CN104560315A - Composite sodium-based lubricating grease and preparation method thereof - Google Patents
Composite sodium-based lubricating grease and preparation method thereof Download PDFInfo
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Abstract
The invention discloses composite sodium-based lubricating grease and a preparation method thereof. By the weight of the lubricating grease, the compound sodium-based lubricating grease comprises the following components: 65-95% of lubricating base oil, 5-30% of a composite sodium-based thickener and 0.2-15% of graphene. The composite sodium-based lubricating grease disclosed by the invention has excellent properties such as high temperature resistance, water resistance, adhesivity, colloid stability, extreme pressure antiwear property, long lubricating life, corrosion resistance and salt fog resistance.
Description
Technical field
The present invention relates to a kind of lubricant material, specifically relate to a kind of composite sodium-based lubricating grease and preparation method thereof.
Background technology
In sodium base grease, introduce the acid compound or its salt class of a small amount of low molecule can obtain the composite sodium-based lubricating grease of dropping point higher than simple soda soap.As added a small amount of Whitfield's ointment soda soap in fatty acid sodium soap lubricating grease and being heated to 257 DEG C, sodium base grease dropping point can be made to raise.In the lubricating grease containing 5-35% fatty acid sodium soap, add 0.1-5% vinylformic acid sodium salt simultaneously, the solubleness of soda soap in water can be reduced as US2468098; In US2591586, the people such as Morway finds that propenal and derivative thereof also can prepare composite sodium-based lubricating grease with polymer acid.The pressed powder that different-grain diameter distributes adds in lubricating grease by CN101153236A, not only increases the water repelling property of lubricating grease, also improves extreme pressure anti-wear; CN1557922A has prepared by adding clean water in sodium base grease the moisture sodium base grease containing 8-30% clean water, this fat is a kind of substantially pollution-free to environment, high lubricating effect, substantially pollution-free to friction pair, high lubricating effect, has thermal equilibrium effect and the lubricant that can be applicable to heavy loading sliding surface bearing with low cost to friction pair; CN102021068A has prepared a kind of sodium aluminate soap grease for ship, be applicable to marine propeller and Floating Crane and snagboat, dropping point more than 75 DEG C, there is good water resisting property, protective and rust-preventing characteristic, existing proper lubrication effect, there is corrosion-resisting function again, and there is the function lowering mechanicalness noise.
In recent years in order to improve the performance of composite sodium-based lubricating 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 composite sodium-based lubricating grease newly and preparation method thereof.
The present inventor finds under study for action, Graphene is especially joined in base oil in initial reaction stage as the part of viscosifying agent, react with composite sodium-based viscosifying agent one and generate the composite sodium-based lubricating grease of graphene-containing, the composite sodium-based lubricating grease obtained not only has good conductivity, and the method obviously can shorten the composite sodium-based preparation of greases time.
An aspect of of the present present invention provides a kind of composite sodium-based lubricating grease, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite sodium-based 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 70-90%, the composite sodium-based viscosifying agent of 8-25%, the Graphene of 1-10%.
A second aspect of the present invention provides a kind of composite sodium-based preparation of greases method, and the method comprises: Graphene, composite sodium-based viscosifying agent and part basis oil are mixed, 180-230 DEG C of constant temperature refining, cooling, add surplus base oil, add necessary additive, obtain finished product.
A third aspect of the present invention provides a kind of composite sodium-based preparation of greases method, and the method comprises:
By Graphene, base oil, polymer acid mixing, heating, be warming up to 80-105 DEG C, add sodium hydroxide, carry out saponification reaction, then add low molecular acid and carry out compound, be warming up to 200-220 DEG C, add remaining base oil and be cooled to 90-130 DEG C, add necessary additive afterwards, be milled into fat, obtain finished product.
A fourth aspect of the present invention provides the obtained composite sodium-based lubricating grease of aforesaid method.
Composite sodium-based lubricating grease provided by the invention, there is the resistance of oxidation of raising, high dropping point, good mechanical stability, high-temperature and reversible, preferably pumping, excellent thermostability, water resisting property and colloid stability, and have good consistency with other lubricating grease.This Graphene is added fashionable at the preliminary stage of fat processed, it makes 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 improves into fat speed, shortens saponification time.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 sodium-based lubricating grease, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite sodium-based 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 70-90%, the composite sodium-based viscosifying agent of 8-25%, the Graphene of 1-10%.
In composite sodium-based lubricating grease of the present invention, the large usage quantity of Graphene, with composite sodium-based viscosifying agent jointly as viscosifying agent, and unconventional conductive agent, the composite sodium-based lubricating grease of gained is made to maintain the advantage of general sodium 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 by the preliminary stage of Graphene at fat processed is added, make greatly to improve into fat speed, shorten saponification time, but also make the composite sodium-based lubricating 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.
Described hyperacoustic frequency is preferably 25-40kHz.
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: above-mentioned 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 sodium-based viscosifying agent of the present invention can be reacted by acid and sodium hydroxide 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 carboxylic acid of described low molecular acid can be carbonatoms be 4-12, is preferably the mixing acid of one or more in phenylformic acid, terephthalic acid, hexanodioic acid, nonane diacid, sebacic acid.The mol ratio of polymer acid and low molecular acid is preferably 1:0.1-2.
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 one or more in Viscotrol C, rapeseed oil, peanut oil, soya-bean oil etc.Synthetic oil can be one or more in 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, the content of each composition of composite sodium-based lubricating grease calculates according to charging capacity to be determined, wherein, and content=100% × (weight of the weight+low molecular acid sodium of polymer acid sodium)/lubricating grease gross weight of composite sodium-based viscosifying agent.
According to a second aspect of the invention, the invention provides a kind of composite sodium-based preparation of greases method, the method comprises: Graphene, composite sodium-based viscosifying agent and part basis oil are mixed, 180-230 DEG C of constant temperature refining, cooling, add surplus base oil, add necessary additive, obtain finished product.
Wherein, the consumption of Graphene, composite sodium-based viscosifying agent, base oil makes the composite sodium-based lubricating grease of gained, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite sodium-based viscosifying agent of 5-30%, the Graphene of 0.2-15%.
Under preferable case, the consumption of Graphene, composite sodium-based viscosifying agent, base oil makes the composite sodium-based lubricating grease of gained, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 70-90%, the composite sodium-based 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 composite sodium-based preparation of greases method, the method comprises:
By Graphene, part basis oil, polymer acid mixing, heating, be warming up to 80-105 DEG C, add sodium hydroxide, carry out saponification reaction, then add low molecular acid and carry out compound, be warming up to 200-220 DEG C, add residue base oil and be cooled to 90-130 DEG C, add necessary additive afterwards, be milled into fat, obtain finished product.
Wherein, the temperature of described saponification reaction is preferably 80-105 DEG C, and the time of the saponification reaction that polymer acid carries out and the saponification reaction that low molecular acid carries out all is preferably 1-3 hour.
Described sodium hydroxide preferably uses liquid caustic soda.
The time of described refining is preferably 5-25 minute.
Wherein, the consumption of Graphene, composite sodium-based viscosifying agent, base oil makes the composite sodium-based lubricating grease of gained, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite sodium-based viscosifying agent of 5-30%, the Graphene of 0.2-15%.
Under preferable case, the consumption of Graphene, composite sodium-based viscosifying agent, base oil makes the composite sodium-based lubricating grease of gained, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 70-90%, the composite sodium-based viscosifying agent of 8-25%, the Graphene of 1-10%.
Part basis oil: residue 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, lubricating grease provided by the invention can be prepared by the following method:
By Graphene, about 2/3 base oil and polymer acid add in fat still processed, stir be warming up to 80-90 DEG C, add liquid caustic soda, be warming up to 100-110 DEG C of saponification reaction 1h-3h, then add low molecular acid saponification reaction 1h-3h; Continue the dehydration that heats up, after rising to the highest refining temperature 200-220 DEG C, keep 5-20min; Add residue base oil to put into when coolship makes it rapidly cooling to 80-100 DEG C and add additive, to be milled 2-4 one-tenth fat by three-roller.
The main difference of the composite sodium-based preparation of greases method that composite sodium-based preparation of greases method provided by the invention and prior art provide is that saponification reaction is carried out under Graphene exists, and therefore can carry out with reference to prior art about other operations of this preparation process and condition.
Fourth aspect present invention provides the composite sodium-based lubricating grease obtained by the preparation method of the above-mentioned third aspect.
Compared with the composite sodium-based lubricating grease obtained with the preparation method provided by second aspect, the composite sodium-based lubricating grease that fourth aspect provides has better high thermal resistance, water resisting property and adhesivity, colloid stability and extreme pressure anti-wear.
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.
Composite sodium-based preparation of greases:
Feed composition: Graphene 10.4g; 500SN base oil 720g(100 DEG C of viscosity is 10mm
2/ s); Sodium hydroxide 11.28g; Phenylformic acid 16.84g; 12-oxystearic acid 41.14g; Oxidation inhibitor T5015.6g; Add in fat still processed by 10.4 grams of Graphenes, 540 grams of base oils and 41.14 grams of 12-oxystearic acids, heated and stirred, when temperature rises to 80 DEG C, adds the alkali lye containing 11.28 grams of sodium hydroxide, after saponification reaction 0.1h; 16.84 grams of phenylformic acid saponification reaction 0.1h are added again in system; 5min is kept after being warming up to 190 DEG C; Add 180 grams of base oils and put into and add 5.6 grams of oxidation inhibitor T501 when coolship makes it rapidly cooling to 100 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-hydroxyl sodium stearate 5.5 % by weight; Sodium Benzoate 2.5 % by weight; Graphene 1.3 % by weight; Lubricating base oil 90 % by weight; Oxidation inhibitor 0.7 % 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.
Composite sodium-based preparation of greases:
Feed composition: Graphene 31.2g; 150BS base oil 420g(100 DEG C of viscosity is 31mm
2/ s); Sodium hydroxide 23.26g; Terephthalic acid 13.40g; 12-oxystearic acid 121.18g; Di-iso-octyldiphenylamine 1.8g;
Add in fat still processed by 31.2 grams of Graphenes, 210 grams of base oils and 121.18 grams of 12-oxystearic acids, heated and stirred, when temperature rises to 90 DEG C, adds the alkali lye containing 23.26 grams of sodium hydroxide, after saponification reaction 0.1h; 13.40 grams of terephthalic acid saponification reaction 0.1h are added again in system; 15min is kept after being warming up to 200 DEG C; Add 210 grams of base oils and put into and add 1.8 grams of di-iso-octyldiphenylamines when coolship makes it rapidly cooling to 110 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-hydroxyl sodium stearate 21.68 % by weight; Para-phthalic sodium 2.82 % by weight; Graphene 5.2 % by weight; Lubricating base oil 70 % 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.
Composite sodium-based preparation of greases:
Feed composition: Graphene 60g; PAO6 synthetic hydrocarbon oil 444g(100 DEG C of viscosity is 5.8mm
2/ s); Sodium hydroxide 17.26g; Sebacic acid 21.19g; Stearic acid 59.6g; Phenyl-a-naphthylamine 6g;
Add in fat still processed by 60 grams of Graphenes, 296 grams of base oils and 59.6 grams of stearic acid, heated and stirred, when temperature rises to 100 DEG C, adds the alkali lye containing 17.26 grams of sodium hydroxide, saponification reaction 0.1h; 21.19 grams of sebacic acid saponification reaction 0.1h are added again in system; 5min is kept after being warming up to 210 DEG C; Add 148 grams of base oils and put into and add 6 grams of phenyl-a-naphthylamine when coolship makes it rapidly cooling 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: sodium stearate 10.7 % by weight; Sebacic acid sodium 4.3 % by weight; Graphene 10 % by weight; Lubricating base oil 74 % by weight; Oxidation inhibitor 1 % by weight.
Embodiment 4
The preparation of graphene oxide is with embodiment 1.
The preparation of Graphene: add 5ml hydrazine hydrate (mass concentration is 85%) 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.
Composite sodium-based preparation of greases:
Feed composition: Graphene 56g; The mixing oil 644g(100 DEG C viscosity of 150BS and 500SN is 14mm
2/ s); Sodium hydroxide 19.89g; Phenylformic acid 39.59g; Stearic acid 45.79g; Oxidation inhibitor T5014g;
Add in fat still processed by 56 grams of Graphenes, 444 grams of base oils and 45.79 grams of stearic acid, heated and stirred, when temperature rises to 95 DEG C, adds the alkali lye containing 19.89 grams of sodium hydroxide, saponification reaction 0.1h; 39.59 grams of phenylformic acid saponification reaction 0.1h are added again in system; 10min is kept after being warming up to 200 DEG C; Add 200 grams of base oils and put into and add 4 grams of oxidation inhibitor T501 when coolship makes it rapidly cooling to 115 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: sodium stearate 10.7 % by weight; Sebacic acid sodium 4.3 % by weight; Graphene 10 % by weight; Lubricating base oil 74 % by weight; Oxidation inhibitor 1 % by weight.
Comparative example 1
Material component: except not graphene-containing, all the other are with embodiment 4
Composite sodium-based lubricating grease is prepared according to the method for embodiment 4, unlike, do not add Graphene in composite sodium-based preparation of greases process.Product performance are as shown in table 3.
Comparative example 2
Feed composition is with embodiment 4
Composite sodium-based lubricating grease is prepared according to the method for embodiment 4, unlike, whole Graphene adds with oxidation inhibitor T501.Product performance are as shown in table 3.
Comparative example 3
Composite sodium-based lubricating grease is prepared according to the method for embodiment 4, unlike, Graphene is replaced by the crystalline flake graphite of identical weight.Product performance are as shown in table 3.
Embodiment 5
The preparation of Graphene is with embodiment 1
Material component: with embodiment 4
Add in fat still processed by 444 grams of base oils and 45.79 grams of stearic acid, heated and stirred, when temperature rises to 95 DEG C, adds the alkali lye containing 19.89 grams of sodium hydroxide, saponification reaction 0.1h; 39.59 grams of phenylformic acid saponification reaction 0.1h are added in system; In system, add 56 grams of Graphenes again, after being warming up to 200 DEG C, keeping 10min; Add 200 grams of base oils and put into and add 4 grams of oxidation inhibitor T501 when coolship makes it rapidly cooling to 115 DEG C and stir, grind 2 times by three-roller and become fat.Product performance are as shown in table 3.
Embodiment 6
Composite sodium-based lubricating 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 sodium-based lubricating 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 (18)
1. a composite sodium-based lubricating grease, is characterized in that, with lubricating grease weight for benchmark, comprises following component: the lubricating base oil of 65-95%, the composite sodium-based viscosifying agent of 5-30%, the Graphene of 0.2-15%.
2. composite sodium-based lubricating grease according to claim 1, wherein, lubricating grease weight is benchmark, comprises following component: the lubricating base oil of 70-90%, the composite sodium-based viscosifying agent of 8-25%, the Graphene of 1-10%.
3. composite sodium-based lubricating 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 sodium-based lubricating 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 sodium-based lubricating grease according to claim 1 and 2, wherein, described composite sodium-based viscosifying agent is reacted by acid and sodium hydroxide 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 4-12.
6. composite sodium-based lubricating grease according to claim 5, wherein, described polymer acid be 1:0.1-2 with the mol ratio of low molecular acid.
7. the composite sodium-based lubricating 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 phenylformic acid, terephthalic acid, nonane diacid, sebacic acid.
8. the composite sodium-based lubricating grease according to claim 5 or 6, wherein, it is 80-105 DEG C that the condition of described saponification reaction comprises temperature.
9. according to the composite sodium-based lubricating grease in claim 1-8 described in any one, wherein, 100 DEG C of kinematic viscosity of described lubricating base oil are 5-60mm
2/ s.
10. according to the composite sodium-based lubricating grease in claim 1-9 described in any one, wherein, the additive of this composite sodium-based lubricating grease also containing 0.5-15 % by weight.
11. 1 kinds of composite sodium-based preparation of greases methods, the method comprises:
Graphene, base oil are mixed with polymer acid, heat, be warming up to 80-105 DEG C, add sodium hydroxide, carry out saponification reaction, then add low molecular acid and carry out compound, be warming up to 200-220 DEG C, add remaining base oil and be cooled to 90-130 DEG C, add necessary additive afterwards, be milled into fat, obtain finished product, 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 4-12.
12. preparation methods according to claim 11, wherein, the temperature of described saponification reaction is 80-105 DEG C, and the time of the saponification reaction that polymer acid carries out and the saponification reaction that low molecular acid carries out is 1-3 hour.
13. preparation methods according to claim 11 or 12, wherein, the consumption of Graphene, composite sodium-based viscosifying agent, base oil makes the composite sodium-based lubricating grease of gained, with lubricating grease weight for benchmark, comprise following component: the lubricating base oil of 65-95%, the composite sodium-based viscosifying agent of 5-30%, the Graphene of 0.2-15%.
14. according to the preparation method in claim 11-13 described in any one, wherein, with molar ratio computing, and polymer acid: low molecular acid=1:0.1-2.
15. according to the preparation method in claim 11-14 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 phenylformic acid, terephthalic acid, nonane diacid, sebacic acid.
16. according to the preparation method in claim 11-15 described in any one, and wherein, described Graphene can disperse in 1ml base oil and non-setting maximum is 8-12mg.
17. according to the preparation method in claim 11-16 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 sodium-based lubricating grease that preparation method in 18. claim 11-17 described in any one obtains.
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| CN106590820A (en) * | 2015-10-15 | 2017-04-26 | 中国石油化工股份有限公司 | Sodium-based lubricating grease and preparation method thereof |
| CN106590823A (en) * | 2015-10-15 | 2017-04-26 | 中国石油化工股份有限公司 | Composite sodium base 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 |
| CN107384559A (en) * | 2017-08-01 | 2017-11-24 | 太原理工大学 | A kind of stratiform potassium magnesium phosphate sodium base 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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| CN107384559A (en) * | 2017-08-01 | 2017-11-24 | 太原理工大学 | A kind of stratiform potassium magnesium phosphate sodium base grease composition 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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