CN101077988B - Method for preparing nano expanded graphite lubricating oil additive - Google Patents
Method for preparing nano expanded graphite lubricating oil additive Download PDFInfo
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- CN101077988B CN101077988B CN2007100622476A CN200710062247A CN101077988B CN 101077988 B CN101077988 B CN 101077988B CN 2007100622476 A CN2007100622476 A CN 2007100622476A CN 200710062247 A CN200710062247 A CN 200710062247A CN 101077988 B CN101077988 B CN 101077988B
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Abstract
The present invention relates to a process for preparing nanometer expandable graphite additive for lubricating oil. The process includes the following steps: (1) preparing expandable graphite worm; (2) preparing expandable graphite powder; and (3) performing a non-equilibrium grinding in a high energy ball mill by using the expandable graphite powder as raw materials, using GCr 15 bearing steel ball as the grinding body during grinding, the mass ratio of the steel ball and the expandable graphite being 4:1-10:1, the rotating speed of the ball mill being 100-160rpm, the grinding time being 30-100h; using alcohol as a ball milling medium so as to prevent the expandable graphite from coagulating during the grinding period; (4) preparing a lubricant: adding the nanometer expandable graphite additive into SJ 15W-40 type Kunlun lubricating oil, with the added amount being 2-7 wt% of the oil, preparing the lubricant. The lubricating oil with the nanometer expandable graphite additive has excellent friction-reduction and anti-friction performance in a wider temperature range and can effectively increase the service life of the friction pair.
Description
Technical field
The present invention relates to a kind of preparation method of nano expanded graphite lubricating oil additive.This additive material is added in the lubricating oil, shows excellent anti-wear and wear-resistant performance in wide temperature range, can effectively delay the work-ing life of friction pair.
Background technology
Wearing and tearing are one of three big principal modes of material failure.Friction then can consume a large amount of energy, it is reported, the 50%-70% of disposable energy consumption is relevant with friction in the world.The frictional wear of mechanical part also can cause very serious environmental pollution when bringing a large amount of losses of the material and the energy.Because nano-powder material has
Than tableCharacteristics such as area is big, high diffusibility and fusing point are low, therefore, it can significantly improve the friction pair friction and wear behavior during as the special lubricating oil additive.The carbon material that with graphite is representative is used widely in tribological field.Utilize the dimensional effect of nano material,, can further improve the tribological property of carbon material the carbon material nanometer." Nano diamond is inquired in the anti-friction wear-resistant mechanism at friction pair interface " (diamond and grinding materials and grinding tool engineering, 2001.4 (124): 4～10, Wang Yanhui etc.) literary composition is pointed out, between the ferrous materials friction pair, add and contain Nano diamond particulate lubricating oil, it is about 50% that frictional coefficient is reduced, and power consumption obviously reduces.Recently, " a kind of lubricating oil that contains nano-sheet graphite " (Chinese patent CN 1632082 A) are added into sheet nano graphite in the lubricating oil, have improved the antifriction antiwear ability and the supporting capacity of lubricating oil effectively.But the problem that there is the Applicable temperature narrow range in above-mentioned carbon nanomaterial during as lubricating oil additive, lost efficacy easily when temperature is higher.
Expanded graphite is the new carbon that natural graphite obtains after intercalation processing.Because the high temperature puffing effect, the distance between graphite linings and the layer is widened, and more easy glide has excellent more low rubbing characteristics.
Summary of the invention
The problem that has the Applicable temperature narrow range when overcoming carbon nanomaterial, lost efficacy easily when temperature is higher as lubricating oil additive, the invention provides a kind of nano expanded graphite lubricating oil additive and preparation method thereof, this nano expanded graphite lubricating oil additive, not only tribological property excellence, and broad application temperature range.
The technical solution adopted for the present invention to solve the technical problems is: be raw material with the expanded graphite, adopt high-energy ball-milling process to prepare the nano expanded graphite powder, utilize the porousness and the lipophilicity of expanded graphite, effectively slow down the degree of lubricating oil, thereby expand effective operating temperature range of lubricating oil in comparatively high temps generation deterioration.The preparation method of this nano expanded graphite lubricating oil additive may further comprise the steps:
(1) preparation of expanded graphite worm: handle the acquisition expanded graphite worm by natural flake graphite being carried out intercalation, washing, high temperature puffing etc.;
A. raw materials used is that granularity is the thin natural flake graphite of 180-220 purpose;
B. intercalator is the vitriol oil of concentration 90-98%, and oxygenant is the hydrogen peroxide of concentration 30%, at room temperature intercalation processing 8-15 minute;
C. the product water behind the intercalation is washed till pH value 7-9, afterwards, dried 1.5-2 hour down at 90-110 ℃ again, carry out high temperature puffing and handle under 800-1000 ℃ temperature, obtaining expansion multiple is 100-150 expanded graphite worm doubly;
(2) preparation of expanded graphite powder: above-mentioned expanded graphite worm is placed alcohol solvent, employing constant temperature timing electric mixer carries out 20-40 minute stirring with 200-400 rev/min revolution to it, and it is broken into about 1～3 micron expanded graphite powder of granularity;
(3) preparation of nano expanded graphite: adopting the expanded graphite powder is starting material, carries out non-equilibrium grinding in high energy ball mill; Grinding element during ball milling is the GCr15 steel ball of bearing steel, and the mass ratio of steel ball and expanded graphite (being ratio of grinding media to material) is 4: 1～10: 1, and the rotating speed of ball mill is 100～160 rev/mins, and the ball milling time is 30～100 hours; For expanded graphite during preventing ball milling condenses, select for use ethanol as ball-milling medium.
The invention has the beneficial effects as follows: the nano expanded graphite slip additive not only can show significant anti-wear and wear-resistant performance at normal temperatures, but also by utilizing self hole adsorpting lubrication medium, effectively slow down the degree of lubricating oil, thereby expand effective operating temperature range of lubricating oil in comparatively high temps generation deterioration.
Embodiment
Embodiment
The preparation of expanded graphite worm: under laboratory condition, adopt chemical method to prepare expanded graphite.Wherein, raw materials used be granularity be the thin natural flake graphite of 200 purposes (purity: 99.9%, the place of production: Shandong Nan Shu graphite company), intercalator is the vitriol oil of concentration 98%, and oxygenant is the hydrogen peroxide of concentration 30%.Intercalation processing is 10 minutes under about 25 ℃ room temperature, then, the product water behind the intercalation is washed till pH value 8, afterwards, dries 2 hours down at 100 ℃ again, carries out high temperature puffing and handle under 900 ℃ temperature.Obtaining expansion multiple is about 100 times expanded graphite worm.
The preparation of expanded graphite powder: with expansion multiple is that about 100 times expanded graphite worm places alcohol solvent, employing Changzhou state China JJ-3 type constant temperature timing electric mixer stirrer carries out about 30 minutes stirring with 300 rev/mins revolution to it, and it is broken into about 1～3 micron expanded graphite powder of granularity.
The preparation of nano expanded graphite powder: under laboratory condition, adopting prepared expanded graphite powder is starting material, preparation nano expanded graphite powder in the GN-2 type high energy ball mill that the new instrument in Shenyang mechanical ﹠ electrical equipment factory produces.Grinding element during ball milling is the GCr15 steel ball of bearing steel, and the mass ratio of steel ball and expanded graphite (being ratio of grinding media to material) is 5: 1, and the rotating speed of ball mill is 120 rev/mins, and the ball milling time is 50 hours.For intermediate phase micro mist during preventing ball milling condenses, select for use ethanol as ball-milling medium.
Lubricant formulation: in the lubricating oil of SJ 15W-40 type the Kunlun, add the nano expanded graphite slip additive powder of 3% (in massfraction), be deployed into lubricant.For guarantee that nano expanded graphite fully disperses in lubricating oil, the employing sorbitol anhydride oleate is a dispersion agent.
Tribological property is estimated
Adopt the omnipotent friction wear testing machine of MMU-5G type to carry out the tribology test.Wherein, the experiment load be 200 newton, rotating speed is 300 rev/mins, test period is 1 hour, two kinds to the mill material be respectively sprayed molybdenum alloy coat and 45# steel.Differing temps tribology test-results is as shown in table 1.
Experimental result shows: compare with pure base oil, when adding nano expanded graphite powder of the present invention in the lubricating oil, than under the high-load, normal temperature and high temperature all have tangible antifriction antiwear effect.
The tribology test-results of table 1 differing temps nano-graphite lubricant additive
Claims (1)
1. the preparation method of a nano expanded graphite lubricating oil additive is characterized in that:
(1) preparation of expanded graphite worm: by natural flake graphite being carried out intercalation, washing, high temperature puffing processing acquisition expanded graphite worm;
A. raw materials used is that granularity is the thin natural flake graphites of 200 purposes;
B. intercalator is the vitriol oil of concentration 90-98%, and oxygenant is the hydrogen peroxide of concentration 30%, at room temperature intercalation processing 8-15 minute;
C. the product water behind the intercalation is washed till pH value 7-9, afterwards, dried 1.5-2 hour down at 90-110 ℃ again, carry out high temperature puffing and handle under 800-1000 ℃ temperature, obtaining expansion multiple is 100-150 expanded graphite worm doubly;
(2) preparation of expanded graphite powder: above-mentioned expanded graphite worm is placed alcohol solvent, employing constant temperature timing electric mixer carries out 20-40 minute stirring with 200-400 rev/min revolution to it, and it is broken into the expanded graphite powder of 1～3 micron of granularity;
(3) preparation of nano expanded graphite: adopting the expanded graphite powder is starting material, in high energy ball mill, carry out non-equilibrium grinding, grinding element during ball milling is the GCr15 steel ball of bearing steel, the mass ratio of steel ball and expanded graphite is 4: 1～10: 1, the rotating speed of ball mill is 100～160 rev/mins, and the ball milling time is 30～100 hours; For expanded graphite during preventing ball milling condenses, select for use ethanol as ball-milling medium;
(4) lubricant formulation: in the lubricating oil of SJ15W-40 type the Kunlun, add the nano expanded graphite slip additive powder of counting 2-7% with massfraction, be deployed into lubricant; For guarantee that nano expanded graphite fully disperses in lubricating oil, the employing sorbitol anhydride oleate is a dispersion agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007100622476A CN101077988B (en) | 2007-06-29 | 2007-06-29 | Method for preparing nano expanded graphite lubricating oil additive |
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| CN2007100622476A CN101077988B (en) | 2007-06-29 | 2007-06-29 | Method for preparing nano expanded graphite lubricating oil additive |
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| CN101077988A CN101077988A (en) | 2007-11-28 |
| CN101077988B true CN101077988B (en) | 2011-07-27 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671591B (en) * | 2009-09-29 | 2012-09-05 | 燕山大学 | Method for preparing nano-graphite/molybdenum disulfide composite powder lubricant additive |
| CN101713298B (en) * | 2009-11-05 | 2012-03-07 | 昆山金发液压机械有限公司 | Hydraulic motor provided with friction pair with nanometer graphite layer and method for processing nanometer graphite layer |
| CN101812351B (en) * | 2010-04-01 | 2013-08-14 | 江苏工业学院 | Lubricating oil additive based on single-layer or more-layer graphene |
| CN101948639B (en) * | 2010-08-31 | 2012-11-21 | 长沙族兴新材料股份有限公司 | Method for preparing high floating value floating aluminum silver paste |
| CN103374434A (en) * | 2012-04-28 | 2013-10-30 | 夏华松 | Preparation method of expanded graphite lubricating oil |
| CN104726169B (en) * | 2013-12-19 | 2017-09-26 | 中国科学院过程工程研究所 | It is a kind of to be used to improve lubricating oil of friction member abrasion-resistant surface and preparation method thereof |
| CN111004665B (en) * | 2019-11-23 | 2022-05-17 | 凯盛石墨碳材料有限公司 | Preparation method of graphite-based nano titanium dioxide lubricating oil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1587034A (en) * | 2004-07-15 | 2005-03-02 | 同济大学 | Process for preparing nano porous graphite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1587034A (en) * | 2004-07-15 | 2005-03-02 | 同济大学 | Process for preparing nano porous graphite |
Non-Patent Citations (2)
| Title |
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| 刘德伟等.丁腈橡胶/膨胀石墨导电纳米复合材料的制备和性能.《精细化工》.2005,第22卷(第7期),第485-488页. * |
| 张瑞军等.高能球磨处理对碳质中间相结构及高温摩擦特性的影响.《润滑与密封》.2006,(第6期),第29-31页. * |
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