CN104560290B - A kind of composite barium-base grease composition and preparation method thereof - Google Patents
A kind of composite barium-base grease composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of composite barium-base grease and preparation method thereof.On the basis of lubricating grease weight, the composite barium-base grease includes following components：65 95% lubricating base oil, 5 30% composite barium-base thickening agent, 0.2 15% graphene.The composite barium-base grease has the performances such as excellent heat-resisting quantity, water-resistance and adhesiveness, colloid stability, extreme pressure anti-wear, lubricating life, anticorrosive property and resistance to saltfog.
Description
Technical field
It is specifically to be related to a kind of composite barium-base grease composition and its system the present invention relates to a kind of lubricant material
Preparation Method.
Background technology
Composite barium-base grease is that the compound barium soap for reacting generation by two or more acid and barium hydroxide is thickened
What refined medium-viscosity mineral oil was made, with good water-resistance, higher dropping point and certain barrier propterty.By tristearin
Sour barium is thickened Ba-grease-ZB10-2, the water-resistance and resistance to pressure of the fat made from the synthetic oil for transformer cut of low condensation point
It is all very strong, it is good to the adhesive force and protective value of metal surface, while it is practically insoluble in the organic solvents such as gasoline and alcohol, it is one
Plant excellent waterproof, anti-solvent, protection and encapsulant.
Also there are many reports both at home and abroad to composite barium-base grease：As US2033148, US2417433A are at large reported
The production method of composite barium-base grease；CN102021067A be prepared for it is a kind of there is preferable water-resistance and sealing, it is anti-low
Warm nature energy and rust-preventing characteristic good ships aluminium Ba-grease；CN1160754A uses oil based on high viscosity mineral oil,
Aliphatic acid and decanedioic acid are thickening agent, and aromatic amine and lithium salicylate are composite antioxidant, and add filler and antirust agent uses one
Footwork is prepared for a kind of multiple-effect composite barium-base profit with excellent high temperatures, oxidation stability, water-resistance and extreme pressure anti-wear
Consistent lubricant.
In recent years in order to improve the performance of composite barium-base grease, substantial amounts of research is have also been made in terms of additive, for example
Antioxidant, extreme pressure anti-wear additives, antirust agent etc..Nano material is also gradually available in the application of lubricating grease, such as nano silicon, receive
Rice diamond, nano titanium oxide, nano zine oxide etc., but the correlation of the application still without graphene in lubricating grease is ground so far
Study carefully.
The content of the invention
It is an object of the invention to provide a kind of new composite barium-base grease and preparation method thereof.
The present inventor is had found under study for action, and a part for graphene as thickening agent is added in base oil,
Especially it is added in base oil and is reacted with composite barium-base thickening agent one in initial reaction stage, the composite barium-base profit of generation graphene-containing
Consistent lubricant, resulting composite barium-base grease not only has good electric conductivity, and this method can substantially shorten compound
The preparation time of Ba-grease.
An aspect of of the present present invention provides a kind of composite barium-base grease, on the basis of lubricating grease weight, including with the following group
Point：65-95% lubricating base oil, 5-30% composite barium-base thickening agent, 0.2-15% graphene.
Under preferable case, on the basis of lubricating grease weight, including following components：70-93% lubricating base oil, 8-25%'s
Composite barium-base thickening agent, 1-10% graphene.
The second aspect of the present invention provides a kind of preparation method of composite barium-base grease, and this method includes：By graphite
Alkene, composite barium-base thickening agent and part basis oil are well mixed, and in 170-220 DEG C of constant temperature refining, cooling adds remaining basis
Oil, adds necessary additive, obtains finished product.
The third aspect of the present invention provides a kind of preparation method of composite barium-base grease, and this method includes：
Part basis oil, graphene, polymer acid and low molecular acid are mixed, heated, 80-105 DEG C is warming up to, hydrogen is added
Barium monoxide, carries out saponification, 170-220 DEG C is warming up to after reaction completely, adds remaining base oil and is cooled to 100-130
DEG C, necessary additive is added afterwards, fat is milled into, and obtains finished product；Wherein described acid is the mixed of polymer acid and low molecular acid
Acid is closed, the polymer acid is the aliphatic acid and/or hydroxy fatty acid that carbon number is C12-C25, and the low molecular acid is carbon
Atomicity is 6-10 carboxylic acid.
The fourth aspect of the present invention provides composite barium-base grease made from the above method.
The composite barium-base grease that the present invention is provided, with high dropping point, good mechanical stability, higher anti-oxidant
Property, high-temperature and reversible, preferable pumping, excellent heat endurance, water-resistance and colloid stability, and have with other lubricating grease
Good compatibility.In addition, being added by the preliminary stage by graphene in fat processed so that graphene causes thickening as nucleus
Agent depends on around it structure for forming class micelle, and this synergy between graphene and soap molecule enhances soap molecule and consolidated
Change the ability of base oil, greatly improve into fat speed, shorten saponification time, and enable the fat to be competent in various electricity
Machine, generator, air blower, transportation, the lubrication of iron and steel enterprise and other various industrial equipments, be particularly suitable for use in it is various compared with
The lubrication of the friction part of plant equipment under high-temperature wet condition.
Embodiment
An aspect of of the present present invention provides a kind of composite barium-base grease, on the basis of lubricating grease weight, including with the following group
Point：65-95% lubricating base oil, 5-30% composite barium-base thickening agent, 0.2-15% graphene.
Under preferable case, on the basis of lubricating grease weight, including following components：70-93% lubricating base oil, 8-25%'s
Composite barium-base thickening agent, 1-10% graphene.
In the composite barium-base grease of the present invention, the consumption of graphene can be common with composite barium-base thickening agent with larger
As thickening agent, and unconventional conductive agent, one side are so that gained composite barium-base grease maintains general composite barium-base profit
The advantage of consistent lubricant, such as good colloid stability, high temperatures, low temperature properties, extreme pressure anti-wear, while the addition of graphene is more carried
Its high oxidation resistance.On the other hand the preliminary stage by graphene in fat processed is added so that greatly improve into fat speed,
Saponification time is shortened, so that obtained composite barium-base grease can be competent in high temperature, high speed, high load capacity, many water
Deng harsh working condition.
Graphene is a kind of new material for the individual layer laminated structure being made up of carbon atom, be it is current it is most thin in the world be but also most
Hard nano material, its thermal conductivity factor is up to 5300W/mK, higher than CNT and diamond, and its resistivity ratio copper or
Silver is lower, is the minimum material of current resistivity in the world.Because graphene is substantially a kind of transparent, good conductor,
Manufacture transparent touch screen, even tabula rasa, solar cell are adapted to, it is multiple that it is widely used in nanoelectronics, nanometer
The fields such as compound, battery, ultracapacitor, hydrogen storage and biologic applications.
In the present invention, the graphene can be the graphene of existing all size, can also may be used by commercially available
To be obtained by existing various methods.Under preferable case, the graphene is obtained by the method comprised the following steps：
Graphite flakes and sodium nitrate, the concentrated sulfuric acid are well mixed in ice bath, potassium permanganate are slowly added under stirring, in 5-
Stirring reaction at 20 DEG C, is warming up to 30-45 DEG C of continuation stirring reaction, then adds deionized water dilution.Added into system
Hydrogen peroxide solution reduces potassium permanganate, then through pickling, wash, be dried to obtain graphene oxide.By obtained graphene oxide
Be added to the water progress ultrasonication after, add hydrazine hydrate, oil bath reaction fully after, obtained black flocculent deposit through washing,
Suction filtration, drying, the powder finally obtained as graphene.The frequency of ultrasonic wave is preferably 20-40kHz.
The graphene obtained using the above method（Referred to as make graphene by oneself）With commercially available graphene in particle diameter distribution, conduction
There is significant advantage in property, stability and dispersiveness, specific performance index see the table below 1.
Table 1
| Commercially available graphene | Make graphene by oneself | |
| Particle diameter, nm | 100~3000 | 80~800 |
| Electrical conductivity, S/cm | 500 | 700-900 |
| Decomposition temperature, DEG C | 410 | 430-480 |
| Being capable of scattered and non-setting maximum, mg in 1ml base oils | 5 | 8-12 |
Note：Base oil is base oil used in following embodiments 1, if precipitation is after disperseing in terms of 60 minutes.Above-mentioned particle diameter is adopted
With dynamic light scattering particle size analyzer Dynapro Titan TC（Producer：Wyatt Technology）Measure.Electrical conductivity is used
Bel BEC-950 laboratories resistivity meter is measured.Decomposition temperature uses thermogravimetric analyzer SDT-Q600（Producer：U.S. TA
Instrument companies）Measure.It is same as below.
The composite barium-base thickening agent of the present invention can be reacted by acid with barium hydroxide to be generated, the acid for polymer acid and
The mixed acid of low molecular acid, the polymer acid is the aliphatic acid and/or hydroxy fatty acid that carbon number is C12-C25, can be with
It is one or more mixtures in laurate, palmitic acid, stearic acid, 12- hydroxy stearic acids, preferably stearic acid, 12- hydroxyls is hard
Resin acid；The low molecular acid can be the dicarboxylic acids that carbon number is 6-10, preferably terephthalic acid (TPA), azelaic acid, the last of the ten Heavenly stems two
One or more of mixed acid in acid.The weight ratio preferably 1 of polymer acid and low molecular acid:0.1-1.
Lubricating base oil used in the present invention can be mineral oil, vegetable oil, artificial oil or their mixture, 100 DEG C
Kinematic viscosity is 5-60mm2/ s, preferably 10-30mm2/s.Vegetable oil can be castor oil, rapeseed oil, peanut oil, soya-bean oil etc..Close
Can be poly-a-olefin oil into oil（PAO）, Esters oil, fluorocarbon oil, silicone oil etc..
Various additives, such as antioxidant, extreme pressure anti-wear additives, antirust agent can also be contained in lubricating grease of the present invention.Its
In, the preferred arylamine kind antioxidant of antioxidant accounts for the 0.01-5% of lubricating grease gross weight, preferably 0.1-2.5%, can be diphenylamines,
At least one of phenyl-α-naphthylamine and di-iso-octyldiphenylamine, preferably di-iso-octyldiphenylamine.Extreme pressure anti-wear additives account for lubricating grease
The 0.5-12% of gross weight, preferably 0.5-5%, can be two thio Acidic phosphates zinc, two thio dialkyl amido formic acid molybdenums, two
Thio dialkyl amido lead formate, triphenylphosphorothionate, organic molybdenum complex compound, olefine sulfide, molybdenum disulfide, polytetrafluoroethyl-ne
Alkene, D2EHDTPA molybdenum, chlorinated paraffin, dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide, fluorographite, carbonic acid
At least one of calcium and zinc oxide；Antirust agent accounts for the 0.01-4.5% of lubricating grease gross weight, preferably 0.1-2%, can be oil
At least one of barium sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid.
In the present invention, the content of the component of each in grease composition is calculated according to inventory to be obtained.Wherein, composite barium-base is thick
Content=100% of agent ×（The weight of the weight of polymer acid barium+low molecular acid barium）/ lubricating grease gross weight.
According to the second aspect of the invention, the invention provides a kind of preparation method of composite barium-base grease, this method
Including：Graphene, composite barium-base thickening agent and part basis oil is well mixed, in 170-220 DEG C of constant temperature refining, cool down, plus
Enter remaining base oil, add necessary additive, obtain finished product.
Wherein, the consumption of graphene, composite barium-base thickening agent and base oil makes the composite barium-base grease of gained, to lubricate
On the basis of fat weight, including following components：65-95% lubricating base oil, 5-30% composite barium-base thickening agent, 0.2-15%'s
Graphene.
Under preferable case, the consumption of graphene, composite barium-base thickening agent and base oil causes gained composite barium-base grease,
On the basis of lubricating grease weight, including following components：70-93% lubricating base oil, 8-25% composite barium-base thickening agent, 1-
10% graphene.
According to the third aspect of the invention we, the invention provides a kind of preparation method of composite barium-base grease, this method
Including：
Base oil, graphene, polymer acid and low molecular acid are mixed, heated, 80-105 DEG C is warming up to, hydroxide is added
Barium, carries out saponification, 170-220 DEG C is warming up to after reaction completely, adds remaining base oil and is cooled to 100-130 DEG C, it
After add necessary additive, be milled into fat, obtain finished product.
Graphene, polymer acid, low molecular acid, the consumption of barium hydroxide and base oil cause gained composite barium-base lubrication
Fat, on the basis of lubricating grease weight, including following components：65-95% lubricating base oil, 5-30% composite barium-base thickening agent,
0.2-15% graphene.
Under preferable case, graphene, polymer acid, low molecular acid, the consumption of barium hydroxide and base oil cause gained multiple
Ba-grease is closed, on the basis of lubricating grease weight, including following components：70-93% lubricating base oil, 8-25% compound barium
Base thickening agent, 1-10% graphene.
The oily weight with remaining base oil of part basis is than preferably 1/2-2/3：1/3-1/2.
The mol ratio of the total amount and barium hydroxide of polymer acid and low molecular acid is preferably stoichiometric proportion, wherein hydroxide
The amount of barium can also excess 1-10 weight %.
The temperature that polymer acid, low molecular acid and barium hydroxide carry out saponification is preferably 80-105 DEG C, and the time is preferred
For 0.5-1 hours.
Refining temperature is preferably 170-220 DEG C, and the time is preferably 5-10 minutes.
The composite barium-base grease that the preparation method for the composite barium-base grease that the present invention is provided is provided with prior art
Preparation method is main difference is that saponification is carried out in the presence of graphene, therefore on other operations of the preparation process
Prior art is referred to condition to carry out.
A preferred embodiment of the invention, the composite barium-base grease that the present invention is provided can be by with lower section
It is prepared by method：
Graphene, polymer acid, low molecular acid are added in 2/3 or so base oil, stirring mixing, heat temperature raising,
When temperature rises to 80-105 DEG C, start to be slowly added to barium hydroxide, carry out compound saponification 0.5h-1h；Continue to heat and rise
When temperature is to 170-220 DEG C, 5-10min is kept；Add remaining base oil and be cooled to 100-130 DEG C, add additive, pass through three
Roller machine mills 2-4 times into fat.
Fourth aspect present invention provides the composite barium-base grease as made from above-mentioned third aspect method.
Compared with the composite barium-base grease as made from the preparation method that second aspect is provided, it is compound that fourth aspect is provided
Ba-grease has more preferable heat-resisting quantity, water-resistance and adhesiveness, colloid stability and extreme pressure anti-wear.
In the present invention, the content of the component of each in grease composition is calculated according to inventory to be obtained.Wherein, composite barium-base is thick
Content=100% of agent ×（The weight of the weight of polymer acid barium+low molecular acid barium）/ lubricating grease gross weight.
The present invention is further illustrated for following embodiment, but and is not so limited the present invention.Following examples
In, dropping point is measured using GB/T3498 methods, and cone penetration is measured using GB/T269 methods, and oxidation stability uses SH/T0325
Method is measured, and Stencil oil-dividing is measured using SH/T0324 methods, and anticorrosive property is measured using GB/T5018 methods, and water drenches number of dropouts
Measured using SH/T0109 methods, tetra-ball machine test PB is measured using SH/T0202 methods, and tetra-ball machine test PD uses SH/
T0202 methods are measured, and copper corrosion performance is measured using GB/T7326 methods, and electric conductivity is measured using SH/T0596 methods, is rubbed
Coefficient is wiped to measure using SH/T0847.
Embodiment 1
The preparation of graphene oxide：
1g graphite flakes and 0.5g sodium nitrate are well mixed with the 23ml concentrated sulfuric acids in ice bath, 3g is slowly added under stirring
Potassium permanganate, temperature is maintained at 10 DEG C of 1h stirred below, and then mixture stirs 0.5h at 35 DEG C, then adds 50ml deionizations
Water dilutes, during release substantial amounts of heat, enter to exercise temperature in ice bath less than 100 DEG C, add 50ml water, mixture stirring
0.5h, adds 200ml deionized waters and further dilutes.10ml 30 weight % aqueous hydrogen peroxide solution reduction is added afterwards
Potassium permanganate.Finally, mixture mass concentration is 5% hydrochloric acid（400ml）Washing and filtering, to remove metal ion.Then use
0.5L deionized waters go deacidification, and graphene oxide is made in 60 DEG C of dry 24h.
The preparation of graphene：
0.1g graphene oxides obtained above are added to ultrasonic disperse in 100ml water（Ultrasonic frequency is 30kHz）
5ml hydrazine hydrates are added after 30min（Mass concentration is 85%）, 100 DEG C of reaction 24h of oil bath, the black flocculent deposit warp finally obtained
The powder as graphene obtained after washing, suction filtration, drying, the performance of graphene is as shown in table 2 below.
The preparation of composite barium-base grease：
Raw material components：Graphene 15g；500SN base oils 640g（100 DEG C of viscosity are 10mm2/s）；Barium hydroxide
78.2g；Terephthalic acid (TPA) 27.6g；12- hydroxy stearic acids 49.2g；Antioxidant T5018g.
430 grams of base oils, 15 grams of graphenes and 49.2 grams of 12- hydroxy stearic acids, 27.6 grams of terephthalic acid (TPA)s are added to
In fat kettle processed, heating stirring, when temperature rises to 85 DEG C, starts to be slowly added to 78.2 grams of barium hydroxides, carries out compound soap
Change；180 DEG C are warming up to after having reacted, 5min is kept；Add 210 grams of base oils and be cooled to 8 grams of antioxidant T501 of addition after 120 DEG C
And stir, 2 times are ground into fat by three-roller.Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment is obtained, on the basis of lubricating grease weight, constitute and be：The weight of 12- hydroxy stearic acids barium 7.8
Measure %；The weight % of terephthalic acid (TPA) barium 6.5；The weight % of graphene 1.9；The weight % of lubricating base oil 82.8；The weight % of antioxidant 1.0.
Embodiment 2
The preparation be the same as Example 1 of graphene oxide.
The preparation of graphene：
Graphene oxide made from 0.1g is added to ultrasonic disperse in 100ml water（Ultrasonic frequency is 35kHz）30min
5ml hydrazine hydrates are added afterwards（Mass concentration is 85%）, 100 DEG C of oil bath reaction 24h, the black flocculent deposit finally obtained through washing,
The powder as graphene obtained after suction filtration, drying, the performance of graphene is as shown in table 2 below.
The preparation of composite barium-base grease：
Raw material components：Graphene 30g；150BS base oils 200g（100 DEG C of viscosity are 31mm2/s）；Barium hydroxide
48.9g；Decanedioic acid 21g；12- hydroxy stearic acids 30.8g；Antioxidant di-iso-octyldiphenylamine 1g.
100 grams of base oils, 30 grams of graphenes, 30.8 grams of 12- hydroxy stearic acids and 21 grams of decanedioic acid are added to fat kettle processed
In, heating stirring when temperature rises to 105 DEG C, starts to be slowly added to 48.9 grams of barium hydroxides, carries out compound saponification；So
After be warming up to 210 DEG C, keep 5min；Add 100 grams of base oils and be cooled to 1 gram of antioxidant di-iso-octyldiphenylamine of addition after 90 DEG C
And stir, 3 times are ground into fat by three-roller.Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment is obtained, on the basis of lubricating grease weight, constitute and be：12- hydroxy stearic acids barium 12.4
Weight %；The weight % of decanedioic acid barium 11.5；The weight % of graphene 9.9；The weight % of lubricating base oil 65.9；The weight % of antioxidant 0.3.
Embodiment 3
The preparation be the same as Example 1 of graphene oxide.
The preparation of graphene：
Graphene oxide made from 0.1g is added to ultrasonic disperse in 100ml water（Ultrasonic frequency is 40kHz）30min
5ml hydrazine hydrates are added afterwards（Mass concentration is 85%）, 100 DEG C of oil bath reaction 24h, the black flocculent deposit finally obtained through washing,
The powder as graphene obtained after suction filtration, drying, the performance of graphene is as shown in table 2 below.
The preparation of composite barium-base grease：
Compound material component：Graphene 46g；PAO6 synthetic hydrocarbon oils 600g（100 DEG C of viscosity are 5.8mm2/s）；Eight water hydrogen-oxygens
Change barium 29.2g；Biphenyl dicarboxylic acid 10g；12- stearic acid 30.8g；4g antioxidant T501.
500 grams of base oils, 46 grams of graphenes, 30.8 grams of 12- hydroxy stearic acids and 10 grams of biphenyl dicarboxylic acids are added to system
In fat kettle, heating stirring, when temperature rises to 90 DEG C, starts to be slowly added to 29.2 grams of baryta waters, carries out compound soap
Change；220 DEG C are then heated to, 5min is kept；100 grams of base oils of addition, which are cooled to after 120 DEG C, to be added 4 grams of antioxidant T501 and stirs
Mix uniform, 2 times are ground into fat by three-roller.Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment is obtained, on the basis of lubricating grease weight, constitute and be：The weight of 12- hydroxy stearic acids barium 5.4
Measure %；The weight % of biphenyl dicarboxylic acid barium 2.2；The weight % of graphene 6.5；The weight % of lubricating base oil 85.3；The weight % of antioxidant 0.6.
Embodiment 4
The preparation be the same as Example 1 of graphene oxide.
The preparation of graphene：
Graphene oxide made from 0.1g is added to ultrasonic disperse in 100ml water（Ultrasonic frequency is 25kHz）30min
5ml hydrazine hydrates are added afterwards（Mass concentration is 85%）, 100 DEG C of oil bath reaction 24h, the black flocculent deposit finally obtained through washing,
The powder as graphene obtained after suction filtration, drying, the performance of graphene is as shown in table 2 below.
The preparation of composite barium-base grease：
Raw material components：Graphene 46g；150BS and 500SN miscella 600g（100 DEG C of viscosity are 14mm2/s）；Eight water
Barium hydroxide 81.2g；Benzoic acid 25g；Stearic acid 30g；4g antioxidant T501.
300 grams of base oils, 46 grams of graphenes, 30 grams of stearic acid and 25 grams of benzoic acid are added in fat kettle processed, heating is stirred
Mix, when temperature rises to 95 DEG C, start slowly to add 81.2 grams of barium hydroxides, carry out compound saponification；It is continuously heating to 210
DEG C, keep 5min；300 grams of base oils of addition, which are cooled to after 120 DEG C, to be added 4 grams of antioxidant T501 and stirs, and passes through three rollers
Machine grinds 3 times into fat.Properties of product are as shown in table 3.
In the lubricating grease that the present embodiment is obtained, on the basis of lubricating grease weight, constitute and be：The weight % of barium stearate 4.9；Benzene
The weight % of barium formate 10.2；The weight % of graphene 6.0；The weight % of lubricating base oil 78.4；The weight % of antioxidant 0.5.
Comparative example 1
Material component：In addition to not graphene-containing, remaining be the same as Example 4
Method according to embodiment 4 prepares composite barium-base grease, unlike, the preparation process of composite barium-base grease
In be added without graphene.Properties of product are as shown in table 3.
Comparative example 2
Raw material components be the same as Example 4
Method according to embodiment 4 prepares composite barium-base grease, unlike, whole graphenes are with antioxidant T501 mono-
Rise and add.Gained grease product performance is as shown in table 3.
Comparative example 3
Method according to embodiment 4 prepares composite barium-base grease, unlike, graphene by identical weight scale stone
Ink is replaced.Gained grease product performance is as shown in table 3.
Embodiment 5
Method according to embodiment 4 prepares composite barium-base grease, unlike, additive adds 12g dialkyl disulfides
For carbamic acid molybdenum, 4g antioxidant T501 and BTA fatty amine 4g.Gained grease product performance is as shown in table 3.
In the lubricating grease that the present embodiment is obtained, on the basis of lubricating grease weight, constitute and be：The weight % of barium stearate 4.8；Benzene
The weight % of barium formate 10.0；The weight % of graphene 5.9；The weight % of lubricating base oil 76.8；Molybdenum dialkyldithiocarbamacompositions 1.5
Weight %；The weight % of BTA fatty amine 0.5；The weight % of antioxidant 0.5.
Embodiment 6
Method according to embodiment 4 prepares composite barium-base grease, unlike, graphene is used commercially available from Beijing Ji'an
The model specification for believing science and trade Co., Ltd is G20 graphene product（Purity>95%, graphene size 100-200nm）,
Gained grease product performance is as shown in table 3.
Table 2
Table 3：PERFORMANCE OF GREASES
The composite barium-base grease that can be seen that the present invention from the result of above-mentioned table 3 has excellent heat-resisting quantity, water resistant
The performance such as property and adhesiveness, colloid stability, extreme pressure anti-wear, lubricating life, anticorrosive property and resistance to saltfog.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (15)
1. a kind of composite barium-base grease, it is characterised in that on the basis of lubricating grease weight, including following components：65-95%'s
Each component content sum is in lubricating base oil, 5-30% composite barium-base thickening agent, 0.2-15% graphene, lubricating grease
100%, the preparation method of the composite barium-base grease includes：Part basis oil, graphene, polymer acid and low molecular acid are mixed
Close, heat, be warming up to 80-105 DEG C, add barium hydroxide, carry out saponification, being warming up to 170-220 DEG C after reaction completely enters
Row refining, adds remaining base oil and is cooled to 100-130 DEG C, necessary additive is added afterwards, fat is milled into, obtains into
Product；Wherein described acid is polymer acid and the mixed acid of low molecular acid, and the polymer acid is the fat that carbon number is C12-C25
Fat acid and/or hydroxy fatty acid, the low molecular acid is the carboxylic acid that carbon number is 6-10.
2. composite barium-base grease according to claim 1, wherein, on the basis of lubricating grease weight, including following components：
70-93% lubricating base oil, 8-25% composite barium-base thickening agent, 1-10% graphene.
3. composite barium-base grease according to claim 1 or 2, wherein, the graphene can divide in 1ml base oils
Scattered and non-setting amount is 8-12mg.
4. composite barium-base grease according to claim 1 or 2, wherein, the particle diameter of the graphene is 80-800nm, electricity
Conductance is 700-900S/cm, and decomposition temperature is 430-480 DEG C.
5. composite barium-base grease according to claim 1 or 2, wherein, the time of the saponification is small for 0.5-1
When, the time of the refining is 5-10 minutes.
6. composite barium-base grease according to claim 1 or 2, wherein, the weight of the polymer acid and low molecular acid
Than for 1:0.1-1.
7. composite barium-base grease according to claim 1 or 2, wherein, the polymer acid be laurate, palmitic acid,
One or more in stearic acid, 12- hydroxy stearic acids；The low molecular acid is in terephthalic acid (TPA), azelaic acid, decanedioic acid
It is one or more.
8. composite barium-base grease according to claim 1 or 2, wherein, 100 DEG C of kinematic viscosity of the lubricating base oil
For 5-60mm2/s。
9. composite barium-base grease according to claim 1 or 2, wherein, the composite barium-base grease also contains 0.5-15
Weight % additive.
10. a kind of preparation method of composite barium-base grease, this method includes：
Part basis oil, graphene, polymer acid and low molecular acid are mixed, heated, 80-105 DEG C is warming up to, hydroxide is added
Barium, carries out saponification, and being warming up to 170-220 DEG C after reaction completely is refined, and adds remaining base oil and is cooled to 100-
130 DEG C, necessary additive is added afterwards, fat is milled into, finished product is obtained；Wherein described acid is polymer acid and low molecular acid
Mixed acid, the polymer acid is the aliphatic acid and/or hydroxy fatty acid that carbon number is C12-C25, and the low molecular acid is
Carbon number is 6-10 carboxylic acid；
Graphene, polymer acid, low molecular acid, the consumption of barium hydroxide and base oil cause gained composite barium-base grease, with
On the basis of lubricating grease weight, including following components：65-95% lubricating base oil, 5-30% composite barium-base thickening agent, 0.2-
Each component content sum is 100% in 15% graphene, lubricating grease.
11. preparation method according to claim 10, wherein, the time of the saponification is 0.5-1 hours, the refining
The time of system is 5-10 minutes.
12. the preparation method according to claim 10 or 11, wherein, the weight ratio of the polymer acid and low molecular acid is
1:0.1-1。
13. the preparation method according to claim 10 or 11, wherein, the polymer acid is laurate, palmitic acid, tristearin
One or more in acid, 12- hydroxy stearic acids；The low molecular acid is one kind in terephthalic acid (TPA), azelaic acid, decanedioic acid
Or it is a variety of.
14. the preparation method according to claim 10 or 11, wherein, the graphene can disperse in 1ml base oils
And non-setting amount is 8-12mg.
15. the preparation method according to claim 10 or 11, wherein, the particle diameter of the graphene is 80-800nm, conductance
Rate is 700-900S/cm, and decomposition temperature is 430-480 DEG C.
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| CN106590824B (en) * | 2015-10-15 | 2019-08-16 | 中国石油化工股份有限公司 | Composite barium-base grease and preparation method thereof |
| CN105219504A (en) * | 2015-10-23 | 2016-01-06 | 中国石油化工股份有限公司 | A kind of composite barium-base grease composition and method of making the same |
| CN109563429A (en) * | 2016-08-08 | 2019-04-02 | Nok克鲁勃株式会社 | Lubricant composition |
| WO2018196474A1 (en) | 2017-04-28 | 2018-11-01 | 杭州高烯科技有限公司 | Paper ball-like graphene microsphere, composite material thereof, and preparation method therefor |
| CN107033994A (en) * | 2017-05-03 | 2017-08-11 | 杭州高烯科技有限公司 | A kind of Ba-grease containing spitball shape graphene microballoon and preparation method thereof |
| CN113150858B (en) * | 2021-03-24 | 2022-08-19 | 苏州艾古新材料有限公司 | Composite barium-based lubricating grease and preparation method thereof |
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