CN104959627B - Nano copper powder used as lubricating oil additive and preparation method thereof - Google Patents
Nano copper powder used as lubricating oil additive and preparation method thereof Download PDFInfo
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Abstract
The invention relates to nano copper powder used as a lubricating oil additive and a preparation method thereof. For an existing nano copper powder preparation method, obtained nano copper is prone to agglomeration, the particle size is difficult to control, the particles are larger, and the activity is low. The preparation method comprises the steps that copper sulfate pentahydrate and ethylenediamine tetraacetic acid are added into distilled water to obtain a solution A, and sodium hypophosphite is added into the distilled water to obtain a solution B; the solution A is stirred under water bath heating, the solution B is poured into the solution A, the solution A and the solution B react at a constant temperature to obtain the copper powder, the copper powder is washed, collected and placed in storage liquid, and ultrasonic dispersion is conducted on the copper powder; freezing treatment is conducted on the storage liquid with the copper powder to obtain a frozen object, vacuum freezing drying is conducted on the frozen object to obtain black freeze-dried nano copper powder, and the black freeze-dried nano copper powder is stored in a vacuum seal mode. According to the nano copper powder used as the lubricating oil additive and the preparation method thereof, the obtained nano copper powder is free of hard aggregation, higher in purity, larger in specific area, stronger in surface activity and smaller in diameter, and it is verified through experiments that the freeze-dried nano copper powder in lubricating oil is easy to stably disperse.
Description
Technical field
The invention belongs to nano-powder material technical field is and in particular to a kind of copper nanoparticle as lube oil additive
And preparation method thereof.
Background technology
Copper nanoparticle has good anti-wear and wear-resistant performance as lube oil additive, can be used for quality lubricant, especially
Lubrication in the case of suitably heavily loaded, vulgar and high-temperature vibrating.In recent years, the method preparing copper nanoparticle becomes Jiao of people's research
Point.The method preparing copper nanoparticle at present has Physical and chemical method two big class, and Physical has mechanical crushing method, arc discharge
Method, atom vapor sedimentation etc.；Chemical method has microemulsion method, gamma-ray irradiation method, pyrolysismethod, liquid phase reduction etc..Wherein, liquid
Phase reducing process is because its experimental facilities and low raw-material cost, preparation technology are brief, the product proportion of goods damageds are relatively low, the industrial metaplasia of easy realization
The features such as product, obtains wide prospect.Copper is generated by chemical reaction, in order to preferably improve the purity of copper nanoparticle, Duo Shuoyan
Studying carefully personnel adds part chelating agent to protect product in preparation process, then carries out vacuum drying treatment.But these preparations are received
The method of rice copper powder has a disadvantage in that
1st, Nanometer Copper is easily reunited, and particle diameter is difficult to control to, and granule is larger；
2nd, in the latter stage of dried, between granule, the surface tension of aqueous water can make to produce larger drawing between powder granule
Power, leads to powder body that hard aggregation occurs；
3rd, Nanometer Copper easily aoxidizes, easy pollution products during collection；
4th, prepared powder body is crystal structure, and activity is low.
5th, it is not easy to stable dispersion long in lubricating oil as lube oil additive.
Content of the invention
It is an object of the invention to provide a kind of copper nanoparticle as lube oil additive and preparation method thereof, prepared
Copper nanoparticle chemical composition is pure, uniform particle sizes, hard aggregation-free, and activity is high.
The technical solution adopted in the present invention is:
The preparation method of the copper nanoparticle as lube oil additive it is characterised in that:
Realized by following steps:
Step one: weigh the copper sulphate pentahydrate of 12.5 g and the ethylenediaminetetraacetic acid of 3.65 g, be added to 300 ml in the lump
Obtain solution a in distilled water, stir；
The sodium hypophosphite weighing 12.71 g is added in 200 ml distilled water and obtains solution b, stirs；
Step 2: heating in water bath is carried out to solution a and b, after being warming up to 60～70 c, turning with 650～750 r/min
Speed is stirred to solution a, and solution b is poured in solution a, and isothermal reaction 1～1.5 h obtains copper powder；
Step 3: use distilled water wash copper powder, then be collected by centrifugation with the rotating speed of 1100～1800 r/min, be placed in storage liquid
Middle ultrasonic disperse 15～30 min；
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars in freeze dryer
Vacuum lyophilization, water vessel temperature -55～-60 c, vacuum 0.01～0.018 mbar, freeze-drying time 15～24 h, obtain
To the lyophilizing copper nanoparticle of black, vacuum sealing preservation.
In step one, in solution b, it is possible to additionally incorporate surfactant, surfactant is the polyvinylpyrrolidine of 0.12 g
Ketone or the stearic acid of 0.32 g.
In step 3, storage liquid is the alcohol water mixed solution of 40～50 ml, by ethanol and distilled water with the volume ratio of 1:4
It is mixed to get.
In step 4, freezing processing method is selected from:
(1) container is loaded with the depth of 5.5～7.5 mm, freeze-drying machine partition board directly freezes, solidification point is -40
c；
(2) container is loaded with the depth of 8～10 mm, on freeze-drying machine partition board, take out when water vessel temperature drops to -55 c
Vacuum quick freezing；
(3) it is added to Quick freezing in liquid nitrogen.
It is used as the copper nanoparticle that the preparation method of the copper nanoparticle of lube oil additive is obtained as mentioned.
The invention has the advantages that
1st, product grain fine uniform, hard aggregation-free；
2nd, process is simple, and product easily collecting preserves it is ensured that products pure degree；
3rd, prepared powder granule is the copper nanoparticle of no metallic luster, and activity is high.
4th, it is easy to, with surface modifier, physics, chemisorbed occur, improve it in the long stable dispersion of lubricating oil.
Brief description
Fig. 1 is the xrd figure of cu nano-particle.
Fig. 2 is the tem photo of sample.
Specific embodiment
With reference to specific embodiment, the present invention will be described in detail.
The preparation method of the copper nanoparticle as lube oil additive according to the present invention, is realized by following steps:
Step one: weigh the copper sulphate pentahydrate of 12.5 g and the ethylenediaminetetraacetic acid of 3.65 g, be added to 300 ml in the lump
Obtain solution a in distilled water, stir；
The sodium hypophosphite weighing 12.71 g is added in 200 ml distilled water and obtains solution b, stirs；
Step 2: heating in water bath is carried out to solution a and b, after being warming up to 60～70 c, turning with 650～750 r/min
Speed is stirred to solution a, and solution b is poured in solution a, and isothermal reaction 1～1.5 h obtains copper powder；
Step 3: use distilled water wash copper powder, then be collected by centrifugation with the rotating speed of 1100～1800 r/min, be placed in storage liquid
Middle ultrasonic disperse 15～30 min；
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars in freeze dryer
Vacuum lyophilization, water vessel temperature -55～-60 c, vacuum 0.01～0.018 mbar, freeze-drying time 15～24 h, obtain
To the lyophilizing copper nanoparticle of black, vacuum sealing preservation.
In step one, in solution b, it is possible to additionally incorporate surfactant, surfactant is the polyvinylpyrrolidine of 0.12 g
Ketone or the stearic acid of 0.32 g.
In step 3, storage liquid is the alcohol water mixed solution of 40～50 ml, by ethanol and distilled water with the volume ratio of 1:4
It is mixed to get.
In step 4, freezing processing method is selected from:
(1) container is loaded with the depth of 5.5～7.5 mm, freeze-drying machine partition board directly freezes, solidification point is -40
c；
(2) container is loaded with the depth of 8～10 mm, on freeze-drying machine partition board, take out when water vessel temperature drops to -55 c
Vacuum quick freezing；
(3) it is added to Quick freezing in liquid nitrogen.
The present invention prepares copper nanoparticle using lyophilization, lyophilization course of reaction solution be in freeze in the state of enter
OK, solvent is made directly to distil under vacuum, solute retains.In the latter stage of dried, between granule, the surface of aqueous water is opened
Power can make to produce larger gravitation between powder granule, thus lead to powder body occur hard aggregation, and the premise of lyophilization be make molten
Matter is dispersed in the solution, and solute is fixed on and freezes in solvent, and with the distillation of freeze water, ethanol molecule, solute is gradually
Separate out, overcome the gravitation producing during aqueous water volatilization, cause grain diameter to be difficult to control to, therefore obtain after vacuum freeze-drying
For hard aggregation-free, even particle size and Nanometer Copper powder body tiny, that activity is high.
The lyophilizing copper nanoparticle that the present invention obtains has larger surface activity, is uniformly dispersed so that it is as lubrication
It is easy to carry out surface modification during oil additive, improve adsorption rate between copper nanoparticle and surface modifier, adsorption effect, thus
Reach copper nanoparticle long stably dispersing in lubricating oil, the think of of next step is provided as lube oil additive for Nanometer Copper
, there is more excellent prospects for commercial application on road.
Embodiment 1:
Step one: weigh the copper sulphate pentahydrate of 12.5 g and the ethylenediaminetetraacetic acid of 3.65 g, be added to 300 ml in the lump
Obtain solution a in distilled water, stir；
The sodium hypophosphite weighing 12.71 g is added in 200 ml distilled water and obtains solution b, stirs；
Step 2: heating in water bath is carried out to solution a and b, after being warming up to 60 c, with the rotating speed of 750 r/min to solution a
It is stirred, solution b is poured in solution a, isothermal reaction 1h, obtain copper powder；
Step 3: use distilled water wash copper powder, then be collected by centrifugation with the rotating speed of 1800 r/min, be placed in ultrasonic in storage liquid
Dispersion 15min；
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars in freeze dryer
Vacuum lyophilization, water vessel temperature -60 c, vacuum 0.01mbar, freeze-drying time 24 h, obtain the lyophilizing nanometer of black
Copper powder, vacuum sealing preserves.
In step 3, storage liquid is the alcohol water mixed solution of 40 ml, is mixed with the volume ratio of 1:4 by ethanol and distilled water
Obtain.
In step 4, freezing processing method is: loads container with the depth of 7.5 mm, directly freezes on freeze-drying machine partition board
Knot, solidification point is -40 c.
Embodiment 2:
Step one: weigh the copper sulphate pentahydrate of 12.5 g and the ethylenediaminetetraacetic acid of 3.65 g, be added to 300 ml in the lump
Obtain solution a in distilled water, stir；
The sodium hypophosphite weighing 12.71 g is added in 200 ml distilled water and obtains solution b, stirs；
Step 2: heating in water bath is carried out to solution a and b, after being warming up to 65 c, with the rotating speed of 700 r/min to solution a
It is stirred, solution b is poured in solution a, isothermal reaction 1h, obtain copper powder；
Step 3: use distilled water wash copper powder, then be collected by centrifugation with the rotating speed of 11500 r/min, be placed in super in storage liquid
Sound disperses 20min；
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars in freeze dryer
Vacuum lyophilization, water vessel temperature -58 c, vacuum 0.014 mbar, freeze-drying time 20 h, the lyophilizing obtaining black is received
Rice copper powder, vacuum sealing preserves.
In step one, in solution b, it is possible to additionally incorporate surfactant, surfactant is the polyvinylpyrrolidine of 0.12 g
Ketone.
In step 3, storage liquid is the alcohol water mixed solution of 45 ml, is mixed with the volume ratio of 1:4 by ethanol and distilled water
Obtain.
In step 4, freezing processing method is: loads container with the depth of 8～10 mm, on freeze-drying machine partition board, is catching
Hydrophone temperature drops to evacuation quick freezing during -55 c.
Embodiment 3:
Step one: weigh the copper sulphate pentahydrate of 12.5 g and the ethylenediaminetetraacetic acid of 3.65 g, be added to 300 ml in the lump
Obtain solution a in distilled water, stir；
The sodium hypophosphite weighing 12.71 g is added in 200 ml distilled water and obtains solution b, stirs；
Step 2: heating in water bath is carried out to solution a and b, after being warming up to 65 c, with the rotating speed of 700 r/min to solution a
It is stirred, solution b is poured in solution a, isothermal reaction 1 h, obtain copper powder；
Step 3: use distilled water wash copper powder, then be collected by centrifugation with the rotating speed of 1500 r/min, be placed in ultrasonic in storage liquid
Disperse 20 min；
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars in freeze dryer
Vacuum lyophilization, water vessel temperature -58 c, vacuum 0.014mbar, freeze-drying time 20 h, obtain the lyophilizing nanometer of black
Copper powder, vacuum sealing preserves.
In step one, in solution b, it is possible to additionally incorporate surfactant, surfactant is the stearic acid of 0.32 g.
In step 3, storage liquid is the alcohol water mixed solution of 45 ml, is mixed with the volume ratio of 1:4 by ethanol and distilled water
Obtain.
In step 4, freezing processing method is: is added to Quick freezing in liquid nitrogen.
Embodiment 4:
Step one: weigh the copper sulphate pentahydrate of 12.5 g and the ethylenediaminetetraacetic acid of 3.65 g, be added to 300 ml in the lump
Obtain solution a in distilled water, stir；
The sodium hypophosphite weighing 12.71 g is added in 200 ml distilled water and obtains solution b, stirs；
Step 2: heating in water bath is carried out to solution a and b, after being warming up to 70 c, with the rotating speed of 650r/min, solution a is entered
Row stirring, solution b is poured in solution a, and isothermal reaction 1.5 h obtains copper powder；
Step 3: use distilled water wash copper powder, then be collected by centrifugation with the rotating speed of 1100 r/min, be placed in ultrasonic in storage liquid
Disperse 30 min；
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars in freeze dryer
Vacuum lyophilization, water vessel temperature -55 c, vacuum 0.018 mbar, freeze-drying time 15h, obtain the lyophilizing nanometer of black
Copper powder, vacuum sealing preserves.
In step one, in solution b, it is possible to additionally incorporate surfactant, surfactant is the polyvinylpyrrolidine of 0.12 g
Ketone.
In step 3, storage liquid is the alcohol water mixed solution of 50 ml, is mixed with the volume ratio of 1:4 by ethanol and distilled water
Obtain.
In step 4, freezing processing method is: is added to Quick freezing in liquid nitrogen.
Using x-ray diffraction instrument and transmission electron microscope, product grain is carried out with purity, droplet measurement, the scanning of xrd
Scope is 10 ~ 80, and the scanning speed of its angle of diffraction 2 θ is 4/min；100,000,140,000 times of the amplification of tem is (see accompanying drawing 1-
2).
It can be seen that 4 sample particle particle diameter fine uniform from Fig. 2, between granule, there is no hard aggregation, good dispersion, shape
Looks are similar to spheroid.It is below purity and the size of sample:
Present disclosure is not limited to cited by embodiment, and those of ordinary skill in the art pass through to read description of the invention
And any equivalent conversion that technical solution of the present invention is taken, the claim being the present invention covered.
Claims (4)
1. be used as lube oil additive copper nanoparticle preparation method it is characterised in that:
Realized by following steps:
Step one: weigh the copper sulphate pentahydrate of 12.5 g and the ethylenediaminetetraacetic acid of 3.65 g, be added to 300 ml distillations in the lump
Obtain solution a in water, stir；
The sodium hypophosphite weighing 12.71 g is added in 200 ml distilled water and obtains solution b, stirs；
Step 2: heating in water bath is carried out to solution a and b, after being warming up to 60～70 c, with the rotating speed pair of 650～750 r/min
Solution a is stirred, and solution b is poured in solution a, and isothermal reaction 1～1.5 h obtains copper powder；
Step 3: use distilled water wash copper powder, then be collected by centrifugation with the rotating speed of 1100～1800 r/min, be placed in super in storage liquid
Sound disperses 15～30 min；
Step 4: copper powder is carried out freezing processing and obtains scars together with storage liquid, by scars in freeze dryer vacuum
Lyophilization, water vessel temperature -55～-60 c, vacuum 0.01～0.018 mbar, freeze-drying time 15～24 h, obtain black
The lyophilizing copper nanoparticle of color, vacuum sealing preserves.
2. the copper nanoparticle as lube oil additive according to claim 1 preparation method it is characterised in that:
In step one, in solution b, it is possible to additionally incorporate surfactant, surfactant be 0.12 g Polyvinylpyrrolidone or
The stearic acid of 0.32 g.
3. the copper nanoparticle as lube oil additive according to claim 2 preparation method it is characterised in that:
In step 3, storage liquid is the alcohol water mixed solution of 40～50 ml, is mixed with the volume ratio of 1:4 by ethanol and distilled water
Obtain.
4. the copper nanoparticle as lube oil additive according to claim 3 preparation method it is characterised in that:
In step 4, freezing processing method is selected from:
(1) container is loaded with the depth of 5.5～7.5 mm, freeze-drying machine partition board directly freezes, solidification point is -40 c；
(2) container, evacuation on freeze-drying machine partition board, when water vessel temperature drops to -55 c are loaded with the depth of 8～10 mm
Quick freezing；
(3) it is added to Quick freezing in liquid nitrogen.
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| CN107335810A (en) * | 2017-05-30 | 2017-11-10 | 胡建锋 | A kind of preparation method of lyophilized copper nanoparticle |
| CN111112639B (en) * | 2020-01-02 | 2023-04-07 | 西安工业大学 | Nanoscale spherical silver particles with room-temperature antifriction effect and preparation method thereof |
| CN113355146A (en) * | 2021-06-18 | 2021-09-07 | 西安工业大学 | Preparation method of graphene-loaded copper nanoparticles for lubricating oil additive |
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| KR20020069271A (en) * | 2001-02-24 | 2002-08-30 | 주식회사 맥스그린 | Solid Phase Lubricating Additive by using nanoparticles of copper alloy |
| CN1536058A (en) * | 2003-04-08 | 2004-10-13 | 北京化工大学 | Lubricating oil additive containing oleophilic nano copper powder |
| KR20070035174A (en) * | 2005-09-27 | 2007-03-30 | 주식회사 듀라씰 | Lubricant composition for restoring abraded metal surface |
| CN101966590B (en) * | 2010-10-09 | 2013-11-06 | 朱光明 | Method for preparing nanometer metal copper powder through liquid-phase arc discharge |
| CN102198513A (en) * | 2011-05-27 | 2011-09-28 | 中南大学 | Method for preparing nano copper particle |
| KR101314990B1 (en) * | 2011-09-19 | 2013-10-04 | 장신우 | Manufacturing method of conductive copper powder |
| CN104028778B (en) * | 2014-06-25 | 2016-05-25 | 东北大学 | A kind of method of preparing fast nanometer copper particle |
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