CN104479815B - 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 lubricant composition and preparation method thereof is and in particular to a kind of polyureas base grease combines
Thing.Belong to technical field of lubricant.
Background technology
The essence of friction process is the consumption of energy and the loss process of material, according to statistics 80% machine failure be due to
The abrasion of parts causes, and lubrication is one of wear-resistant most effective approach of anti-attrition.Most of lubricants are many to add at present
Plant additive to improve performance, each lifting of lubricant quality is nearly all the result of Development of Additives.
Because micro-nano granules can form one layer of relatively low thin film of coefficient of friction it is possible to friction surface in friction surface
Carry out a certain degree of accumulation filled up and repair, thus reducing the wear extent of friction pair, reducing friction surface heat simultaneously, prolong
The service life of long friction pair, thus the use of micro-nano granules additive increasingly causes the concern of people in recent years.
At present, polyureas base grease relies on its good resistance to elevated temperatures, anti-radiation, water-resistance, colloid stability, with
And the performance such as longer bearing life favored using producer by great majority, but its anti-attrition abrasion resistance and extreme pressure property effect are poor
Limit its application to a certain extent again.
Patent application CN101173199A discloses a kind of self-repair carbamido consistent grease and preparation method thereof, will be a certain amount of
Selfreparing nanoparticle is added in polyureas base grease, effectively increases bearing capacity and the wearability of polyureas base grease
Energy, 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, Wear vesistance and carrying in polyurea grease
Performance is improved, but four balls experiment in, PB value in below 500N, PD value in below 4000N, more than wear scar diameter 0.6mm,
Still there is certain gap with practical application request.
Content of the invention
Problems to be solved by the invention
It is high that the anti-attrition anti-wear effect existing for existing common urea-base grease is poor, urea groups structure that is generating does not have carrying
The ability of load, the problems such as easily cause fretting wear, the technical problem to be solved is to provide a kind of grease group
Compound and preparation method thereof.Described lubricant composition has advantages below：1. relatively low coefficient of friction and prominent extreme pressure resist
Mill property, can bear load duty for a long time；2. preferable applied at elevated temperature performance, using will not coking and loss under high temperature；3. excellent
Different oxidation stability, colloid stability and Corrosion Protection, and preparation process is simple is it is easy to industrialized production and control.
For solution to problem
The present invention provides a kind of lubricant composition, comprises following components：
(a) polyureas base grease；
(b) antiwear additive；
(c) antioxidant；
(d) viscosifier；
(e) micro-nano granules additive,
With the quality of polyureas base grease (a) for 100% meter, the addition of antiwear additive (b) is 0.5-5 mass %；Antioxygen
The addition of agent (c) is 0.1-3 mass %；The addition of viscosifier (d) is 1-8 mass %；Micro-nano granules additive (e)
Addition is 2-10 mass %.
In lubricant composition of the present invention, described polyureas base grease (a) is prepared by the following method：With institute
On the basis of stating polyureas base grease (a) gross mass, (1) is by the diisocyanate Hybrid Heating of the base oil of 32-45% and 2-4%
Dissolving；(2) by the 18-amine. Hybrid Heating dissolving of remaining base oil and 0.3-1%, 0.1-1% aniline and 0.8- are added afterwards
2.5% cyclohexylamine, stirring and dissolving；(3) the solution mix and blend being obtained the solution that (1) obtains with (2), is cooled down after heating and thermal insulation
Grind homogenizing degassing, obtain polyureas base grease (a).
In lubricant composition of the present invention, the base oil in described polyureas base grease (a) is poly alpha olefin
Base oil, one or more of Esters oil, one or more of preferably PAO40, PAO100, aromatic ester, polyol ester, more
It is preferably one or more of trimellitate, trihydroxymethylpropanyl ester, neopentyl polyol ester.
In lubricant composition of the present invention, with the quality of polyureas base grease (a) for 100% meter, antiwear additive (b)
Addition be 1-3 mass %；The addition of antioxidant (c) is 0.5-2.5 mass %；The addition of viscosifier (d) is 3-5 matter
Amount %；The addition of micro-nano granules additive (e) is 2-8 mass %.
In lubricant composition of the present invention, described antiwear additive (b) is borate antiwear additive, preferably three potassium borates
Neutral dispersion liquid.
In lubricant composition of the present invention, described antioxidant (c) is amine or phenolic antioxidant, preferably right,
P- dioctyl diphenylamine, octyl group butyl diphenylamines, naphthylamines, DBPC 2,6 ditertiary butyl p cresol or double (3,5- di-t-butyl -4- hydroxyl
One or more of base benzyl) thioether.
In lubricant composition of the present invention, described viscosifier (d) are polyisobutylene, ethylene-propylene copolymer or poly- methyl
One or more of acrylate.
In lubricant composition of the present invention, described micro-nano granules additive (e) are politef and nanometer
The compositionss of Calcium Carbonate, wherein politef are 1 with the mass ratio of nano-calcium carbonate:4～4:1, preferably 1:2～2:1.
In lubricant composition of the present invention, the mean diameter of described politef is less than 5 μm；Nano-calcium carbonate
Mean diameter be less than 0.02 μm.
The present invention also provides a kind of preparation method of lubricant composition of the present invention, in described polyureas base grease
In (a), add described antiwear additive (b), antioxidant (c), viscosifier (d) and micro-nano granules additive (e), mixed,
Obtain described lubricant composition.
The effect of invention
Under the lubricant composition high temperature of the present invention will not coking and loss, and oxidation stability is good.The lubrication of the present invention
Oil/fat composition also has excellent anti-water drenching energy, colloid stability and longer bearing service life, and excellent combination property can
For the mechanical lubrication agent of operating under the bad working environments such as high temperature, serious wear, heavy duty, humidity, deep-etching and high speed or superelevation
The bearing lubrication of speed operating, such as oil drilling, high-speed electric expreess locomotive bearing, steel plant's continuous casting machine bearing, automobile bearing, constant velocity universal
Section and the lubrication of precision instrumentation；The preparation process is simple of the lubricant composition of the present invention, is easy to commercial production
And control.
Specific embodiment
As described above, more preferable high-temperature stability is had than traditional lithium saponify using fat based on polyureas base grease,
It is more suitable for for high temperature lubricating.
Preferably, described polyureas base grease (a) is prepared in the following manner：With described polyureas base grease gross mass
On the basis of, the base oil of 32-45% is mixed by (1) with the diisocyanate of 2-4%, is heated to 60-80 DEG C of dissolving；(2) will remain
Remaining base oil is mixed with the 18-amine. of 0.3-1%, is heated to 60-80 DEG C of dissolving, adds 0.1-1% aniline and 0.8- afterwards
2.5% cyclohexylamine, stirring is allowed to dissolve；(3) the solution mix and blend that the solution that (1) obtains is obtained with (2), and be warming up to
130-160 DEG C, insulation；Cooling is ground homogenizing degassing and is obtained.
The present invention passes through, from the fatty amine of proper ratio, cycloalkanes amine and aromatic amine and di-isocyanate reaction, to prepare
The polyureas base grease of excellent combination property, the wherein aromatic amine of proper proportion, make polyureas base grease mechanical stability,
Oxidation stability is enhanced；And the fatty amine of proper proportion and cycloalkanes amine then ensure that polyureas base grease thickening ability and
Resistance to elevated temperatures.
Wherein, base oil be poly alpha olefin base oil, one or more of Esters oil；It is preferably PAO40, PAO100, virtue
One or more of fragrant ester, polyol ester, more preferably trimellitate, trihydroxymethylpropanyl ester, in neopentyl polyol ester
One or more.
In the lubricant composition of the present invention, with the quality of polyureas base grease (a) for 100% meter, antiwear additive (b) plus
Entering amount is 0.5-5 mass %, preferably 1-3 mass %.
In the lubricant composition of the present invention, preferably antiwear additive (b) is borate antiwear additive, and preferably three potassium borates are neutral
Dispersion liquid.It has very high thermo oxidative stability, for a long time using still very stable under 150 DEG C of high temperature, substantially sees not
To colloid and greasy filth.And, borate is by electronic and ionic group's displacement and to have adsorbed extreme pressure, wear-resistant and anti-attrition effect, both
Not damaging rubbing surface metal, do not consume the additive in oil product yet, even if being got off by friction, also can be adsorbed again by electrophoresis
Go, service life is very long.
In the lubricant composition of the present invention, with the quality of polyureas base grease (a) for 100% meter, antioxidant (c) plus
Entering amount is 0.1-3 mass %, preferably 0.5-2.5 mass %.
The antioxidant (c) of the present invention preferably employs amine or phenolic antioxidant, preferably right, p- dioctyl diphenylamine, pungent
One of base butyl diphenylamines, naphthylamines, DBPC 2,6 ditertiary butyl p cresol or double (3,5- di-tert-butyl-4-hydroxyl benzyl) thioether
Or it is multiple.Above-mentioned antioxidant and other additives of the present invention have preferable compatibility, can improve the oxygen of the present composition
Change stability, and extend its service life.
In the lubricant composition of the present invention, with the quality of polyureas base grease (a) for 100% meter, viscosifier (d) add
Measure as 1-8 mass %, preferably 3-5 mass %.
The viscosifier (d) of the present invention be preferably one of polyisobutylene, ethylene-propylene copolymer or polymethacrylates or
Multiple.Above-mentioned viscosifier can improve adhesiveness and the anti-water drenching energy of lubricant composition of the present invention.
In the lubricant composition of the present invention, with the quality of polyureas base grease (a) for 100% meter, micro-nano granules add
Plus the addition of agent (e) is 2-10 mass %, preferably 2-8 mass %.
Micro-nano granules additive (e) of the present invention are preferably the compositionss of politef and nano-calcium carbonate, wherein
Politef is 1 with the mass ratio of nano-calcium carbonate:4-4:1, preferably 1:2-2:1.Politef coefficient of friction is solid
Minimum in body material, polyureas base grease adds the compositionss of politef and nano-calcium carbonate, can be in friction table
Face forms the relatively low thin film of one layer of coefficient of friction, and friction surface polishing scratch is carried out a certain degree of fill up and repair, gather in addition
Tetrafluoroethene and nano-calcium carbonate also have certain extreme-pressure anti-wear synergism, thus adopt politef and nano-calcium carbonate
Calcium is additive, contributes to improving the wear-resistant, anti-attrition of polyureas base grease and load-carrying properties, and contributes to reducing bearing in high temperature
The coefficient of friction working under environment, reducing energy consumption and reduce grease consumption, extend the service life of grease.
Described politef mean diameter is less than 5 μm, preferably smaller than 3 μm, and politef has good chemistry peace
Qualitative and heat stability, can improve oxidation stability and the chemical resistance of polyureas base grease.
Described nano-calcium carbonate mean diameter is less than 0.02 μm, and preferably smaller than 0.01 μm, nano-calcium carbonate is due to particle
Super-refinement, its crystal structure and Electronic Structure there occurs change, and grease therefore can be made to possess preferable extreme pressure and resist
Mill Wear vesistance.
Borate family antiwear additive, politef, nano-calcium carbonate and polyureas base grease have preferable compatibility and
Adaptability, compensate for that polyureas base grease anti-attrition anti-wear effect is poor, defect that is can not carrying high load capacity, expands it and applies model
Enclose.
Preferably, the present invention also provides a kind of preparation method according to lubricant composition of the present invention, described
In polyureas base grease (a), add described antiwear additive (b), antioxidant (c), viscosifier (d) and micro-nano granules additive
E (), is mixed, obtain described lubricant composition.
It is highly preferred that described mixed process is to stir each group decilitre temperature to 100-110 DEG C, constant temperature stirs 40min-1h,
Homogenizing is ground in cooling.
Embodiment
Embodiments of the invention presented below, it is only used for explaining and descriptive purpose, is not intended to limit the present invention.Implementing
In example, " part " refers to " mass parts ".
Embodiment 1
In grease compounding kettle by 420 parts of trimellitate TMT-4 (Liaocheng Rui Jie Chemical Co., Ltd., similarly hereinafter) with
35.04 parts of diphenyl methane -4,4- diisocyanate (Ai Ke reagent) mixes, and is heated to 70 DEG C of dissolvings；Simultaneously at another
512 parts of polyalphaolefin SpectraSyn 40 and 7.92 parts of 18-amine. (Shanghai to prosperous Chemical Co., Ltd.) is added to mix in reactor
Close, be heated to 70 DEG C of dissolvings, add 6.67 parts of aniline (Shandong Hai Hua limited company) and 17.76 parts of cyclohexylamine (south afterwards
Lead to beneficial same Chemical Co., Ltd.), stirring is allowed to dissolve；Mixed solution in reactor is quickly put in modulation kettle, opens wind
Machine, after constant temperature stirs 10 minutes, is warming up to 150 DEG C, is incubated 20 minutes；Cooling is ground homogenizing degassing and is obtained polyureas base grease.
100 parts of above-mentioned polyureas base grease is added in the normal-pressure reaction kettle of pre-wash, heat up stirring, adds
1.5 part of three potassium borate neutral oil dispersion liquid Octopol PTB (Tiarco Chemical Company, Inc. is similarly hereinafter), 0.5 part
Butyl/octyl diphenylamine Irganox L57 (Basf Chemical Company, similarly hereinafter), 5 parts of polyisobutylene viscosifier PB-
2400 (Daelim Industrial Co.Ltd Petrochemical Division, similarly hereinafter), 3 parts of polytetrafluoroethylene PTFEs
L101-1 (Su Wei group Solvay), similarly hereinafter) and 2 parts of nano-calcium carbonates (Zhejiang Province Changshan Jinxiong Co., Ltd, similarly hereinafter), mixing is stirred
Mix, then be warming up to 110 DEG C, constant temperature stirs 40min, cool down out kettle, homogenizing grinds packaging, obtains lubricant composition I.
Embodiment 2
100 parts of above-mentioned polyureas base grease is added in the normal-pressure reaction kettle of pre-wash, heat up stirring, adds 1
Part three potassium borate neutral oil dispersion liquid Octopol PTB, 1 part of butyl/octyl diphenylamine Irganox L57,4 parts of viscosifier second third
Copolymer T614 (Run Da chemical industry Co., Ltd of Jinzhou City), 2 parts of politef and 3 parts of nano-calcium carbonates, mix and blend,
It is warming up to 110 DEG C again, constant temperature stirs 40min, cools down out kettle, homogenizing grinds packaging, obtains lubricant composition II.
Comparative example 1
Except the politef in embodiment 1 is replaced with traditional antiwear additive tricresyl phosphate, nano-calcium carbonate is replaced
Beyond zinc diamyldithiocarbamate, according to the same manner as in Example 1, prepare lubricant composition III.
Comparative example 2
Except replacing with addition to politef by 2 parts of nano-calcium carbonates, according to the same manner as in Example 1, prepare profit
Grease composition IV.
Comparative example 3
Except viscosifier addition is replaced by 1 part, politef addition is replaced by 10 especially, by with embodiment 1 phase
Same method, prepares lubricant composition V.
Table 1 lists the performance test data of foregoing grease composition I, II, III, IV and V.
Table 1 lubricant composition I, II, III, IV and V performance test data
In Table 1, can be seen that with respect to traditional extreme pressure anti-wear additives by embodiment 1, embodiment 2 and comparative example 1 data,
Micro-nano granules politef and nano-calcium carbonate can make the wear-resistant, wearability of polyureas base grease and load-carrying properties more excellent
Different, show four higher ball PB values and PD value, less wear scar diameter and low-friction coefficient.In addition comparative example 2 and reality are passed through
Apply example 1, the data of embodiment 2 compares and can draw, add the nano-calcium carbonate of proper ratio that lubricant composition I, II can be made resistance to
Mill load-carrying properties are more excellent, illustrate that nano-calcium carbonate and politef have certain extreme-pressure anti-wear under this additional proportion
Concertedness.
The present composition has relatively low water and drenches number of dropouts, Stencil oil-dividing amount and oxidative pressure fall, show its resistance to water,
Colloid stability and oxidation stability are excellent.A large amount of sulfur phosphorus extreme pressure anti-wear additives are added in the lubricant composition of comparative example 1, its
Active sulfur P elements can accelerate the oxidation of polyureas base grease, thus its oxidative pressure drop data is bigger than normal.
With respect to embodiment 1, comparative example 3 water resistant is drenched data and is increased, and anti-water drenching can weaken, and this shows that viscosifier remove itself
Can increase outside grease adhesiveness moreover it is possible to improve the anti-water drenching of grease to a certain extent.Although in addition, in comparative example 3
Add more superfine powder of polytetrafluoroethylene, but reduction trend but in its four ball experiment PB and PD value, four ball milling speckles are straight
Footpath and coefficient of friction become big, and that is, extreme-pressure anti-wear, Wear vesistance die down, this is because on the one hand adding substantial amounts of solid particle to add
Agent, is easily caused granule and disperses inequality in grease, coalesce in bulk, increased the roughness of lubricated surface, on the other hand poly-
The seriality of grease, the above lubrication effect all having slackened polyureas base grease when tetrafluoroethene amount of particles is larger, are isolated
Really, coefficient of friction is led to increase, wear scar diameter increases.In addition politef and nano-calcium carbonate ratios of calcium content are inharmonious, funeral
Lose extreme-pressure anti-wear synergism, be also the reason lead to grease PB and PD value to be deteriorated.
Claims (14)
1. a kind of lubricant composition is it is characterised in that comprise following components：
(a) polyureas base grease；
(b) antiwear additive；
(c) antioxidant；
(d) viscosifier；
(e) micro-nano granules additive,
With the quality of polyureas base grease (a) for 100% meter, the addition of antiwear additive (b) is 0.5-5 mass %；Antioxidant (c)
Addition be 0.1-3 mass %；The addition of viscosifier (d) is 1-8 mass %；The addition of micro-nano granules additive (e)
Measure as 2-10 mass %；
Wherein, described micro-nano granules additive (e) are the compositionss of politef and nano-calcium carbonate, described polytetrafluoroethyl-ne
Alkene is 1 with the mass ratio of nano-calcium carbonate:4～4:1.
2. lubricant composition according to claim 1 it is characterised in that described polyureas base grease (a) pass through with
Lower section method preparation：On the basis of described polyureas base grease (a) gross mass, (1) is by the two of the base oil of 32-45% and 2-4%
Isocyanates Hybrid Heating dissolves；(2) by the 18-amine. Hybrid Heating dissolving of remaining base oil and 0.3-1%, add afterwards
0.1-1% aniline and 0.8-2.5% cyclohexylamine, stirring and dissolving；(3) solution being obtained the solution that (1) obtains with (2) is mixed and stirs
Mix, homogenizing degassing is ground in cooling after heating and thermal insulation, obtains polyureas base grease (a).
3. lubricant composition according to claim 2 is it is characterised in that base in described polyureas base grease (a)
Plinth oil for poly alpha olefin base oil, one or more of Esters oil.
4. lubricant composition according to claim 3 is it is characterised in that base in described polyureas base grease (a)
Plinth oil is one or more of PAO40, PAO100, aromatic ester, polyol ester.
5. lubricant composition according to claim 4 is it is characterised in that base in described polyureas base grease (a)
Plinth oil is one or more of trimellitate, trihydroxymethylpropanyl ester, neopentyl polyol ester.
6. the lubricant composition according to any one of Claims 1 to 5 is it is characterised in that with polyureas base grease (a)
Quality is 100% meter, and the addition of antiwear additive (b) is 1-3 mass %；The addition of antioxidant (c) is 0.5-2.5 mass %；
The addition of viscosifier (d) is 3-5 mass %；The addition of micro-nano granules additive (e) is 2-8 mass %.
7. the lubricant composition according to any one of Claims 1 to 5 is it is characterised in that described antiwear additive (b) is boric acid
Salt antiwear additive.
8. lubricant composition according to claim 7 is it is characterised in that described antiwear additive (b) is three potassium borates neutrality
Dispersion liquid.
9. the lubricant composition according to any one of Claims 1 to 5 is it is characterised in that described antioxidant (c) is amine
Or phenolic antioxidant.
10. lubricant composition according to claim 9 is it is characterised in that described antioxidant (c) is right, p- dioctyl
Diphenylamines, octyl group butyl diphenylamines, naphthylamines, DBPC 2,6 ditertiary butyl p cresol or double (3,5- di-tert-butyl-4-hydroxyl benzyl) sulfur
One or more of ether.
11. lubricant compositions according to any one of Claims 1 to 5 are it is characterised in that described viscosifier (d) are poly-
One or more of isobutene., ethylene-propylene copolymer or polymethacrylates.
12. lubricant compositions according to any one of Claims 1 to 5 it is characterised in that described politef with receive
The mass ratio of rice Calcium Carbonate is 1:2～2:1.
13. lubricant compositions according to claim 12 are it is characterised in that the mean diameter of described politef is little
In 5 μm；The mean diameter of nano-calcium carbonate is less than 0.02 μm.
The preparation method of the lubricant composition described in a kind of 14. any one of claim 1～13 is it is characterised in that described
In polyureas base grease (a), add described antiwear additive (b), antioxidant (c), viscosifier (d) and micro-nano granules additive
E (), is mixed, obtain described lubricant composition.
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| CN105038913B (en) * | 2015-06-30 | 2018-03-02 | 上海禾泰特种润滑科技股份有限公司 | Lubricant compositions and preparation method thereof |
| CN105038914B (en) * | 2015-06-30 | 2018-09-18 | 上海禾泰特种润滑科技股份有限公司 | Gearbox lubrication agent composition and preparation method thereof |
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| CN111394151A (en) * | 2020-04-27 | 2020-07-10 | 中国石油化工股份有限公司 | Urea-based lubricating grease composition and preparation method thereof |
| CN112552981B (en) * | 2020-11-12 | 2022-03-25 | 江南大学 | Food-grade lubricating grease and application thereof |
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| CN101307269A (en) * | 2008-07-11 | 2008-11-19 | 哈尔滨工业大学 | Composite titan-based grease and method for preparing same |
| CN102839040A (en) * | 2011-06-22 | 2012-12-26 | 中国石油天然气股份有限公司 | Heavy-duty self-repairing open gear grease |
| CN103113969A (en) * | 2013-02-21 | 2013-05-22 | 尹继辉 | Modified composite titanium-based grease of micron-nano particles and preparation method thereof |
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