CN109401825A - A kind of polyureas base protective grease of containing graphene and preparation method thereof - Google Patents
A kind of polyureas base protective grease of containing graphene and preparation method thereof Download PDFInfo
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- CN109401825A CN109401825A CN201811264735.XA CN201811264735A CN109401825A CN 109401825 A CN109401825 A CN 109401825A CN 201811264735 A CN201811264735 A CN 201811264735A CN 109401825 A CN109401825 A CN 109401825A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/06—Mixtures of thickeners and additives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2217/045—Polyureas; Polyurethanes
- C10M2217/0456—Polyureas; Polyurethanes used as thickening agents
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The present invention is a kind of polyureas base grease and preparation method thereof of containing graphene, the lubricating grease is by base oil, account for the polyurea thickening agent of lubricating grease total weight 8%~20%, 0.1%~15% graphene, and 0~8% functional additive composition, graphene be by with participated in saponification after organic amine pre-reaction.The urea-base grease for the containing graphene for using this method to prepare can guarantee that graphene is uniformly distributed in lubricating grease in the form of single layer or thin layer, and its atomic structure of carbon is restored.The lubricating grease has excellent protective performance, can be used for a long time under marine environment.
Description
Technical field
The present invention relates to polyureas base protective greases of a kind of containing graphene and preparation method thereof, belong to the system of lubriation material
Standby technical field.
Background technique
With the rapid development of marine economy, the marine vehicles movable device such as naval vessel proposes more its lubriation material
High antirust, anticorrosion requirement.It is found according to practical experience, the existing common structure for protecting additive to lubricating grease, physics and chemistry
Performance or lubrication abrasion resistance have detrimental effect, if consistency reduces, mechanical stability decline etc..Graphene has ultra-thin lamella
Structure and chemical inertness can form Physical barriers between metal surface and active medium, to effectively obstruct water, salt fog
Deng pass through, prevent the media contact of metallic matrix and corrosivity or oxidisability, good protective action played to base material.
Graphene will not destroy the structure of lubricating grease as grease additive and can be improved the anti-wear and wear-resistant performance of lubricating grease, because
This is a kind of promising protection additive.The mechanism acted on by graphene to metal protection is it is found that expected anti-in order to reach
Effect is protected, graphene sheet layer is needed to be dispersed evenly in medium in the form of a large amount of thin layers.However, due to piece interlayer Van der Waals force
Effect, graphene is easy to happen lamella stacking in the medium, rather than is distributed in medium with thin layer state, so being not easy shape
At continuous whole protective layer.Therefore, preparing well dispersed graphene lubricating grease using effective preparation process is to realize stone
The protection of black alkene, abrasion resistance key.In addition, the graphene raw material generallyd use is the graphene of chemical method preparation, it is to pass through
The graphene oxide of strong oxidation reaction preparation, graphene oxide hydrophily is strong, has directly as additive to protective performance
Adverse effect restores its chemical inertness for needing to carry out reduction treatment to it when protecting additive.
In the document in graphene lubricating grease field, using graphene as grease additive by the wide of lubricating area
General concern, but in these reports, graphene is generallyd use as wear-resistant, lubricating additive, and more concerns pass through graphene
Addition improves the lubrication abrasion resistance of lubricating grease.Such as Patent No. CN103289802, CN201410648151.8 etc., another party
Face is exactly the conductive and heat-conductive physical characteristic using graphite, prepares thermally conductive or conducting function lubricating grease.Such as
CN105802717A.2016. it for the grease structure of invention, generallys use graphene and the progress of common lithium saponify is compound
Prepare graphene lubricating grease (CN104560264A).In the literature, the patent of only one report graphene polyureas base grease
Document, the graphene polyureas base grease simple process of the patent protection, is only mixed in polyureas base grease for graphene
At the conduction and greasy property for being more concerned about graphene lubricating grease in rouge raw material, and in the patent document, not more about
The examination of protective performance.Theoretically graphene sheet layer structure can play the protective action of isolation medium, however use graphene
So far there are no relevant reports for the research of protection additive as lubricating grease.
Summary of the invention
For the present invention exactly on the basis of the above-mentioned prior art, design provides a kind of polyureas base of novel containing graphene
Lubricating grease and preparation method thereof can be in marine environment the purpose is to have both the comprehensive performances such as good protective performance, abrasion resistance
It is used for a long time.
The it is proposed of this kind of technical solution is derived from us and has paid close attention to graphene at work as lubricating grease protection additive
A possibility that, and practice is combined by theoretical, this kind of graphene polyureas base grease is devised, and carry out to its preparation process
Improvement is continued to optimize, a kind of graphene polyureas base grease with prominent salt fog protective performance has been obtained.
The purpose of the present invention is achieved through the following technical solutions:
Technical solution of the present invention proposes a kind of polyureas base grease of containing graphene, it is characterised in that: the lubricating grease
Chemical component and weight percent are as follows: thickening agent 8~20%, graphene or its modified product 0.1%~5%, based on surplus
Oil；
The thickening agent is polyureas base, chemical general formula are as follows:
Wherein: n=1,3 or 5, which be prepared by organic amine and di-isocyanate reaction, wherein organic amine
In amido and diisocyanate in cyanic acid aliphatic radical molar ratio be 1.03~1.3: 1；
One or two kinds of mixture during the base oil is mineral oil, Synthin is oily；
The graphene is the graphene oxide prepared using chemical oxidization method,
The modified product of the graphene is the graphene nanometer sheet using long-chain organic matter/polymer-modified.It is lubricating
It can sufficiently be removed in oil, stable suspersion, the modified product of graphene oxide or graphene is by the pre-reaction with organic amine, into one
Step participates in saponification, is uniformly distributed in thickening agent network of fibers, and graphene chemical structure is restored.
Further, the chemical component and weight percent of the lubricating grease are as follows: thickening agent 8~20%, graphene or its modification
Product 0.1%~5%, rust-inhibiting additive 1%~3%, oil based on surplus；
The antirust agent is barium sulfonate/succinic acid one or two mixture.
Further, the extreme-pressure anti-friction additive of weight percent 1~5% is added in the lubricating grease.
Technical solution of the present invention also proposed the method for preparing above-mentioned polyureas base grease, it is characterised in that: this method
Steps are as follows:
Step 1: weighing each component in lubricating grease according to the ratio, base oil is divided into two parts, makes organic amine, isocyanide respectively
Acid esters sufficiently dissolves；
Ultrasound is carried out Step 2: graphene or its modified product are added in a base oil for be used to dissolve organic amine
Dispersion, 100~1000W of ultrasonic power, 20~60min of ultrasonic time, then organic amine is added in base oil, it is heated to organic amine
Solution temperature, mechanical stirring allows graphene or its modified product and organic amine to carry out 20~300min of pre-reaction, obtains organic
Amine oil solution；
Step 3: isocyanates is added in another base oil, heating stirring is uniform, obtains isocyanates oil solution；
Step 4: by isocyanates oil solution and organic amine oil solution hybrid reaction, reaction temperature is maintained at 90~120 DEG C
Between, the reaction time is 1~2.5h；
Step 5: after reaction, by reaction product in 100~180 DEG C of condition 1~3h of constant temperature, cooled to room temperature,
Then additive is added, mixes, be ground to uniformly, obtain graphene polyureas base grease.
The technical scheme is that being obtained in research work by deep theoretical research and a large amount of experimental exploring
Final grease composition and preparation process condition.According to the preventing mechanism of graphene, graphene is due to its ultra-thin lamella
Structure can form Physical barriers between metal surface and active medium, so that passing through for water, salt fog etc. is effectively obstructed,
The media contact for preventing metallic matrix and corrosivity or oxidisability, plays good protective action to base material.Therefore, it prepares
Graphene lubricating grease first has to guarantee that graphene can be present in lubricating grease with lamellar form, and is dispersed in lubricating grease
In, to form closely knit continuous protective barrier.
It is directly scattered in lubricating oil using graphene oxide, it is highly polar due to graphene oxide, make it in lubricating oil
Middle dispersion stabilization is bad, stands 2 hours and sedimentation layering (as shown in Fig. 1) just occurs.Organic amine is utilized in the present invention
The strong basicity of oil solution, pre-processes graphene oxide, and obtained graphene oil solution has good stably dispersing
Property, can guarantee 60 days almost without sedimentation (as shown in Fig. 1), graphene sheet layer being uniformly dispersed (such as Fig. 2 institute in lubricating oil
Show).In addition, by pretreatment after graphene oxide chemical structure have occurred reduction (result refer to attached drawing 3, pretreatment before and after
The XPS analysis result of graphene).
Method according to SH/T0081 carries out salt fog Performance Assessment and corruption to polyureas base grease prepared by distinct methods
Failure analysis is lost, graphene lubricating grease will be not added with, prepare graphene lubrication without pre-reaction graphene lubricating grease and pre-reaction
Rouge is applied to 45# steel surface, carries out salt fog performance test in property salt fog cabinet in a standard.Three kinds of test piece shapes by different number of days
State is as shown in Figure 4, the results showed that, be not added with graphene lubricating grease (such as Fig. 4 left figure) and without pre-reaction graphene lubricating grease (such as
Scheme in Fig. 4) there is corrosion by 20 days rear surfaces, and the graphene lubricating grease of pre-reaction passes through 60 days salt fog performance table of merit rating
Face is almost without obvious evidence of corrosion (such as figure right figure).In addition, without pre-reaction preparation graphene lubricating grease protective performance compared to
Decline instead before addition, fine etch pit uniformly occurs in steel disc after 20 days salt fogs, furthermore in some positions
There is big and deep corrosion pit, whether fine hot spot or big corrosion pit, which are all significantly more than, is not added with oxidation
The steel disc of graphene.This is because graphene there is no sufficiently restoring, exists, hydrophily still in the form of graphene oxide
By force, it is easy to provide the channel of contact metal testing plate to hydrone.
The advantages of technical solution of the present invention, is:
The present invention is for above-mentioned prior art situation and needs and designs and provide a kind of containing graphene polyureas base grease
And preparation method thereof, since the dispersion mixing technique to graphene in lubricating grease preparation process is sufficiently improved, the polyureas
Graphene is dispersed in lubricating grease in base grease with lamellar form, and chemical structure has obtained abundant reduction, therefore,
Graphene is on the one hand lipophilic to be improved, and without obvious hydrophily, is on the other hand formd continuous closely knit protective barrier, can be delayed
The approach of the contact metal such as hydrone, oxygen molecule.Therefore, the salt fog protective performance of lubricating grease has obtained great promotion, protection
Effect can be suitable with protection additive.In addition, usually used protection additive can be to the structure of lubricating grease and other reasons
Changing performance has undesirable influence, is influenced less, also to anti-wear and wear-resistant performance using graphene on the conventional physico-chemical properties of lubricating grease
It is promoted, therefore, is moistened using optimization technique using graphene as the protection of the protection available excellent combination property of additive
Consistent lubricant.
Detailed description of the invention
(left: graphene oxide directly disperses the graphene lubricating oil digital photo that Fig. 1 is prepared for different dispersing modes；It is right:
After graphene oxide dispersion after pre-reaction)
Fig. 2 is dispersed optical micrograph of the graphene platelet in lubricating oil after ultrasound and pre-reaction
Fig. 3 is (left: before pre-reaction by the XPS map of graphene before and after pre-reaction；It is right: after pre-reaction)
Fig. 4 is that the steel disc of different lubricating grease coating (is followed successively by is not added with from left to right by salt spray test rear surface state
Graphene lubricating grease, 20 days；Without pre-reaction graphene lubricating grease, 20 days；Pre-reaction graphene lubricating grease, 60 days)
Specific embodiment
Technical solution of the present invention is further described below with reference to embodiment:
Graphene oxide used in the examples is prepared using Hummers method, salt fog protective performance in embodiment
Establishing criteria method SH/T0081 is tested, four ball abrasion resistances are tested according to standard method SH/T0204.
The following are the embodiments of the polyureas base grease of graphene:
Embodiment 1
The step of preparing the polyureas base grease of graphene are as follows: 1g graphene oxide is added in 519g base oil, is surpassed
Sound 30min (ultrasonic power 500w), then 32.4g octadecylamine and 15.25g n-octyl amine are added into base oil, 80 DEG C are heated to, is stirred
It mixes 60min. and weighs 400g base oil again, 29.5gMDI is added, heating makes its thawing.Reaction kettle, mixing is added in two groups of solution
Stirring, 100 DEG C of stirring 60min discharging are put into 150 DEG C of baking ovens and post-process 2 hours, by three-roll grinder grinding 2~3 times at
Rouge, properties of product are as shown in appendix 1.
Wherein, poly- carbamido thickening agent is two polyureas in embodiment 1.
Embodiment 2
The step of preparing the polyureas base grease of graphene are as follows: 5g graphene oxide is added in 495g base oil, is surpassed
Sound 20min (ultrasonic power 1000w), then 51.28g octadecylamine and 18.5g para-totuidine are added into base oil, it is heated to 80
DEG C, stirring 120min. weighs 400g base oil again, and 30.1gTDI is added, and heating makes its thawing.Reaction is added in two groups of solution
Kettle is mixed, and 90 DEG C of stirring 120min discharging is put into 180 DEG C of baking ovens and post-processes 1 hour, 2 are ground by three-roll grinder~
3 times at rouge, properties of product are as shown in appendix 1.
Wherein, poly- carbamido thickening agent is two polyureas in embodiment 2.
Embodiment 3
The step of preparing the polyureas base grease of graphene are as follows: 25g graphene oxide is added in 425g base oil, is surpassed
Sound 60min (ultrasonic power 100w), then 63.7g lauryl amine and 32.9g para-totuidine are added into base oil, 80 DEG C are heated to,
Stirring 300min. weighs 400g base oil again, and 53.4gTDI is added, and heating makes its thawing.Reaction kettle is added in two groups of solution, is mixed
Close stirring, 110 DEG C of stirring 90min discharging is put into 100 DEG C of baking ovens and post-processes 3 hours, by three-roll grinder grinding 2~3 times at
Rouge, properties of product are as shown in appendix 1.Wherein, poly- carbamido thickening agent is two polyureas in embodiment 3.
Embodiment 4
The step of preparing the polyureas base grease of graphene are as follows: 30g graphene oxide is added in 400g base oil, is surpassed
Sound 40min (ultrasonic power 500w), then 67.5g lauryl amine and 51g decyl amine are added into base oil, 80 DEG C are heated to, stirring
60min. weighs 370g base oil again, and 81.3gMDI is added, and heating makes its thawing.Reaction kettle is added in two groups of solution, mixing is stirred
Mix, 100 DEG C of stirring 60min discharging is put into 120 DEG C of baking ovens and post-processes 2.5 hours, by three-roll grinder grind 2~3 times at
Rouge, properties of product are as shown in appendix 1.Wherein, poly- carbamido thickening agent is two polyureas in embodiment 4.
Comparative example 1
Preparation not the polyureas base grease of containing graphene the step of are as follows: into 520g base oil be added 32.4g octadecylamine and
15.25g n-octyl amine is heated to 80 DEG C, and stirring 60min. weighs 400g base oil again, and 29.5gMDI is added, and heating makes its thawing.
Reaction kettle is added in two groups of solution, is mixed, 100 DEG C of stirring 60min dischargings are put into 150 DEG C of baking ovens and post-process 2 hours, lead to
It crosses three-roll grinder and grinds 2~3 times into rouge, properties of product are as shown in appendix 1.Wherein, poly- carbamido thickening agent is two in comparative example 1
Polyureas.
Comparative example 2
The step of preparing the polyureas base grease of the graphene without pre-reaction are as follows: 1g graphene oxide is added to 519g base
In plinth oil, then 32.4g octadecylamine and 15.25g n-octyl amine are added into base oil, are heated to 80 DEG C.400g base oil is weighed again,
29.5gMDI is added, heating makes its thawing.Reaction kettle is added in two groups of solution, is mixed, 100 DEG C of stirring 60min dischargings are put
Enter 150 DEG C of baking ovens to post-process 2 hours, grinds 2~3 times into rouge by three-roll grinder, properties of product are as shown in appendix 1.Wherein,
Poly- carbamido thickening agent is two polyureas in comparative example 2.
1. containing graphene of subordinate list, two polyurea grease protects abrasion resistance
Embodiment 5
The step of preparing the polyureas base grease of graphene are as follows: the graphene additive of oleic acid modified is prepared first, it is typical
Ground disperses 0.1g graphene oxide in 200ml ethyl alcohol/DMF, ultrasonic 30min, and then suspension, machine is added in 1g oleic acid
Tool is stirred to react 5h, rinses, and filtering, grinding obtains the graphene powder of oleic acid modified after drying.By the graphite of 30g oleic acid modified
Alkene is added in 400g base oil, ultrasonic 30min (ultrasonic power 500w), then into base oil be added 12.65g ethylenediamine and
77.8g lauryl amine is heated to 80 DEG C, and stirring 60min. weighs 350 base oils again, and 105.1gMDI is added, and heating makes its thawing.
Reaction kettle is added in two groups of solution, is mixed, 90 DEG C of stirring 150min, 2.0g diphenylamines (20g oil) is added, then react
30min, discharging are put into 150 DEG C of baking ovens and post-process 2 hours, grind 2~3 times into rouge by three-roll grinder, properties of product are for example attached
Shown in table 2.Wherein, poly- carbamido thickening agent is four polyureas in embodiment 5.
Embodiment 6
The step of preparing the polyureas base grease of graphene are as follows: 10g graphene oxide is added in 500g base oil, is surpassed
Sound 30min (ultrasonic power 500w), then 9.14g hexamethylene diamine and 43.5g octadecylamine are added into base oil, 80 DEG C are heated to, is stirred
It mixes 60min. and weighs 410 base oils again, 27.4gTDI is added, heating makes its thawing.Reaction kettle is added in two groups of solution, mixing is stirred
It mixes, 100 DEG C of stirring 90min, discharges, be put into 180 DEG C of baking ovens and post-process 2 hours, grind 2~3 times into rouge by three-roll grinder,
Properties of product are as shown in subordinate list 2.Wherein, poly- carbamido thickening agent is four polyureas in embodiment 6.
Embodiment 7
The step of preparing the polyureas base grease of graphene are as follows: prepare the graphene additive of stearic acid grafted, allusion quotation first
Type, it disperses 0.1g graphene oxide in 200ml ethyl alcohol/DMF, ultrasonic 30min, and then 1g stearic acid is added and is suspended
Liquid, mechanic whirl-nett reaction 5h are rinsed, and filtering, grinding obtains the graphene powder of stearic acid grafted after drying.8g stearic acid is connect
Branch graphene be added in 442g base oil, ultrasonic 30min (ultrasonic power 500w), then into base oil be added 22.2g oneself
Diamines and 60.6g decyl amine are heated to 80 DEG C, and stirring 60min. weighs 400g base oil again, and 66.1gTDI is added, and heating melts it
Change.Reaction kettle is added in two groups of solution, is mixed, 100 DEG C of stirring 60min, it is small to be put into 120 DEG C of baking oven post-processings 2 for discharging
When, 2~3 times are ground into rouge by three-roll grinder, and properties of product are as shown in subordinate list 2.Wherein, polyureas base is thickened in embodiment 7
Agent is four polyureas.
Embodiment 8
The step of preparing the polyureas base grease of graphene are as follows: 50g graphene oxide is added in 450g base oil, is surpassed
Sound 30min (ultrasonic power 500w), then 5.33g ethylenediamine and 50.26g octadecylamine are added into base oil, 80 DEG C are heated to, is stirred
It mixes 60min. and weighs 400g base oil again, 44.4gMDI is added, heating makes its thawing.Reaction kettle, mixing is added in two groups of solution
Stirring, 100 DEG C of stirring 60min, discharging are put into 150 DEG C of baking ovens and post-process 2 hours, by three-roll grinder grinding 2~3 times at
Rouge, properties of product are as shown in subordinate list 2.Wherein, poly- carbamido thickening agent is four polyureas in embodiment 8.
2. containing graphene of subordinate list, four polyurea grease protects abrasion resistance
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | |
| Diamines | Ethylenediamine | Hexamethylene diamine | Hexamethylene diamine | Ethylenediamine |
| Monoamine | Lauryl amine | Octadecylamine | Decyl amine | Octadecylamine |
| Isocyanates | MDI | TDI | TDI | MDI |
| Salt fog performance/day | 65 | 67 | 70 | 64 |
| Abrasion resistance/mm | 0.70 | 0.65 | 0.68 | 0.70 |
Embodiment 9
The step of preparing the polyureas base grease of graphene are as follows: 50g graphene oxide is added in 450g base oil, is surpassed
Sound 30min (ultrasonic power 500w), then 9.6g ethylenediamine and 45.2g lauryl amine are added into base oil, 80 DEG C are heated to, stirring
60min. weighs 400g base oil again, and 60g MDI is added, and heating makes its thawing.Reaction kettle is added in two groups of solution, mixing is stirred
It mixes, 100 DEG C of stirring 60min, discharges, be put into 150 DEG C of baking ovens and post-process 2 hours, grind 2~3 times into rouge by three-roll grinder,
Properties of product are as shown in subordinate list 3.Wherein, poly- carbamido thickening agent is six polyureas in embodiment 9.
Embodiment 10
The step of preparing the polyureas base grease of graphene are as follows: 40g graphene oxide is added in 410g base oil, is surpassed
Sound 30min (ultrasonic power 500w), then 26.4g hexamethylene diamine and 64.5g octadecylamine are added into base oil, 80 DEG C are heated to, is stirred
It mixes 60min. and weighs 400g base oil again, 59.6g TDI is added, heating makes its thawing.Reaction kettle, mixing is added in two groups of solution
Stirring, 100 DEG C of stirring 60min, discharging are put into 160 DEG C of baking ovens and post-process 2 hours, by three-roll grinder grinding 2~3 times at
Rouge, properties of product are as shown in subordinate list 3.Wherein, poly- carbamido thickening agent is six polyureas in embodiment 10.
Embodiment 11
The step of preparing the polyureas base grease of graphene are as follows: 30g graphene oxide is added in 450g base oil, is surpassed
Sound 30min (ultrasonic power 500w), then 26g hexamethylene diamine and 35.8g decyl amine are added into base oil, 80 DEG C are heated to, stirring
60min. weighs 400g base oil again, and 58.5g TDI is added, and heating makes its thawing.Reaction kettle is added in two groups of solution, mixing is stirred
It mixes, 100 DEG C of stirring 60min, discharges, be put into 180 DEG C of baking ovens and post-process 2 hours, grind 2~3 times into rouge by three-roll grinder,
Properties of product are as shown in subordinate list 3.Wherein, poly- carbamido thickening agent is six polyureas in embodiment 11.
Embodiment 12
The step of preparing the polyureas base grease of graphene are as follows: 10g graphene oxide is added in 390g base oil, is surpassed
Sound 30min (ultrasonic power 500w), then 16.8g ethylenediamine and 79.2g octadecylamine are added into base oil, 80 DEG C are heated to, is stirred
It mixes 60min. and weighs 400g base oil again, 105g MDI is added, heating makes its thawing.Reaction kettle, mixing is added in two groups of solution
Stirring, 100 DEG C of stirring 60min, discharging are put into 150 DEG C of baking ovens and post-process 2 hours, by three-roll grinder grinding 2~3 times at
Rouge, properties of product are as shown in subordinate list 3.Wherein, poly- carbamido thickening agent is six polyureas in embodiment 12.
3. containing graphene of subordinate list, six polyurea grease protects abrasion resistance
| Embodiment 9 | Embodiment 10 | Embodiment 11 | Embodiment 12 | |
| Diamines | Ethylenediamine | Hexamethylene diamine | Hexamethylene diamine | Ethylenediamine |
| Monoamine | Lauryl amine | Octadecylamine | Decyl amine | Octadecylamine |
| Isocyanates | MDI | TDI | TDI | MDI |
| Salt fog performance/day | 66 | 62 | 71 | 68 |
| Abrasion resistance/mm | 0.72 | 0.70 | 0.62 | 0.65 |
By the performance of lubricating grease in embodiment it can be seen that prepared lubricating grease is homogeneous paste, protective performance is very
Excellent, salt fog performance reaches 60 days or more, and abrasion resistance is excellent, and wear scar diameter is lower than 0.75mm, can satisfy marine environment
The protection of the components such as bearing lubricates use demand.
Claims (4)
1. a kind of polyureas base grease of containing graphene, it is characterised in that: the chemical component and weight percent of the lubricating grease are as follows:
Thickening agent 8~20%, graphene or its modified product 0.1%~5%, oil based on surplus；
The thickening agent is polyureas base, chemical general formula are as follows:
Wherein: n=1,3 or 5, which be prepared by organic amine and di-isocyanate reaction, wherein in organic amine
The molar ratio of cyanic acid aliphatic radical in amido and diisocyanate is 1.03~1.3: 1；
One or two kinds of mixture during the base oil is mineral oil, Synthin is oily；
The graphene is the graphene oxide prepared using chemical oxidization method,
The modified product of the graphene is the graphene nanometer sheet using long-chain organic matter/polymer-modified.
2. the polyureas base grease of containing graphene according to claim 1, it is characterised in that: the chemical component of the lubricating grease
And weight percent are as follows: thickening agent 8~20%, graphene or its modified product 0.1%~5%, rust-inhibiting additive 1%~3%,
It is oily based on surplus；
The antirust agent is barium sulfonate/succinic acid one or two mixture.
3. the polyureas base grease of containing graphene according to claim 1 or 2, it is characterised in that: be added in the lubricating grease
The extreme-pressure anti-friction additive of weight percent 1~5%.
4. the method for preparing polyureas base grease described in claim 1, it is characterised in that: the step of this method is as follows:
Step 1: weighing each component in lubricating grease according to the ratio, base oil is divided into two parts, makes organic amine, isocyanates respectively
Sufficiently dissolution；
Ultrasound point is carried out Step 2: graphene or its modified product are added in a base oil for be used to dissolve organic amine
It dissipates, 100~1000W of ultrasonic power, 20~60min of ultrasonic time, then organic amine is added in base oil, be heated to organic amine
Solution temperature, mechanical stirring allow graphene or its modified product and organic amine to carry out 20~300min of pre-reaction, obtain organic amine
Oil solution；
Step 3: isocyanates is added in another base oil, heating stirring is uniform, obtains isocyanates oil solution；
Step 4: by isocyanates oil solution and organic amine oil solution hybrid reaction, reaction temperature be maintained at 90~120 DEG C it
Between, the reaction time is 1~2.5h；
Step 5: after reaction, by reaction product in 100~180 DEG C of condition 1~3h of constant temperature, cooled to room temperature, then
Additive is added, mixes, be ground to uniformly, obtain graphene polyureas base grease.
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