WO2014189065A1 - Lubrifiant a base d'eau - Google Patents

Lubrifiant a base d'eau Download PDF

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Publication number
WO2014189065A1
WO2014189065A1 PCT/JP2014/063398 JP2014063398W WO2014189065A1 WO 2014189065 A1 WO2014189065 A1 WO 2014189065A1 JP 2014063398 W JP2014063398 W JP 2014063398W WO 2014189065 A1 WO2014189065 A1 WO 2014189065A1
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WO
WIPO (PCT)
Prior art keywords
water
graphite
graphene oxide
sliding
sp1go
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PCT/JP2014/063398
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English (en)
Japanese (ja)
Inventor
博 木之下
勇太 仁科
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国立大学法人岡山大学
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Priority to JP2015518269A priority Critical patent/JPWO2014189065A1/ja
Publication of WO2014189065A1 publication Critical patent/WO2014189065A1/fr

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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
    • C10M173/00—Lubricating compositions containing more than 10% water
    • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
    • 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
    • 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
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • 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
    • 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
    • C10N2040/20—Metal working
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants

Definitions

  • the present invention relates to an aqueous lubricant containing graphene oxide.
  • oil-based materials such as machine oil and machining oil are used as lubricants.
  • a coating made of a highly lipophilic material is provided on the contact surface.
  • a carbon atom-containing inorganic material such as graphite, diamond-like carbon, or carbon nanotube as a highly lipophilic material (see, for example, Patent Document 1).
  • these coatings are formed on the inner surface of the surface texturing by innumerable recesses formed on the contact surface.
  • Oil-based lubricants are extremely inexpensive and are widely used. However, when an oil-based lubricant is used as, for example, cutting oil, it is necessary to degrease the workpiece, and various chemicals for this degreasing treatment are necessary, and it is easy to increase the cost in the post-treatment. It was.
  • oil-based lubricants have a problem of flammability
  • water-soluble lubricants that are used by mixing with water are also used recently.
  • a cleaning process using an appropriate chemical is necessary, and an aqueous lubricant that can be easily post-processed has been demanded.
  • an aqueous lubricant containing a nanocarbon material such as fullerene in an aqueous solvent see, for example, Patent Document 2
  • processing in which ultrafine particles such as fullerene and carbon nanotubes are dispersed in water containing a surfactant has been proposed.
  • water-based lubricants in which carbon materials such as fullerenes are dispersed originally have low dispersibility of carbon materials such as fullerenes in water, so various additives such as surfactants are necessary and are flammable.
  • various additives such as surfactants are necessary and are flammable.
  • one of the inventors of the present invention has invented a production method that makes it possible to produce graphene oxide highly dispersed in water at a lower cost than before.
  • the inventors of the present invention have been studying the use of graphene oxide produced by this production method. As a result, they have found that it can be used as a lubricant, and have achieved the present invention.
  • the aqueous lubricant of the present invention is an aqueous lubricant in which graphene oxide formed by exfoliating graphite and exfoliating it from graphite is dispersed in water.
  • the exfoliation treatment is performed by mixing graphite with an aqueous solution containing an oxidizing agent. In this way, peeling is caused by oxidizing graphite.
  • the aqueous lubricant of the present invention is also characterized by the following points.
  • the graphite should be fine powder with an average particle size of 100 ⁇ m or less.
  • (3) Graphite should contain graphene oxide at a concentration of 0.01 wt% or more as a fine powder with an average particle size of 50 ⁇ m or less.
  • an aqueous lubricant using graphene oxide that is highly dispersed in water can be used as a lubricant without using an extra additive. Furthermore, in the water-based lubricant of the present invention, graphene oxide itself is harmless in post-treatment after use as a lubricant, so that it can be disposed of easily and at low cost.
  • (A) is an SEM image of the sliding surface of the ball after 60,000 sliding tests with a friction tester in the case of 1 wt% SP1GO dispersed water.
  • (B) is the sliding surface of (a). It is a measurement result of carbon element component distribution by energy dispersive X-ray spectroscopic analysis (EDX).
  • (A) is an SEM image of the sliding surface of the substrate (SUS304) after 60,000 sliding tests with a friction tester in the case of 1 wt% SP1GO dispersed water
  • (b) is (a) 3 is a measurement result of a carbon element component distribution by energy dispersive X-ray spectroscopy (EDX) on a sliding surface of the steel.
  • the aqueous lubricant of the present invention is an aqueous lubricant in which graphene oxide obtained by subjecting graphite to exfoliation and exfoliating from graphite is dispersed in water.
  • exfoliation is caused by mixing graphite in an aqueous solution containing an oxidizing agent to oxidize the graphite.
  • the graphene oxide formed by peeling from graphite into water to form an aqueous lubricant, the graphene oxide can be suitably maintained in a dispersed state without any other additive, and used as a lubricant. Can function.
  • graphene oxide itself is harmless and functions as a lubricant even without other additives, it can be disposed of easily and at low cost in post-treatment after use as a lubricant. If necessary, graphene oxide can be decomposed by adding an appropriate acid to the waste liquid after use as a lubricant, and the graphene oxide itself can be lost.
  • the graphite to be exfoliated is desirably a fine powder having an average particle diameter of 100 ⁇ m or less, and preferably a fine powder having an average particle diameter of 50 ⁇ m or less.
  • the average particle size of graphite By setting the average particle size of graphite to 100 ⁇ m or less, the average particle size of graphene oxide also becomes 100 ⁇ m or less, and the graphene oxide concentration in the aqueous lubricant can be used as a lubricant by setting it to 0.1 wt% or more.
  • the average particle size of graphite is set to 50 ⁇ m or less, the average particle size of graphene oxide also becomes 50 ⁇ m or less, and the concentration of graphene oxide in an aqueous lubricant can be set to 0.01 wt% or more and can be used as a lubricant. That is, by using graphene oxide having a smaller diameter, the concentration of graphene oxide can be reduced, and the amount of graphene oxide used can be reduced, so that a less expensive aqueous lubricant can be provided.
  • a friction tester was used as a method for evaluating the aqueous lubricant of the present invention.
  • the friction tester used in this example is composed of a flat substrate, a ball arranged in contact with the upper surface of the substrate, and a sliding mechanism for reciprocatingly sliding the ball on the substrate. .
  • the ball is reciprocated on the substrate without rotating at all.
  • the material of the substrate is SUS304 and the surface is smoothed by grinding.
  • the material of the ball is a very hard ball for bearings (tansten carbide), with a 1 mm radius.
  • the ball sliding conditions were such that the sliding distance for one cycle was about 2 mm and the sliding time for one cycle was about 0.2 seconds. That is, the sliding speed is approximately 0.02 m / s.
  • graphene oxide graphene oxide created by oxidizing graphite called “SP1” and graphene oxide created by oxidizing graphite called “X100” were used.
  • SP1GO graphene oxide created by oxidizing graphite
  • X100GO graphene oxide created by oxidizing graphite
  • the raw material graphite is irradiated with microwaves using a microwave oven, and then the graphite irradiated with the microwaves is mixed with an oxidizing agent composed of sulfuric acid, sodium nitrate, and potassium permanganate. It was oxidized by mixing with an aqueous solution to produce exfoliation as graphene oxide.
  • an oxidizing agent composed of sulfuric acid, sodium nitrate, and potassium permanganate. It was oxidized by mixing with an aqueous solution to produce exfoliation as graphene oxide.
  • an aqueous graphene oxide solution having high water dispersibility can be prepared, and an inexpensive graphene oxide aqueous solution can be provided.
  • FIG. 1 shows a scanning electron microscope (SEM) photograph of SP1GO and X100GO dropped on a silicon oxide film substrate.
  • SP1GO is over 50 ⁇ m in one large size, but X100GO is about 5 ⁇ m in size.
  • the difference in size is caused by the size of the raw graphite powder, and it is desirable to adjust the size of the graphite powder so that a desired size can be obtained.
  • graphite is desirably a fine powder having an average particle size of 100 ⁇ m or less, and preferably has an average particle size of 50 ⁇ m or less.
  • SP1GO and X100GO were subjected to the following comparative tests as dispersed water adjusted to a desired concentration.
  • FIG. 2 (a) as a comparative test of purified water alone, SP1GO dispersed water, X100GO dispersed water, and a commercially available water-soluble lubricant, 60,000 reciprocating slides were performed using the friction tester described above. It shows the coefficient of friction change.
  • the SP1GO dispersion water and the X100GO dispersion water each had a concentration of 1 wt%, and the commercially available water-soluble lubricant was a 1% aqueous solution.
  • the friction coefficient of purified water is 0.4 or more, and the friction coefficient of the water-soluble lubricant is around 0.1.
  • the friction coefficients of SP1GO dispersion water and X100GO dispersion water are each around 0.05, indicating that the friction coefficient is lower than that of the water-soluble lubricant and extremely good lubrication characteristics.
  • Fig. 2 (b) shows the change in the friction coefficient when the reciprocating slide is performed 60,000 times with a friction tester as a comparative test based on the difference in SP1GO concentration in SP1GO dispersed water. As a comparative example, only purified water is shown.
  • the friction coefficient of 1wt% SP1GO dispersed water is the lowest at 0.05, the friction coefficient of 0.1wt% SP1GO dispersed water is around 0.1, and 0.01wt% SP1GO dispersed water. It can be seen that the coefficient of friction finally exceeds 0.3. Thus, it was confirmed that there was a lubricating effect even at 0.01 wt%, compared with that of purified water alone. However, if the same level of performance as that of a commercially available water-soluble lubricant is required, the concentration of SP1GO dispersed water is desirably 0.1 wt% or more.
  • Fig. 2 (c) shows the coefficient of friction change when reciprocating 60,000 times with a friction tester as a comparative test based on the difference in X100GO concentration in X100GO dispersed water. As a comparative example, only purified water is shown.
  • the friction coefficient of 1 wt% X100GO dispersed water and the friction coefficient of 0.1wt% X100GO dispersed water are approximately the same, about 0.05 at first, and finally about 0.1.
  • the friction coefficient of 0.01wt% X100GO dispersed water is about 0.15 at first and finally about 0.1, and the friction coefficient of 0.001wt% X100GO dispersed water is almost the same as that of purified water alone. I understand.
  • X100GO dispersed water has a friction reducing effect at a concentration of 0.01 wt% or more.
  • X100GO dispersed water is more effective than SP1GO dispersed water is that the average particle size of X100GO is smaller than that of SP1GO, as is apparent from FIG. Conceivable. That is, by using graphene oxide having a particle size as small as possible, it is possible to obtain a graphene oxide dispersed water with a lower concentration, and further cost reduction can be achieved.
  • FIG. 3 shows a cross-sectional curve obtained by measuring the sliding surface of the substrate (SUS304) after 60,000 sliding tests with a friction tester using a confocal laser microscope.
  • FIG. 3A shows the case of purified water only
  • FIG. 3B shows the case of 1 wt% SP1GO dispersed water.
  • FIG. 4 shows an SEM image of the sliding surface of the ball after only 60,000 sliding tests with a friction tester in the case of purified water only.
  • the arrow line in Fig.4 (a) has shown the sliding direction.
  • FIG. 4B is an enlarged SEM image of a part of FIG. The balls are cleaned in acetone using an ultrasonic cleaner after the sliding test.
  • the broken line circled portion is the sliding surface of the ball, which is approximately 300 ⁇ m in size and flat, and it can be seen that it is worn. When calculated geometrically, the wear depth is about 5 ⁇ m.
  • the ball is synthesized by sintering fine particles of tungsten carbide. From the enlarged view of FIG. 4B, it can be seen that the fine particles are missing and defective.
  • FIG. 5 shows an SEM image of the sliding surface of the ball after 60,000 sliding tests with a friction tester in the case of 1 wt% SP1GO dispersed water.
  • the arrow line in Fig.5 (a) has shown the sliding direction.
  • FIG. 5B is an enlarged SEM image of a part of FIG. The balls are cleaned in acetone using an ultrasonic cleaner after the sliding test.
  • FIG. 5A it can be seen that a dark streak pattern is formed along the sliding direction.
  • FIG. 5B the gaps between the tungsten carbide particles are clearly observed even in the dark imaged area, as if the permeable thin film is adsorbed on the surface. Looks like.
  • Fig. 6 (a) is an SEM image of the sliding surface of the ball after 60,000 sliding tests with a friction tester in the case of 1wt% SP1GO dispersed water
  • Fig. 6 (b) shows Fig. 6 (b).
  • the measurement result of the carbon element component distribution by the energy dispersive X-ray-spectroscopy (EDX) in the sliding surface of a) is shown.
  • the vertical direction is the sliding direction.
  • Fig. 7 (a) is an SEM image of the sliding surface of the substrate (SUS304) after 60,000 sliding tests with a friction tester in the case of 1wt% SP1GO dispersed water.
  • Fig. 7 (b) The measurement result of the carbon element component distribution by the energy dispersive X-ray-spectroscopy (EDX) in the sliding surface of Fig.7 (a) is shown. 7A and 7B, the vertical direction is the sliding direction.
  • EDX energy dispersive X-ray-spectroscopy
  • FIG. 7B also shows that a lot of carbon components are contained in the place darkly shown in FIG. 7A.
  • the water-based lubricant of the present invention is composed only of water and graphene oxide, but an appropriate preservative, pH adjusting solution, or the like may be added for commercialization.
  • FIG. 8 shows the test results with a friction tester when the ball material is SUS304.
  • the material of the substrate is SUS304, and the surface is smoothed by grinding.
  • the ball had a radius of 1 mm, and the sliding condition of the ball was that the sliding distance of one cycle was about 2 mm and the sliding cycle was 500 rpm.
  • the load acting on the substrate was 1.8N.
  • FIG. 9 shows an SEM image of the sliding surface of the ball after 60,000 sliding tests with a friction tester using only purified water.
  • FIG. 10 shows an SEM image of the sliding surface of the ball after 60,000 sliding tests with a friction tester in the case of 1 wt% SP1GO dispersed water.
  • FIG. 11 shows a test result by a friction tester when the ball material is SUJ2.
  • the material of the substrate is SUS304, and the surface is smoothed by grinding.
  • the ball had a radius of 1 mm, and the sliding condition of the ball was that the sliding distance of one cycle was about 2 mm and the sliding cycle was 500 rpm.
  • the load acting on the substrate was 1.8N.
  • FIG. 12 shows an SEM image of the sliding surface of the ball after 60,000 sliding tests with a friction tester in the case of purified water alone.
  • FIG. 13 shows an SEM image of the sliding surface of the ball after 60,000 sliding tests with a friction tester in the case of 1 wt% SP1GO dispersed water.
  • DLC diamond-like carbon
  • FIG. 1 the material of the ball was SUS304, the radius of the ball was 1 mm, and the sliding condition of the ball was that the sliding distance of one cycle was about 2 mm and the sliding cycle was 500 rpm.
  • the load acting on the substrate was 11.1N.
  • the square dots ( ⁇ ) indicate the case of DLC substrate-SUS304 ball-purified water only, and the diamond-shaped dots ( ⁇ ) indicate the case of DLC substrate-SUS304 ball-1 wt% SP1GO dispersion water. It was confirmed that the friction coefficient can be reduced by SP1GO dispersed water.
  • the point x indicates the case of single crystal diamond substrate-SUS304 ball-purified water only, and the triangular point ( ⁇ ) indicates single crystal diamond substrate-SUS304 ball-1 wt% SP1GO dispersion. The case of water is shown, and in the single crystal diamond substrate, there was no difference in the friction coefficient.
  • the sliding surface of the substrate is larger in the frictional trace when 1 wt% SP1GO dispersed water shown in FIG. 16B is compared with the frictional trace of purified water alone shown in FIG.
  • the thickness can be reduced to half or less.
  • the water-based lubricant in which graphene oxide is dispersed has excellent characteristics as a lubricant.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

L'invention porte sur un lubrifiant à base d'eau qui est à base d'eau afin de résoudre le problème d'inflammabilité et dans lequel la nécessité d'additifs tels que des tensioactifs peut être réduite au minimum pour réduire le coût associé au traitement du rejet liquide après utilisation. Le lubrifiant à base d'eau selon la présente invention comprend de l'oxyde de graphène, obtenu par mise en oeuvre d'un procédé de séparation sur du graphite et séparation de l'oxyde de graphène du graphite, dispersé dans de l'eau. Le procédé de séparation provoque la séparation par mélange du graphite dans une solution aqueuse contenant un agent d'oxydation et oxydation du graphite. Le graphite est une poudre fine ayant une taille moyenne des grains inférieure ou égale à 100 μm et contient de l'oxyde de graphène en une concentration supérieure ou égale à 0,1 % en poids. Si la taille moyenne des grains du graphite est inférieure ou égale à 50 μm, l'oxyde de graphène est contenu en une concentration supérieure ou égale à 0,01 % en poids.
PCT/JP2014/063398 2013-05-20 2014-05-20 Lubrifiant a base d'eau WO2014189065A1 (fr)

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CN105316077A (zh) * 2015-11-16 2016-02-10 青岛领军节能与新材料研究院 一种石墨烯/氮化碳量子点复合纳米材料及润滑油摩擦改善剂
JP2016098279A (ja) * 2014-11-19 2016-05-30 国立大学法人 岡山大学 水系潤滑液組成物
WO2017199503A1 (fr) * 2016-05-16 2017-11-23 株式会社ダイセル Composition aqueuse lubrifiante et système aqueux de lubrification
CN107603724A (zh) * 2017-09-22 2018-01-19 广西大学 一种石墨烯增效无需排放环保型水基切削液及其制备方法
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CN108117913A (zh) * 2016-11-28 2018-06-05 中国科学院金属研究所 一种球形石墨烯润滑添加剂的制备方法和用途
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JP2016098279A (ja) * 2014-11-19 2016-05-30 国立大学法人 岡山大学 水系潤滑液組成物
JP2018534412A (ja) * 2015-10-15 2018-11-22 ジ オーストラリアン ナショナル ユニヴァーシティーＴｈｅ Ａｕｓｔｒａｌｉａｎ Ｎａｔｉｏｎａｌ Ｕｎｉｖｅｒｓｉｔｙ トラクション駆動流体
US11124734B2 (en) 2015-10-15 2021-09-21 Flex-G Pty Ltd Traction drive fluid
CN105316077A (zh) * 2015-11-16 2016-02-10 青岛领军节能与新材料研究院 一种石墨烯/氮化碳量子点复合纳米材料及润滑油摩擦改善剂
WO2017199503A1 (fr) * 2016-05-16 2017-11-23 株式会社ダイセル Composition aqueuse lubrifiante et système aqueux de lubrification
US10844313B2 (en) 2016-05-16 2020-11-24 Daicel Corporation Water lubricant composition and water lubricating system
JP2018070785A (ja) * 2016-10-31 2018-05-10 国立大学法人 岡山大学 水性媒体用流動抵抗低減剤組成物
CN108117913B (zh) * 2016-11-28 2021-05-18 中国科学院金属研究所 一种球形石墨烯润滑添加剂的制备方法和用途
CN108117913A (zh) * 2016-11-28 2018-06-05 中国科学院金属研究所 一种球形石墨烯润滑添加剂的制备方法和用途
IT201700023496A1 (it) * 2017-03-14 2018-09-14 Vincenzo Tagliaferri Fluidi termovettori ad elevata conducibilità termica.
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