite base solution of a reaction medium in a first refining kettle;
thirdly, preparing the organobentonite thickener in the composite base liquid of the reaction medium in a second refining kettle;
fourthly, compounding the organic bentonite thickener and the composite calcium-based thickener in a blending kettle;
and fifthly, adding and homogenizing the other additives in a blending kettle, blending, degassing and packaging.
9. The method for preparing the composite multi-soap base 260 ℃ high temperature and extreme pressure resistant bearing grease according to claim 8, wherein in the first step, the preparation process of the reaction medium composite base liquid is as follows: sequentially adding synthetic polymers of poly alpha-olefin PAO150, PAO20, PAO40, alkyl naphthalene and synthetic perfluoropolyether into a first refining kettle according to a proportion, dispersing, heating and preparing into uniform medium for standby; sequentially adding synthetic polyol ester, synthetic ester polymer and synthetic partial phenyl ester into a second refining kettle according to the formula proportion, dispersing, heating and preparing into uniform medium for later use;
in the second step, the preparation process of the composite calcium-based thickener comprises the following steps: adding calcium hydroxide into a reaction medium composite base solution in a first refining kettle, dispersing by a high-speed dispersing machine for not less than 40min, heating to 60 ℃, adding C8 acid, dispersing by the high-speed dispersing machine for not less than 20min, then adding 12-hydroxystearic acid, dispersing by the high-speed dispersing machine for not less than 20min, adding C2 acid calcium salt for composite refining, heating to 100 ℃ for reaction and dehydration, heating to 120 ℃, sampling and measuring the free acid-base content of a basic soap sample, regulating and controlling the free alkali content to 0.01-0.05 NaOH (m/m) by using 12-hydroxystearic acid, thickening, adding glycerol when heating to 160 ℃, continuously heating to the maximum refining temperature of 200-220 ℃, and keeping constant temperature for 20min;
in the third step, the preparation process of the organobentonite thickener comprises the following steps: adding organic bentonite into a reaction medium composite base solution in a second refining kettle, dispersing for at least 30min by a high-speed dispersing machine, heating to 50 ℃, adding one or more of water, alcohol and acetone, reacting for 30min, heating to 100 ℃, circularly stirring, removing alcohol and acetone for at least 60min, and standing by after preparation is completed;
in the fourth step, the preparation process of the composite calcium soap thickener comprises the following steps: transferring the composite calcium-based thickener prepared in the first refining kettle and the organobentonite thickener prepared in the second refining kettle to a blending kettle, compositing for 60min at 120-160 ℃ in the blending kettle, and cooling to below 100 ℃;
in the fifth step, the additive adding and homogenizing, blending, degassing and packaging processes are as follows: stirring, circulating and preserving heat of the cooled basic grease in a blending kettle, sequentially adding tin disulfide powder, bismuth oxide, tungsten disulfide, polarized graphite, boron nitride, lanthanum oxide, neodymium oxide and nano calcium carbonate, stirring and circulating for 60min, adding a high-temperature antioxidant and corrosion-resistant additive, then adding a self-repairing additive, fully and circularly dispersing, and finally homogenizing, shearing and degassing to obtain a finished product.
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