CN105018186B - Organic nitrogen molybdenum fullerene lubricant and preparation method thereof - Google Patents
Organic nitrogen molybdenum fullerene lubricant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of organic nitrogen molybdenum fullerene lubricant and preparation method thereof, the lubricant is prepared from by Modified with Polar Monomer Fullerene C20, succinamide, non-sulphur phosphorus organic-molybdenum；Wherein Modified with Polar Monomer Fullerene C20, succinamide, the weight ratio of non-sulphur phosphorus organic-molybdenum are：1：5~8：30~35.Modified with Polar Monomer Fullerene C20 is made up of Fullerene C20, concentrated nitric acid, concentrated hydrochloric acid, castor oil acid reaction.The additive is a kind of organic nitrogen molybdenum fullerene lubricant, it is the lubricating oil particularly friction improver of I. C. engine lubricating oil, antiwear additive and antioxidant, oil-saving effect is notable, due to not containing sulphur, phosphorus, chlorine, the additive also has the advantages that energy-conserving and environment-protective, and production method is simple, cost is low, oil-soluble is good, yield is high.
Description
Technical field
The present invention relates to organic nitrogen molybdenum fullerene lubricant and preparation method thereof, specifically a kind of oil-soluble organic nitrogen
Molybdenum fullerene lubricant class compound and preparation method thereof.
Background technology
Fullerene C20 is due to its unique architectural characteristic, as physics in recent years, chemistry, materialogy and life section
The focus of etc. numerous subjects and related application area research.The torispherical particle that it is made up of concentric completed shell, its layer
Spacing is 0.349nm, is close with the interlamellar spacing 0.336nm of graphite, is all the lubricant of function admirable.
If fullerene is applied in lubricating oil, the antiwear and antifriction characteristic of lubricating oil, effectively protection can be greatly improved
Engine, but because fullerene is solid, the use in lubricating oil is limited.
Non- sulphur phosphorus organic-molybdenum is to apply anti-friction agent most top in lubricating oil, it not only have excellent antifriction performance and
Fabulous high-temperature oxidation resistance, also with good oily molten and dispersive property；Coordinating with fullerene can be significantly in lubricating oil
The wear-resistant of lubricating oil, antifriction, inoxidizability function are improved, can effectively extend the drain period, more effective lasting protection is started
Machine.
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of production method is simple, cost is low, oil-soluble good, yield
High organic nitrogen molybdenum fullerene lubricant and preparation method thereof.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of organic nitrogen molybdenum fullerene lubricant
Preparation method, reacted based on Fullerene C20 with concentrated nitric acid, concentrated hydrochloric acid, add castor oil acid, using regulation pH value
Method, obtains Modified with Polar Monomer fullerene, is then reacted with succinamide, non-sulphur phosphorus organic-molybdenum, takes two step partial pressures to depressurize method, is made
Organic nitrogen molybdenum fullerene lubricant, including step are as follows：
1) synthesis of Modified with Polar Monomer fullerene
Fullerene C20 and concentrated nitric acid, concentrated hydrochloric acid are placed in container, under conditions of 90 DEG C~100 DEG C vacuum react 2~
3 hours, then wash, alcohol is washed, between adjustment pH=6.5~7, add castor oil acid, being 180~200 DEG C in temperature continues instead
Answer 3~4 hours, then vacuum filter, obtains sediment, and alcohol is washed, is washed to neutrality, obtain brown paste rich for Modified with Polar Monomer
Strangle alkene, the Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：Mass ratio=1 of castor oil acid：8.5~10：8.5~10：17~20；
2) synthesis of organic nitrogen molybdenum fullerene lubricant
The Modified with Polar Monomer fullerene of above-mentioned preparation is mixed with succinamide, in 90~100 DEG C of temperature, pressure after stirring
Under the conditions of power 0.2MPa, react 4~5 hours；Be cooled to 50~60 DEG C, add non-sulphur phosphorus organic-molybdenum, heighten temperature to 180~
190 DEG C, continue under pressure permanence condition to react 3~4 hours, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa；Most
After filter, obtain brown color organic nitrogen molybdenum fullerene lubricant, the Modified with Polar Monomer fullerene：Succinamide：Non- sulphur phosphorus is organic
Weight ratio=1 of molybdenum：5~8：30~35.
The step 1) in synthetic reaction vacuum condition be 0.098~0.1MPa.
The step 1) in washing, alcohol adjust pH=7 after washing.
The raw material weight ratio, Modified with Polar Monomer fullerene：Succinamide：Non- sulphur phosphorus organic-molybdenum=1：6：32；Fullerene
C60：Concentrated nitric acid：Concentrated hydrochloric acid：Castor oil acid=1：9：9：18.
Organic nitrogen molybdenum fullerene lubricant prepared by above-mentioned preparation method.
The beneficial effects of the invention are as follows：Prepare the organic nitrogen molybdenum fullerene lubrication with good lubricating properties and splendid wear resistence
Agent, the particularly friction improver of I. C. engine lubricating oil, antiwear additive and antioxidant, oil-saving effect are notable.With section
Energy, low-sulfur, it is low-phosphorous, without chlorine, environmental protection, efficient advantage.
Embodiment
The present invention is described in further detail with reference to embodiment：
The preparation method of the organic nitrogen molybdenum fullerene lubricant of the present invention, with concentrated nitric acid, dense salt based on Fullerene C20
Acid reaction, adds castor oil acid, using the method for regulation pH value, Modified with Polar Monomer fullerene is obtained, then with succinamide, non-sulphur
Phosphorus organic-molybdenum reacts, and takes two step partial pressures to depressurize method, and obtained organic nitrogen molybdenum fullerene lubricant, including step are as follows：
1) synthesis of Modified with Polar Monomer fullerene
Fullerene C20 and concentrated nitric acid, concentrated hydrochloric acid are placed in container, under conditions of 90 DEG C~100 DEG C vacuum react 2~
3 hours, then wash, alcohol is washed, between adjustment pH=6.5~7, add castor oil acid, being 180~200 DEG C in temperature continues instead
Answer 3~4 hours, then vacuum filter, obtains sediment, and alcohol is washed, is washed to neutrality, obtain brown paste rich for Modified with Polar Monomer
Strangle alkene, the Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：Mass ratio=1 of castor oil acid：8.5~10：8.5~10：17~20；
2) synthesis of organic nitrogen molybdenum fullerene lubricant
The Modified with Polar Monomer fullerene of above-mentioned preparation is mixed with succinamide, in 90~100 DEG C of temperature, pressure after stirring
Under the conditions of power 0.2MPa, react 4~5 hours；Be cooled to 50~60 DEG C, add non-sulphur phosphorus organic-molybdenum, heighten temperature to 180~
190 DEG C, continue under pressure permanence condition to react 3~4 hours, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa；Most
After filter, obtain brown color organic nitrogen molybdenum fullerene lubricant, the Modified with Polar Monomer fullerene：Succinamide：Non- sulphur phosphorus is organic
Weight ratio=1 of molybdenum：5~8：30~35.
The step 1) in synthetic reaction vacuum condition be 0.098~0.1MPa.
The step 1) in washing, alcohol adjust pH=7 after washing.
The raw material weight ratio, Modified with Polar Monomer fullerene：Succinamide：Non- sulphur phosphorus organic-molybdenum=1：6：32；Fullerene
C60：Concentrated nitric acid：Concentrated hydrochloric acid：Castor oil acid=1：9：9：18.
Organic nitrogen molybdenum fullerene lubricant prepared by above-mentioned preparation method.
The present invention is Fullerene C20 first to be carried out Modified with Polar Monomer transformation and then effectively coordinated with non-sulphur phosphorus organic-molybdenum；By
Fullerene after modification, its surface can be substantially reduced, and form monomolecular adsorption layer, hydrophilic group towards fullerene surface,
Lipophilic group is outside, and this aspect makes fullerenic particles have lipophile, and oil-soluble non-sulphur phosphorus organic-molybdenum compatibility is combined, and is made
Fullerene adsorption can be dissolved completely in and hinder the collision of fullerene to reunite and again in lubricating oil on the surface of non-sulphur phosphorus organic-molybdenum
Power is precipitated, so as to improve dispersiveness and stability of the organic nitrogen molybdenum fullerene lubricant in lubricating oil.
Organic nitrogen molybdenum fullerene lubricant is dissolved in various lubricating oil in liquid form, and minimized friction coefficient can be reduced to
0.0127；The film forming and bearing capacity of lubricating oil can be significantly improved.Lubrication mechanism is that sliding friction and rolling friction is effective
Fusion.Under lubricating component nominal situation, form a kind of with antifriction, the physics of wear-resistant effect, chemistry suction in friction surface
Membrane, this adsorbed film is sliding friction；Under the harsh operating mode such as high speed, high temperature, high pressure, in the fowler of surface of friction pair
Sliding friction is changed into rolling friction by the alkene factor, closer to one layer of protection engine.
This sliding friction and rolling friction are effectively merged, and are even belonged in our countries in other various countries of the world super
Preceding precedent.
Such a organic nitrogen molybdenum fullerene lubricant, be fullerene together with non-sulphur phosphorus organic-molybdenum organic synthesis, be from
The liquefied compound of subtype, oil-soluble is good, never precipitates.And mesh is without phosphorus without chlorine without sulphur, plus dosage is small, performance is high, is one
Plant rare environmental friendly lubricant.
Domestic at present or even external fullerene lube oil additive is all solid nano type, with dispersant to profit
In lubricating oil, time length can precipitate.
Experimental data shows, this 0.5% organic nitrogen molybdenum fullerene lubricant is added in engine oil, coefficient of friction can
To be reduced to less than 0.0127 (coefficient of friction of conventional engine oil is more than 0.08), 40 kgf of four-ball tester is 60 minutes long to rub
Experiment, wear scar diameter only has the 0.30mm wear scar diameter of oil (conventional engine be 0.50 or so), and temperature reaches 45 degree, not followed by
Height of continuing rising.So following effect can be reached using organic nitrogen molybdenum fullerene lubricant
1st, coefficient of friction is reduced：More than 80% can be reduced.
2nd, engine temperature is reduced：During using common lubricant oil additive, engine temperature can reach 170 DEG C or so,
Additive of the present invention is added, the temperature of engine is just no longer raised to 45 degree.
3rd, fuel oil is saved：Can be with fuel-economizing more than 15%.
4th, the drain period is extended：10000 kilometers or more more oil changes can be extended to.
Embodiment 1
1st, the synthesis of Modified with Polar Monomer fullerene
Fullerene C20 and concentrated nitric acid, concentrated hydrochloric acid are placed in container, in the condition of 100 DEG C of vacuum (pressure=0.10MPa)
It is lower to react 2 hours, then wash, alcohol is washed, adjust pH=6.5, add castor oil acid, be that 180 DEG C of continuation reactions 3 are small in temperature
When, then vacuum filter, obtains pasty mixture, and alcohol is washed, is washed to neutrality, obtains brown paste for Modified with Polar Monomer fowler
Alkene；
Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：Castor oil acid=1：9：9：18 (weight ratios).
2nd, the synthesis of organic nitrogen molybdenum fullerene lubricant
5 grams of the Modified with Polar Monomer fullerene of above-mentioned preparation is mixed for 30 grams with succinamide, after stirring 90 DEG C of temperature,
Under the conditions of pressure 0.2MPa, react 4 hours；50 DEG C are cooled to, non-160 grams of sulphur phosphorus organic-molybdenum is added, heightens temperature to 180 DEG C,
Continue to react 3 hours under pressure permanence condition, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa；Finally filter, obtain
To brown color organic nitrogen molybdenum fullerene lubricant.
The antifriction antiwear of product and the investigation of bearing capacity：Determined using four-ball tester, setting load (bear by 20 DEG C of temperature
Lotus 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, the steel ball used in four-ball test is straight
Footpath 12.7mm GCR steel balls, experiment shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly use
Lubricating oil, wear scar diameter reaches 0.8mm.0.5% (weight) the present embodiment is added in API SN5W/40 lubricating oil and prepares product,
Wear scar diameter reaches 0.30mm, coefficient of friction 0.0119.
Embodiment 2
1st, the synthesis of Modified with Polar Monomer fullerene
Fullerene C20 and concentrated nitric acid, concentrated hydrochloric acid are placed in container, in the condition of 90 DEG C of vacuum (pressure=0.10MPa)
It is lower to react 2.5 hours, then wash, alcohol is washed, adjust pH=7, add castor oil acid, be that 200 DEG C of continuation reactions 3.5 are small in temperature
When, then vacuum filter, obtains pasty mixture, and alcohol is washed, is washed to neutrality, obtains brown paste for Modified with Polar Monomer fowler
Alkene；
Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：Castor oil acid=1：10：10：20 (weight ratios).
2nd, the synthesis of organic nitrogen molybdenum fullerene lubricant
4 grams of the Modified with Polar Monomer fullerene of above-mentioned preparation is mixed for 20 grams with succinamide, in temperature 100 after stirring
DEG C, under the conditions of pressure 0.2MPa, react 5 hours；60 DEG C are cooled to, non-120 grams of sulphur phosphorus organic-molybdenum is added, heightens temperature to 190
DEG C, continue to react 4 hours under pressure permanence condition, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa；Finally filter,
Obtain brown color organic nitrogen molybdenum fullerene lubricant.
The antifriction antiwear of product and the investigation of bearing capacity：Determined using four-ball tester, setting load (bear by 20 DEG C of temperature
Lotus 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, the steel ball used in four-ball test is straight
Footpath 12.7mm GCR steel balls, experiment shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly use
Lubricating oil, wear scar diameter reaches 0.8mm.0.5% (weight) the present embodiment is added in API SN5W/40 lubricating oil and prepares product,
Wear scar diameter reaches 0.31mm, coefficient of friction 0.0125.
Embodiment 3
1st, the synthesis of Modified with Polar Monomer fullerene
Fullerene C20 and concentrated nitric acid, concentrated hydrochloric acid are placed in container, in the condition of 95 DEG C of vacuum (pressure=0.10MPa)
It is lower to react 3 hours, then wash, alcohol is washed, adjust pH=6.5, add castor oil acid, be that 190 DEG C of continuation reactions 4 are small in temperature
When, then vacuum filter, obtains pasty mixture, and alcohol is washed, is washed to neutrality, obtains brown paste for Modified with Polar Monomer fowler
Alkene；
Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：Castor oil acid=1：8.5：9：19 (weight ratios).
2nd, the synthesis of organic nitrogen molybdenum fullerene lubricant
8 grams of the Modified with Polar Monomer fullerene of above-mentioned preparation is mixed for 56 grams with succinamide, after stirring 95 DEG C of temperature,
Under the conditions of pressure 0.2MPa, react 4.5 hours；50 DEG C are cooled to, non-256 grams of sulphur phosphorus organic-molybdenum is added, heightens temperature to 185
DEG C, continue to react 3.5 hours under pressure permanence condition, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa；Finally cross
Filter, obtains brown color organic nitrogen molybdenum fullerene lubricant.
The antifriction antiwear of product and the investigation of bearing capacity：Determined using four-ball tester, setting load (bear by 20 DEG C of temperature
Lotus 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, the steel ball used in four-ball test is straight
Footpath 12.7mm GCR steel balls, experiment shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly use
Lubricating oil, wear scar diameter reaches 0.8mm.0.5% (weight) the present embodiment is added in API SN5W/40 lubricating oil and prepares product,
Wear scar diameter reaches 0.29mm, coefficient of friction 0.0115.
Embodiment 4
1st, the synthesis of Modified with Polar Monomer fullerene
Fullerene C20 and concentrated nitric acid, concentrated hydrochloric acid are placed in container, in the condition of 90 DEG C of vacuum (pressure=0.10MPa)
Lower reaction 3 hours, then washes, alcohol is washed, adjusts pH=7, add castor oil acid, and being 190 DEG C in temperature continues reaction 3 hours,
Then vacuum filter, obtains pasty mixture, and alcohol is washed, is washed to neutrality, obtains brown paste for Modified with Polar Monomer fullerene；
Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：Castor oil acid=1：9：8.7：17 (weight ratios).
2nd, the synthesis of organic nitrogen molybdenum fullerene lubricant
3 grams of the Modified with Polar Monomer fullerene of above-mentioned preparation is mixed for 15 grams with succinamide, after stirring 98 DEG C of temperature,
Under the conditions of pressure 0.2MPa, react 4 hours；60 DEG C are cooled to, non-90 grams of sulphur phosphorus organic-molybdenum is added, heightens temperature to 195 DEG C, is pressed
Continue to react 3 hours under power permanence condition, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa；Finally filter, obtain
Brown color organic nitrogen molybdenum fullerene lubricant.
The antifriction antiwear of product and the investigation of bearing capacity：Determined using four-ball tester, setting load (bear by 20 DEG C of temperature
Lotus 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, the steel ball used in four-ball test is straight
Footpath 12.7mm GCR steel balls, experiment shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly use
Lubricating oil, wear scar diameter reaches 0.8mm.0.5% (weight) the present embodiment is added in API SN5W/40 lubricating oil and prepares product,
Wear scar diameter reaches 0.31mm, coefficient of friction 0.0127.
In summary, present disclosure is not limited in the above embodiments, and the knowledgeable people in same area can
Can propose other embodiments easily within the technological guidance's thought of the present invention, but this embodiment is included in this hair
Within the scope of bright.
Claims (5)
1. a kind of preparation method of organic nitrogen molybdenum fullerene lubricant, it is characterised in that with dense nitre based on Fullerene C20
Acid, concentrated hydrochloric acid reaction, add castor oil acid, using the method for regulation pH value, Modified with Polar Monomer fullerene are obtained, then with succinyl
Amine, the reaction of non-sulphur phosphorus organic-molybdenum, take two step partial pressures to depressurize method, and obtained organic nitrogen molybdenum fullerene lubricant, including step are as follows：
1) synthesis of Modified with Polar Monomer fullerene
Fullerene C20 and concentrated nitric acid, concentrated hydrochloric acid are placed in container, 2~3 are reacted under conditions of 90 DEG C~100 DEG C vacuum small
When, then washing, alcohol are washed, and between adjustment pH=6.5~7, add castor oil acid, and being 180~200 DEG C in temperature continues to react 3
~4 hours, then vacuum filter, obtained sediment, and alcohol is washed, is washed to neutrality, obtained brown paste for Modified with Polar Monomer fowler
Alkene, the Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：Mass ratio=1 of castor oil acid：8.5~10：8.5~10：17~20；
2) synthesis of organic nitrogen molybdenum fullerene lubricant
The Modified with Polar Monomer fullerene of above-mentioned preparation is mixed with succinamide, in 90~100 DEG C of temperature, pressure after stirring
Under the conditions of 0.2MPa, react 4~5 hours；50~60 DEG C are cooled to, non-sulphur phosphorus organic-molybdenum is added, heightens temperature to 180~190
DEG C, continue to react 3~4 hours under pressure permanence condition, then cool to 100 DEG C, be evacuated to pressure to 0.1MPa；Finally cross
Filter, obtains brown color organic nitrogen molybdenum fullerene lubricant, the Modified with Polar Monomer fullerene：Succinamide：Non- sulphur phosphorus organic-molybdenum
Weight ratio=1：5~8：30~35.
2. the preparation method of organic nitrogen molybdenum fullerene lubricant according to claim 1, it is characterised in that the step 1) in
The condition of the vacuum of synthetic reaction is 0.098~0.1MPa.
3. the preparation method of organic nitrogen molybdenum fullerene lubricant according to claim 1, it is characterised in that the step 1) in
Washing, alcohol adjust pH=7 after washing.
4. the preparation method of organic nitrogen molybdenum fullerene lubricant according to claim 1, it is characterised in that the raw material weight
Than Modified with Polar Monomer fullerene：Succinamide：Non- sulphur phosphorus organic-molybdenum=1：6：32；The Fullerene C20：Concentrated nitric acid：Concentrated hydrochloric acid：
Castor oil acid=1：9：9：18.
5. organic nitrogen molybdenum fullerene lubricant prepared by a kind of preparation method as described in claim any one of 1-4.
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| CN106190434B (en) * | 2016-07-04 | 2018-11-02 | 王严绪 | Nitrogen molybdenum complex lube oil additive and preparation method thereof |
| CN109536250B (en) * | 2018-11-02 | 2021-09-14 | 欧陆宝(天津)新材料科技有限公司 | Environment-friendly degradable aluminum and aluminum alloy drawing process lubricant and preparation method thereof |
| CN109679752B (en) * | 2019-01-29 | 2021-10-15 | 汉能（青岛）润滑科技有限公司 | Degradable lubricating oil adopting permeation layer technology and preparation method thereof |
| CN109929624B (en) * | 2019-04-25 | 2020-02-07 | 上海鑫灵精细化工有限公司 | Composition of fatty acid diesel antiwear agent and preparation method thereof |
| CN110564484A (en) * | 2019-09-16 | 2019-12-13 | 连云港爱华能源科技发展有限公司 | Antiwear repairing agent for engine oil |
| CN111269741A (en) * | 2020-03-11 | 2020-06-12 | 上海金山廊林实业有限公司 | Composition of friction modifier for vehicle engine oil |
| CN111718776A (en) * | 2020-07-31 | 2020-09-29 | 锐典科技有限公司 | Composite additive for lubricating oil |
| CN112080331A (en) * | 2020-09-24 | 2020-12-15 | 苏州金钼润成润滑科技有限公司 | Organic nitrogen zirconium fullerene lubricant and preparation method thereof |
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| CN1406164A (en) * | 2000-03-06 | 2003-03-26 | 耶达研究与开发有限公司 | Hollow fullerene-like nanoparticles as solid lubricants in composite metal matrices |
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Effective date of registration: 20220211 Address after: 5-3, independent courtyard of Dahua Chunshan Mingyue phase I, No. 3186, Keji Avenue, Jinbei street, Lin'an District, Hangzhou, Zhejiang Patentee after: Huayi Jinwei (Hangzhou) energy Co.,Ltd. Address before: 300384 floor 16, building 2, Dingjia Park, No. 2, Lanyuan Road, Huayuan Industrial Park, Nankai District, Tianjin Patentee before: Wang Yanxu |
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