CN104017627A - Method for preparing modified graphene oxide anti-wear agent - Google Patents
Method for preparing modified graphene oxide anti-wear agent Download PDFInfo
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- CN104017627A CN104017627A CN201410269485.4A CN201410269485A CN104017627A CN 104017627 A CN104017627 A CN 104017627A CN 201410269485 A CN201410269485 A CN 201410269485A CN 104017627 A CN104017627 A CN 104017627A
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Abstract
The invention relates to a method for preparing a modified graphene oxide anti-wear agent. The method disclosed by the invention comprises the following steps: adding graphene oxide and a compound containing boron, molybdenum, calcium, copper and rare earth elements into a three-mouth flask, adding an organic solvent into the container, stirring, heating, adding concentrated sulphuric acid serving as a catalyst to react, heating to the boiling point temperature of the solvent to evaporate the solvent, putting the product into a vacuum drying oven to obtain the modified graphene oxide anti-wear agent. The method disclosed by the invention has the advantages that the problems that oily lubricants and solid lubricants are high in cost, strict in service condition, troublesome in replacement, not friendly to environment due to produced wastes and the like are solved; by utilizing the characteristics that the graphene oxide is ultrathin, ultrahard, ultra lubricative and resistant to corrosion and high temperature, the novel anti-wear agent with excellent performances is prepared through the surface modification of the elements with the anti-wear property; by means of the product, the lubricating property of the lubricants can be remarkably improved, the friction and the wear of the mechanical movement surface are reduced by a big margin and the efficacies of saving material and energy are provided.
Description
Technical field
The invention belongs to lubrication technical field, particularly a kind of preparation method of modified graphene oxide anti-wear agent.
Background technology
According to internal authority mechanism statistics, Material Wear, corrosion and fatigue three lossies account for 30% of gross industrial output value, and frictional wear is ubiquitous spontaneous phenomenon.Frictionloss the primary energy source in the world approximately 1/3rd, wearing and tearing are to cause one of three kinds of topmost forms of material and damage of facilities and inefficacy, lubricated be the effective technology that reduces friction, reduces or avoid wearing and tearing.Development have good wear resistance, high bearing capacity, to wear surface there is certain repairing effect, to adding up according to internal authority mechanism, Material Wear, corrosion and fatigue three lossies account for 30% of gross industrial output value, and frictional wear is ubiquitous spontaneous phenomenon.Frictionloss the primary energy source in the world approximately 1/3rd, wearing and tearing are to cause one of three kinds of topmost forms of material and damage of facilities and inefficacy, lubricated be the effective technology that reduces friction, reduces or avoid wearing and tearing.Development has good wear resistance, high bearing capacity, wear surface is had to the lubrication technology of certain repairing effect, environmentally safe or less contamination, is one of important topic of contemporary chemistry and Materials science and tribology.
It is mainly the organic compound of sulfur-bearing, chlorine and phosphorus that traditional extreme pressure grease improves extreme pressure and antiwear behavior, although extreme pressure property is better, sulphur, chlorine and phosphorus compound can produce corrosion and problem of environmental pollution.And the efficient extreme pressure anti-wear additives of the zinc dialkyl dithiophosphate of widespread use (ZDDP), the needs that now seemed and be difficult to adapt to the situation development.This be because: (1) element Zn can make some alloy bearing (mainly referring to argentiferous, plumbous parts) produce galvanic corrosion; (2) under the operating mode higher than 160 degree, can lose anti-oxidant and extreme pressure and antiwear behavior because sharply decomposing.Therefore, searching can overcome the circumscribed novel extreme pressure anti-wear additives of ZDDP has become the focus of lubricating grease research and development.
In solid lubricant, for a long time, the lubricant of industrial use mainly contains two kinds: oily lubricant and solid lubricant, but they have, cost is high, working conditions is harsher, change trouble, produce the problems such as waste pollution environment.Graphite, as features such as solid lubrication additive are wide with its source, price is low, solid lubricant effect is good, is widely used in the existing century-old history of industrial production.But the superfine graphite using and the particle size of molybdenum disulfide powder are micron-scale, and shortcoming is that mixing uniformity is poor, and utilization ratio is low, and addition is high.
Grapheme material has the shape of super large than (plane sizes/Thickness Ratio), and has kept the basic conduction property of graphite and good lubricated, corrosion-resistant, high-temperature stability.Research shows, Graphene is the highest material of intensity in the middle of the material of finding at present, has inherent physical strength and similar graphite compared with low-shearing power, and has a layer constructional feature, so be good solid lubricant.
Summary of the invention
The object of the invention is to overcome above-mentioned defect, develop a kind of preparation method of modified graphene oxide anti-wear agent.
Technical scheme of the present invention is:
A kind of preparation method of modified graphene oxide anti-wear agent, its technical characteristics is to add the compound of graphene oxide and boracic, molybdenum, calcium, copper, rare earth element in there-necked flask, in said vesse, add organic solvent stirring heating, then add the vitriol oil as catalyzer reaction, the boiling point that is warming up to solvent steams solvent, product is put into vacuum drying oven dry, obtain modified graphene oxide anti-wear agent.
Described graphene oxide is prepared by Hummers method.
The compound of described boracic, molybdenum, calcium, copper, rare earth element refers to boric acid, lanthanum borate, boric acid molybdenum, lime borate, one or more in copper borate.
The weight ratio of the compound of described graphene oxide and boracic, molybdenum, calcium, copper, rare earth element is 1: 0.5-3.
Described organic solvent is sherwood oil, water, ethanol, benzene, normal hexane, chloroform.
The weight of described concentrated sulfuric acid catalyst is the 0.1-0.5% of reactant.
Described temperature of reaction 60-150 DEG C, the reaction times is 2-8h.
The vacuum-drying temperature of described product is 20-80 DEG C.
Advantage of the present invention and effect are to utilize the characteristic of ultra-thin, superhard, super lubricated, corrosion-resistant, the high-temperature stability of graphene oxide, utilize abundant hydroxyl and the carboxyl in graphene oxide surface, use the element compound with abrasion resistance to carry out modification to it by chemical process, by thering is the surface modification of abrasion resistance element, prepare the New Kind of Anti-Abrasion agent of excellent performance, this product can significantly improve the lubricity of lubricant, significantly reduce the friction and wear on mechanical movement surface, there is material-saving and energy-conservation effect.
Other concrete advantages of the present invention and effect will go on to say below.
Embodiment
Embodiment 1:
In 250mL there-necked flask, add 1.2g graphene oxide and 3.6g boric acid, then add 30ml petroleum ether and stirring to add the 0.024g vitriol oil, be warming up to 60 DEG C of condensing reflux reaction 8h, then steam solvent.Product is put into 80 DEG C of vacuum drying ovens and be dried to obtain pale solid, be boric acid modified graphene oxide.Be added in common lubricating grease according to 0.05% ratio, wear scar diameter is reduced to 0.38 from 0.96 of blank fat, and wear rate has reduced 60%, and frictional coefficient drops to 0.04 from 0.106 of blank fat, and frictional coefficient has reduced 60%.
Graphene oxide is prepared by Hummers method, belongs to and adopts prior art preparation, therefore omit concrete preparation method.
Embodiment 2:
In 250mL there-necked flask, add 1g graphene oxide and 0.5g lime borate, then add 70ml normal hexane to be heated with stirring to 60 DEG C and add 0.005g to drip the vitriol oil, continue to be warming up to 150 DEG C of condensing reflux reaction 2h, then steam solvent.Product is put into 20 DEG C of vacuum drying ovens and be dried to obtain pale solid, be lime borate modified graphene oxide.Be added in common lubricating grease according to 0.5% ratio, wear scar diameter is reduced to 0.20 from 0.96 of blank fat, and wear rate has reduced 80%, and frictional coefficient drops to 0.02 from 0.106 of blank fat, and frictional coefficient has reduced 80%.
Embodiment 3:
In 250mL there-necked flask, add 1g graphene oxide and 1.5g lanthanum borate then to add 50ml ethanol to be heated with stirring to 80 DEG C and add the 0.020g vitriol oil, continue to be warming up to 130 DEG C of condensing reflux reaction 5h, then steam solvent.Product is put into 60 DEG C of vacuum drying ovens dry that pale solid is lanthanum borate graphene oxide.Be added in common lubricating grease according to 0.1% ratio, wear scar diameter is reduced to 0.28 from 0.96 of blank fat, and wear rate reduces by 70% left and right, and frictional coefficient drops to 0.04 from 0.106 of blank fat, and frictional coefficient has reduced by 60% left and right.
Embodiment 4:
In 250mL there-necked flask, add 1g graphene oxide and 1.2g copper borate then to add 10ml ethanol to be heated with stirring to 40 DEG C and add the 0.023g vitriol oil, continue to be warming up to 120 DEG C of condensing reflux reaction 4h, then steam solvent.Product is put into 40 DEG C of vacuum drying ovens and be dried to obtain pale solid, be copper borate modified graphene oxide.Be added in common lubricating grease according to 0.08% ratio, wear scar diameter is reduced to 0.28 from 0.96 of blank fat, and wear rate drops to 70% of blank, and frictional coefficient drops to 0.02 from 0.106 of blank fat, and frictional coefficient has reduced 80%.
The modified graphene oxide anti-wear agent that obtains of application the present invention, the ratio being added in lubricant is 0.05%-0.5%, and the wear rate blank fat of comparing has reduced 50-100%, and the frictional coefficient blank fat of comparing has reduced 50-100%.
Check embodiment 1-4, can find out, modified graphene is added in common lubricating grease, by four-ball friction and wear test machine, it carried out to four ball frictional wear experiments, and the condition of experiment is: pressure 392N; Rotating speed 1200r/min; Time 3600s.
Result shows to have significantly and reduce wear through the graphene oxide of modification, reduces effect of frictional coefficient.
Table 1: additive and the base oil sign under different ratios
Claims (9)
1. the preparation method of a modified graphene oxide anti-wear agent, it is characterized in that adding the compound of graphene oxide and boracic, molybdenum, calcium, copper, rare earth element in there-necked flask, in said vesse, add organic solvent stirring heating, then add the vitriol oil as catalyzer reaction, the boiling point that is warming up to solvent steams solvent, product is put into vacuum drying oven dry, obtain modified graphene oxide anti-wear agent.
2. the preparation method of a kind of modified graphene oxide anti-wear agent according to claim 1, prepared by the graphene oxide Hummers method described in it is characterized in that.
3. the preparation method of a kind of modified graphene oxide anti-wear agent according to claim 1, the compound that it is characterized in that described boracic, molybdenum, calcium, copper, rare earth element refers to boric acid, lanthanum borate, boric acid molybdenum, lime borate, one or more in copper borate.
4. according to the preparation method of a kind of modified graphene oxide anti-wear agent described in claim 1 or 3, it is characterized in that the weight ratio of the compound of described graphene oxide and boracic, molybdenum, calcium, copper, rare earth element is: 1: 0.5-3.
5. the preparation method of a kind of modified graphene oxide anti-wear agent according to claim 1, is characterized in that described organic solvent is sherwood oil, water, ethanol, benzene, normal hexane, chloroform.
6. the preparation method of a kind of modified graphene oxide anti-wear agent according to claim 1, is characterized in that described temperature of reaction 60-150 DEG C.
7. the preparation method of a kind of modified graphene oxide anti-wear agent according to claim 1, the 0.1-0.5% that the weight that it is characterized in that described concentrated sulfuric acid catalyst is reactant.
8. the preparation method of a kind of modified graphene oxide anti-wear agent according to claim 1, is characterized in that the described reaction times is 2-8h.
9. the preparation method of a kind of modified graphene oxide anti-wear agent according to claim 1, the vacuum-drying temperature that it is characterized in that product is 20-80 DEG C, be 6-12h time of drying.
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Cited By (12)
| 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 |
| CN105112124A (en) * | 2015-08-14 | 2015-12-02 | 中航联合石墨烯技术有限公司 | Graphene or graphene oxide based lubricant composition, and preparation method and application thereof |
| CN105154170A (en) * | 2015-09-21 | 2015-12-16 | 西南石油大学 | Preparation method of nanometer boehmite composite oxidized graphene antiwear 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 |
| CN106221859A (en) * | 2016-07-07 | 2016-12-14 | 重庆德领科技有限公司 | Modified graphene lubricating oil of high dispersive performance and preparation method thereof |
| CN106221858A (en) * | 2016-07-07 | 2016-12-14 | 重庆德领科技有限公司 | A kind of modified graphene lubricating oil of polymolecularity and high-affinity and preparation method thereof |
| CN107090327A (en) * | 2017-04-21 | 2017-08-25 | 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 |
| CN109233938A (en) * | 2018-10-22 | 2019-01-18 | 深圳大学 | Modified graphene and preparation method thereof and lubricating oil |
| CN109233937A (en) * | 2018-10-16 | 2019-01-18 | 郭健 | Graphene oxide lubricating additive and its application in wear-resistant automatic transmission fluid |
| CN109294704A (en) * | 2018-10-16 | 2019-02-01 | 郭健 | Wear-resistant automatic transmission fluid and its preparation process |
| CN110373247A (en) * | 2019-07-18 | 2019-10-25 | 南京理工大学 | Functional graphene/montmorillonite/boric acid lanthanide composite material lube oil additive |
| CN111286393A (en) * | 2020-03-13 | 2020-06-16 | 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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| CN103275787A (en) * | 2013-05-31 | 2013-09-04 | 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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| US20050187115A1 (en) * | 2003-05-15 | 2005-08-25 | Jet-Lube, Inc. | Resin bonded particulate anti-seize agent, lubricating system made therefrom and methods of making and using same |
| CN103275787A (en) * | 2013-05-31 | 2013-09-04 | 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 |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105112124A (en) * | 2015-08-14 | 2015-12-02 | 中航联合石墨烯技术有限公司 | Graphene or graphene oxide based lubricant composition, and preparation method and application thereof |
| 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 |
| CN105154170A (en) * | 2015-09-21 | 2015-12-16 | 西南石油大学 | Preparation method of nanometer boehmite composite oxidized graphene antiwear 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 |
| CN106221858A (en) * | 2016-07-07 | 2016-12-14 | 重庆德领科技有限公司 | A kind of modified graphene lubricating oil of polymolecularity and high-affinity and preparation method thereof |
| CN106221859A (en) * | 2016-07-07 | 2016-12-14 | 重庆德领科技有限公司 | Modified graphene lubricating oil of high dispersive performance and preparation method thereof |
| CN107090327A (en) * | 2017-04-21 | 2017-08-25 | 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 |
| 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 |
| CN109233937A (en) * | 2018-10-16 | 2019-01-18 | 郭健 | Graphene oxide lubricating additive and its application in wear-resistant automatic transmission fluid |
| CN109294704A (en) * | 2018-10-16 | 2019-02-01 | 郭健 | Wear-resistant automatic transmission fluid and its preparation process |
| CN109233938A (en) * | 2018-10-22 | 2019-01-18 | 深圳大学 | Modified graphene and preparation method thereof and lubricating 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 |
| CN110373247A (en) * | 2019-07-18 | 2019-10-25 | 南京理工大学 | Functional graphene/montmorillonite/boric acid lanthanide composite material lube oil additive |
| CN111286393A (en) * | 2020-03-13 | 2020-06-16 | 中国科学院过程工程研究所 | Rare earth wear-resistant lubricating grease and preparation method thereof |
| 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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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 |