CN104560315B - A kind of composite sodium-based lubricating grease and preparation method thereof - Google Patents
A kind of composite sodium-based lubricating grease and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of composite sodium-based lubricating grease and preparation method thereof.On the basis of lubricating grease weight, the composite sodium-based lubricating grease includes following components：65 95% lubricating base oil, 5 30% composite sodium-based thickening agent, 0.2 15% graphene.The composite sodium-based lubricating grease of the present invention 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 sodium-based lubricating grease and its preparation side the present invention relates to a kind of lubricant material
Method.
Background technology
The acid compound or its salt class of a small amount of low molecule is introduced in sodium base grease can obtain dropping point higher than simple soda soap
Composite sodium-based lubricating grease.As added a small amount of salicylic acid soda soap in fatty acid sodium soap lubricating grease and being heated to 257 DEG C, sodium base can be made
Grease dropping point is raised.0.1-5% acrylic acid sodium salts are added in the lubricating grease containing 5-35% fatty acid sodium soaps simultaneously, can be dropped
Solubility of the low soda soap in water such as US2468098；Morway et al. has found that methacrylaldehyde and its derivative also may be used in US2591586
Composite sodium-based lubricating grease is prepared with polymer acid.The solid powder that different-grain diameter is distributed is added to lubricating grease by CN101153236A
In, the water repelling property of lubricating grease is not only increased, extreme pressure anti-wear is also improved；CN1557922A passes through into sodium base grease
Addition clean water is prepared for the aqueous sodium base grease containing 8-30% clean waters, and the fat is a kind of substantially pollution-free to environment, profit
Sliding effect is good, high lubricating effect substantially pollution-free to friction pair, has thermal balance to act on and with low cost can fit to friction pair
Lubriation material for heavy load sliding bearing；CN102021068A is prepared for a kind of sodium aluminate soap grease for ship, it is adaptable to
Marine propeller and Floating Crane and dredger, more than 75 DEG C of dropping point, with good water-resistance, protective and rust-preventing characteristic,
Existing proper lubrication effect, there is corrosion-resisting function again, and with the function of lowering mechanicalness noise.
In recent years in order to improve the performance of composite sodium-based lubricating 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 sodium-based lubricating grease and preparation method thereof.
The present inventor has found under study for action, using graphene as thickening agent a part especially in initial reaction stage
It is added in base oil, the composite sodium-based lubricating grease for the generation graphene-containing that reacted with composite sodium-based thickening agent one is resulting
Composite sodium-based lubricating grease not only has good electric conductivity, and this method can substantially shorten the system of composite sodium-based lubricating grease
The standby time.
An aspect of of the present present invention provides a kind of composite sodium-based lubricating grease, on the basis of lubricating grease weight, including with the following group
Point：65-95% lubricating base oil, 5-30% composite sodium-based thickening agent, 0.2-15% graphene.
Under preferable case, on the basis of lubricating grease weight, including following components：70-90% lubricating base oil, 8-25%'s
Composite sodium-based thickening agent, 1-10% graphene.
The second aspect of the present invention provides a kind of composite sodium-based preparation of greases method, and this method includes：By graphite
Alkene, composite sodium-based thickening agent and part basis oil are well mixed, and in 180-230 DEG C of constant temperature refining, cooling adds surplus basis
Oil, adds necessary additive, obtains finished product.
The third aspect of the present invention provides a kind of composite sodium-based preparation of greases method, and this method includes：
Graphene, base oil, polymer acid are mixed, heated, 80-105 DEG C is warming up to, sodium hydroxide is added, soap is carried out
Change reaction, then add low molecular acid and be combined, be warming up to 200-220 DEG C, add remaining base oil and be cooled to 90-130
DEG C, necessary additive is added afterwards, fat is milled into, and obtains finished product.
The fourth aspect of the present invention provides composite sodium-based lubricating grease made from the above method.
The composite sodium-based lubricating grease that the present invention is provided, the oxidation resistance with raising, high dropping point, good machinery are stabilized
Property, high-temperature and reversible, preferable pumping, excellent heat endurance, water-resistance and colloid stability, and have with other lubricating grease
Good compatibility.By the graphene when the preliminary stage of fat processed is added, it causes thickening agent to depend on its week as nucleus
The structure to form class micelle is enclosed, this synergy between graphene and soap molecule enhances the energy of the molecules immobilized base oil of soap
Power, greatly improves into fat speed, shortens saponification time.The fat is enabled to be competent in various motors, generator, air blast
Machine, transportation, the lubrication of iron and steel enterprise and other various industrial equipments, are particularly suitable for use in various higher temperature wet conditions
The lubrication of the friction part of lower plant equipment.
Embodiment
An aspect of of the present present invention provides a kind of composite sodium-based lubricating grease, on the basis of lubricating grease weight, including with the following group
Point：65-95% lubricating base oil, 5-30% composite sodium-based thickening agent, 0.2-15% graphene.
Under preferable case, on the basis of lubricating grease weight, including following components：70-90% lubricating base oil, 8-25%'s
Composite sodium-based thickening agent, 1-10% graphene.
The present invention composite sodium-based lubricating grease in, the large usage quantity of graphene, with composite sodium-based thickening agent collectively as
Thickening agent, and unconventional conductive agent, on the one hand cause the composite sodium-based lubricating grease of gained to maintain the excellent of general sodium base grease
Point, such as good colloid stability, high temperatures, low temperature properties, extreme pressure anti-wear resist while the addition of graphene more improves it
Oxidability.On the other hand added so that greatly improve into fat speed, shortened by the preliminary stage by graphene in fat processed
Saponification time, so that can be competent in high temperature, high speed, high load capacity, many water etc. severe for obtained composite sodium-based lubricating grease
Carve 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 the ultrasonic wave is preferably 25-40kHz.
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：Above-mentioned base oil is base oil used in following embodiments 1, if precipitation is after disperseing in terms of 60 minutes.Above-mentioned grain
Footpath uses dynamic light scattering particle size analyzer Dynapro Titan TC（Producer：Wyatt Technology）Measure.Electrical conductivity
Measured using Bel BEC-950 laboratories resistivity meter.Decomposition temperature uses thermogravimetric analyzer SDT-Q600（Producer：U.S. TA
Instrument companies）Measure.It is same as below.
The composite sodium-based thickening agent of the present invention can be reacted by acid with sodium 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 carboxylic acid that carbon number is 4-12, preferably benzoic acid, terephthalic acid (TPA), adipic acid, nonyl
One or more of mixed acid in diacid, decanedioic acid.The mol ratio of polymer acid and low molecular acid is preferably 1:0.1-2.
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.During vegetable oil can be castor oil, rapeseed oil, peanut oil, soya-bean oil etc.
It is one or more.Artificial oil can be poly-a-olefin oil（PAO）, Esters oil, fluorocarbon oil, the one or more in 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.The present invention
In, the content of composite sodium-based each composition of lubricating grease is determined according to inventory calculating, wherein, the content of composite sodium-based thickening agent=
100%×（The weight of the weight of polymer acid sodium+low molecular acid sodium）/ lubricating grease gross weight.
According to the second aspect of the invention, the invention provides a kind of composite sodium-based preparation of greases method, this method
Including：Graphene, composite sodium-based thickening agent and part basis oil is well mixed, in 180-230 DEG C of constant temperature refining, cool down, plus
Enter surplus base oil, add necessary additive, obtain finished product.
Wherein, graphene, composite sodium-based thickening agent, the consumption of base oil cause the composite sodium-based lubricating grease of gained, to moisten
On the basis of consistent lubricant weight, including following components：65-95% lubricating base oil, 5-30% composite sodium-based thickening agent, 0.2-15%
Graphene.
Under preferable case, graphene, composite sodium-based thickening agent, the consumption of base oil cause the composite sodium-based lubrication of gained
Fat, on the basis of lubricating grease weight, including following components：70-90% lubricating base oil, 8-25% composite sodium-based thickening agent,
1-10% graphene.
According to the third aspect of the invention we, the invention provides a kind of composite sodium-based preparation of greases method, this method
Including：
Graphene, part basis oil, polymer acid are mixed, heated, 80-105 DEG C is warming up to, adds sodium hydroxide, enter
Row saponification, then adds low molecular acid and is combined, be warming up to 200-220 DEG C, adds remaining base oil and is cooled to 90-
130 DEG C, necessary additive is added afterwards, fat is milled into, finished product is obtained.
Wherein, the temperature of the saponification is preferably 80-105 DEG C, saponification and low molecule that polymer acid is carried out
The time for the saponification that acid is carried out is both preferably 1-3 hours.
The sodium hydroxide preferably uses liquid caustic soda.
The time of the refining is preferably 5-25 minutes.
Wherein, graphene, composite sodium-based thickening agent, the consumption of base oil cause the composite sodium-based lubricating grease of gained, to moisten
On the basis of consistent lubricant weight, including following components：65-95% lubricating base oil, 5-30% composite sodium-based thickening agent, 0.2-15%
Graphene.
Under preferable case, graphene, composite sodium-based thickening agent, the consumption of base oil cause the composite sodium-based lubrication of gained
Fat, on the basis of lubricating grease weight, including following components：70-90% lubricating base oil, 8-25% composite sodium-based thickening agent,
1-10% graphene.
Part basis oil：Remaining base oil=50-75:25-50.
The mol ratio of polymer acid and low molecular acid is 1：0.1-2.
A preferred embodiment of the invention, the lubricating grease that the present invention is provided can be prepared by the following method：
Graphene, 2/3 or so base oil and polymer acid are added in fat kettle processed, stirring is warming up to 80-90 DEG C, addition
Liquid caustic soda, is warming up to 100-110 DEG C of saponification 1h-3h, adds low molecular acid saponification 1h-3h；Continue the dehydration that heats up, treat
5-20min is kept after rising to 200-220 DEG C of highest refining temperature；Adding remaining base oil and being put into cooler pan makes it quickly cool down
Additive is added during to 80-100 DEG C, 2-4 times is milled into fat by three-roller.
The composite sodium-based lubricating grease that the composite sodium-based preparation of greases method 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.
Fourth aspect present invention provides the composite sodium-based lubricating grease as made from the preparation method of the above-mentioned third aspect.
Compared with the composite sodium-based lubricating grease as made from the preparation method that second aspect is provided, it is compound that fourth aspect is provided
Sodium base grease has more preferable heat-resisting quantity, water-resistance and adhesiveness, colloid stability and extreme pressure anti-wear.
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.
Composite sodium-based preparation of greases：
Raw material components：Graphene 10.4g；500SN base oils 720g（100 DEG C of viscosity are 10mm2/s）；Sodium hydroxide
11.28g；Benzoic acid 16.84g；12- hydroxy stearic acids 41.14g；Antioxidant T5015.6g；By 10.4 grams of graphenes, 540 grams of bases
Plinth oil and 41.14 grams of 12- hydroxy stearic acids are added in fat kettle processed, and heating stirring, when temperature rises to 80 DEG C, adds and contains 11.28 grams
After the alkali lye of sodium hydroxide, saponification 0.1h；16.84 grams of benzoic acid saponification 0.1h are added into system again；It is warming up to
5min is kept after 190 DEG C；Add 180 grams of base oils and be put into cooler pan 5.6 grams of addition when making it rapidly cooling to 100 DEG C and resist
Oxygen agent T501 is simultaneously stirred, and 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- hydroxyl sodium stearates 5.5
Measure %；The weight % of sodium benzoate 2.5；The weight % of graphene 1.3；The weight % of lubricating base oil 90；The weight % of antioxidant 0.7.
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.
Composite sodium-based preparation of greases：
Raw material components：Graphene 31.2g；150BS base oils 420g（100 DEG C of viscosity are 31mm2/s）；Sodium hydroxide
23.26g；Terephthalic acid (TPA) 13.40g；12- hydroxy stearic acids 121.18g；Di-iso-octyldiphenylamine 1.8g；
31.2 grams of graphenes, 210 grams of base oils and 121.18 grams of 12- hydroxy stearic acids are added in fat kettle processed, heating is stirred
Mix, when temperature rises to 90 DEG C, add after the alkali lye containing 23.26 grams of sodium hydroxides, saponification 0.1h；Added again into system
13.40 grams of terephthalic acid (TPA) saponification 0.1h；15min is kept after being warming up to 200 DEG C；Add 210 grams of base oils and be put into cold
1.8 grams of di-iso-octyldiphenylamines are added when but making it rapidly cooling to 110 DEG C in disk to stir, and are ground 3 times by three-roller
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：12- hydroxyl sodium stearates 21.68
Weight %；The weight % of para-phthalic sodium 2.82；The weight % of graphene 5.2；The weight % of lubricating base oil 70；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.
Composite sodium-based preparation of greases：
Raw material components：Graphene 60g；PAO6 synthetic hydrocarbon oils 444g（100 DEG C of viscosity are 5.8mm2/s）；Sodium hydroxide
17.26g；Decanedioic acid 21.19g；Stearic acid 59.6g；Phenyl-α-naphthylamine 6g；
60 grams of graphenes, 296 grams of base oils and 59.6 grams of stearic acid are added in fat kettle processed, heating stirring, when temperature liter
To 100 DEG C, the alkali lye containing 17.26 grams of sodium hydroxides, saponification 0.1h are added；21.19 grams of last of the ten Heavenly stems are added into system again
Diacid saponification 0.1h；5min is kept after being warming up to 210 DEG C；Add 148 grams of base oils and being put into cooler pan makes its fast
6 grams of phenyl-α-naphthylamines are added when speed is cooled to 120 DEG C and are stirred, 3 times are ground into fat by three-roller.Properties of product are such 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 odium stearate 10.7；The last of the ten Heavenly stems
The weight % of diacid sodium 4.3；The weight % of graphene 10；The weight % of lubricating base oil 74；The weight % of antioxidant 1.
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
For 25kHz）5ml hydrazine hydrates are added after 30min（Mass concentration is 85%）, 100 DEG C of reaction 24h of oil bath, the black wadding finally obtained
The powder as graphene that shape precipitation is obtained after washing, suction filtration, drying, the performance of graphene is as shown in table 2 below.
Composite sodium-based preparation of greases：
Raw material components：Graphene 56g；150BS and 500SN miscella 644g（100 DEG C of viscosity are 14mm2/s）；Hydrogen-oxygen
Change sodium 19.89g；Benzoic acid 39.59g；Stearic acid 45.79g；Antioxidant T5014g；
56 grams of graphenes, 444 grams of base oils and 45.79 grams of stearic acid are added in fat kettle processed, heating stirring, when temperature liter
To 95 DEG C, the alkali lye containing 19.89 grams of sodium hydroxides, saponification 0.1h are added；39.59 grams of benzoic acid soaps are added into system again
Change reaction 0.1h；10min is kept after being warming up to 200 DEG C；Add 200 grams of base oils and being put into cooler pan makes it quickly cool down
To adding 4 grams of antioxidant T501 at 115 DEG C and stirring, 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 odium stearate 10.7；The last of the ten Heavenly stems
The weight % of diacid sodium 4.3；The weight % of graphene 10；The weight % of lubricating base oil 74；The weight % of antioxidant 1.
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 sodium-based lubricating grease, unlike, composite sodium-based preparation of greases process
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 sodium-based lubricating grease, unlike, whole graphenes are with antioxidant T501 mono-
Rise and add.Properties of product are as shown in table 3.
Comparative example 3
Method according to embodiment 4 prepares composite sodium-based lubricating grease, unlike, graphene by identical weight scale stone
Ink is replaced.Properties of product are as shown in table 3.
Embodiment 5
The preparation be the same as Example 1 of graphene
Material component：Be the same as Example 4
444 grams of base oils and 45.79 grams of stearic acid are added in fat kettle processed, heating stirring, when temperature rises to 95 DEG C, addition
Alkali lye containing 19.89 grams of sodium hydroxides, saponification 0.1h；39.59 grams of benzoic acid saponification 0.1h are added into system；Again
56 grams of graphenes are added into system, 10min is kept after being warming up to 200 DEG C；Add 200 grams of base oils and be put into cooler pan
4 grams of antioxidant T501 are added when making it rapidly cooling to 115 DEG C and are stirred, 2 times are ground into fat by three-roller.Product
Can be as shown in table 3.
Embodiment 6
Method according to embodiment 4 prepares composite sodium-based lubricating 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 sodium-based lubricating 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 sodium-based lubricating grease, it is characterised in that on the basis of lubricating grease weight, including following components：65-95%'s
Lubricating base oil, 5-30% composite sodium-based thickening agent, 0.2-15% graphene, the composite sodium-based preparation of greases method
Including：Graphene, base oil are mixed with polymer acid, heated, 80-105 DEG C is warming up to, sodium hydroxide is added, saponification is carried out
Reaction, then adds low molecular acid and is combined, be warming up to 200-220 DEG C, add remaining base oil and be cooled to 90-130 DEG C,
Necessary additive is added afterwards, fat is milled into, finished product is obtained, and the polymer acid is the fat that carbon number is C12-C25
Acid and/or hydroxy fatty acid, the low molecular acid is the carboxylic acid that carbon number is C4-C12.
2. composite sodium-based lubricating grease according to claim 1, wherein, on the basis of lubricating grease weight, including following components：
70-90% lubricating base oil, 8-25% composite sodium-based thickening agent, 1-10% graphene.
3. composite sodium-based lubricating grease according to claim 1 or 2, wherein, the graphene can divide in 1ml base oils
Scattered and non-setting maximum is 8-12mg.
4. composite sodium-based lubricating 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 sodium-based lubricating grease according to claim 1 or 2, wherein, the temperature of the saponification is 80-105 DEG C,
The time for the saponification that the saponification and low molecular acid that polymer acid is carried out are carried out is 1-3 hours.
6. composite sodium-based lubricating grease according to claim 1 or 2, wherein, the polymer acid with low molecular acid with rubbing
You are than being 1:0.1-2.
7. composite sodium-based lubricating 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 benzoic acid, terephthalic acid (TPA), azelaic acid, the last of the ten Heavenly stems
One or more in diacid.
8. composite sodium-based lubricating 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 sodium-based lubricating grease according to claim 1 or 2, wherein, the composite sodium-based lubricating grease also contains 0.5-15
Weight % additive.
10. a kind of composite sodium-based preparation of greases method, this method includes：
Graphene, base oil are mixed with polymer acid, heated, 80-105 DEG C is warming up to, sodium hydroxide is added, saponification is carried out anti-
Should, then add low molecular acid and be combined, be warming up to 200-220 DEG C, add remaining base oil and be cooled to 90-130 DEG C, it
After add necessary additive, be milled into fat, obtain finished product, the polymer acid is the aliphatic acid that carbon number is C12-C25
And/or hydroxy fatty acid, the low molecular acid is the carboxylic acid that carbon number is C4-C12；
Graphene, base oil, polymer acid, the consumption of sodium hydroxide and low molecular acid cause the composite sodium-based lubricating grease of gained,
On the basis of lubricating grease weight, including following components：65-95% lubricating base oil, 5-30% composite sodium-based thickening agent,
0.2-15% graphene.
11. preparation method according to claim 10, wherein, the temperature of the saponification is 80-105 DEG C, macromolecule
The time for the saponification that the saponification and low molecular acid that acid is carried out are carried out is 1-3 hours.
12. the preparation method according to claim 10 or 11, wherein, with molar ratio computing, polymer acid：Low molecular acid=1：
0.1-2。
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 benzoic acid, terephthalic acid (TPA), azelaic acid, decanedioic acid
In one or more.
14. the preparation method according to claim 10 or 11, wherein, the graphene can disperse in 1ml base oils
And non-setting maximum 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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| CN105087125A (en) * | 2015-08-11 | 2015-11-25 | 新乡市恒星化工有限责任公司 | Method for preparing lubricating grease special for engineering mechanical equipment |
| CN106590820B (en) * | 2015-10-15 | 2019-08-16 | 中国石油化工股份有限公司 | Sodium base grease and preparation method thereof |
| CN106590823B (en) * | 2015-10-15 | 2019-08-16 | 中国石油化工股份有限公司 | Composite sodium-based lubricating grease and preparation method thereof |
| CN107287012A (en) * | 2017-06-21 | 2017-10-24 | 长兴德烯科技有限公司 | A kind of composite sodium-based lubricating grease containing spitball shape graphene microballoon and preparation method thereof |
| CN107384559B (en) * | 2017-08-01 | 2020-07-14 | 太原理工大学 | Layered potassium magnesium phosphate sodium-based lubricating grease composition and preparation method thereof |
| CN112048354A (en) * | 2020-09-23 | 2020-12-08 | 上海虎头化工有限公司 | Long-acting high-temperature lubricating grease and preparation method thereof |
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| CN1283766C (en) * | 2004-02-09 | 2006-11-08 | 张义伦 | Lubricant for heavy-duty slide bearing |
| JP5330773B2 (en) * | 2008-07-07 | 2013-10-30 | 昭和シェル石油株式会社 | Grease composition for resin lubrication |
| US8222190B2 (en) * | 2009-08-19 | 2012-07-17 | Nanotek Instruments, Inc. | Nano graphene-modified lubricant |
| CN103289802A (en) * | 2013-06-05 | 2013-09-11 | 扬州大学 | Preparation method of graphene lubricating grease |
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