CN103589478B - Lubricating oil containing illite/montmorillonite clay nano powder and preparation method thereof - Google Patents
Lubricating oil containing illite/montmorillonite clay nano powder and preparation method thereof Download PDFInfo
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- CN103589478B CN103589478B CN201310488088.1A CN201310488088A CN103589478B CN 103589478 B CN103589478 B CN 103589478B CN 201310488088 A CN201310488088 A CN 201310488088A CN 103589478 B CN103589478 B CN 103589478B
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Abstract
The invention discloses a lubricating oil containing illite/montmorillonite clay nano powder and a preparation method thereof, belonging to the field of new application of phyllosilicate clay minerals. The lubricating oil is composed of oleic acid modified illite/montmorillonite clay nano powder and III type base oil, wherein the oleic acid modified illite/montmorillonite clay nano powder accounts for 0.5-2.5 wt% of the lubricating oil. The preparation method comprises the following steps: (1) crushing natural illite/montmorillonite clay minerals, and adding water to obtain a slurry; (2) regulating the pH value of the slurry, and dispersing; (3) screening the slurry through a sieve; (4) grinding the undersieve slurry to obtain a nano slurry; (5) adding oleic acid for modification; (6) drying the modified nano slurry to obtain nano dry powder; and (7) mixing the nano dry powder with III type base oil to obtain the lubricating oil containing illite/montmorillonite clay nano powder. By using the illite/montmorillonite clay nano powder as the additive, the lubricating oil has the advantages of favorable friction and wear resistance, environment friendliness and no pollution.
Description
Technical field
The present invention relates to a kind of lubricating oil containing illite/montmorillonite clay nano powder and preparation method thereof, particularly relate to and a kind of modified Iraq/Mongolia clay is added in III class base oil as additive, to improve lubricating oil of the wear Characteristics of III class base oil and preparation method thereof, belong to the new opplication field of clay of laminar silicate mineral.
Background technology
Making rapid progress of machine and mechanical means, require that lubricating oil can adapt to various different operating mode, as high temperature, low temperature, vacuum, high radiation, high-load and corrosive medium etc., also require longer work-ing life and stability in storage etc. simultaneously, therefore rely on the performance of lubricating oil itself to be difficult to meet these requirements.Lubricating oil additive is one of main path addressed these problems.Compared with traditional lubricating oil additive, the additive of nanoscale is far above conventional lubrication oil additive in oil film strength, suspension density and degree of uniformity etc., and therefore, nanometer lubricating additive is the Main Trends of The Development of following slip additive.
Nanometer lubricating additive by sources can be divided into synthesis with natural two large classes.Be main mainly with the compound of S, P, Pb or simple substance in the nanometer additive of synthesis, these elements are not only easy causes burn into shorten workpiece work-ing life to metal works friction position, but also to environment.At present, a lot of scientific worker using natural mineral clay powder as additive application to (as serpentine, wilkinite, kaolinite, sepiolite, attapulgite, talcum, agalmatolite and schungite etc.) in lubricating oil, achieve certain achievement in research, this depends primarily on the silicate minerals that these mineral grains belong to stratiform, these particle depositions are on surface of friction, prevent the direct contact between friction workpiece, friction is only occurred over just between the laminate structure of mineral, thus reduction rub, reduce wear.But these mineral grains are in a micron grade mostly, therefore cannot repair the crack and micropore that are present in friction workpiece surface, cause antiwear and antifriction effect not very good.
Summary of the invention
For the defect that existing lubrication oil antiwear friction reducing effect is unsatisfactory, the object of the present invention is to provide a kind of lubricating oil containing illite/montmorillonite clay nano powder and preparation method thereof, described lubricating oil adopts illite/montmorillonite clay nano powder as additive, there is good wear Characteristics, and environmental friendliness, pollution-free.
Object of the present invention is realized by following technical scheme:
Containing the lubricating oil of illite/montmorillonite clay nano powder, described lubricating oil is made up of the illite/montmorillonite clay nano powder of oleic acid modification and III class base oil, and wherein, the illite/montmorillonite clay nano powder of oleic acid modification accounts for 0.5 ~ 2.5% of lubricating oil total mass.
The preparation method of the lubricating oil containing illite/montmorillonite clay nano powder of the present invention, step is as follows:
(1) preparation of slurry: become particle diameter to be less than the Iraq/Mongolia clay pit fritter of 5cm natural Iraq/Mongolia clay mineral Mechanical Crushing; Iraq/Mongolia clay pit fritter is soaked 12h, obtains Iraq/Mongolia clay slip; Wherein, solids in pulp amount is 45wt%;
(2) disperse: the pH value regulating Iraq/Mongolia clay slip is 9, adds dispersion agent, and adopt sand milling dispersion machine to carry out smashing slurry dispersion; Wherein, the add-on of dispersion agent is the 1.5wt% of solid content in described slip; The rotating speed of sand milling dispersion machine is 1000rpm, and churning time is 30min;
(3) sieve: the slip after step (2) being disperseed crosses 500 mesh sieves, obtain minus mesh slurry;
(4) grind: adopt high-energy-density Ball-stirring mill to grind minus mesh slurry, wherein the delivery rate of pump is 3L/min, and grinding medium is the ZrO of diameter 0.4 ~ 0.6mm
2ceramic fine bead, grinding medium filling ratio is 85%, and mill speed is 1400rpm, and milling time is 2 ~ 6h; Nanometer slurry is obtained after grinding;
(5) modification: the slip that step (4) obtains is moved in round-bottomed flask, under agitation add oleic acid, continue to stir 40min after adding oleic acid, then first use washes of absolute alcohol 3 times, use washed with de-ionized water again 3 times, wherein oleic acid add-on is the 4wt% of solids in pulp amount; Obtain modified nanometer slurry;
(6) dry: moved to by the modified nanometer slurry that step (5) obtains in vacuum environment dry, wherein drying temperature is 60 DEG C, and time of drying is 24h, obtains the Iraq/Mongolia clay nano dry powder of modification;
(7) mix: the Iraq/Mongolia clay nano dry powder of modification step (6) obtained mixes with III class base oil, disperses each 0.5h through ultrasonic disperse and high speed shear, namely obtain the lubricating oil containing illite/montmorillonite clay nano powder of the present invention; Wherein velocity of shear is 6000rpm; The Iraq/Mongolia clay nano dry powder of modification accounts for 0.5 ~ 2.5% of lubricating oil total mass, and all the other are III class base oil;
Step (2) regulates during the pH value of Iraq/Mongolia clay slip and preferably adopts NaOH or H
2sO
4solution;
Step (2) described dispersion agent is preferably WF-211 dispersion agent (polycarboxylate sodium's multipolymer).
Beneficial effect
Lubricating oil of the present invention adopts illite/montmorillonite clay nano powder as additive, has the following advantages:
(1) there is the feature of layer silicate mineral as slip additive of other type.
Illite/montmorillonite clay nano powder has natural laminate structure, this microcosmic laminate structure is more conducive to clay nanoparticle and covers friction workpiece surface, thus stop the direct contact of friction workpiece, friction is occurred over just between the laminate structure of mineral grain microcosmic, thus reduction rub, reduce wear.
(2) feature of nano particle slip additive is had concurrently, and environmental friendliness, pollution-free.
Illite/montmorillonite clay nano powder has the feature of nanoparticle additives as lubricating oil additive, is namely 1. conducive to its stablizing and dispersion in lubricating oil, strengthens the stability in storage of made lubricating oil; 2. because the dimensional effect of nano particle contributes to the absorption of particle at friction workpiece surface; 3. chemically reactive is high, is conducive at friction instantaneous high-temperature, the raw friction chemical reaction of elevated pressure and forms friction selfreparing protective membrane; 4. being conducive to nanoclay particles is filled in the friction crack of workpiece surface and micropore, repairs friction workpiece surface, makes friction process more stable, easilier forms continuous, homogeneous selfreparing protective membrane at friction workpiece surface.
Accompanying drawing explanation
Fig. 1 is the particulate accumulation distribution plan of embodiment 1 ~ 4; Wherein, 2h-embodiment 1,3h-embodiment 2,4h-embodiment 3,6h-embodiment 4;
Fig. 2 is the friction coefficient curve figure containing illite/montmorillonite clay nano powder lubricating oil described in embodiment 1 ~ 5;
Fig. 3 is illite/montmorillonite clay nano powder content when being 0.0wt%, the 3D skeleton diagram of surface of friction pair after friction
Fig. 4 is illite/montmorillonite clay nano powder content when being 2.0wt%, the 3D skeleton diagram of surface of friction pair after friction.
Embodiment
Below in conjunction with the drawings and specific embodiments in detail the present invention is described in detail, but is not limited thereto.
In following examples, equipment used is as follows:
Sand milling dispersion machine: Shenzhen three Xing Feirong Machinery Co., Ltd. SDF-400 type;
High-energy-density Ball-stirring mill: Switzerland Bulher (Bu Le) company SuperFlow12 type;
In embodiment, III class base oil used is the 40# base oil that China PetroChemical Corporation produces.
In embodiment, dispersion agent WF-211 used is that Shanghai Xin Yang Chemical Co., Ltd. produces.
Embodiment 1
(1) preparation of slurry: become particle diameter to be less than the Iraq/Mongolia clay pit fritter of 5cm natural Iraq/Mongolia clay mineral Mechanical Crushing; By 450g Iraq/Mongolia clay and the mixing of 550g water, then soak 12h, obtain Iraq/Mongolia clay slip;
(2) disperse: adopt the NaOH solution of 0.1mol/L to regulate the pH value of Iraq/Mongolia clay slip to be 9, add 6.75g dispersion agent WF-211, and adopt sand milling dispersion machine to carry out smashing slurry dispersion; Wherein, the add-on of dispersion agent WF-211 is the 1.5wt% of solid content in described slip; The rotating speed of sand milling dispersion machine is 1000rpm, and churning time is 30min;
(3) sieve: the slip after step (2) being disperseed crosses 500 mesh sieves, obtain minus mesh slurry;
(4) grind: adopt high-energy-density Ball-stirring mill to grind minus mesh slurry, wherein the delivery rate of pump is 3L/min, and grinding medium is the ZrO of diameter 0.6mm
2ceramic fine bead, grinding medium filling ratio is 85%, and mill speed is 1400rpm, and milling time is 2h; Nanometer slurry is obtained after grinding; The particulate accumulation distribution plan of described slip is as shown in 2h curve in Fig. 1, and can find out that the particle being less than 100nm accounts for 64%, grain graininess reaches nano level;
(5) modification: move in round-bottomed flask by the slip that step (4) obtains, continues to stir 40min after under agitation adding 18g oleic acid, then first uses washes of absolute alcohol 3 times, then use washed with de-ionized water 3 times, obtain modified nanometer slurry;
(6) dry: moved to by the modified nanometer slurry that step (5) obtains in vacuum drying oven dry, wherein drying temperature is 60 DEG C, and time of drying is 24h, obtains the Iraq/Mongolia clay nano dry powder of modification.
(7) mix: get the modified Iraq/Mongolia clay nano dry powder of 1g and 199g III class base oil and be placed in round-bottomed flask and mix, each 0.5h is disperseed through ultrasonic disperse and high speed shear, can obtain containing illite/montmorillonite clay nano powder massfraction is the lubricating oil of 0.5wt%, and wherein velocity of shear is 6000rpm.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: in step (4), milling time is 3h, the particulate accumulation distribution plan of its nanometer slurry prepared is as shown in 3h curve in Fig. 1, can find out that the particle being less than 100nm accounts for 67%, grain graininess reaches nano level; Get the modified illite/montmorillonite clay nano powder of 2g and 198g III class base oil in step (7), preparing containing illite/montmorillonite clay nano powder massfraction is the lubricating oil of 1.0wt%.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: in step (4), milling time is 4h, and the particulate accumulation distribution plan of described slip is as shown in 4h curve in Fig. 1, and can find out that the particle being less than 100nm accounts for 70%, grain graininess reaches nano level; Get the modified illite/montmorillonite clay nano powder of 3g and 197g III class base oil in step (7), preparing containing illite/montmorillonite clay nano powder massfraction is the lubricating oil of 1.5wt%.
Embodiment 4
The difference of the present embodiment and embodiment 1 is: in step (4), milling time is 6h, and the particulate accumulation distribution plan of described slip is as shown in 6h curve in Fig. 1, and can find out that the particle being less than 100nm accounts for 72%, grain graininess reaches nano level; Get the modified illite/montmorillonite clay nano powder of 4g and 196g III class base oil in step (7), preparing containing illite/montmorillonite clay nano powder massfraction is the lubricating oil of 2.0wt%.
Embodiment 5
The difference of the present embodiment and embodiment 1 is: in step (4), milling time is 6h, and in step (4), milling time is 6h, and can find out that the particle being less than 100nm accounts for 72% from the particulate accumulation distribution plan of described slip, grain graininess reaches nano level; Get the modified illite/montmorillonite clay nano powder of 5g and 194g III class base oil in step (7), preparing containing illite/montmorillonite clay nano powder massfraction is the lubricating oil of 2.5wt%.
In embodiment 1 ~ 5, the frictional behaviour of lubricating oil adopts MRS-10A type four ball frictional testing machines to carry out frictional behaviour detection, detects data as shown in Fig. 2,3 and 4.Friction steel ball is standard secondary steel ball (GCr15, Φ 12.7mm, HRC59-61, w (Fe): 96.50-97.49%; W (C): 0.95-1.05%; W (Si): 0.15-0.35%; W (Cr): 1.30-1.65%; W (Mn): 0.20-0.40%; W (S) :≤0.02%; W (P) :≤0.027%); Experiment condition is: experiment load 400N, rotating speed 1450rpm, fraction time 60min.
Fig. 2 shows the friction coefficient curve figure containing different mass mark illite/montmorillonite clay nano powder lubricating oil in each embodiment.Compared with the lubricating oil not adding illite/montmorillonite clay nano powder, the lubricating oil average friction coefficient containing illite/montmorillonite clay nano powder all has reduction in various degree; Especially when content is 2.0wt%, average friction coefficient minimum (0.030), reduces 60% (0.075 → 0.030), and this illustrates that illite/montmorillonite clay nano powder has good wear Characteristics as slip additive.
Fig. 3 is illite/montmorillonite clay nano powder content is 0.0wt%, and when namely not adding illite/montmorillonite clay nano powder, friction steel ball is by the 3D skeleton diagram of surface of friction pair after rubbing; Fig. 4 is illite/montmorillonite clay nano powder content when being 2.0wt%, and friction steel ball is by the 3D skeleton diagram of surface of friction pair after rubbing.As seen from the figure, compared with the lubricating oil not adding illite/montmorillonite clay nano powder, by the friction steel ball surface planeness of the oil lubrication containing illite/montmorillonite clay nano powder better, ditch dug with a plow is more shallow, roughness is less (446.94nm → 201.07nm), this illustrates that illite/montmorillonite clay nano powder has the ability of good improvement frictional contact surface.
The present invention includes but be not limited to above embodiment, every any equivalent replacement of carrying out under the principle of spirit of the present invention or local improvement, all will be considered as within protection scope of the present invention.
Claims (3)
1. the preparation method containing the lubricating oil of illite/montmorillonite clay nano powder, it is characterized in that, described lubricating oil is made up of the illite/montmorillonite clay nano powder of oleic acid modification and III class base oil, and wherein, the illite/montmorillonite clay nano powder of oleic acid modification accounts for 0.5 ~ 2.5% of lubricating oil total mass;
Preparation method's step is as follows:
(1) preparation of slurry: become particle diameter to be less than the Iraq/Mongolia clay pit fritter of 5 cm natural Iraq/Mongolia clay mineral Mechanical Crushing; Iraq/Mongolia clay pit fritter is soaked 12 h, obtains Iraq/Mongolia clay slip; Wherein, solids in pulp amount is 45 wt%;
(2) disperse: the pH value regulating Iraq/Mongolia clay slip is 9, adds dispersion agent, and adopt sand milling dispersion machine to carry out smashing slurry dispersion; Wherein, the add-on of dispersion agent is 1.5 wt% of solid content in described slip; The rotating speed of sand milling dispersion machine is 1000 rpm, and churning time is 30 min;
(3) sieve: the slip after step (2) being disperseed crosses 500 mesh sieves, obtain minus mesh slurry;
(4) grind: adopt high-energy-density Ball-stirring mill to grind minus mesh slurry, wherein the delivery rate of pump is 3 L/min, and grinding medium is the ZrO of diameter 0.4 ~ 0.6 mm
2ceramic fine bead, grinding medium filling ratio is 85 %, and mill speed is 1400 rpm, and milling time is 2 ~ 6 h; Nanometer slurry is obtained after grinding;
(5) modification: the slip that step (4) obtains is moved in round-bottomed flask, under agitation add oleic acid, after adding oleic acid, continue stirring 40 min, then first use washes of absolute alcohol 3 times, use washed with de-ionized water again 3 times, wherein oleic acid add-on is 4 wt% of solids in pulp amount; Obtain modified nanometer slurry;
(6) dry: moved to by the modified nanometer slurry that step (5) obtains in vacuum environment dry, wherein drying temperature is 60 DEG C, and time of drying is 24 h, obtains the Iraq/Mongolia clay nano dry powder of modification;
(7) mix: the Iraq/Mongolia clay nano dry powder of modification step (6) obtained mixes with III class base oil, through ultrasonic disperse and each 0.5 h of high speed shear dispersion, namely obtain the described lubricating oil containing illite/montmorillonite clay nano powder; Wherein velocity of shear is 6000 rpm; The Iraq/Mongolia clay nano dry powder of modification accounts for 0.5 ~ 2.5% of lubricating oil total mass, and all the other are III class base oil.
2. according to claim 1 containing the preparation method of the lubricating oil of illite/montmorillonite clay nano powder, it is characterized in that, step (2) regulates during the pH value of Iraq/Mongolia clay slip and adopts NaOH or H
2sO
4solution.
3., according to claim 1 containing the preparation method of the lubricating oil of illite/montmorillonite clay nano powder, it is characterized in that, step (2) described dispersion agent is WF-211 dispersion agent.
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| CN105176647B (en) * | 2015-10-14 | 2018-01-09 | 苏州市晶协高新电子材料有限公司 | A kind of wire cutting oil and preparation method thereof |
| CN105855277A (en) * | 2016-05-02 | 2016-08-17 | 中国环境科学研究院 | Preparation method of clay mineral material and method for reducing bio-availability of heavy metal in soil and water body |
| CN106244292B (en) * | 2016-08-02 | 2019-01-25 | 陕西科技大学 | A method of hydroxyl magnesium silicate micro-nano lubricant is prepared using natural crystal |
| CN110465261B (en) * | 2019-08-16 | 2022-08-30 | 内蒙古电力(集团)有限责任公司内蒙古电力科学研究院分公司 | Manufacturing process and application of adsorbent for recycling and regenerating waste transformer oil |
| CN114378111A (en) * | 2021-11-30 | 2022-04-22 | 西安建筑科技大学 | Device and method for removing loess heavy metal pollution based on electrodynamics and mineralogy |
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| CN102947429A (en) * | 2010-03-26 | 2013-02-27 | 爱思开润滑油株式会社 | Lubricating oil composition for reducing friction comprising nanoporous particles |
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| CN102947429A (en) * | 2010-03-26 | 2013-02-27 | 爱思开润滑油株式会社 | Lubricating oil composition for reducing friction comprising nanoporous particles |
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| Title |
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| 摩擦磨损自修复润滑油添加剂研究进展;刘谦等;《润滑与密封》;150-153;20060228(第2期);150-153 * |
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