CN104560290A - Composite barium-based lubricating grease composition and preparation method thereof - Google Patents
Composite barium-based lubricating grease composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite barium-based lubricating grease composition and a preparation method thereof. By taking the weight of the lubricating grease as a benchmark, the composite barium-based lubricating grease composition comprises the following components: 65-95% of lubricating base oil, 5-30% of a composite barium-based thickening agent and 0.2-15% of graphene. The composite barium-based lubricating grease has excellent high temperature resistance, water resistance, adhesion, colloidal stability, extreme pressure antiwear property, anti-corrosion property, salt and spray resistance and the like and long lubricating life.
Description
Technical field
The present invention relates to a kind of lubricant material, specifically relate to a kind of composite barium-base grease composition and method of making the same.
Background technology
Composite barium-base grease reacts by two or more acid and hydrated barta the medium-viscosity mineral oil that the compound barium soap multiviscosisty that generates refines to make, and has good water resisting property, higher dropping point and certain barrier propterty.Barium based grease-the ZB10-2 obtained by the synthetic oil for transformer cut of the low condensation point of barium stearate multiviscosisty; the water resisting property of this fat and resistance to pressure are all very strong; to the sticking power of metallic surface and protective value good; it is dissolved in the organic solvent such as gasoline and alcohol hardly simultaneously, is a kind of excellent waterproof, solvent resistant, protection and sealing material.
Also a lot of report is had both at home and abroad: as US2033148, US2417433A at large report the production method of composite barium-base grease to composite barium-base grease; CN102021067A has prepared one and has had better water resisting property and stopping property, cold resistance energy and rust-preventing characteristic good ships aluminium barium based grease; CN1160754A adopts oil based on high viscosity mineral oil, lipid acid and sebacic acid are viscosifying agent, aromatic amine and lithium salicylate are composite antioxidant, and add filler and rust-preventive agent to have adopted single stage method to prepare a kind of the multiple-effect composite barium-base grease with excellent high temperatures, oxidation stability, water resisting property and extreme pressure anti-wear.
In recent years in order to improve the performance of composite barium-base grease, in additive, have also been made large quantifier elimination, such as oxidation inhibitor, extreme pressure anti-wear additives, rust-preventive agent etc.Nano material gradually in the application of lubricating grease, as nano silicon, Nano diamond, nano titanium oxide, nano zine oxide etc., but does not still have the correlative study of the application of Graphene in lubricating grease so far yet.
Summary of the invention
The object of the present invention is to provide a kind of new composite barium-base grease and preparation method thereof.
The present inventor finds under study for action, Graphene is joined in base oil as the part of viscosifying agent, especially join in base oil in initial reaction stage and react with composite barium-base viscosifying agent one, generate the composite barium-base grease of graphene-containing, the composite barium-base grease obtained not only has good conductivity, and the method obviously can shorten the preparation time of composite barium-base grease.
An aspect of of the present present invention provides a kind of composite barium-base grease, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite barium-base viscosifying agent of 5-30%, the Graphene of 0.2-15%.
Under preferable case, with lubricating grease weight for benchmark, comprise following component: the lubricating base oil of 70-93%, the composite barium-base viscosifying agent of 8-25%, the Graphene of 1-10%.
A second aspect of the present invention provides a kind of preparation method of composite barium-base grease, and the method comprises: Graphene, composite barium-base viscosifying agent and part basis oil are mixed, 170-220 DEG C of constant temperature refining, cooling, add remaining base oil, add necessary additive, obtain finished product.
A third aspect of the present invention provides a kind of preparation method of composite barium-base grease, and the method comprises:
Part basis oil, Graphene, polymer acid and low molecular acid are mixed, heats, be warming up to 80-105 DEG C, add hydrated barta, carry out saponification reaction, be warming up to 170-220 DEG C after reacting completely, add remaining base oil and be cooled to 100-130 DEG C, add necessary additive afterwards, be milled into fat, obtain finished product; Wherein said acid is the mixing acid of polymer acid and low molecular acid, lipid acid and/or the hydroxy fatty acid of described polymer acid to be carbonatoms be C12-C25, the carboxylic acid of described low molecular acid to be carbonatoms be 6-10.
A fourth aspect of the present invention provides the obtained composite barium-base grease of aforesaid method.
Composite barium-base grease provided by the invention, there is high dropping point, good mechanical stability, higher oxidation-resistance, high-temperature and reversible, preferably pumping, excellent thermostability, water resisting property and colloid stability, and have good consistency with other lubricating grease.In addition, by the preliminary stage of Graphene at fat processed is added, Graphene is made to make viscosifying agent depend on the structure forming class micelle around it as nucleus, this synergy between Graphene and soap molecule enhances the ability of the molecules immobilized base oil of soap, greatly improve into fat speed, shorten saponification time, and make this fat can be competent in the lubrication of various motor, generator, gas blower, transportation, iron and steel enterprise and other various industrial equipments, be specially adapted to the lubrication at the friction position of mechanical means under various comparatively high temps wet condition.
Embodiment
An aspect of of the present present invention provides a kind of composite barium-base grease, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite barium-base viscosifying agent of 5-30%, the Graphene of 0.2-15%.
Under preferable case, with lubricating grease weight for benchmark, comprise following component: the lubricating base oil of 70-93%, the composite barium-base viscosifying agent of 8-25%, the Graphene of 1-10%.
In composite barium-base grease of the present invention, the consumption of Graphene can be larger, with composite barium-base viscosifying agent jointly as viscosifying agent, and unconventional conductive agent, gained composite barium-base grease is made to maintain the advantage of general composite barium-base grease on the one hand, as good colloid stability, high temperatures, low temperature properties, extreme pressure anti-wear etc., more improve its resistance of oxidation adding of Graphene simultaneously.On the other hand the preliminary stage of Graphene at fat processed is added, makes greatly to improve into fat speed, shorten saponification time, but also make the composite barium-base grease obtained can be competent in high temperature, at a high speed, the harsh working condition such as high loading, many water.
Graphene is a kind of novel material of the individual layer sheet structure be made up of carbon atom, be at present in the world the thinnest be the hardest nano material also, its thermal conductivity is up to 5300W/mK, higher than carbon nanotube and diamond, and its resistivity than copper or silver lower, be the material that at present resistivity is minimum in the world.Because Graphene is in fact a kind of transparent, good conductor, also be applicable to for manufacturing transparent touch screen, tabula rasa or even solar cell, it is widely used in the fields such as nanoelectronics, nano-complex, battery, ultracapacitor, hydrogen storage and biologic applications.
In the present invention, described Graphene can be the Graphene of existing all size, by commercially available, also can be obtained by existing various method.Under preferable case, described Graphene is obtained by the method comprised the following steps:
Graphite flakes and SODIUMNITRATE, the vitriol oil are mixed in ice bath, under stirring, slowly adds potassium permanganate, stirring reaction at 5-20 DEG C, be warming up to 30-45 DEG C and continue stirring reaction, then add deionized water dilution.In system, add superoxol reduction potassium permanganate, then obtain graphene oxide through pickling, washing, drying.Be added to the water by obtained graphene oxide after carrying out ultrasonication, add hydrazine hydrate, after oil bath sufficient reacting, the black flocks obtained is through washing, suction filtration, drying, and the powder finally obtained is Graphene.Hyperacoustic frequency is preferably 20-40kHz.
The Graphene (being called self-control Graphene) adopting aforesaid method to obtain has significant advantage with commercially available Graphene in size distribution, electroconductibility, stability and dispersiveness, and specific performance index sees the following form 1.
Table 1
| Commercially available Graphene | Self-control Graphene | |
| Particle diameter, nm | 100～3000 | 80～800 |
| Specific conductivity, S/cm | 500 | 700-900 |
| Decomposition temperature, DEG C | 410 | 430-480 |
| Can disperse and non-setting maximum in 1ml base oil, mg | 5 | 8-12 |
Whether note: base oil is following embodiment 1 base oil used, precipitate to disperse latter 60 minutes.Above-mentioned particle diameter adopts dynamic light scattering particle size analyser Dynapro Titan TC(producer: Wyatt Technology) record.Specific conductivity adopts Bel BEC-950 laboratory resistivity meter to record.Decomposition temperature adopts thermogravimetric analyzer SDT-Q600(producer: TA instrument company of the U.S.) record.Identical below.
Composite barium-base viscosifying agent of the present invention can be reacted by acid and hydrated barta and generate, described acid is the mixing acid of polymer acid and low molecular acid, lipid acid and/or the hydroxy fatty acid of described polymer acid to be carbonatoms be C12-C25, can be one or more mixtures in lauric acid, palmitinic acid, stearic acid, 12-oxystearic acid, preferred stearic acid, 12-oxystearic acid; The di-carboxylic acid of described low molecular acid can be carbonatoms be 6-10, is preferably the mixing acid of one or more in terephthalic acid, nonane diacid, sebacic acid.The weight ratio of polymer acid and low molecular acid is preferably 1:0.1-1.
The present invention's lubricating base oil used can be mineral oil, vegetables oil, synthetic oil or their mixture, and 100 DEG C of kinematic viscosity are 5-60mm
2/ s, preferred 10-30mm
2/ s.Vegetables oil can be Viscotrol C, rapeseed oil, peanut oil, soya-bean oil etc.Synthetic oil can be poly-a-olefin oil (PAO), Esters oil, fluorocarbon oil, silicone oil etc.
Can also various additive be contained, as oxidation inhibitor, extreme pressure anti-wear additives, rust-preventive agent etc. in lubricating grease of the present invention.Wherein, the preferred arylamine kind antioxidant of oxidation inhibitor, accounts for the 0.01-5% of lubricating grease gross weight, preferred 0.1-2.5%, can be at least one in pentanoic, phenyl-a-naphthylamine and di-iso-octyldiphenylamine, preferred di-iso-octyldiphenylamine.Extreme pressure anti-wear additives accounts for the 0.5-12% of lubricating grease gross weight, preferred 0.5-5% can be at least one in dithio Acidic phosphates zinc, dithio dialkyl amido formic acid molybdenum, dithio dialkyl amido lead formiate, triphenylphosphorothionate, organic molybdenum complex compound, olefine sulfide, molybdenumdisulphide, tetrafluoroethylene, thiophosphoric acid molybdenum, clorafin, dibutyl dithiocaarbamate antimony, tungsten disulfide, Selenium Sulfide, fluorographite, calcium carbonate and zinc oxide; Rust-preventive agent accounts for the 0.01-4.5% of lubricating grease gross weight, preferred 0.1-2%, can be at least one in barium mahogany sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid.
In the present invention, in grease composition, the content of each component calculates according to charging capacity.Wherein, content=100% × (weight of the weight+low molecular acid barium of polymer acid barium)/lubricating grease gross weight of composite barium-base viscosifying agent.
According to a second aspect of the invention, the invention provides a kind of preparation method of composite barium-base grease, the method comprises: Graphene, composite barium-base viscosifying agent and part basis oil are mixed, 170-220 DEG C of constant temperature refining, cooling, add remaining base oil, add necessary additive, obtain finished product.
Wherein, the consumption of Graphene, composite barium-base viscosifying agent and base oil makes the composite barium-base grease of gained, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite barium-base viscosifying agent of 5-30%, the Graphene of 0.2-15%.
Under preferable case, the consumption of Graphene, composite barium-base viscosifying agent and base oil makes gained composite barium-base grease, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 70-93%, the composite barium-base viscosifying agent of 8-25%, the Graphene of 1-10%.
According to a third aspect of the invention we, the invention provides a kind of preparation method of composite barium-base grease, the method comprises:
Base oil, Graphene, polymer acid and low molecular acid are mixed, heats, be warming up to 80-105 DEG C, add hydrated barta, carry out saponification reaction, be warming up to 170-220 DEG C after reacting completely, add remaining base oil and be cooled to 100-130 DEG C, add necessary additive afterwards, be milled into fat, obtain finished product.
The consumption of Graphene, polymer acid, low molecular acid, hydrated barta and base oil makes gained composite barium-base grease, with lubricating grease weight for benchmark, comprise following component: the lubricating base oil of 65-95%, the composite barium-base viscosifying agent of 5-30%, the Graphene of 0.2-15%.
Under preferable case, the consumption of Graphene, polymer acid, low molecular acid, hydrated barta and base oil makes gained composite barium-base grease, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 70-93%, the composite barium-base viscosifying agent of 8-25%, the Graphene of 1-10%.
Part basis oil is preferably 1/2-2/3:1/3-1/2 with the weight ratio of remaining base oil.
The total amount of polymer acid and low molecular acid and the mol ratio of hydrated barta are preferably stoichiometric ratio, and wherein the amount of hydrated barta also can excessive 1-10 % by weight.
The temperature that polymer acid, low molecular acid and hydrated barta carry out saponification reaction is preferably 80-105 DEG C, and the time is preferably 0.5-1 hour.
Refining temperature is preferably 170-220 DEG C, and the time is preferably 5-10 minute.
The difference that the preparation method of the composite barium-base grease that the preparation method of composite barium-base grease provided by the invention and prior art provide is main is that saponification reaction is carried out under Graphene exists, therefore about this preparation process other operation and condition can carry out with reference to prior art.
A preferred embodiment of the invention, composite barium-base grease provided by the invention can be prepared by the following method:
Graphene, polymer acid, low molecular acid are joined in the base oil of about 2/3, is uniformly mixed, heat temperature raising, when temperature rises to 80-105 DEG C, start slowly to add hydrated barta, carry out compound saponification reaction 0.5h-1h; When continuing to be heated to 170-220 DEG C, keep 5-10min; Add remaining base oil and be cooled to 100-130 DEG C, add additive, being milled by three-roller becomes fat 2-4 time.
Fourth aspect present invention provides by the obtained composite barium-base grease of above-mentioned third aspect method.
Compared with the composite barium-base grease obtained with the preparation method provided by second aspect, the composite barium-base grease that fourth aspect provides has better high thermal resistance, water resisting property and adhesivity, colloid stability and extreme pressure anti-wear.
In the present invention, in grease composition, the content of each component calculates according to charging capacity.Wherein, content=100% × (weight of the weight+low molecular acid barium of polymer acid barium)/lubricating grease gross weight of composite barium-base viscosifying agent.
The present invention is further illustrated for following embodiment, but therefore do not limit the present invention.In following examples, dropping point adopts GB/T3498 method to record, cone penetration adopts GB/T269 method to record, oxidation stability adopts SH/T0325 method to record, Stencil oil-dividing adopts SH/T0324 method to record, non-corrosibility adopts GB/T5018 method to record, water drenches number of dropouts and adopts SH/T0109 method to record, tetra-ball machine test PB adopts SH/T0202 method to record, tetra-ball machine test PD adopts SH/T0202 method to record, copper corrosion performance adopts GB/T7326 method to record, and electroconductibility adopts SH/T0596 method to record, and frictional coefficient adopts SH/T0847 to record.
Embodiment 1
The preparation of graphene oxide:
1g graphite flakes and 0.5g SODIUMNITRATE are mixed in ice bath with the 23ml vitriol oil, 3g potassium permanganate is slowly added under stirring, temperature remains on less than 10 DEG C and stirs 1h, then mixture stirs 0.5h at 35 DEG C, then adds the dilution of 50ml deionized water, releases a large amount of heat in process, carry out making temperature lower than 100 DEG C in ice bath, add 50ml water, mixture stirs 0.5h, then adds 200ml deionized water and dilute further.Add the aqueous hydrogen peroxide solution reduction potassium permanganate of 30 % by weight of 10ml afterwards.Finally, mixture mass concentration is hydrochloric acid (400ml) washing and filtering of 5%, to remove metal ion.Then acid is removed, 60 DEG C of dry 24h with 0.5L deionized water, obtained graphene oxide.
The preparation of Graphene:
5ml hydrazine hydrate (mass concentration is 85%) is added after above-mentioned for 0.1g obtained graphene oxide being joined ultrasonic disperse in 100ml water (ultrasonic frequency is 30kHz) 30min, oil bath 100 DEG C reaction 24h, the powder that the black flocks finally obtained obtains after washing, suction filtration, drying is Graphene, and the performance of Graphene is as shown in table 2 below.
The preparation of composite barium-base grease:
Feed composition: Graphene 15g; 500SN base oil 640g(100 DEG C of viscosity is 10mm
2/ s); Barium hydroxide 78.2g; Terephthalic acid 27.6g; 12-oxystearic acid 49.2g; Oxidation inhibitor T5018g.
430 grams of base oils, 15 grams of Graphenes and 49.2 grams of 12-oxystearic acids, 27.6 grams of terephthalic acids are joined in fat still processed, heated and stirred, when temperature rises to 85 DEG C, start slowly to add 78.2 grams of barium hydroxides, carry out compound saponification; Be warming up to 180 DEG C after having reacted, keep 5min; Add and add 8 grams of oxidation inhibitor T501 after 210 grams of base oils are cooled to 120 DEG C and stir, grind 2 times by three-roller and become fat.Product performance are as shown in table 3.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: 12-oxystearic acid barium 7.8 % by weight; Terephthalic acid barium 6.5 % by weight; Graphene 1.9 % by weight; Lubricating base oil 82.8 % by weight; Oxidation inhibitor 1.0 % by weight.
Embodiment 2
The preparation of graphene oxide is with embodiment 1.
The preparation of Graphene:
5ml hydrazine hydrate (mass concentration is 85%) is added after the graphene oxide that 0.1g is obtained is joined ultrasonic disperse in 100ml water (ultrasonic frequency is 35kHz) 30min, oil bath 100 DEG C reaction 24h, the powder that the black flocks finally obtained obtains after washing, suction filtration, drying is Graphene, and the performance of Graphene is as shown in table 2 below.
The preparation of composite barium-base grease:
Feed composition: Graphene 30g; 150BS base oil 200g(100 DEG C of viscosity is 31mm
2/ s); Barium hydroxide 48.9g; Sebacic acid 21g; 12-oxystearic acid 30.8g; Oxidation inhibitor di-iso-octyldiphenylamine 1g.
100 grams of base oils, 30 grams of Graphenes, 30.8 grams of 12-oxystearic acids and 21 grams of sebacic acid are joined in fat still processed, heated and stirred, when temperature rises to 105 DEG C, start slowly to add 48.9 grams of barium hydroxides, carry out compound saponification; Then be warming up to 210 DEG C, keep 5min; Add and add 1 gram of oxidation inhibitor di-iso-octyldiphenylamine after 100 grams of base oils are cooled to 90 DEG C and stir, grind 3 times by three-roller and become fat.Product performance are as shown in table 3.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: 12-oxystearic acid barium 12.4 % by weight; Sebacic acid barium 11.5 % by weight; Graphene 9.9 % by weight; Lubricating base oil 65.9 % by weight; Oxidation inhibitor 0.3 % by weight.
Embodiment 3
The preparation of graphene oxide is with embodiment 1.
The preparation of Graphene:
5ml hydrazine hydrate (mass concentration is 85%) is added after the graphene oxide that 0.1g is obtained is joined ultrasonic disperse in 100ml water (ultrasonic frequency is 40kHz) 30min, oil bath 100 DEG C reaction 24h, the powder that the black flocks finally obtained obtains after washing, suction filtration, drying is Graphene, and 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 oil 600g(100 DEG C of viscosity is 5.8mm
2/ s); Barium hydroxide 29.2g; Biphenyl dicarboxylic acid 10g; 12-stearic acid 30.8g; 4g oxidation inhibitor T501.
500 grams of base oils, 46 grams of Graphenes, 30.8 grams of 12-oxystearic acids and 10 grams of biphenyl dicarboxylic acids are joined in fat still processed, heated and stirred, when temperature rises to 90 DEG C, start slowly to add 29.2 grams of baryta waters, carry out compound saponification; Then be warming up to 220 DEG C, keep 5min; Add and add 4 grams of oxidation inhibitor T501 after 100 grams of base oils are cooled to 120 DEG C and stir, grind 2 times by three-roller and become fat.Product performance are as shown in table 3.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: 12-oxystearic acid barium 5.4 % by weight; Biphenyl dicarboxylic acid barium 2.2 % by weight; Graphene 6.5 % by weight; Lubricating base oil 85.3 % by weight; Oxidation inhibitor 0.6 % by weight.
Embodiment 4
The preparation of graphene oxide is with embodiment 1.
The preparation of Graphene:
5ml hydrazine hydrate (mass concentration is 85%) is added after the graphene oxide that 0.1g is obtained is joined ultrasonic disperse in 100ml water (ultrasonic frequency is 25kHz) 30min, oil bath 100 DEG C reaction 24h, the powder that the black flocks finally obtained obtains after washing, suction filtration, drying is Graphene, and the performance of Graphene is as shown in table 2 below.
The preparation of composite barium-base grease:
Feed composition: Graphene 46g; The mixing oil 600g(100 DEG C viscosity of 150BS and 500SN is 14mm
2/ s); Barium hydroxide 81.2g; Phenylformic acid 25g; Stearic acid 30g; 4g oxidation inhibitor T501.
300 grams of base oils, 46 grams of Graphenes, 30 grams of stearic acid and 25 grams of phenylformic acid are joined in fat still processed, heated and stirred, when temperature rises to 95 DEG C, start slowly to add 81.2 grams of barium hydroxides, carry out compound saponification; Continue to be warming up to 210 DEG C, keep 5min; Add and add 4 grams of oxidation inhibitor T501 after 300 grams of base oils are cooled to 120 DEG C and stir, grind 3 times by three-roller and become fat.Product performance are as shown in table 3.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: barium stearate 4.9 % by weight; Barium dibenzoate 10.2 % by weight; Graphene 6.0 % by weight; Lubricating base oil 78.4 % by weight; Oxidation inhibitor 0.5 % by weight.
Comparative example 1
Material component: except not graphene-containing, all the other are with embodiment 4
Composite barium-base grease is prepared according to the method for embodiment 4, unlike, do not add Graphene in the preparation process of composite barium-base grease.Product performance are as shown in table 3.
Comparative example 2
Feed composition is with embodiment 4
Composite barium-base grease is prepared according to the method for embodiment 4, unlike, whole Graphene adds with oxidation inhibitor T501.Gained grease product performance is as shown in table 3.
Comparative example 3
Composite barium-base grease is prepared according to the method for embodiment 4, unlike, Graphene is replaced by the crystalline flake graphite of identical weight.Gained grease product performance is as shown in table 3.
Embodiment 5
Prepare composite barium-base grease according to the method for embodiment 4, add 12g molybdenum dialkyldithiocarbamacompositions, the oxidation inhibitor T501 of 4g and benzotriazole aliphatic amide 4g unlike, additive.Gained grease product performance is as shown in table 3.
In the lubricating grease that the present embodiment obtains, with lubricating grease weight for benchmark, consist of: barium stearate 4.8 % by weight; Barium dibenzoate 10.0 % by weight; Graphene 5.9 % by weight; Lubricating base oil 76.8 % by weight; Molybdenum dialkyldithiocarbamacompositions 1.5 % by weight; Benzotriazole aliphatic amide 0.5 % by weight; Oxidation inhibitor 0.5 % by weight.
Embodiment 6
Composite barium-base grease is prepared according to the method for embodiment 4, unlike, Graphene uses to be purchased believes from Ji'an, Beijing graphene product (the purity >95% that the model specification of science and trade limited liability company is G20, Graphene size 100-200nm), gained grease product performance is as shown in table 3.
Table 2
Table 3: PERFORMANCE OF GREASES
As can be seen from the result of above-mentioned table 3, composite barium-base grease of the present invention has the performances such as excellent high thermal resistance, water resisting property and adhesivity, colloid stability, extreme pressure anti-wear, lubricating life, non-corrosibility and resistance to salt(spray)fog.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (17)
1. a composite barium-base grease, is characterized in that, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite barium-base viscosifying agent of 5-30%, the Graphene of 0.2-15%.
2. composite barium-base grease according to claim 1, wherein, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 70-93%, the composite barium-base viscosifying agent of 8-25%, the Graphene of 1-10%.
3. composite barium-base grease according to claim 1 and 2, wherein, described Graphene can disperse in 1ml base oil and non-setting maximum is 8-12mg.
4. according to the composite barium-base grease in claim 1-3 described in any one, wherein, the particle diameter of described Graphene is 80-800nm, and specific conductivity is 700-900S/cm, and decomposition temperature is 430-480 DEG C.
5. composite barium-base grease according to claim 1 and 2, wherein, described composite barium-base viscosifying agent is reacted by acid and hydrated barta and generates, described acid is the mixing acid of polymer acid and low molecular acid, lipid acid and/or the hydroxy fatty acid of described polymer acid to be carbonatoms be C12-C25, the carboxylic acid of described low molecular acid to be carbonatoms be 6-10.
6. composite barium-base grease according to claim 5, wherein, the weight ratio of described polymer acid and low molecular acid is 1:0.1-1.
7. the composite barium-base grease according to claim 5 or 6, wherein, described polymer acid is one or more in lauric acid, palmitinic acid, stearic acid, 12-oxystearic acid; Described low molecular acid is one or more in terephthalic acid, nonane diacid, sebacic acid.
8. according to the composite barium-base grease in claim 1-7 described in any one, wherein, 100 DEG C of kinematic viscosity of described lubricating base oil are 5-60mm
2/ s.
9. according to the composite barium-base grease in claim 1-8 described in any one, wherein, the additive of this composite barium-base grease also containing 0.5-15 % by weight.
10. a preparation method for composite barium-base grease, the method comprises:
Part basis oil, Graphene, polymer acid and low molecular acid are mixed, heats, be warming up to 80-105 DEG C, add hydrated barta, carry out saponification reaction, be warming up to 170-220 DEG C after reacting completely to refine, add remaining base oil and be cooled to 100-130 DEG C, add necessary additive afterwards, be milled into fat, obtain finished product; Wherein said acid is the mixing acid of polymer acid and low molecular acid, lipid acid and/or the hydroxy fatty acid of described polymer acid to be carbonatoms be C12-C25, the carboxylic acid of described low molecular acid to be carbonatoms be 6-10.
11. preparation methods according to claim 10, wherein, the time of described saponification reaction is 0.5-1 hour, and the time of described refining is 5-10 minute.
12. preparation methods according to claim 10 or 11, wherein, the consumption of Graphene, polymer acid, low molecular acid, hydrated barta and base oil makes gained composite barium-base grease, with lubricating grease weight for benchmark, comprise following component: the lubricating base oil of 65-95%, the composite barium-base viscosifying agent of 5-30%, the Graphene of 0.2-15%.
13. according to the preparation method in claim 10-12 described in any one, and wherein, the weight ratio of described polymer acid and low molecular acid is 1:0.1-1.
14. according to the preparation method in claim 10-13 described in any one, and wherein, described polymer acid is one or more in lauric acid, palmitinic acid, stearic acid, 12-oxystearic acid; Described low molecular acid is one or more in terephthalic acid, nonane diacid, sebacic acid.
15. according to the preparation method in claim 10-14 described in any one, and wherein, described Graphene can disperse in 1ml base oil and non-setting maximum is 8-12mg.
16. according to the preparation method in claim 10-15 described in any one, and wherein, the particle diameter of described Graphene is 80-800nm, and specific conductivity is 700-900S/cm, and decomposition temperature is 430-480 DEG C.
The composite barium-base grease that preparation method in 17. claim 10-16 described in any one obtains.
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Cited By (6)
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| 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 |
| CN106590824A (en) * | 2015-10-15 | 2017-04-26 | 中国石油化工股份有限公司 | Composite barium-based lubricating grease and preparation method thereof |
| 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 |
| CN109563429A (en) * | 2016-08-08 | 2019-04-02 | Nok克鲁勃株式会社 | Lubricant composition |
| CN113150858A (en) * | 2021-03-24 | 2021-07-23 | 苏州艾古新材料有限公司 | Composite barium-based lubricating grease and preparation method thereof |
| US11225414B2 (en) | 2017-04-28 | 2022-01-18 | Hangzhou Gaoxi Technology Co., Ltd. | Paper ball-like graphene microsphere, composite material thereof, and preparation method therefor |
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| CN106590824A (en) * | 2015-10-15 | 2017-04-26 | 中国石油化工股份有限公司 | Composite barium-based lubricating grease and preparation method thereof |
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| CN113150858A (en) * | 2021-03-24 | 2021-07-23 | 苏州艾古新材料有限公司 | Composite barium-based lubricating grease and preparation method thereof |
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