CN106433861A - Lubricating grease - Google Patents
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- CN106433861A CN106433861A CN201510479753.XA CN201510479753A CN106433861A CN 106433861 A CN106433861 A CN 106433861A CN 201510479753 A CN201510479753 A CN 201510479753A CN 106433861 A CN106433861 A CN 106433861A
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Abstract
The present invention relates to a lubricating grease, which comprises base oil, 12-hydroxystearic acid, lithium hydroxide, potassium hydroxide, petroleum calcium sulfonate, rosin, vegetable oil, (NH4)xMoS2, a first solid additive, a second solid additive, a first composite modifier comprising trioctylmethylammonium bromide, glycerol and polytetrafluoroethylene, a second composite modifier comprising diphenylamine, 2,6-di-tert-butyl and benzotriazole, and a third composite modifier comprising sulfurized cottonseed oil T404, bis(2-mercapto-4-n-propylamino-1,3,5-triazine)thioether and bis(2-mercapto-4-cyclopentylamino-1, 3,5-triazine)thioether. The lubricating grease of the present invention has advantages of good sealing performance, strong corrosion resistance, excellent anti-wear performance, and excellent anti-extreme pressure performance.
Description
Technical field
The present invention relates to lubricating oil field, particularly to a kind of grease.
Background technology
China's grease industry develops rapidly in recent years, and grease industry has become China's chemicals industry mainstay.China's grease total output in 2012 reaches surprising 44.40 ten thousand ton, account for more than the 40% of global grease yield, the ranking whole world first, simultaneously grease great variety of goods include lithium saponify, calcium grease, aluminium base fat, bentonite grease etc., substantially can meet whole nation all trades and professions demand.Wherein have the call, range of application is the widest for lithium saponify, accounts for the 70% about of whole yield.
CN100389183C (2008-5-21) discloses a kind of lithium base grease in high drop point and preparation method thereof, but this PERFORMANCE OF GREASES still has much room for improvement.
Content of the invention
It is an object of the invention to provide a kind of good seal performance, corrosion resistance are strong, have excellent anti-attrition and the grease of anti-extreme pressure energy.
The above-mentioned technical purpose of the present invention technical scheme is that：
A kind of grease, it is prepared from by the raw material that following parts by weight are major constituent：
Base oil 88-95 part；
Ten dihydroxystearic acid 4-7 parts；
Lithium hydrate 0.05-1.25 part；
Potassium hydroxide 0.8-2.4 part；
Calcium mahogany sulfonate 5-10 part；
Colophonium 2-6 part；
Vegetable oil 8-15 part；
(NH4)xMoS2
7-13 part；
First solid additive 3-7 part；
Second solid additive 1.5-6 part；
In mass ratio 1：3-4：First composite regulator 6-9 part of the tricaprylmethyl ammonium bromide of 1-2 proportioning, glycerol and politef composition；
In mass ratio 1：2-4：Second composite regulator 7-11 part of the diphenylamines of 1-3 proportioning, 2,6- di-t-butyl and BTA composition；
In mass ratio 1：0.5-0.8：The 3rd composite regulator 8-14 part of sulfuration cottonseed oil T404 of 1.3-1.7 proportioning, two (2- sulfydryl -4- n-propylamine base -1,3,5- triazine) thioethers and two (2- sulfydryl -4- Aminocyclopentane base -1,3,5- triazine) thioether composition；
Described base oil is to compare 1 according to weight：3-5：The mixture of the paraffinic base, cycloalkyl and polyalphaolefin of 2-4 composition；The viscosity when 60 DEG C for the described base oil is 100-300cSt, 230-250 DEG C of open flash point, and pour point is in -10 DEG C of -40-；
The total base number of described calcium mahogany sulfonate is 300-350；
The specific surface area of described politef is 2-6m2/g；
The particle size range of the first solid additive is 0.8-5 micron；Wherein, the granule of 0.8-1 micron accounts for the 20-40% of described solid additive gross weight；The granule of 1-2 micron accounts for the 10-30% of described solid additive gross weight；The granule of balance of 3-5 micron；
Described first solid additive is following Formulas I polymer, wherein MwFor 6.10 × 106, MnFor 2.0 × 106, molecular weight distributing index is 3.1：
I.
Described second solid additive is for the molybdenum disulfide nano ball of particle diameter 10-20 nanometer and the regulation grain of particle diameter 6-9 micron according to mass ratio 1:The mixture of 2-5 composition.
The mixture of paraffinic base of the present invention, cycloalkyl and polyalphaolefin is the mixture of paraffin base oil, naphthenic base oils and polyalphaolefin base；The Lithium hydrate of the present invention prepares generation compositing lithio ester with monocarboxylic acid or dicarboxylic acids through in-situ chemical reaction；(NH4)xMoS2In chemical reaction, preparation generates monolithic layer MoS in the original location2, interlayer slip effect is played by the effect of described first solid additive and Second addition simultaneously, improves lubricity, wear resistence and the sealing property of grease.
Meanwhile, after the present invention the first composite regulator proportioning, there is excellent dispersion, coagulate the soup and anti-wear and wear-resistant performance；There is after described second composite regulator proportioning antioxidation and bright and clean corrosion-resistant function；After described 3rd composite regulator proportioning, there are good anti-extreme pressure and anti wear properties；Three kinds of composite regulators are combined and can be reached synergistic function；
First solid additive of different-grain diameter and species and the second solid additive are while increasing Lubricating Greases extreme pressure and anti-wear performance, grease can also be given with water repelling property and anti-wear lubricating performance so that disclosure satisfy that underwater operation requires with the machinery equipment of grease of the present invention.
Base oil according to proportioning of the present invention composition, after combining with the various additives of the present invention and regulator, the grease made is made to have the performance of high temperature resistant (more than 300 DEG C) and low temperature resistant (less than -40 DEG C) concurrently, multiple special occasions can be used for, under for example northern working environment of high temperature such as high temperature wire drawing and low temperature, all there is preferable mobility, greasy property, resistance to high temperature oxidation and surface antirust function.
Preferably, described regulation grain is one or more of micro powder graphite, Calcium Carbonate, copper powder or tungsten disulfide.
Preferably, also including polyacrylate -2- cross linked polymer and impregnating fluid in mass ratio 1 in grease:The 4th composite regulator 3-7 part of 1-4 composition；
The preparation method of described polyacrylate -2- cross linked polymer is：
(1) prepared polymer P (MMA-MAh)-PEG6000 30-40 part, regulation liquid 40-60 part form first and just mix liquid by weight；The described liquid that adjusts is to include the carbonic allyl ester solution that concentration is the sodium perchlorate of the 0.4-0.7mol/L and concentration N- butyl benzimidazole for 0.3-0.8mol/L；MMA in described polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, MAh is maleic anhydride, P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, and PEG6000 is the Polyethylene Glycol that molecular weight is 6000；
(2) add 2-7 part ten dihydroxystearic acid in described first just mixed liquid, be heated to 30-45 DEG C of reaction 5-9min under nitrogen protection；
(3) deionized water obtains polyacrylate -2- cross linked polymer after rinsing and being dried.
Polyacrylate -2- cross linked polymer using present invention preparation has excellent hot property and dimensional stability, enables grease to possess more excellent sealing property, corrosion resistance, anti-attrition and anti-extreme pressure.
Preferably, described anti-corrosion liquid making method：
A. AVC 10-18 part, sodium fluoride 20-40 part, ammonium acid fluoride 30-60 part, potassium permanganate 10-20 part, Neutral potassium chromate 40-50 part are added by weight in order successively；Stirring 5-10min, obtains second and just mixes liquid；
B. and then in order toward in described second just mixed liquid add zinc phosphate 15-25 part, sodium nitrate 8-18 part, praseodymium chloride 5-12 part, ethylenediaminetetraacetic acid 10-16 part, malic acid 7-14 part, dodecyl phenenyl sulfate 8-12 part, nickel sulfate 6-13 part, triethanolamine 15-25 part successively, stir 1-4min.
Inventor finds, during the preparation of impregnating fluid mix and blend, the order that various composition is added has an impact to the performance of grease.Impregnating fluid according to the preparation of the inventive method order of addition makes the stability of grease more preferably, with more wearability and anti-corrosive properties.
Preferably, also including potassium borohydride 1-3 part, bicyclohexane simultaneously -18- crown- 6 4-6 part and dibenzyl xenol polyoxyethylene polyoxypropylene ether 5-8 part in described impregnating fluid.
Inventor finds, adds the impregnating fluid of described material, can make when preparing grease that grease stability, sealing and corrosion resistance are good, storage time is long.
Preferably, preparation of greases method includes：
A. in order successively by ten dihydroxystearic acid 4-7 parts, calcium mahogany sulfonate 5-10 part, Colophonium 2-6 part, vegetable oil 8-15 part, (NH4)xMoS2
7-13 part, first solid additive 3-7 part and second solid additive 1.5-6 part add in 88-95 part base oil, ultrasonic disperse, it is subsequently adding Lithium hydrate 0.05-1.25 part, potassium hydroxide 0.8-2.4 part and dicarboxylic acids 10-20 part, be heated to 60-80 DEG C of reaction 10-15min and obtain the first reactant liquor；
B. sequentially add in mass ratio 1 in order toward in described first reactant liquor：3-4：First composite regulator 6-9 part of the tricaprylmethyl ammonium bromide of 1-2 proportioning, glycerol and politef composition；In mass ratio 1：2-4：Second composite regulator 7-11 part of the diphenylamines of 1-3 proportioning, 2,6- di-t-butyl and BTA composition；It is warming up to 85-95 DEG C of reaction 20-30min for the first time, be then incubated 1-2h for the first time；Then heat up dehydration for second to 120-150 DEG C, then second insulation 15-20min；Add in mass ratio 1：0.5-0.8：The 3rd composite regulator 8-14 part of sulfuration cottonseed oil T404 of 1.3-1.7 proportioning, two (2- sulfydryl -4- n-propylamine base -1,3,5- triazine) thioethers and two (2- sulfydryl -4- Aminocyclopentane base -1,3,5- triazine) thioether composition；Third time is warming up to 180-200 DEG C, cooling, obtains grease.
The good seal performance of the grease prepared by ad hoc approach of the present invention, corrosion resistance are strong, have excellent anti-attrition and anti-extreme pressure energy.
Preferably, described grease preparation also includes step C:After adding described 3rd composite regulator temperature reaction, it is cooled to 90-120 DEG C, add described 4th composite regulator 3-7 part, then circulation stirring, homogenizing is processed, degassing, obtain grease.
Preferably, described step B is additionally included in after insulation terminates for the first time adds fire retardant 4-8 part, described fire retardant is according to mass ratio 1:2-3:The ammonium pyrophosphate of 1-4 composition, boric acid and melamine cyanurate.
Inventor finds, adds described fire retardant in the time between first time insulation and second heat up, and while grease of the present invention can be enable to keep its anti-extreme pressure, obtains anti-flammability incombustible in 800 DEG C of hot plates.
In sum, the invention has the advantages that：
1st, the good seal performance of the grease of the present invention, corrosion resistance is strong, have excellent anti-attrition and anti-extreme pressure energy；
2nd, the additive of different-grain diameter and species, particularly first solid additive is while increasing Lubricating Greases extreme pressure and anti-wear performance, grease can also be given with water repelling property and anti-wear lubricating performance so that disclosure satisfy that underwater operation requires with the machinery equipment of grease of the present invention；
3rd, according to the base oil of proportioning of the present invention composition, after combining with the various additives of the present invention and regulator, the grease made is made to have the performance of high temperature resistant (more than 300 DEG C) and low temperature resistant (less than -40 DEG C) concurrently, multiple special occasions can be used for, under for example northern working environment of high temperature such as high temperature wire drawing and low temperature, all there is preferable mobility, greasy property, resistance to high temperature oxidation and surface antirust function；
4th, add described fire retardant in the time between first time insulation and second heat up, while grease of the present invention can be enable to keep its anti-extreme pressure, obtain anti-flammability incombustible in 800 DEG C of hot plates.
Embodiment
Below by embodiment, the invention will be further described.It should be understood that embodiment of the present invention methods described is only used for the present invention is described, rather than limitation of the present invention, under the concept thereof of the present invention, the scope of protection of present invention is broadly fallen into the simple modifications of preparation method of the present invention.The all raw materials used in embodiment and solvent are purchased from Sigma Biochemical and
Organic Compounds for Research and Diagnostic Clinical Reagents company.
Formula
I
The preparation embodiment of polymer：
1) in 250mL flask with three necks,round bottom, add 1,5- naphthyridines (30mmol), potassium iodide (50mmol), potassium iodate (50mmol) and glacial acetic acid (150mL), are stirred at room temperature and so that it is dissolved, and are then heated to 80 DEG C and react 6 hours.It is cooled to room temperature, filters, filter cake uses water, saturation Na successively2CO3, saturation Na2S2O3Fully wash with water, obtain the solid product of white solid.
2) in 100mL flask with three necks,round bottom, add step 1) product (4mmol), 2- methyl -3- butyne-2-alcohol (12mmol) and NEt3(40mL), stir, substitute gas twice, then deaerate 30 minutes, add Pd (PPh under hydrogen shield3)2Cl2(0.1mmol), PPh3(0.3mmol) with CuI (0.8mmol), overnight, TLC display reaction completely, terminates to react heating reflux reaction.It is cooled to room temperature, filters, precipitation is washed three times with EA.It is filtrated to get white solid, not purified be directly used in next step.
3) in 100mL round bottom single-necked flask, add step 2) product (2.4mmol), powder potassium hydroxide (7.2 mmol) and 60 milliliters of isopropanol, the lower back flow reaction of argon protection 4 hours, terminate to react.It is cooled to room temperature, rotary evaporation removes isopropanol, obtains faint yellow solid.
4) in 250mL flask with three necks,round bottom, add the magnesium silk (0.1mol) shearing and two iodine, substitute gas twice.With the oxolane (10mL) that needle tubing injection is dry, stir-activating 30 minutes, it is slowly added dropwise oxolane (25mL) solution of bromoethane (0.1mol), keep solution micro-boiling.Completion of dropping, is heated to reflux l hour.It is cooled to room temperature, is slowly added dropwise oxolane (20mL) solution of phenylacetylene (0.1mol), exit in time, until system is not having bubble to emerge, be heated to reflux 2 hours.It is cooled to room temperature, it is slowly added dropwise oxolane (20mL) solution of dichlorodimethylsilane (0.05mol), completion of dropping, it is heated to reflux 3 hours, it is cooled to room temperature, add water (50mL) and acetic acid second cruel (50mL), separate organic layer, aqueous layer with ethyl acetate extracts (50mL × 2), merge organic layer, anhydrous sodium sulfate drying, filter, decompression removes solvent, obtain light yellow solid, solid is dissolved in the normal hexane of a small amount of boiling, is subsequently cooled to -30 DEG C one hour, filter, obtain beige solid.
5) in 250mL flask with three necks,round bottom, add naphthalene (37.6mmol), substitute gas twice, argon ball is protected.With the oxolane (24mL) that needle tubing injection is dry, stir and be allowed to dissolve, hydrogen deaerates half an hour.Under the protection of argon ball, it is rapidly added lithium piece (36mmol), stir 6 hours under room temperature, obtain blackish green viscous solution.In another 100mL flask with three necks,round bottom, step 4) product (8mmol), hydrogen balloon protects.With the oxolane (40mL) that needle tubing injection is dry, stir to dissolving, deaerate half an hour.Then solution of silane is slowly dropped in naphthalene lithium (about 20 minutes), completion of dropping, wraps up this flask with aluminium-foil paper, be cooled to -10 DEG C.Oxolane (33mL) solution (about 30 minutes) of dropwise Deca anhydrous zinc chloride (40mmol) in this naphthalene lithium/solution of silane, stirs 20 minutes.It is further continued for being cooled to -78 DEG C, promptly adds oxolane (16mL) solution of NBS (20mmol) with needle tubing, add continuation stirring 1 hour.Take out reaction bulb from cryostat, cold soln is lentamente poured into the NH of semi-saturation containing 150mL4Claq. in the conical flask (250mL) of solution, it is extracted with ethyl acetate (50mL × 3).Merge organic layer, use half saturated Na successively2S2O3(50mL), water (100mL) and saturated aqueous common salt (50mL × 2) washing, anhydrous Na2SO4It is dried.Short silicagel column post filter, decompression removes solvent, and the purification (silica gel, petroleum ether) of column chromatography obtains 0.9 gram of white solid.
6) in 50mL flask with three necks,round bottom, add step 5) product (1mmol), step 3) product (1mmol), toluene (10mL) and triethylamine (3mL), stirring time argon-degassed 30 minutes.Add Pd (PPh under argon protection3)4(50mg) with CuI (20mg), it is heated to 60 DEG C, react three days.It is cooled to room temperature, filter, remove solvent under reduced pressure.Residue CHCl3(3mL) it is completely dissolved, methanol (35mL) separates out, and refilters and obtains polymer solids.This program in triplicate, in order to remove the polymer of remaining unreacted monomer and low-molecular-weight.It is vacuum dried 1 hour at 60 DEG C, obtain white granular solid 97mg.Described Formulas I polymer is as follows,
Wherein MwFor 6.10 × 106, MnFor 2.0 × 106, molecular weight distributing index is 3.1.
1HNMR (300 MHz, DMSO), δ: 9.16 (s, 2H, CH); 8.57 (s,
2H, CH); 7.37 (d, 4H, CH); 7.35 (d, 2H, CH); 7.17 (d, 4H, CH); 0.14 (s, 6H, CH3).
Embodiment one：
A. in order successively by 4 parts of ten dihydroxystearic acid, 5 parts of calcium mahogany sulfonate, 2 parts of Colophonium, 8 parts of vegetable oil, (NH4)xMoS2
7 parts, 3 parts of the first solid additive and 1.5 parts of the second solid additive add in 88 parts of base oils, and ultrasonic disperse is subsequently adding 0.05 part of Lithium hydrate, 2.4 parts of potassium hydroxide and 20 parts of dicarboxylic acids, are heated to 60 DEG C of reaction 10min and obtain the first reactant liquor；
Wherein, base oil is to compare 1 according to weight：3：The mixture of the paraffinic base, cycloalkyl and polyalphaolefin of 4 compositions；The viscosity when 60 DEG C for the base oil is 100cSt, 230 DEG C of open flash point, and pour point is at -40 DEG C；
The total base number of calcium mahogany sulfonate is 300；
The specific surface area of politef is 2m2/g；
The particle size range of the first solid additive is 0.8-5 micron；Wherein, the granule of 0.8-1 micron accounts for the 20% of solid additive gross weight；The granule of 1-2 micron accounts for the 10% of solid additive gross weight；Balance of 3 microns of granule；
Second solid additive is for the molybdenum disulfide nano ball of 10 nanometers of particle diameter and the tungsten disulfide of particle diameter 6-9 micron according to mass ratio 1:The mixture of 2 compositions.
B. sequentially add in mass ratio 1 in order toward in the first reactant liquor：3：6 parts of first composite regulator of the tricaprylmethyl ammonium bromide of 2 proportionings, glycerol and politef composition；In mass ratio 1：2：7 parts of second composite regulator of the diphenylamines of 3 proportionings, 2,6- di-t-butyl and BTA composition；It is warming up to 85 DEG C of reaction 20min for the first time, be then incubated 1h for the first time；Then heat up dehydration for second to 120 DEG C, then second insulation 15min；Add in mass ratio 1：0.5：8 parts of 3rd composite regulator of sulfuration cottonseed oil T404 of 1.7 proportionings, two (2- sulfydryl -4- n-propylamine base -1,3,5- triazine) thioethers and two (2- sulfydryl -4- Aminocyclopentane base -1,3,5- triazine) thioether composition；Third time is warming up to 180 DEG C, cooling, obtains grease.
Embodiment two：
In order successively by 7 parts of ten dihydroxystearic acid, 10 parts of calcium mahogany sulfonate, Colophonium 2-6 part, 15 parts of vegetable oil, (NH4)xMoS2
13 parts, 7 parts of the first solid additive and 6 parts of the second solid additive add in 88-95 part base oil, and ultrasonic disperse is subsequently adding 1.25 parts of Lithium hydrate, 0.8 part of potassium hydroxide and 10 parts of dicarboxylic acids, are heated to 80 DEG C of reaction 15min and obtain the first reactant liquor；
Wherein, base oil is to compare 1 according to weight：5：The mixture of the paraffinic base, cycloalkyl and polyalphaolefin of 2 compositions；The viscosity when 60 DEG C for the base oil is 100-300cSt, 250 DEG C of open flash point, and pour point is at -10 DEG C；
The total base number of calcium mahogany sulfonate is 350；
The specific surface area of politef is 6m2/g；
The particle size range of the first solid additive is 0.8-5 micron;Wherein, the granule of 0.8-1 micron accounts for the 40% of solid additive gross weight；The granule of 1-2 micron accounts for the 30% of solid additive gross weight；Balance of 5 microns of granule；
Second solid additive is for the molybdenum disulfide nano ball of 20 nanometers of particle diameter and the micro powder graphite of 9 microns of particle diameter according to mass ratio 1:The mixture of 2-5 composition.
Sequentially add in mass ratio 1 in order toward in the first reactant liquor：4：9 parts of first composite regulator of the tricaprylmethyl ammonium bromide of 1 proportioning, glycerol and politef composition；In mass ratio 1： 4：Second composite regulator 7- part of the diphenylamines of 1 proportioning, 2,6- di-t-butyl and BTA composition；It is warming up to 95 DEG C of reaction 30min for the first time, be then incubated 2h for the first time；Then heat up dehydration for second to 150 DEG C, then second insulation 20min；Add in mass ratio 1：0.8：14 parts of 3rd composite regulator of sulfuration cottonseed oil T404 of 1.3 proportionings, two (2- sulfydryl -4- n-propylamine base -1,3,5- triazine) thioethers and two (2- sulfydryl -4- Aminocyclopentane base -1,3,5- triazine) thioether composition；Third time is warming up to 200 DEG C, cooling, obtains grease.
Embodiment three：
In order successively by 5 parts of ten dihydroxystearic acid, 7 parts of calcium mahogany sulfonate, 4 parts of Colophonium, 12 parts of vegetable oil, (NH4)xMoS2
9 parts, 5 parts of the first solid additive and 4 parts of the second solid additive add in 92 parts of base oils, and ultrasonic disperse is subsequently adding 0.95 part of Lithium hydrate, 1.4 parts of potassium hydroxide and 15 parts of dicarboxylic acids, are heated to 70 DEG C of reaction 12min and obtain the first reactant liquor；
Wherein, base oil is to compare 1 according to weight：4：The mixture of the paraffinic base, cycloalkyl and polyalphaolefin of 3 compositions；The viscosity when 60 DEG C for the base oil is 200cSt, 240 DEG C of open flash point, and pour point is at -20 DEG C；
The total base number of calcium mahogany sulfonate is 330；
The specific surface area of politef is 4m2/g；
The particle size range of the first solid additive is 0.8-5 micron;Wherein, the granule of 0.8-1 micron accounts for the 30% of solid additive gross weight;The granule of 1-2 micron accounts for the 20% of solid additive gross weight；The granule of balance of 3-5 micron；
Second solid additive is for the molybdenum disulfide nano ball of 15 nanometers of particle diameter and the Calcium Carbonate of 8 microns of particle diameter according to mass ratio 1:The mixture of 3 compositions.
Sequentially add in mass ratio 1 in order toward in the first reactant liquor：3：7 parts of first composite regulator of the tricaprylmethyl ammonium bromide of 1 proportioning, glycerol and politef composition；In mass ratio 1：3：9 parts of second composite regulator of the diphenylamines of 2 proportionings, 2,6- di-t-butyl and BTA composition；It is warming up to 90 DEG C of reaction 25min for the first time, be then incubated 1.2h for the first time；Then heat up dehydration for second to 130 DEG C, then second insulation 18min；Add in mass ratio 1：0.7：12 parts of 3rd composite regulator of sulfuration cottonseed oil T404 of 1.5 proportionings, two (2- sulfydryl -4- n-propylamine base -1,3,5- triazine) thioethers and two (2- sulfydryl -4- Aminocyclopentane base -1,3,5- triazine) thioether composition；Third time is warming up to 190 DEG C, cooling, obtains grease.
Example IV：
With embodiment one, except for the difference that in grease, also include polyacrylate -2- cross linked polymer and impregnating fluid in mass ratio 1:5 parts of 4th composite regulator of 3 compositions；After grease preparation also includes adding the 3rd composite regulator temperature reaction, it is cooled to 100 DEG C, add 6 parts of the 4th composite regulator, then circulation stirring, homogenizing is processed, degassing, obtain grease.
The preparation method of polyacrylate -2- cross linked polymer is：
(1) 35 parts of prepared polymer P (MMA-MAh)-PEG6000 by weight, 50 parts of regulation liquid form first and just mix liquid；Adjusting liquid is to include the carbonic allyl ester solution that concentration is the sodium perchlorate of the 0.5mol/L and concentration N- butyl benzimidazole for 0.3-0.8mol/L；MMA in polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, and MAh is maleic anhydride, and P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, and PEG6000 is the Polyethylene Glycol that molecular weight is 6000；
(2) add 4 part of ten dihydroxystearic acid in first just mixed liquid, be heated to 38 DEG C of reaction 5-9min under nitrogen protection；
(3) deionized water obtains polyacrylate -2- cross linked polymer after rinsing and being dried.
Anti-corrosion liquid making method：
A. 15 parts of AVC, 28 parts of sodium fluoride, 50 parts of ammonium acid fluoride, 15 parts of potassium permanganate, 47 parts of Neutral potassium chromate are added by weight in order successively；Stirring 8min, obtains second and just mixes liquid；
B. and then in order toward in second just mixed liquid add 19 parts of zinc phosphate, 12 parts of sodium nitrate, 9 parts of praseodymium chloride, 14 parts of ethylenediaminetetraacetic acid, 11 parts of malic acid, 10 parts of dodecyl phenenyl sulfate, 8 parts of nickel sulfate, 20 parts of triethanolamine successively, stir 3min.
Embodiment five：
With embodiment one, except for the difference that in grease, also include polyacrylate -2- cross linked polymer and impregnating fluid in mass ratio 1:3 parts of 4th composite regulator of 1 composition；After grease preparation is additionally included in addition the 3rd composite regulator temperature reaction, it is cooled to 90 DEG C, add 3 parts of the 4th composite regulator, then circulation stirring, homogenizing is processed, degassing, obtain grease.
The preparation method of polyacrylate -2- cross linked polymer is：
(1) 30 parts of prepared polymer P (MMA-MAh)-PEG6000 by weight, 40 parts of regulation liquid form first and just mix liquid；Adjusting liquid is to include the carbonic allyl ester solution that concentration is the sodium perchlorate of the 0.4mol/L and concentration N- butyl benzimidazole for 0.3mol/L；MMA in polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, and MAh is maleic anhydride, and P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, and PEG6000 is the Polyethylene Glycol that molecular weight is 6000；
(2) add 2 part of ten dihydroxystearic acid in first just mixed liquid, be heated to 30 DEG C of reaction 5min under nitrogen protection；
(3) deionized water obtains polyacrylate -2- cross linked polymer after rinsing and being dried.
Anti-corrosion liquid making method：
Add 10 parts of AVC, 20 parts of sodium fluoride, 30 parts of ammonium acid fluoride, 10 parts of potassium permanganate, 50 parts of Neutral potassium chromate by weight in order successively；Stirring 5min, obtains second and just mixes liquid；
Then add 15 parts of zinc phosphate, 8 parts of sodium nitrate, 5 parts of praseodymium chloride, 10 parts of ethylenediaminetetraacetic acid, 7 parts of malic acid, 8 parts of dodecyl phenenyl sulfate, 6 parts of nickel sulfate, 25 parts of triethanolamine successively toward in second just mixed liquid in order, stir 1min.
Embodiment six：
With embodiment one, except for the difference that in grease, also include polyacrylate -2- cross linked polymer and impregnating fluid in mass ratio 1:7 parts of 4th composite regulator of 4 compositions；After grease preparation is additionally included in addition the 3rd composite regulator temperature reaction, it is cooled to 120 DEG C, add 7 parts of the 4th composite regulator, then circulation stirring, homogenizing is processed, degassing, obtain grease.
The preparation method of polyacrylate -2- cross linked polymer is：
(1) 40 parts of prepared polymer P (MMA-MAh)-PEG6000 by weight, 60 parts of regulation liquid form first and just mix liquid；Adjusting liquid is to include the carbonic allyl ester solution that concentration is the sodium perchlorate of the 0.7mol/L and concentration N- butyl benzimidazole for 0.8mol/L；MMA in polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, and MAh is maleic anhydride, and P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, and PEG6000 is the Polyethylene Glycol that molecular weight is 6000；
(2) add 7 part of ten dihydroxystearic acid in first just mixed liquid, be heated to 45 DEG C of reaction 9min under nitrogen protection；
(3) deionized water obtains polyacrylate -2- cross linked polymer after rinsing and being dried.
Anti-corrosion liquid making method：
Add 18 parts of AVC, 40 parts of sodium fluoride, 60 parts of ammonium acid fluoride, 20 parts of potassium permanganate, 40 parts of Neutral potassium chromate by weight in order successively；Stirring 10min, obtains second and just mixes liquid；
Then add 25 parts of zinc phosphate, 18 parts of sodium nitrate, 12 parts of praseodymium chloride, 16 parts of ethylenediaminetetraacetic acid, 14 parts of malic acid, 12 parts of dodecyl phenenyl sulfate, 13 parts of nickel sulfate, 15 parts of triethanolamine successively toward in second just mixed liquid in order, stir 4min.
Embodiment seven：
Same example IV, except for the difference that also includes 1 part of potassium borohydride, bicyclohexane simultaneously 64 parts of -18- crown- and 8 parts of dibenzyl xenol polyoxyethylene polyoxypropylene ether in impregnating fluid.
Step B is additionally included in after insulation terminates for the first time and adds 4 parts of fire retardant, and fire retardant is according to mass ratio 1:2:The ammonium pyrophosphate of 4 compositions, boric acid and melamine cyanurate.
Embodiment eight：
With embodiment five, except for the difference that in impregnating fluid, also include 3 parts of potassium borohydride, bicyclohexane simultaneously 66 parts of -18- crown- and 5 parts of dibenzyl xenol polyoxyethylene polyoxypropylene ether.
Step B is additionally included in after insulation terminates for the first time and adds 8 parts of fire retardant, and fire retardant is according to mass ratio 1: 3:The ammonium pyrophosphate of 1 composition, boric acid and melamine cyanurate.
Embodiment nine：
With embodiment six, except for the difference that in impregnating fluid, also include 2 parts of potassium borohydride, bicyclohexane simultaneously 65 parts of -18- crown- and 7 parts of dibenzyl xenol polyoxyethylene polyoxypropylene ether.
Step B is additionally included in after insulation terminates for the first time and adds fire retardant 4-8 part, and fire retardant is according to mass ratio 1:2:The ammonium pyrophosphate of 1 composition, boric acid and melamine cyanurate.
Comparative example one：
With embodiment one, except for the difference that wherein do not contain the first solid additive, Colophonium, vegetable oil and (NH4)xMoS2.
Comparative example two：
With embodiment two, except for the difference that wherein do not contain the first solid additive.
Comparative example three：
With embodiment three, except for the difference that out of order but directly by 4 parts of ten dihydroxystearic acid, 4 parts of calcium mahogany sulfonate, 7 parts of Colophonium, 16 parts of vegetable oil, (NH4)xMoS2
6 parts, 7 parts of the second solid additive (without the first solid additive) is all simultaneously introduced in 98 parts of base oils together, ultrasonic disperse, it is subsequently adding 0.04 part of Lithium hydrate, 2.5 parts of potassium hydroxide and 23 parts of dicarboxylic acids, be heated to 90 DEG C of reaction 8min and obtain the first reactant liquor.
Wherein, PB, PD, ZMZ represent the extreme pressure and antiwear behavior of grease.Water drenches number of dropouts and water resistant sprayability represents sealing and the water repelling property of grease.
PB is maximum nonseizure load, refers under test conditions, make test steel ball that seizing maximum nonseizure load not occur, it represents film strength.
PD is sintering load, refers under test conditions, make test steel ball that the minimum load of sintering to occur, it represents the maximal work ability of lubricant.
ZMZ is integrated abrasion value, is that lubricant makes abrasion be reduced to an index of the anti-extreme pressure ability of minimum under institute's application of load.
As can be seen from the table, grease sealing performance of the present invention is good, corrosion resistance is strong, have excellent anti-attrition and anti-extreme pressure energy, also has excellent temperature tolerance, water-resistance and rustless property simultaneously.
Claims (10)
1. a kind of grease is it is characterised in that it is prepared from by the raw material that following parts by weight are major constituent：
Base oil 88-95 part；
Ten dihydroxystearic acid 4-7 parts；
Lithium hydrate 0.05-1.25 part；
Potassium hydroxide 0.8-2.4 part；
Calcium mahogany sulfonate 5-10 part；
Colophonium 2-6 part；
Vegetable oil 8-15 part；
(NH4)xMoS27-13 part；
First solid additive 3-7 part；
Second solid additive 1.5-6 part；
In mass ratio 1：3-4：First composite regulator 6-9 part of the tricaprylmethyl ammonium bromide of 1-2 proportioning, glycerol and politef composition；
In mass ratio 1：2-4：Second composite regulator 7-11 part of the diphenylamines of 1-3 proportioning, 2,6- di-t-butyl and BTA composition；
In mass ratio 1：0.5-0.8：The 3rd composite regulator 8-14 part of sulfuration cottonseed oil T404 of 1.3-1.7 proportioning, two (2- sulfydryl -4- n-propylamine base -1,3,5- triazine) thioethers and two (2- sulfydryl -4- Aminocyclopentane base -1,3,5- triazine) thioether composition；
Described base oil is to compare 1 according to weight：3-5：The mixture of the paraffinic base, cycloalkyl and polyalphaolefin of 2-4 composition；
The particle size range of the first solid additive is 0.8-5 micron；Wherein, the granule of 0.8-1 micron accounts for the 20-40% of described solid additive gross weight；The granule of 1-2 micron accounts for the 10-30% of described solid additive gross weight；The granule of balance of 3-5 micron；
Described second solid additive is for the molybdenum disulfide nano ball of particle diameter 10-20 nanometer and the regulation grain of particle diameter 6-9 micron according to mass ratio 1:The mixture of 2-5 composition；
Described first solid additive is following Formulas I polymer, wherein MwFor 6.10 × 106, MnFor 2.0 × 106, molecular weight distributing index is 3.1：
I.
2. a kind of grease according to claim 1 it is characterised in that：Described regulation grain is one or more of micro powder graphite, Calcium Carbonate, copper powder or tungsten disulfide.
3. a kind of grease according to claim 2 it is characterised in that：Polyacrylate -2- cross linked polymer and impregnating fluid in mass ratio 1 is also included in grease:The 4th composite regulator 3-7 part of 1-4 composition；
The preparation method of described polyacrylate -2- cross linked polymer is：
(1) prepared polymer P (MMA-MAh)-PEG6000 30-40 part, regulation liquid 40-60 part form first and just mix liquid by weight；The described liquid that adjusts is to include the carbonic allyl ester solution that concentration is the sodium perchlorate of the 0.4-0.7mol/L and concentration N- butyl benzimidazole for 0.3-0.8mol/L；MMA in described polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, MAh is maleic anhydride, P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, and PEG6000 is the Polyethylene Glycol that molecular weight is 6000；
(2) add 2-7 part ten dihydroxystearic acid in described first just mixed liquid, be heated to 30-45 DEG C of reaction 5-9min under nitrogen protection；
(3) deionized water obtains polyacrylate -2- cross linked polymer after rinsing and being dried.
4. a kind of grease according to claim 3 it is characterised in that：Described anti-corrosion liquid making method：Add AVC 10-18 part, sodium fluoride 20-40 part, ammonium acid fluoride 30-60 part, potassium permanganate 10-20 part, Neutral potassium chromate 40-50 part by weight in order successively；Stirring 5-10min, obtains second and just mixes liquid；
Then add zinc phosphate 15-25 part, sodium nitrate 8-18 part, praseodymium chloride 5-12 part, ethylenediaminetetraacetic acid 10-16 part, malic acid 7-14 part, dodecyl phenenyl sulfate 8-12 part, nickel sulfate 6-13 part, triethanolamine 15-25 part successively toward in described second just mixed liquid in order, stir 1-4min.
5. a kind of grease according to claim 4 it is characterised in that：Potassium borohydride 1-3 part, bicyclohexane simultaneously -18- crown- 6 4-6 part and dibenzyl xenol polyoxyethylene polyoxypropylene ether 5-8 part is also included in described impregnating fluid.
6. a kind of preparation of greases method according to any one of claim 1-5 is it is characterised in that it includes step：
In order successively by ten dihydroxystearic acid 4-7 parts, calcium mahogany sulfonate 5-10 part, Colophonium 2-6 part, vegetable oil 8-15 part, (NH4)xMoS2
7-13 part, first solid additive 3-7 part and second solid additive 1.5-6 part add in 88-95 part base oil, ultrasonic disperse, it is subsequently adding Lithium hydrate 0.05-1.25 part, potassium hydroxide 0.8-2.4 part and dicarboxylic acids 10-20 part, be heated to 60-80 DEG C of reaction 10-15min and obtain the first reactant liquor；
Sequentially add in mass ratio 1 in order toward in described first reactant liquor：3-4：First composite regulator 6-9 part of the tricaprylmethyl ammonium bromide of 1-2 proportioning, glycerol and politef composition；In mass ratio 1：2-4：Second composite regulator 7-11 part of the diphenylamines of 1-3 proportioning, 2,6- di-t-butyl and BTA composition；It is warming up to 85-95 DEG C of reaction 20-30min for the first time, be then incubated 1-2h for the first time；Then heat up dehydration for second to 120-150 DEG C, then second insulation 15-20min；Add in mass ratio 1：0.5-0.8：The 3rd composite regulator 8-14 part of sulfuration cottonseed oil T404 of 1.3-1.7 proportioning, two (2- sulfydryl -4- n-propylamine base -1,3,5- triazine) thioethers and two (2- sulfydryl -4- Aminocyclopentane base -1,3,5- triazine) thioether composition；Third time is warming up to 180-200 DEG C, cooling, obtains grease.
7. a kind of preparation of greases method according to any one of claim 1-5 it is characterised in that：Step C is also included after described step B：After adding described 3rd composite regulator temperature reaction, it is cooled to 90-120 DEG C, add described 4th composite regulator 3-7 part, then circulation stirring, homogenizing is processed, degassing, obtain grease.
8. a kind of preparation of greases method according to claim 7 it is characterised in that：Described step B is additionally included in after insulation terminates for the first time and adds fire retardant 4-8 part, and described fire retardant is according to mass ratio 1:2-3:The ammonium pyrophosphate of 1-4 composition, boric acid and melamine cyanurate.
9. a kind of polymer that can be used for grease is it is characterised in that as shown in following formula I：
I
Wherein MwFor 6.10 × 106, MnFor 2.0 × 106, molecular weight distributing index is 3.1.
10. application in terms of preparing lubricating oil for the Formulas I polymer described in claim 9.
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| CN111808660A (en) * | 2020-06-19 | 2020-10-23 | 中国石油化工股份有限公司 | Low-friction-coefficient composite calcium sulfonate lubricating grease composition and preparation method thereof |
| CN111849590A (en) * | 2020-06-19 | 2020-10-30 | 中国石油化工股份有限公司 | Low-noise mixed soap-based lubricating grease composition and preparation method thereof |
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