CN104479815A - Lubrication grease composition and preparation method thereof - Google Patents
Lubrication grease composition and preparation method thereof Download PDFInfo
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Abstract
The invention provides a lubrication grease composition and a preparation method thereof. The lubrication grease composition comprises the following components: (a) polturea-based grease; (b) an antiwear agent; (c) an antioxidant; (d) a thickening agent; (e) a micro-nano granular additive. By taking the weight percentage of the polturea-based grease (a) as 100%, the addition amount of the antiwear agent (b) is 0.5-5wt%, the addition amount of the antioxidant (c) is 0.1-3wt%, the addition amount of the thickening agent (d) is 1-8wt%; the addition amount of the micro-nano granular additive (e) is 2-10wt%. The lubrication grease composition is excellent in comprehensive performance, can be used as lubricants of machines which operate in poor conditions with high temperature, severe abrasion, heavy load, humidity and high corrosion, and can be used for lubricating high-speed or ultrahigh-speed operation.
Description
Technical field
The present invention relates to a kind of grease composition and preparation method thereof, be specifically related to a kind of Polyurea grease composition.Belong to technical field of lubricant.
Background technology
The essence of friction process is the consumption of energy and the loss process of material, and the machine failure of 80% is because the wearing and tearing of component cause according to statistics, and lubrication is one of wear-resistant most effective way of anti-attrition.Current most of lubricant adds multiple additives to improve performance, and each lifting of lubricant quality is nearly all the result of Development of Additives.
Because micro-nano granules can form the lower film of one deck frictional coefficient at friction surface, and filling up and repairing to a certain degree can be carried out to friction surface, thus reduce the abrasion loss of friction pair, reduce gathering of friction surface heat simultaneously, extend the work-ing life of friction pair, thus the use of micro-nano granules additive causes the concern of people day by day in recent years.
At present, polyurea based lubricating grease relies on its good resistance to elevated temperatures, anti-radiation, water resisting property, colloid stability, and the performance such as longer bearing life by great majority use producer favor, but its anti-attrition abrasion resistance and extreme pressure property weak effect limit again its application to a certain extent.
Patent application CN101173199A discloses a kind of self-repair carbamido consistent grease and preparation method thereof, join in polyurea based lubricating grease by a certain amount of selfreparing nanoparticle, effectively improve supporting capacity and the wear resisting property of polyurea based lubricating grease, but the nanoparticle selected and polyurea grease bad adaptability, the Stencil oil-dividing of prepared product is larger.
Patent application CN103740443A adds micron order fluorographite in polyurea grease, and Wear vesistance and load-carrying properties are improved, but in four ball experiments, PB value is at below 500N, PD value is at below 4000N, and more than wear scar diameter 0.6mm, still has certain gap with practical application request.
Summary of the invention
the problem that invention will solve
The ability that the anti-attrition anti-wear effect existed for existing common urea-base grease is poor, urea groups structure that is that generate does not have carrying high loading, easily cause the problems such as frictional wear, technical problem to be solved by this invention is to provide a kind of grease composition and preparation method thereof.Described grease composition has the following advantages: 1. lower frictional coefficient and outstanding extreme pressure anti-wear, can bear load duty for a long time; 2. good applied at elevated temperature performance, using under high temperature can not coking and loss; 3. excellent oxidation stability, colloid stability and Corrosion Protection, and preparation technology is simple, is easy to suitability for industrialized production and control.
for the scheme of dealing with problems
The invention provides a kind of grease composition, comprise following component:
(a) polyurea based lubricating grease;
(b) anti-wear agent;
(c) oxidation inhibitor;
(d) tackifier;
(e) micro-nano granules additive,
In the quality of polyurea based lubricating grease (a) for 100%, the add-on of anti-wear agent (b) is 0.5-5 quality %; The add-on of oxidation inhibitor (c) is 0.1-3 quality %; The add-on of tackifier (d) is 1-8 quality %; The add-on of micro-nano granules additive (e) is 2-10 quality %.
In grease composition of the present invention, described polyurea based lubricating grease (a) is prepared by the following method: with described polyurea based lubricating grease (a) total mass for benchmark, the vulcabond Hybrid Heating of the base oil of 32-45% and 2-4% is dissolved by (1); (2) the stearylamine Hybrid Heating of remaining base oil and 0.3-1% is dissolved, add 0.1-1% aniline and 0.8-2.5% hexahydroaniline afterwards, stirring and dissolving; (3) the solution mix and blend that the solution (1) obtained and (2) obtain, after heating and thermal insulation, cooling grinding homogeneous is degassed, obtains polyurea based lubricating grease (a).
In grease composition of the present invention, base oil in described polyurea based lubricating grease (a) be poly-alpha olefins base oil, Esters oil one or more, be preferably one or more in PAO40, PAO100, aromatic ester, polyol ester, be more preferably one or more in trimellitate, trihydroxymethylpropanyl ester, neopentyl polyol ester.
In grease composition of the present invention, in the quality of polyurea based lubricating grease (a) for 100%, the add-on of anti-wear agent (b) is 1-3 quality %; The add-on of oxidation inhibitor (c) is 0.5-2.5 quality %; The add-on of tackifier (d) is 3-5 quality %; The add-on of micro-nano granules additive (e) is 2-8 quality %.
In grease composition of the present invention, described anti-wear agent (b) is borate anti-wear agent, is preferably the neutral dispersion liquid of three potassium borates.
In grease composition of the present invention, described oxidation inhibitor (c) is amine or phenolic antioxidant, preferably right, p-dioctyl diphenylamine, octyl group butyl pentanoic, naphthylamines, 2, one or more in 6-ditertbutylparacresol or two (3,5-di-tert-butyl-4-hydroxyl benzyl) thioether.
In grease composition of the present invention, described tackifier (d) are polyisobutene, one or more in ethylene-propylene copolymer or polymethacrylate.
In grease composition of the present invention, the composition that described micro-nano granules additive (e) is tetrafluoroethylene and nano-calcium carbonate, wherein the mass ratio of tetrafluoroethylene and nano-calcium carbonate is 1:4 ~ 4:1, is preferably 1:2 ~ 2:1.
In grease composition of the present invention, the median size of described tetrafluoroethylene is less than 5 μm; The median size of nano-calcium carbonate is less than 0.02 μm.
The present invention also provides a kind of preparation method of grease composition of the present invention, in described polyurea based lubricating grease (a), add described anti-wear agent (b), oxidation inhibitor (c), tackifier (d) and micro-nano granules additive (e), mix, obtain described grease composition.
the effect of invention
Can not coking and loss under grease composition high temperature of the present invention, and oxidation stability is good.Grease composition of the present invention also has excellent anti-water drenching energy, colloid stability and longer bearing work-ing life, excellent combination property, the bearing lubrication of the power lubrication agent operated under can be used for the bad working environments such as high temperature, serious wear, heavy duty, humidity, deep-etching and high speed or ultra-high speed running, the such as lubrication of oil drilling, high-speed electric expreess locomotive bearing, Steel Plant's continuous caster bearing, automobile bearing, constant velocity cardan joint and precision instrumentation; The preparation technology of grease composition of the present invention is simple, is extremely easy to industrial production and control.
Embodiment
As mentioned above, based on adopting polyurea based lubricating grease, fat has better high-temperature stability than traditional lithium saponify, is more suitable for high temperature lubricating.
Preferably, described polyurea based lubricating grease (a) is prepared in the following manner: with described polyurea based lubricating grease total mass for benchmark, the base oil of 32-45% mixes with the vulcabond of 2-4% by (1), is heated to 60-80 DEG C of dissolving; (2) remaining base oil is mixed with the stearylamine of 0.3-1%, be heated to 60-80 DEG C of dissolving, add 0.1-1% aniline and 0.8-2.5% hexahydroaniline afterwards, stir and make it to dissolve; (3) the solution mix and blend that the solution (1) obtained and (2) obtain, and be warming up to 130-160 DEG C, insulation; Homogeneous is degassed obtains in cooling grinding.
The present invention is by selecting the aliphatic amide of proper ratio, cycloalkanes amine and aromatic amine and di-isocyanate reaction, prepare the polyurea based lubricating grease of excellent combination property, the wherein aromatic amine of suitable proportion, makes the mechanical stability of polyurea based lubricating grease, oxidation stability is strengthened; Aliphatic amide and the cycloalkanes amine of suitable proportion then ensure that polyurea based grease thickening ability and resistance to elevated temperatures.
Wherein, base oil be poly-alpha olefins base oil, Esters oil one or more; Be preferably PAO40, PAO100, aromatic ester, one or more in polyol ester, one or more more preferably in trimellitate, trihydroxymethylpropanyl ester, neopentyl polyol ester.
In grease composition of the present invention, in the quality of polyurea based lubricating grease (a) for 100%, the add-on of anti-wear agent (b) is 0.5-5 quality %, is preferably 1-3 quality %.
In grease composition of the present invention, preferred anti-wear agent (b) is borate anti-wear agent, is preferably the neutral dispersion liquid of three potassium borates.It has very high thermo-oxidative stability, and under 150 DEG C of high temperature, long-time use is still very stable, substantially can't see colloid and greasy filth.Further, borate is by electronic and ionic group's displacement and has adsorbed extreme pressure, wear-resistant and anti-attrition effect, and neither damage surface of friction metal, also do not consume the additive in oil product, even if rubbed, also can be adsorbed up by electrophoresis, work-ing life is very long again.
In grease composition of the present invention, in the quality of polyurea based lubricating grease (a) for 100%, the add-on of oxidation inhibitor (c) is 0.1-3 quality %, is preferably 0.5-2.5 quality %.
Oxidation inhibitor (c) of the present invention preferably adopts amine or phenolic antioxidant, preferably right, one or more in p-dioctyl diphenylamine, octyl group butyl pentanoic, naphthylamines, 2,6 ditertiary butyl p cresol or two (3,5-di-tert-butyl-4-hydroxyl benzyl) thioether.Above-mentioned oxidation inhibitor and other additives of the present invention have good compatibleness, can improve the oxidation stability of the present composition, and extend its work-ing life.
In grease composition of the present invention, in the quality of polyurea based lubricating grease (a) for 100%, tackifier (d) add-on is 1-8 quality %, is preferably 3-5 quality %.
Tackifier (d) of the present invention be preferably in polyisobutene, ethylene-propylene copolymer or polymethacrylate one or more.Above-mentioned tackifier can improve adhesivity and the anti-water drenching energy of grease composition of the present invention.
In grease composition of the present invention, in the quality of polyurea based lubricating grease (a) for 100%, the add-on of micro-nano granules additive (e) is 2-10 quality %, is preferably 2-8 quality %.
Micro-nano granules additive (e) of the present invention is preferably the composition of tetrafluoroethylene and nano-calcium carbonate, and wherein the mass ratio of tetrafluoroethylene and nano-calcium carbonate is 1:4-4:1, is preferably 1:2-2:1.Tetrafluoroethylene frictional coefficient is minimum in solid material, the composition of tetrafluoroethylene and nano-calcium carbonate is added in polyurea based lubricating grease, the lower film of one deck frictional coefficient can be formed at friction surface, and filling up and repairing to a certain degree is carried out to friction surface polishing scratch, in addition tetrafluoroethylene and nano-calcium carbonate also have certain extreme-pressure anti-wear synergy, thus tetrafluoroethylene and nano-calcium carbonate is adopted to be additive, contribute to improving the wear-resistant of polyurea based lubricating grease, anti-attrition and load-carrying properties, and contribute to reducing the frictional coefficient that works in high temperature environments of bearing, reduce energy consumption and reduce lubricating grease consumption, extend the work-ing life of lubricating grease.
Described tetrafluoroethylene median size is less than 5 μm, is preferably less than 3 μm, and tetrafluoroethylene has good chemical stability and thermostability, can improve oxidation stability and the chemical resistance of polyurea based lubricating grease.
Described nano-calcium carbonate median size is less than 0.02 μm, is preferably less than 0.01 μm, and nano-calcium carbonate is due to the super-refinement of particle, and its crystalline structure and Electronic Structure there occurs change, and lubricating grease therefore can be made to possess good extreme pressure and antiwear and reducing friction performance.
Borate family anti-wear agent, tetrafluoroethylene, nano-calcium carbonate and polyurea based lubricating grease have good compatibleness and adaptability, compensate for the defect that polyurea based lubricating grease anti-attrition anti-wear effect is poor, can not carry high loading, expand its range of application.
Preferably, the present invention also provides a kind of preparation method according to grease composition of the present invention, in described polyurea based lubricating grease (a), add described anti-wear agent (b), oxidation inhibitor (c), tackifier (d) and micro-nano granules additive (e), mix, obtain described grease composition.
More preferably, described mixing process is stirred to 100-110 DEG C for each component being heated up, and constant temperature stirs 40min-1h, cooling grinding homogeneous.
Embodiment
Below provide embodiments of the invention, its object only for explaining and illustrating, does not limit the present invention.In an embodiment, " part " refers to " mass parts ".
Embodiment 1
In grease compounding still, the trimellitate TMT-4 (Liaocheng Rui Jie Chemical Co., Ltd., lower same) of 420 parts and ditan-4, the 4-vulcabond (Ai Ke reagent) of 35.04 parts are mixed, be heated to 70 DEG C of dissolvings; In another reactor, add 512 parts of polyalphaolefin SpectraSyn 40 mix with the stearylamine (Shanghai is prosperous Chemical Co., Ltd. extremely) of 7.92 parts simultaneously, be heated to 70 DEG C of dissolvings, add 6.67 parts of aniline (Shandong Hai Hua limited-liability company) and 17.76 parts of hexahydroaniline (the Nantong same Chemical Co., Ltd. of benefit) afterwards, stir and make it to dissolve; Mixing solutions in reactor is dropped in modulation kettle fast, opens blower fan, after constant temperature stirs 10 minutes, be warming up to 150 DEG C, be incubated 20 minutes; Homogeneous is degassed obtains polyurea based lubricating grease in cooling grinding.
The above-mentioned polyurea based lubricating grease of 100 parts is joined in the normal-pressure reaction kettle cleaned in advance, heat up and stir, add 1.5 part of three potassium borate neutral oil dispersion liquid Octopol PTB (Tiarco Chemical Company, Inc. lower same), 0.5 part of butyl/octyl diphenylamine Irganox L57 (Basf Chemical Company, lower same), 5 parts of polyisobutene tackifier PB-2400 (Daelim Industrial Co.Ltd PetrochemicalDivision, lower same), 3 parts of polytetrafluoroethylene PTFE L101-1 (Su Wei group Solvay), lower same) and 2 parts of nano-calcium carbonate (Zhejiang Province Changshan Jinxiong Co., Ltd, lower same), mix and blend, be warming up to 110 DEG C again, constant temperature stirs 40min, cool out still, homogeneous grinding packaging, obtain grease composition I.
Embodiment 2
The above-mentioned polyurea based lubricating grease of 100 parts is joined in the normal-pressure reaction kettle cleaned in advance, heat up and stir, add 1 part of three potassium borate neutral oil dispersion liquid Octopol PTB, 1 part of butyl/octyl diphenylamine IrganoxL57,4 parts of tackifier ethylene-propylene copolymer T614 (Run Da chemical industry limited liability company of Jinzhou City), 2 parts of tetrafluoroethylene and 3 parts of nano-calcium carbonates, mix and blend, be warming up to 110 DEG C again, constant temperature stirs 40min, cool out still, homogeneous grinding packaging, obtains grease composition II.
Comparative example 1
Except the tetrafluoroethylene in embodiment 1 is replaced with traditional anti-wear agent tritolyl phosphate, nano-calcium carbonate replaces with beyond zinc diamyldithiocarbamate, by the method identical with embodiment 1, prepares grease composition III.
Comparative example 2
Except replacing with except tetrafluoroethylene by 2 parts of nano-calcium carbonates, by the method identical with embodiment 1, prepare grease composition IV.
Comparative example 3
Except tackifier add-on is replaced by 1 part, tetrafluoroethylene add-on is replaced by 10 especially, by the method identical with embodiment 1, prepares grease composition V.
Table 1 lists the performance test data of foregoing grease composition I, II, III, IV and V.
Table 1 grease composition I, II, III, IV and V performance test data
In Table 1, as can be seen from embodiment 1, embodiment 2 and comparative example 1 data, relative to traditional extreme pressure anti-wear additives, micro-nano granules tetrafluoroethylene and nano-calcium carbonate can make wear-resistant, the wear resistance of polyurea based lubricating grease and load-carrying properties more excellent, show four higher ball PB values and PD value, less wear scar diameter and low-friction coefficient.In addition compare can draw by the data of comparative example 2 and embodiment 1, embodiment 2, the nano-calcium carbonate adding proper ratio can make the wear-resisting load-carrying properties of grease composition I, II more excellent, illustrates that nano-calcium carbonate and tetrafluoroethylene have certain extreme-pressure anti-wear synergetic property under this additional proportion.
The present composition has lower water pouring number of dropouts, Stencil oil-dividing amount and oxidative pressure and falls, and shows that its water tolerance, colloid stability and oxidation stability are excellent.Add a large amount of sulphur phosphorus extreme pressure anti-wear additives in the grease composition of comparative example 1, its active sulphur phosphoric can accelerate the oxidation of polyurea based lubricating grease, and thus its oxidative pressure drop data is bigger than normal.
Relative to embodiment 1, comparative example 3 water resistant is drenched data and is increased, and anti-water drenching can weaken, and this shows that tackifier are except itself can increase lubricating grease adhesivity, can also improve the anti-water drenching of lubricating grease to a certain extent.In addition, although add more superfine powder of polytetrafluoroethylene in comparative example 3, but but there is reduction trend in its four ball experiment PB and PD value, four ball milling spot diameters and frictional coefficient become large, i.e. extreme-pressure anti-wear, Wear vesistance dies down, this is because add a large amount of solid particulate additives on the one hand, easily cause particle in lubricating grease, disperse inequality, be agglomerated into block, add the roughness of lubricated surface, on the other hand during polytetrafluoroethylene granule large usage quantity, isolate the continuity of lubricating grease, below the lubricant effect of polyurea based lubricating grease has all been slackened, frictional coefficient is caused to increase, wear scar diameter increases.In addition tetrafluoroethylene and nano-calcium carbonate ratios of calcium content inharmonious, lose extreme-pressure anti-wear synergy, be also cause lubricating grease PB and PD value variation reason.
Claims (10)
1. a grease composition, is characterized in that comprising following component:
(a) polyurea based lubricating grease;
(b) anti-wear agent;
(c) oxidation inhibitor;
(d) tackifier;
(e) micro-nano granules additive,
In the quality of polyurea based lubricating grease (a) for 100%, the add-on of anti-wear agent (b) is 0.5-5 quality %; The add-on of oxidation inhibitor (c) is 0.1-3 quality %; The add-on of tackifier (d) is 1-8 quality %; The add-on of micro-nano granules additive (e) is 2-10 quality %.
2. grease composition according to claim 1, it is characterized in that, described polyurea based lubricating grease (a) is prepared by the following method: with described polyurea based lubricating grease (a) total mass for benchmark, the vulcabond Hybrid Heating of the base oil of 32-45% and 2-4% is dissolved by (1); (2) the stearylamine Hybrid Heating of remaining base oil and 0.3-1% is dissolved, add 0.1-1% aniline and 0.8-2.5% hexahydroaniline afterwards, stirring and dissolving; (3) the solution mix and blend that the solution (1) obtained and (2) obtain, after heating and thermal insulation, cooling grinding homogeneous is degassed, obtains polyurea based lubricating grease (a).
3. grease composition according to claim 2, it is characterized in that, base oil in described polyurea based lubricating grease (a) be poly-alpha olefins base oil, Esters oil one or more, be preferably one or more in PAO40, PAO100, aromatic ester, polyol ester, be more preferably one or more in trimellitate, trihydroxymethylpropanyl ester, neopentyl polyol ester.
4. the grease composition according to any one of claims 1 to 3, is characterized in that, in the quality of polyurea based lubricating grease (a) for 100%, the add-on of anti-wear agent (b) is 1-3 quality %; The add-on of oxidation inhibitor (c) is 0.5-2.5 quality %; The add-on of tackifier (d) is 3-5 quality %; The add-on of micro-nano granules additive (e) is 2-8 quality %.
5. the grease composition according to any one of Claims 1 to 4, is characterized in that, described anti-wear agent (b) is borate anti-wear agent, is preferably the neutral dispersion liquid of three potassium borates.
6. the grease composition according to any one of Claims 1 to 5, it is characterized in that, described oxidation inhibitor (c) is amine or phenolic antioxidant, preferably right, p-dioctyl diphenylamine, octyl group butyl pentanoic, naphthylamines, 2, one or more in 6-ditertbutylparacresol or two (3,5-di-tert-butyl-4-hydroxyl benzyl) thioether.
7. the grease composition according to any one of claim 1 ~ 6, is characterized in that, described tackifier (d) are polyisobutene, one or more in ethylene-propylene copolymer or polymethacrylate.
8. the grease composition according to any one of claim 1 ~ 7, it is characterized in that, the composition that described micro-nano granules additive (e) is tetrafluoroethylene and nano-calcium carbonate, wherein the mass ratio of tetrafluoroethylene and nano-calcium carbonate is 1:4 ~ 4:1, is preferably 1:2 ~ 2:1.
9. grease composition according to claim 8, is characterized in that, the median size of described tetrafluoroethylene is less than 5 μm; The median size of nano-calcium carbonate is less than 0.02 μm.
10. the preparation method of the grease composition described in an any one of claim 1 ~ 9, it is characterized in that, in described polyurea based lubricating grease (a), add described anti-wear agent (b), oxidation inhibitor (c), tackifier (d) and micro-nano granules additive (e), mix, obtain described grease composition.
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