CN109054960A - A kind of friction improver and preparation method thereof containing mesoporous nano carbon - Google Patents
A kind of friction improver and preparation method thereof containing mesoporous nano carbon Download PDFInfo
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- CN109054960A CN109054960A CN201811201561.2A CN201811201561A CN109054960A CN 109054960 A CN109054960 A CN 109054960A CN 201811201561 A CN201811201561 A CN 201811201561A CN 109054960 A CN109054960 A CN 109054960A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/16—Naphthenic acids
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
- C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
- C10M2219/066—Thiocarbamic type compounds
- C10M2219/068—Thiocarbamate metal salts
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/045—Metal containing thio derivatives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/25—Internal-combustion engines
Abstract
The present invention relates to technical field of nano material, specially a kind of friction improver and preparation method thereof containing mesoporous nano carbon.The present invention passes through first by base oil, part ashless dispersant, nano artificial graphite is prepared into after nano artificial graphite particle and mixes again with other components, and mixture first is further continued for stirring using high-speed mixer after ultrasonic wave disperses, mesoporous nano carbon and nano artificial graphite are subjected to dispersion cladding processing, there can be good dispersibility in base oil and lubricating oil, long-term suspension, it does not settle, oil circuit will not be blocked, thermal stability is good, friction reducing effect is good, and it can mutually be fused with various lubricating oil, with high temperature-resistant high-speed high load capacity, it can avoid carbon distribution to generate, lubricity between significant increase engine each metal parts, it is capable of forming effective physical absorption protective film and chemical reaction protective film, reduce the high abrasion between each component of engine, extend engine life.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of friction improver containing mesoporous nano carbon and its
Preparation method.
Background technique
Since the 21th century, China's car ownership rapid growth, in relation to automotive safety, environmental protection and energy-efficient regulation,
Standard is increasingly strengthened, and vehicular engine dynamic property, economy and emission performance is pushed constantly to improve.Wherein automobile power is played
The automobile engine lubricating oil of key effect is a kind of oil product that dosage is maximum in motor vehicle lubricants, consumption is most.In recent years, with
Engine lubricating oil operating condition it is more and more harsher, the specification kind of engine lubricating oil is more and more, and quality class makes
It is also higher and higher with performance and price.
Toyota Motor company was once tested according to 10 operating condition oil consumption mileages measurement standard, the results showed that is started
The fricting loss power of machine is about as much as the 40% of vehicle effective output, and wherein cylinder sleeve and piston, piston ring rub
It wears to fail to keep an appointment and accounts for the 50%-60% of engine total friction head.In order to improve the friction, lubrication state of engine, reduce friction damage
Lose, save fuel consumption and extend engine service life, in addition to the basic oil product to lubricating oil constantly bring forth new ideas optimization and
It promotes and applies outside peace and quiet, high-quality fuel oil, the use of high-quality oil additives is a kind of effective method.
Oil additives is the most effective substance for improving engine friction and lubrication property and being used widely, native land
The inside and outside research and development and popularization and application for always attaching great importance to oil additives.Oil additives mainly includes peace and quiet dispersion
Agent, viscosity index improver, extreme pressure additive, friction improver, antirust agent, oiliness improver, pour-point depressant, disappears at antioxidant anticorrosive agent
Infusion etc..
Common friction improver mainly includes following several in lubricating oil: Long carbon chain fatty acid, fatty alcohol and its esters；
Fatty amine and its derivative；Organic boric acid ester and borate；Organic molybdenum or graphite.Wherein, Long carbon chain fatty acid, fat
There is certain corrosivity to easily cause piston chemically if control is bad for alcohol and its esters, fatty amine and its derivative
Corrosive wear；The thermal oxidation stability of organic boric acid ester and borate, water stability and durability are poor；Molybdenum disulfide and
That there are particles is larger for natural graphite, and pattern is inconsistent, causes friction reducing effect unstable, and is easy that coagulation is precipitated for a long time, with
Cause is quickly invalidated, or even blocking strainer causes the side effects such as fuel feeding difficulty.
Summary of the invention
That there are thermal stability is poor for existing friction improver by the present invention, is easy sedimentation blocking oil circuit, and friction reducing effect is general
The problems such as, it is good to provide a kind of good thermal stability, not easily settled blocking oil circuit, friction reducing effect, and can mutually fuse with various lubricating oil,
With high temperature-resistant high-speed high load capacity, the friction improver containing mesoporous nano carbon of the characteristics such as carbon distribution generation is avoided.
To achieve the above object, the present invention uses following technical scheme.
A kind of friction improver containing mesoporous nano carbon, is made of each raw material component of following mass percentage:
The mesoporous nano carbon of 0.4-1.8%；The nano artificial graphite of 1.5-5.2%；The ashless dispersant of 0.2-7%；0.2-1.6%'s
Organic molybdenum；The antioxidant of 0-0.5%；Base oil surplus.
Preferably, the mesoporous nano carbon is spherical or cylindrical mesoporous nano carbon, and granularity is less than 100nm.
Preferably, the purity of the nano artificial graphite is greater than 99.5%, and granularity is 0.5 μm.
Preferably, the ashless dispersant is selected from boronation polyisobutene succinimide, polyisobutylene succinic acid ester, benzylamine
At least one of.
Preferably, the organic molybdenum is selected from dialkyl dithiophosphoric acid oxygen molybdenum, nitrogenous dialkyl dithiophosphoric acid
At least one of oxygen molybdenum, molybdenum dialkyldithiocarbamacompositions, molybdenum naphthenate, alkyl salicylate molybdenum.
Preferably, the antioxidant is selected from zinc dialkyl dithiophosphate, 4,4- di-2-ethylhexylphosphine oxide (2,6- di-t-butyls
Phenol), four [β (3,5- di-tert-butyl-hydroxy phenyl the third) acid] pentaerythritol esters, at least one of sulphide amino zinc formate.
Preferably, the base oil is fully synthetic base oil or semi-synthetic base oil, and viscosity index (VI) is 90 < VI <
120。
The preparation method of friction improver of the above containing mesoporous nano carbon, comprising the following steps:
S1, base oil, part ashless dispersant and nano artificial graphite are mixed and is uniformly dispersed, be then ground to afterwards mixed
0.5 μm of partial size D50 < for closing object, obtains nano artificial graphite particle dispersion liquid；
S2, mesoporous nano carbon, remaining ashless dispersant, antioxidant and organic molybdenum are added to the nanometer
It in electrographite particle dispersion, is uniformly dispersed, obtains friction improver.
Preferably, mesoporous nano carbon, remaining ashless dispersant, antioxidant and organic molybdenum are added sequentially to
In the nano artificial graphite particle dispersion liquid, ultrasonic wave disperses 1-2 hours, is then stirred 3-6 hours using high-speed mixer,
Obtain friction improver.
Preferably, above-described mesoporous nano carbon is made by following steps:
S21, phenolic resin and potassium hydroxide are added to the water and is heated to 70-80 DEG C and is stirred continuously, after mixing evenly,
Triblock copolymer is added into mixture and is kept for 70-80 DEG C and is stirred continuously 10-15h, obtains mixed liquor；The hydroxide
The quality of potassium is the 0.9-1% of the quality of phenolic resin；
S22, mixed liquor is placed at 100 DEG C and reacts 24-36h, then the mixed liquor after drying reaction, obtains powder；
S23, powder is placed under inert atmosphere, is warming up to 700 DEG C and constant temperature 2h with the speed of 5 DEG C/min, is received
Rice mesoporous carbon；
S24, it disperses mesoporous nano carbon in petroleum ether, then heats dispersion liquid to 90 DEG C and constant temperature 30min, then
Modifying agent is added into dispersion liquid and dispersion is equal, followed by the solid particle and drying collected in dispersion liquid, obtains modified
Mesoporous nano carbon；The quality of the modifying agent is the 11.5-23.1% of the quality of phenolic resin.
Preferably, the modifying agent is selected from least one of hydrogen peroxide, nitric acid, stearic acid, oleic acid.
Compared with prior art, the beneficial effects of the present invention are:
By the present invention in that have the characteristics that the good mesoporous nano carbon of morphological consistency, the meso-hole structure tool of mesoporous nano carbon
There are good oil suction and oil storage performance, forms oil film by storing lubricating oil in relief hole in friction process, it can be effective
It realizes lubricating action, especially with spherical and cylindrical mesoporous carbon, micro- bearing and micro- rolling can be played in friction process
The effect of pearl can become sliding friction as rolling friction, and synergistic with nano artificial graphite, the physics for forming long stable effect is inhaled
Attached protective film effectively reduces coefficient of friction, reduces the abrasion at each position of engine, especially the engine cold-start stage is violent
Abrasion, extends engine life.And the present invention is surface modified mesoporous nano carbon by modifying agent to increase its parent
Oiliness and dispersion stabilization can preferably improve the performance of friction improver, in addition, the preparation work of mesoporous nano carbon of the invention
Skill is simple, and cost is relatively low, as a kind of new and effective antifriction component, has a vast market foreground.
Nano artificial graphite-phase is than natural graphite, and purity is high, compact structure, orientation is consistent, especially selects spherical high-purity
Nano artificial graphite can play the role of micro- bearing in friction process, while be also equipped with the lubrication effect of the interformational sliding of graphite
Fruit greatly improves the lubricity to engine.Mesoporous nano carbon and nano artificial graphite are synergistic, form good physics
Protective film is adsorbed, engine scuffing is reduced, extends engine life.
The present invention uses ashless dispersant, the insoluble particles object in oil product can be made to keep suspending, and prevent greasy filth from agglomerating
It is deposited with insoluble matter, the viscosity build in lubricating oil use process can also be reduced.
The present invention is especially existed in the operation process of engine high-temperature high pressure high load capacity by adding organic molybdenum
Piston wall, piston rod etc., organic molybdenum chemically reacts, and decomposites MOS2Equal compounds, form chemical reaction
Protective film is covered in wear-resistant friction layer, to have the function that antifriction, wear-resistant, lubrication.
The present invention is by addition antioxidant, during so that friction improver of the invention is hindered oil ageing
Chain reaction, to prevent rapid oxidation of lubricating oil during high temperature lubricating.
The present invention is by being first prepared into nano artificial granular graphite for base oil, part ashless dispersant, nano artificial graphite
It is mixed again with other components after son, and mixture first is further continued for stirring using high-speed mixer after ultrasonic wave disperses 1-2 hours
It mixes 3-6 hours, mesoporous nano carbon and nano artificial graphite is subjected to dispersion cladding processing, can be had in base oil and lubricating oil
Good dispersibility, long-term suspension do not settle, and will not block oil circuit, and thermal stability is good, friction reducing effect is good, and can be with various profits
Lubricating oil mutually fuses, and has high temperature-resistant high-speed high load capacity, can avoid carbon distribution and generates, between significant increase engine each metal parts
Lubricity, be capable of forming effective physical absorption protective film and chemical reaction protective film, reduce each component of engine between
Height abrasion, extends engine life.
Detailed description of the invention
Fig. 1 is the shape appearance figure of modified mesoporous nano carbon made from embodiment 4；
Fig. 2 is the dispersion shape appearance figure of the friction improver containing mesoporous nano carbon under the microscope made from embodiment 4.
Specific embodiment
In order to more fully understand technology contents of the invention, combined with specific embodiments below to technical solution of the present invention
It is described further and illustrates.
Embodiment 1
The rubbing containing mesoporous nano carbon the present embodiment provides a kind of friction improver containing mesoporous nano carbon and this kind
Wipe the preparation method of modifier.
Friction improver containing mesoporous nano carbon described in the present embodiment is by the following raw material system that is calculated in mass percent
It is standby to form:
Mesoporous nano carbon: 0.6%；Nano artificial graphite: 1.8%；Ashless dispersant: 3.5%；Organic molybdenum:
0.4%；Antioxidant: 0%；Base oil: surplus.
Mesoporous nano carbon is spherical or cylindrical mesoporous nano carbon, granularity 25nm.
Nano artificial graphite be high pure spherical electrographite, purity 99.9%, 0.5 μm of granularity.
Ashless dispersant is polyisobutylene succinic acid ester.
Organic molybdenum by etc. quality dialkyl dithiophosphoric acid oxygen molybdenum and molybdenum dialkyldithiocarbamacompositions group
At.
Base oil is fully synthetic base oil, viscosity index (VI) 95.
Specific preparation process is as follows for the friction improver containing mesoporous nano carbon of the present embodiment:
1, the preparation of nano artificial graphite particle
A. ingredient: by 23.425kg base oil, 0.438kg ashless dispersant, 0.45kg spherical faux graphite in proportion according to
Secondary addition high-speed mixer.
B. grinding distribution: being stirred 2 hours with the revolving speed of 1000rpm using high-speed mixer, and mixed liquor is passed through colloid mill
Lapping liquid, is then added in horizontal sand mill and grinds by grinding 3 times, and circular grinding 36 hours.
C. it is classified: being classified above-mentioned lapping liquid using Wet-type centrifugal grader, centrifugal rotational speed 6000rpm, according to centrifugal force
Field classification principle, bulky grain continue to return and continue to grind in horizontal sand mill, and suitable little particle is no longer ground.It follows
Ring grinding is until 0.5 μm of partial size D50 <, as qualified product, obtain nano artificial graphite particle dispersion liquid.
2, the preparation of mesoporous nano carbon
Using triblock copolymer as activating agent, using phenolic resin as carbon source, under hydrothermal conditions, prepare have height have
The mesoporous nano carbon of ordered meso-porous structure (spherical, cylindrical).And it is surface modified with modifying agent to increase its lipophilicity
And the dispersion stabilization in lubricating oil.
Specifically:
A. it prepares: 1.3kg phenolic resin (resorcinol-formaldehyde) and 0.012kg potassium hydroxide being added in 3L water, added
Heat is to 80 DEG C and is stirred continuously, and after stirring 1 hour, 1.6kg triblock copolymer is added, and (polyoxyethylene polyoxypropylene ether three is embedding
Section copolymer), kept for 80 DEG C, and continue stirring 10 hours.Mixed liquor after stirring is added in reaction kettle, is polymerize at 100 DEG C
Reaction 36 hours, takes out 60 DEG C of drying, obtains bronzing powder.This bronzing powder is added in sealing high temperature furnace,
Under nitrogen protection, 700 DEG C is warming up to the speed of 5 DEG C/min, and continue high temperature 2h, obtains mesoporous nano carbon.
B. be modified: the mesoporous nano carbon of the above-mentioned preparation of 0.5kg be added in 30L petroleum ether solution, using ultrasonic wave into
Row dispersion 20 minutes.It is heated to 90 DEG C, and constant temperature 30 minutes.Being slowly added to 0.15kg modifying agent, (modifying agent is by mass ratio
The hydrogen peroxide and oleic acid of 1:10 forms), and this process is dispersed using ultrasonic wave, and it is small to reuse high-speed mixer stirring 1
When.Then, this mixed liquor is added in centrifuge and is centrifuged, remove supernatant, 60 DEG C of drying obtain modified mesoporous nano
Carbon.
3. the preparation of friction improver
The modified mesoporous nano carbon of 0.15kg, 0.438kg ashless dispersant and 0.1kg organic molybdenum is taken successively to add
Enter to 1 gained nano artificial graphite dispersing solution of technique, ultrasonic wave dispersion 1 hour, then proceedes to small using high-speed mixer stirring 4
When, the as friction improver containing mesoporous nano carbon.
Embodiment 2
The rubbing containing mesoporous nano carbon the present embodiment provides a kind of friction improver containing mesoporous nano carbon and this kind
Wipe the preparation method of modifier.
Friction improver containing mesoporous nano carbon described in the present embodiment is by the following raw material system that is calculated in mass percent
It is standby to form: mesoporous nano carbon: 1.2%；Nano artificial graphite: 2.4%；Ashless dispersant: 4.5%；Organic molybdenum:
0.6%；Antioxidant: 0.3%；Base oil: surplus.
Mesoporous nano carbon is spherical or cylindrical nanometer mesoporous carbon, granularity 25nm.
Nano artificial graphite be high pure spherical electrographite, purity 99.9%, 0.5 μm of granularity.
Ashless dispersant is boronation polyisobutene succinimide.
Organic molybdenum by etc. quality dialkyl dithiophosphoric acid oxygen molybdenum and molybdenum dialkyldithiocarbamacompositions group
At.
Antioxidant is zinc dialkyl dithiophosphate.
Base oil is fully synthetic base oil, viscosity index (VI) 95.
Specific preparation process is as follows for the friction improver containing mesoporous nano carbon of the present embodiment:
1. prepared by nano artificial graphite particle
A. ingredient: in proportion successively by 22.75kg base oil, 0.563kg ashless dispersant, 0.6kg spherical faux graphite
High-speed mixer is added.
B. grinding distribution: being stirred 2 hours with the revolving speed of 1000rpm using high-speed mixer, and mixed liquor is passed through colloid mill
Grinding 3 times, then, lapping liquid is added in horizontal sand mill and is ground, and circular grinding 36 hours.
C. it is classified: being classified above-mentioned lapping liquid using Wet-type centrifugal grader, centrifugal rotational speed 6000rpm, according to centrifugal force
Field classification principle, bulky grain continue to return and continue to grind in horizontal sand mill, and suitable little particle is no longer ground.It follows
Ring grinding is until 0.5 μm of partial size D50 <, as qualified product, obtain nano artificial graphite particle dispersion liquid.
2. the preparation of mesoporous nano carbon
A. it prepares: 1.3kg phenolic resin (resorcinol-formaldehyde) and 0.012kg potassium hydroxide being added in 3L water, added
Heat is to 80 DEG C and is stirred continuously, and after stirring 1 hour, 1.6kg triblock copolymer (the polycyclic oxygen second for being 1:5 by mass ratio is added
Alkane-polypropylene oxide-polyethylene oxide triblock copolymer and polyoxyethylene polyoxypropylene ether triblock copolymer form), it protects
80 DEG C are held, and continues stirring 10 hours.Mixed liquor after stirring is added in reaction kettle, polymerization reaction 36 hours, take at 100 DEG C
60 DEG C of drying out, obtain bronzing powder.This bronzing powder is added in sealing high temperature furnace, under nitrogen protection, with 5
DEG C/speed of min is warming up to 700 DEG C, and continues high temperature 2h, obtain mesoporous nano carbon.
B. be modified: the mesoporous nano carbon of the above-mentioned preparation of 0.5kg be added in 30L petroleum ether solution, using ultrasonic wave into
Row dispersion 20 minutes.It is heated to 90 DEG C, and constant temperature 30 minutes.Being slowly added to 0.25kg modifying agent (is 1:3's by mass ratio
Stearic acid and oleic acid form), and this process is dispersed using ultrasonic wave, is reused high-speed mixer and is stirred 1 hour.So
Afterwards, this mixed liquor is added in centrifuge and is centrifuged, remove supernatant, 60 DEG C of drying obtain modified mesoporous nano carbon.
3. the preparation of friction improver
The modified mesoporous nano carbon of 0.3kg, 0.563kg ashless dispersant, 0.075kg antioxidant and 0.15kg is taken to have
Machine molybdenum compound is added sequentially to 1 gained nano artificial graphite dispersing solution of technique, and ultrasonic wave disperses 1 hour, then, continues to use
High-speed mixer stirs 4 hours, the as friction improver containing mesoporous nano carbon.
Embodiment 3
The rubbing containing mesoporous nano carbon the present embodiment provides a kind of friction improver containing mesoporous nano carbon and this kind
Wipe the preparation method of modifier.
Friction improver containing mesoporous nano carbon described in the present embodiment is by the following raw material system that is calculated in mass percent
It is standby to form: mesoporous nano carbon: 1.2%；Nano artificial graphite: 1.8%；Ashless dispersant: 4.0%；Organic molybdenum:
0.8%；Antioxidant: 0.5%；Base oil: surplus.
Mesoporous nano carbon is spherical or cylindrical nanometer mesoporous carbon, granularity 25nm.
Nano artificial graphite be high pure spherical electrographite, purity 99.9%, 0.5 μm of granularity.
Ashless dispersant is boronation polyisobutene succinimide.
The dialkyl dithiophosphoric acid oxygen molybdenum and dialkyldithiocarbamacompositions that organic molybdenum is 1:2 by mass ratio
Molybdenum composition.
Antioxidant is zinc dialkyl dithiophosphate.
Base oil is fully synthetic base oil, viscosity index (VI) 95.
Specific preparation process is as follows for the friction improver containing mesoporous nano carbon of the present embodiment:
1. prepared by nano artificial graphite particle
A. ingredient: in proportion successively by 22.925kg base oil, 0.5kg ashless dispersant, 0.45kg spherical faux graphite
High-speed mixer is added.
B. grinding distribution: being stirred 2 hours with the revolving speed of 1000rpm using high-speed mixer, and mixed liquor is passed through colloid mill
Grinding 3 times, then, lapping liquid is added in horizontal sand mill and is ground, and circular grinding 36 hours.
C. it is classified: being classified above-mentioned lapping liquid using Wet-type centrifugal grader, centrifugal rotational speed 6000rpm, according to centrifugal force
Field classification principle, bulky grain continue to return and continue to grind in horizontal sand mill, and suitable little particle is no longer ground.It follows
Ring grinding is until 0.5 μm of partial size D50 <, as qualified product, obtain nano artificial graphite particle dispersion liquid.
2. the preparation of mesoporous nano carbon
A. it prepares: 1.3kg phenolic resin (resorcinol-formaldehyde) and 0.012kg potassium hydroxide being added in 3L water, added
Heat is to 80 DEG C and is stirred continuously, and after stirring 1 hour, 1.6kg triblock copolymer (the polycyclic oxygen second for being 1:8 by mass ratio is added
Alkane-polypropylene oxide-polyethylene oxide triblock copolymer and polyoxyethylene polyoxypropylene ether triblock copolymer form), it protects
80 DEG C are held, and continues stirring 10 hours.Mixed liquor after stirring is added in reaction kettle, polymerization reaction 36 hours, take at 100 DEG C
60 DEG C of drying out, obtain bronzing powder.This bronzing powder is added in sealing high temperature furnace, under nitrogen protection, with 5
DEG C/speed of min is warming up to 700 DEG C, and continues high temperature 2h, obtain mesoporous nano carbon.
B. be modified: the mesoporous nano carbon of the above-mentioned preparation of 0.5kg be added in 30L petroleum ether solution, using ultrasonic wave into
Row dispersion 20 minutes.It is heated to 90 DEG C, and constant temperature 30 minutes.Being slowly added to 0.3kg modifying agent (is the hard of 1:5 by mass ratio
Resin acid and oleic acid form), and this process is dispersed using ultrasonic wave, is reused high-speed mixer and is stirred 1 hour.Then,
This mixed liquor is added in centrifuge and is centrifuged, supernatant is removed, 60 DEG C of drying obtain modified mesoporous nano carbon.
3. the preparation of friction improver
Take the modified mesoporous nano carbon of 0.3kg, 0.5kg ashless dispersant, 0.125kg antioxidant and 0.2kg organic
Molybdenum compound is added sequentially to 1 gained nano artificial graphite dispersing solution of technique, and ultrasonic wave disperses 1 hour, then, continues to use height
Fast blender stirs 4 hours, the as friction improver containing mesoporous nano carbon.
Embodiment 4
The rubbing containing mesoporous nano carbon the present embodiment provides a kind of friction improver containing mesoporous nano carbon and this kind
Wipe the preparation method of modifier.
Friction improver containing mesoporous nano carbon described in the present embodiment is by the following raw material system that is calculated in mass percent
It is standby to form: mesoporous nano carbon: 1.5%；Nano artificial graphite: 1.5%；Ashless dispersant: 4.2%；Organic molybdenum:
0.8%；Antioxidant: 0.5%；Base oil: surplus.
Mesoporous nano carbon is spherical or cylindrical nanometer mesoporous carbon, granularity 25nm.
Nano artificial graphite be high pure spherical electrographite, purity 99.9%, 0.5 μm of granularity.
Ashless dispersant is boronation polyisobutene succinimide.
The dialkyl dithiophosphoric acid oxygen molybdenum and dialkyldithiocarbamacompositions that organic molybdenum is 1:2 by mass ratio
Molybdenum composition.
The antioxidant is zinc dialkyl dithiophosphate.
The base oil is fully synthetic base oil, viscosity index (VI) 95.
Specific preparation process is as follows for the friction improver containing mesoporous nano carbon of the present embodiment:
1. prepared by nano artificial graphite particle
A. ingredient: 22.875kg base oil, 0.525kg ashless dispersant (half of total dosage), 0.375kg is spherical
Electrographite sequentially adds high-speed mixer in proportion.
B. grinding distribution: being stirred 2 hours with the revolving speed of 1000rpm using high-speed mixer, and mixed liquor is passed through colloid mill
Grinding 3 times, then, lapping liquid is added in horizontal sand mill and is ground, and circular grinding 36 hours.
C. it is classified: being classified above-mentioned lapping liquid using Wet-type centrifugal grader, centrifugal rotational speed 6000rpm, according to centrifugal force
Field classification principle, bulky grain continue to return and continue to grind in horizontal sand mill, and suitable little particle is no longer ground.It follows
Ring grinding is until 0.5 μm of partial size D50 <, as qualified product, obtain nano artificial graphite particle dispersion liquid.
2. the preparation of mesoporous nano carbon
A. it prepares: 1.3kg phenolic resin (resorcinol-formaldehyde) and 0.012kg potassium hydroxide being added in 3L water, added
Heat is to 80 DEG C and is stirred continuously, and after stirring 1 hour, 1.6kg triblock copolymer (the polycyclic oxygen second for being 1:6 by mass ratio is added
Alkane-polypropylene oxide-polyethylene oxide triblock copolymer and polyoxyethylene polyoxypropylene ether triblock copolymer form), it protects
80 DEG C are held, and continues stirring 10 hours.Mixed liquor after stirring is added in reaction kettle, polymerization reaction 36 hours, take at 100 DEG C
60 DEG C of drying out, obtain bronzing powder.This bronzing powder is added in sealing high temperature furnace, under nitrogen protection, with 5
DEG C/speed of min is warming up to 700 DEG C, and continues high temperature 2h, obtain mesoporous nano carbon.
B. be modified: the mesoporous nano carbon of the above-mentioned preparation of 0.5kg be added in 30L petroleum ether solution, using ultrasonic wave into
Row dispersion 20 minutes.It is heated to 90 DEG C, and constant temperature 30 minutes.Being slowly added to 0.3kg modifying agent (is 1:10's by mass ratio
Stearic acid and oleic acid form), and this process is dispersed using ultrasonic wave, is reused high-speed mixer and is stirred 1 hour.So
Afterwards, this mixed liquor is added in centrifuge and is centrifuged, remove supernatant, 60 DEG C of drying obtain modified mesoporous nano carbon, shape
Looks are shown in Fig. 1.
3. the preparation of friction improver
Take the modified mesoporous nano carbon of 0.375kg, 0.525kg ashless dispersant, 0.125kg antioxidant and 0.2kg
Organic molybdenum is added sequentially to 1 gained nano artificial graphite dispersing solution of technique, and ultrasonic wave disperses 1 hour, then, continues to make
4 hours, the as friction improver containing mesoporous nano carbon are stirred with high-speed mixer, dispersion pattern is shown in Fig. 2.
Embodiment 5
The rubbing containing mesoporous nano carbon the present embodiment provides a kind of friction improver containing mesoporous nano carbon and this kind
Wipe the preparation method of modifier.
It is used to prepare each raw materials and consumption of the friction improver containing mesoporous nano carbon in the present embodiment and implements
Example 4 it is identical, prepare that the raw material that mesoporous nano carbon uses is also identical with embodiment 4, the basic phase of preparation method and embodiment 4
Together, the difference is that temperature and time when preparing mesoporous nano carbon is different, specifically:
A. it prepares: 1.3kg phenolic resin (resorcinol-formaldehyde) and 0.012kg potassium hydroxide being added in 3L water, added
Heat is to 100 DEG C and is stirred continuously, and after stirring 1 hour, 1.6kg triblock copolymer (the polycyclic oxygen second for being 1:6 by mass ratio is added
Alkane-polypropylene oxide-polyethylene oxide triblock copolymer and polyoxyethylene polyoxypropylene ether triblock copolymer form), it protects
100 DEG C are held, and continues stirring 6 hours.Mixed liquor after stirring is added in reaction kettle, polymerization reaction 12 hours, take at 115 DEG C
60 DEG C of drying out, obtain bronzing powder.This bronzing powder is added in sealing high temperature furnace, under nitrogen protection, with 5
DEG C/speed of min is warming up to 700 DEG C, and continues high temperature 2h, obtain mesoporous nano carbon.
B. be modified: the method being modified to mesoporous nano carbon is identical as embodiment 4.
Embodiment 6
The rubbing containing mesoporous nano carbon the present embodiment provides a kind of friction improver containing mesoporous nano carbon and this kind
Wipe the preparation method of modifier.
Friction improver containing mesoporous nano carbon described in the present embodiment is by the following raw material system that is calculated in mass percent
It is standby to form: mesoporous nano carbon: 0.4%；Nano artificial graphite: 5.2%；Ashless dispersant: 2.5%；Organic molybdenum:
0.2%；Antioxidant: 0.5%；Base oil: surplus.
Mesoporous nano carbon is spherical or cylindrical nanometer mesoporous carbon, granularity 25nm.
Nano artificial graphite be high pure spherical electrographite, purity 99.9%, 0.5 μm of granularity.
Ashless dispersant is boronation polyisobutene succinimide.
The dialkyl dithiophosphoric acid oxygen molybdenum and dialkyldithiocarbamacompositions that organic molybdenum is 1:2 by mass ratio
Molybdenum composition.
The antioxidant is zinc dialkyl dithiophosphate.
The base oil is semi-synthetic base oil, viscosity index (VI) 90.
The method that the present embodiment prepares the friction improver of the carbon containing mesoporous nano is identical as embodiment 4.
Embodiment 7
The rubbing containing mesoporous nano carbon the present embodiment provides a kind of friction improver containing mesoporous nano carbon and this kind
Wipe the preparation method of modifier.
Friction improver containing mesoporous nano carbon described in the present embodiment is by the following raw material system that is calculated in mass percent
It is standby to form: mesoporous nano carbon: 1.8%；Nano artificial graphite: 1.5%；Ashless dispersant: 7%；Organic molybdenum:
1.6%；Antioxidant: 0.5%；Base oil: surplus.
Mesoporous nano carbon is spherical or cylindrical nanometer mesoporous carbon, granularity 25nm.
Nano artificial graphite be high pure spherical electrographite, purity 99.9%, 0.5 μm of granularity.
Ashless dispersant is boronation polyisobutene succinimide.
The dialkyl dithiophosphoric acid oxygen molybdenum and dialkyldithiocarbamacompositions that organic molybdenum is 1:2 by mass ratio
Molybdenum composition.
The antioxidant is zinc dialkyl dithiophosphate.
The base oil is semi-synthetic base oil, viscosity index (VI) 120.
The method that the present embodiment prepares the friction improver of the carbon containing mesoporous nano is identical as embodiment 4.
Performance characterization is carried out to the friction improver of the carbon containing mesoporous nano of embodiment 1-7 preparation.
1, product index
The physical and chemical index of the friction improver containing mesoporous nano carbon of embodiment 1-7 preparation is detected, detection knot
Fruit is shown in Table 1.
The physical and chemical index of the friction improver containing mesoporous nano carbon of 1 embodiment 1-7 of table preparation
2, product compares the 5W-40SN grades of abrasion resistance influences of shell Huang Heineken synthetic technology machine oil
Each 150ml of friction improver containing mesoporous nano carbon prepared by embodiment 1-7 is added separately to the shell of 4L
In yellow Heineken synthetic technology machine oil, oil classifications 5W-40SN is stirred 10 minutes using high-speed mixer, is obtained improved
Shell Huang Heineken synthetic technology machine oil successively improves machine oil 7 labeled as improvement machine oil 1- respectively.Meanwhile blank control group is set,
For the shell Huang Heineken synthetic technology machine oil that product of the present invention is not added.Then, it is ground using the vertical omnipotent friction of MMW-1P dual display
Damage testing machine and four ball frictional testing machine of MQ-800 type test its tribological property, and testing result is shown in Table 2.
2 tribological property index of table
Note: PB represents maximum nonseizure load, and seizing maximum load does not occur under prescribed conditions, is indicated with N.Sometimes
Referred to as highest film strength.PD represents sintering load, is to be sintered rotating ball with three static balls
Minimum load, indicated with N.
3. product compares the influence that automobile engine tail gas discharges pollutants
Choose the automobile engine for being not added with the friction improver of embodiment 4 and the friction improver for being added to embodiment 4
The tail gas discharging pollutant of automobile engine carry out detection comparison, wherein the automobile of the friction improver of addition embodiment 4
After the Testing index of engine is its friction improver 150ml that embodiment 4 is added, after travelling 1000km, then car tail is carried out
The index of gas detection.Testing result is shown in Table 3.
3 tail gas discharging pollutant index of table
In other embodiments scheme, ashless dispersant is also selected from boronation polyisobutene succinimide, poly- isobutyl
At least one of alkene succinate, benzylamine；Organic molybdenum is also selected from dialkyl dithiophosphoric acid oxygen molybdenum, nitrogenous two
At least one of alkyl dithiophosphoric acid oxygen molybdenum, molybdenum dialkyldithiocarbamacompositions, molybdenum naphthenate, alkyl salicylate molybdenum；
Antioxidant is also selected from zinc dialkyl dithiophosphate, 4,4- di-2-ethylhexylphosphine oxide (2,6- di-tert-butylphenol), four [β (3,5- bis-
Tert-butyl-hydroxy phenyl the third) acid] pentaerythritol ester, at least one of sulphide amino zinc formate；Modifying agent is also selected from
At least one of hydrogen peroxide, nitric acid, stearic acid, oleic acid.
When preparing mesoporous nano carbon, phenolic resin and a small amount of potassium hydroxide are added to the water, such as the quality of potassium hydroxide
It can be the 0.9-1% of the quality of phenolic resin.
It is described above that technology contents of the invention are only further illustrated with embodiment, in order to which reader is easier to understand,
But embodiments of the present invention are not represented and are only limitted to this, any technology done according to the present invention extends or recreation, is sent out by this
Bright protection.
Claims (10)
1. a kind of friction improver containing mesoporous nano carbon, it is characterised in that: by each raw material group of following mass percentage
Divide and be made: the mesoporous nano carbon of 0.4-1.8%；The nano artificial graphite of 1.5-5.2%；The ashless dispersant of 0.2-7%；0.2-
1.6% organic molybdenum；The antioxidant of 0-0.5%；Base oil surplus.
2. the friction improver according to claim 1 containing mesoporous nano carbon, it is characterised in that: the mesoporous nano carbon
For spherical or cylindrical mesoporous nano carbon, granularity is less than 100nm.
3. the friction improver according to claim 1 containing mesoporous nano carbon, it is characterised in that: the nano artificial stone
The purity of ink is greater than 99.5%, and granularity is 0.5 μm.
4. the friction improver according to claim 1 containing mesoporous nano carbon, it is characterised in that: the ashless dispersant
Selected from least one of boronation polyisobutene succinimide, polyisobutylene succinic acid ester, benzylamine.
5. the friction improver according to claim 1 containing mesoporous nano carbon, it is characterised in that: the organic-molybdenum chemical combination
Object is selected from dialkyl dithiophosphoric acid oxygen molybdenum, nitrogenous dialkyl dithiophosphoric acid oxygen molybdenum, molybdenum dialkyldithiocarbamacompositions, ring
At least one of alkanoic acid molybdenum, alkyl salicylate molybdenum.
6. the friction improver according to claim 1 containing mesoporous nano carbon, it is characterised in that: the antioxidant choosing
From zinc dialkyl dithiophosphate, 4,4- di-2-ethylhexylphosphine oxide (2,6- di-tert-butylphenol), four [β (3,5- di-t-butyl -4- hydroxy benzenes
Base the third) acid] pentaerythritol ester, at least one of sulphide amino zinc formate.
7. the friction improver according to claim 1 containing mesoporous nano carbon, it is characterised in that: the base oil is complete
Synthetic base oil or semi-synthetic base oil, and viscosity index (VI) is 90 < VI < 120.
8. a kind of preparation method of the friction improver as described in claim 1 containing mesoporous nano carbon, which is characterized in that packet
Include following steps:
S1, base oil, part ashless dispersant and nano artificial graphite are mixed and is uniformly dispersed, be then ground to mixture afterwards
0.5 μm of partial size D50 <, obtain nano artificial graphite particle dispersion liquid；
S2, mesoporous nano carbon, remaining ashless dispersant, antioxidant and organic molybdenum are added to the nano artificial
It in graphite particle dispersion liquid, is uniformly dispersed, obtains friction improver.
9. the preparation method of the friction improver according to claim 8 containing mesoporous nano carbon, it is characterised in that: step
Mesoporous nano carbon described in S2 is made by following steps:
S21, phenolic resin and potassium hydroxide are added to the water and is heated to 70-80 DEG C and is stirred continuously, after mixing evenly, to mixed
It closes and triblock copolymer is added in object and is kept for 70-80 DEG C and is stirred continuously 10-15h, obtain mixed liquor；The potassium hydroxide
Quality is the 0.9-1% of the quality of phenolic resin；
S22, mixed liquor is placed at 100 DEG C and reacts 24-36h, then the mixed liquor after drying reaction, obtains powder；
S23, powder is placed under inert atmosphere, is warming up to 700 DEG C and constant temperature 2h with the speed of 5 DEG C/min, obtain nanometer Jie
Hole carbon；
S24, it disperses mesoporous nano carbon in petroleum ether, then heats dispersion liquid to 90 DEG C and constant temperature 30min, then to dispersion
Modifying agent is added in liquid and dispersion is equal, followed by the solid particle and drying collected in dispersion liquid, obtains modified nanometer
Mesoporous carbon；The quality of the modifying agent is the 11.5-23.1% of the quality of phenolic resin.
10. the preparation method of the friction improver according to claim 9 containing mesoporous nano carbon, it is characterised in that: institute
It states modifying agent and is selected from least one of hydrogen peroxide, nitric acid, stearic acid, oleic acid.
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