CN104017627B - A kind of preparation method of modified graphene oxide antiwear additive - Google Patents
A kind of preparation method of modified graphene oxide antiwear additive Download PDFInfo
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- CN104017627B CN104017627B CN201410269485.4A CN201410269485A CN104017627B CN 104017627 B CN104017627 B CN 104017627B CN 201410269485 A CN201410269485 A CN 201410269485A CN 104017627 B CN104017627 B CN 104017627B
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Abstract
The present invention relates to the preparation method of a kind of modified graphene oxide antiwear additive.The present invention adds graphene oxide and boracic, molybdenum, calcium, copper, the compound of rare earth element in there-necked flask, the heating of organic stirring solvent is added in said vesse, it is subsequently adding concentrated sulphuric acid as catalyst and to react, the boiling point being warming up to solvent steams solvent, product is put into vacuum drying oven be dried, i.e. obtain modified graphene oxide antiwear additive.Instant invention overcomes oily lubricant and kollag, but they have, and cost is high, use condition is harsher, change trouble, produce the problems such as waste pollution environment.The present invention utilizes graphene oxide lubrication ultra-thin, superhard, super, corrosion-resistant, the characteristic of high-temperature stability, by having the surface modification of abrasion resistance element, prepare the New Kind of Anti-Abrasion agent of excellent performance, this product can significantly improve the greasy property of lubricant, the friction and wear on mechanical movement surface is greatly decreased, there is material-saving and energy-conservation effect.
Description
Technical field
The invention belongs to lubrication technical field, particularly to the preparation side of a kind of modified graphene oxide antiwear additive
Method.
Background technology
Adding up according to internal authority mechanism, Material Wear, corrosion and fatigue three lossy account for total industrial output value
30%, fretting wear is the natural phenomena generally existed.Friction loss once of the world about 1/3rd
Source, abrasion is one of three kinds of topmost forms causing material and damage of facilities and inefficacy, and lubrication is then to reduce
Friction, the most effective technology of abrasion is reduced or avoided.Development have good wear resistance, high bearing capacity,
Wear surface is had certain repair function, adds up according to internal authority mechanism, Material Wear, burn into
Tired three lossies account for the 30% of total industrial output value, and fretting wear is the natural phenomena generally existed.Friction is damaged
The primary energy in the Shi Liao world about 1/3rd, abrasion is to cause material the most main with three kinds of damage of facilities and inefficacy
One of form wanted, lubrication is then to reduce the most effective technology of the abrasion that rubs, is reduced or avoided.Development has good
Good wear resistance, high bearing capacity, wear surface is had certain repair function, environmentally safe or few
The lubrication technology polluted, is one of contemporary chemistry important topic with material science and tribology.
Traditional extreme pressure grease improves extreme pressure and antiwear behavior and is mainly the organic compound of sulfur-bearing, chlorine and phosphorus, to the greatest extent
Pipe extreme pressure property is preferable, but sulfur, chlorine and phosphorus compound can produce corrosion and problem of environmental pollution.And extensively should
Zinc dialkyl dithiophosphate (ZDDP) efficiently extreme pressure anti-wear additives, the most having seemed is difficult to adapt to the situation sends out
The needs of exhibition.This is because: (1) element Zn can make some alloy bearing (referring mainly to argentiferous, lead parts)
Produce electrochemical corrosion；(2) antioxidation and pole can be lost under the operating mode higher than 160 degree because drastically decomposing
Pressure abrasion resistance.Therefore, searching can overcome the circumscribed novel extreme pressure anti-wear additives of ZDDP to become grease
The focus of research and development.
In kollag, for a long time, industrial lubricant mainly has two kinds: oily lubricant and
Kollag, but they have, and cost is high, use condition is harsher, change trouble, produce waste pollution ring
The problems such as border.The spies such as graphite is originated extensively with it as solid lubrication additive, price is low, solid lubricant effect is good
Point, is widely used in commercial production and has gone up the history of a century.But the superfine graphite used and molybdenum disulphide powder
The particle size at end is micron-scale, and shortcoming is that mixing uniformity is poor, and utilization rate is low, and addition is high.
Grapheme material has the shape ratio (plane sizes/thickness ratio) of super large, and maintains substantially leading of graphite
Electrical property and excellent lubrication, corrosion-resistant, high-temperature stability.Research shows, Graphene has now been found that
The material that in the middle of material, intensity is the highest, has mechanical strength and the similar graphite relatively low-shearing force of inherence, and has
There is Rotating fields feature, so being good kollag.
Summary of the invention
It is an object of the invention to overcome drawbacks described above, develop the preparation side of a kind of modified graphene oxide antiwear additive
Method.
The technical scheme is that
The preparation method of a kind of modified graphene oxide antiwear additive, it is mainly characterized by there-necked flask
Add graphene oxide and boracic, molybdenum, calcium, copper, the compound of rare earth element, there was added in said vesse
Machine stirring solvent heats, and is subsequently adding concentrated sulphuric acid and as catalyst and reacts, and the boiling point being warming up to solvent steams molten
Agent, puts into vacuum drying oven by product and is dried, and i.e. obtains modified graphene oxide antiwear additive.
Prepared by described graphene oxide Hummers method.
Described boracic, molybdenum, calcium, copper, the compound of rare earth element refer to boric acid, lanthanum borate, boric acid molybdenum,
Calcium pyroborate, one or more in copper borate.
Described graphene oxide and boracic, molybdenum, calcium, copper, the weight ratio of compound of rare earth element are 1:
0.5-3。
Described organic solvent is petroleum ether, water, ethanol, benzene, normal hexane, chloroform.
The weight of described concentrated sulfuric acid catalyst is the 0.1-0.5% of reactant.
Described reaction temperature 60-150 DEG C, the response time is 2-8h.
The vacuum drying temperature of described product is 20-80 DEG C.
Advantages of the present invention and effect are to utilize graphene oxide lubrication ultra-thin, superhard, super, corrosion-resistant, resistance to
The characteristic of hot properties, utilizes hydroxyl and carboxyl that surface of graphene oxide is abundant, by chemical method with having
It is modified by the element compound of abrasion resistance, by having the surface modification of abrasion resistance element, and preparation
Going out the New Kind of Anti-Abrasion agent of excellent performance, this product can significantly improve the greasy property of lubricant, be greatly decreased
The friction and wear on mechanical movement surface, has material-saving and energy-conservation effect.
Other concrete advantages of the present invention and effect will go on to say below.
Detailed description of the invention
Embodiment 1:
In 250mL there-necked flask, add 1.2g graphene oxide and 3.6g boric acid, be subsequently adding 30ml stone
Oil ether stirring adds 0.024g concentrated sulphuric acid, is warming up to 60 DEG C of condensing reflux reaction 8h, then steams solvent.Will
Product is put into 80 DEG C of vacuum drying ovens and is dried to obtain pale solid, is boric acid modified graphene oxide.According to
0.05% ratio is added in common lubricant fat, and wear scar diameter is reduced to 0.38 from the 0.96 of blank fat, abrasion
Rate decreases 60%, and coefficient of friction drops to 0.04 from the 0.106 of blank fat, and coefficient of friction decreases 60%.
Prepared by graphene oxide Hummers method, belong to employing prior art and prepare, therefore omit concrete
Preparation method.
Embodiment 2:
In 250mL there-necked flask, add 1g graphene oxide and 0.5g Calcium pyroborate, be just subsequently adding 70ml
Hexane is heated with stirring to 60 DEG C of addition 0.005g and drips concentrated sulphuric acid, is continuously heating to 150 DEG C of condensing refluxes reaction 2h,
Then solvent is steamed.Product is put into 20 DEG C of vacuum drying ovens and is dried to obtain pale solid, be Calcium pyroborate and change
Property graphene oxide.Being added in common lubricant fat according to 0.5% ratio, wear scar diameter is from the 0.96 of blank fat
Being reduced to 0.20, wear rate decreases 80%, and coefficient of friction drops to 0.02 from the 0.106 of blank fat, rubs
Wipe coefficient and decrease 80%.
Embodiment 3:
In 250mL there-necked flask, add 1g graphene oxide and 1.5g lanthanum borate is subsequently adding 50ml ethanol
It is heated with stirring to 80 DEG C and adds 0.020g concentrated sulphuric acid, be continuously heating to 130 DEG C of condensing reflux reaction 5h, then
Steam solvent.Product is put into 60 DEG C of vacuum drying ovens be dried pale solid is lanthanum borate graphite oxide
Alkene.Being added in common lubricant fat according to 0.1% ratio, wear scar diameter is reduced to 0.28 from the 0.96 of blank fat,
Wear rate reduces about 70%, and coefficient of friction drops to 0.04 from the 0.106 of blank fat, and coefficient of friction decreases
About 60%.
Embodiment 4:
In 250mL there-necked flask, add 1g graphene oxide and 1.2g copper borate is subsequently adding 10ml ethanol
It is heated with stirring to 40 DEG C and adds 0.023g concentrated sulphuric acid, be continuously heating to 120 DEG C of condensing reflux reaction 4h, then
Steam solvent.Product is put into 40 DEG C of vacuum drying ovens and is dried to obtain pale solid, be copper borate modification oxygen
Functionalized graphene.Being added in common lubricant fat according to 0.08% ratio, wear scar diameter subtracts from the 0.96 of blank fat
Little to 0.28, wear rate drops to the 70% of blank, and coefficient of friction drops to 0.02 from the 0.106 of blank fat,
Coefficient of friction decreases 80%.
The modified graphene oxide antiwear additive that the application present invention obtains, the ratio being added in lubricant is
0.05%-0.5%, wear rate compares more blank fat and decreases 50-100%, and coefficient of friction is compared more blank fat and reduced
50-100%.
Check embodiment 1-4, it can be seen that added by modified graphene in common lubricant fat by four ball frictions
Abrasion tester has carried out four-ball friction and wear experiment to it, and the condition of experiment is: pressure 392N；Rotating speed
1200r/min；Time 3600s.
Result shows, has through modified graphene oxide and significantly decreases abrasion, reduces the merit of coefficient of friction
Effect.
Table 1: additive and base oil sign under different proportion
Claims (4)
1. the preparation method of a modified graphene oxide antiwear additive, it is characterised in that add oxidation in there-necked flask
Graphene and boracic, molybdenum, calcium, copper, the compound of rare earth element, there was added in above-mentioned there-necked flask
Machine stirring solvent heats, and is subsequently adding concentrated sulphuric acid and as catalyst and reacts, and the boiling point being warming up to solvent steams
Go out solvent, product is put into vacuum drying oven and is dried, i.e. obtain modified graphene oxide antiwear additive；Described
Boracic, molybdenum, calcium, copper, the compound of rare earth element refer to boric acid, lanthanum borate, boric acid molybdenum, boric acid
One or more in calcium, copper borate are described graphene oxide and boracic, molybdenum, calcium, copper, dilute
The weight ratio of the compound of earth elements is: 1: 0.5-3, reaction temperature 60-150 DEG C, and the response time is 2-8h,
The weight of described concentrated sulfuric acid catalyst is the 0.1-0.5% of reactant.
The preparation method of a kind of modified graphene oxide antiwear additive the most according to claim 1, it is characterised in that
Prepared by described graphene oxide Hummers method.
The preparation method of a kind of modified graphene oxide antiwear additive the most according to claim 1, it is characterised in that
Described organic solvent is petroleum ether, ethanol, benzene, normal hexane or chloroform.
The preparation method of a kind of modified graphene oxide antiwear additive the most according to claim 1, it is characterised in that
The vacuum drying temperature of product is 20-80 DEG C, and drying time is 6-12h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104449948A (en) * | 2014-11-28 | 2015-03-25 | 上海应用技术学院 | Graphene-oxide-based zinc borate and preparation method thereof |
| CN105112124B (en) * | 2015-08-14 | 2018-05-15 | 中航联合石墨烯技术有限公司 | A kind of lubricant compositions based on graphene or graphene oxide and its preparation method and application |
| CN105154170B (en) * | 2015-09-21 | 2018-04-17 | 西南石油大学 | A kind of preparation method of nm boehmite combined oxidation graphene antifriction lubricant |
| CN106046037A (en) * | 2016-06-07 | 2016-10-26 | 山东源根石油化工有限公司 | Preparation of extreme pressure anti-wear agent and vehicle gear oil containing extreme pressure anti-wear agent |
| CN106221858B (en) * | 2016-07-07 | 2018-12-21 | 重庆德领科技有限公司 | A kind of polymolecularity and the modified graphene lubricating oil of high-affinity and preparation method thereof |
| CN106221859B (en) * | 2016-07-07 | 2018-12-21 | 重庆德领科技有限公司 | The modified graphene lubricating oil and preparation method thereof of polymolecularity energy |
| CN107090327B (en) * | 2017-04-21 | 2019-08-02 | 四川碳世界科技有限公司 | A kind of oleic acid boric acid modification lanthanum-stannic oxide/graphene nano composite lubricating oil and preparation method thereof |
| CN109294704B (en) * | 2018-10-16 | 2021-10-26 | 惠华科技有限公司 | Antiwear automatic gearbox oil and preparation process thereof |
| CN109233937B (en) * | 2018-10-16 | 2021-06-15 | 惠华科技有限公司 | Graphene oxide lubricating additive and application thereof in antiwear automatic transmission oil |
| CN109233938B (en) * | 2018-10-22 | 2021-09-28 | 深圳大学 | Modified graphene, preparation method thereof and lubricating oil |
| CN110373247B (en) * | 2019-07-18 | 2021-09-21 | 南京理工大学 | Functional graphene/montmorillonite/lanthanum borate composite lubricating oil additive |
| CN111286393B (en) * | 2020-03-13 | 2021-06-18 | 中国科学院过程工程研究所 | Rare earth wear-resistant lubricating grease and preparation method thereof |
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| US6960555B2 (en) * | 2003-05-15 | 2005-11-01 | Jet-Lube, Inc | Resin bonded particulate anti-seize agent, lubricating system made therefrom and methods of making and using same |
| CN103275787B (en) * | 2013-05-31 | 2014-12-31 | 太平洋联合(北京)石油化工有限公司 | Sulfur and phosphorous-containing extreme pressure anti-wear reagent and preparation method and application thereof |
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Effective date of registration: 20200102 Address after: 225000 Hongyuan Road, industrial concentration zone, Shaobo Town, Jiangdu District, Yangzhou City, Jiangsu Province Patentee after: Yangzhou Zhi Chuang Enterprise Operation Management Service Co., Ltd. Address before: 225009 No. 88, South University Road, Jiangsu, Yangzhou Patentee before: yangzhou university |
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