CN104959627A - 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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- CN104959627A CN104959627A CN201510425460.3A CN201510425460A CN104959627A CN 104959627 A CN104959627 A CN 104959627A CN 201510425460 A CN201510425460 A CN 201510425460A CN 104959627 A CN104959627 A CN 104959627A
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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, be specifically related 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, is especially suitable for the lubrication in heavily loaded, vulgar and high-temperature vibrating situation.In recent years, the method preparing copper nanoparticle becomes the focus of people's research.The method preparing copper nanoparticle at present has Physical and the large class of chemical method two, 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 reduction because of its experimental facilities and low raw-material cost, preparation technology is brief, the product proportion of goods damageds are lower, easily realize the features such as suitability for industrialized production obtains wide prospect.Generate copper by chemical reaction, in order to better improve the purity of copper nanoparticle, most researcher adds part complexing agent to protect product in preparation process, then carries out vacuum drying treatment.But there is following shortcoming in these methods preparing copper nanoparticle:
1, Nanometer Copper is easily reunited, and particle diameter is difficult to control, and particle is larger;
2, in the latter stage of drying process, between particle, the surface tension of aqueous water can make to produce larger gravitation between powder granule, causes powder generation hard aggregation;
3, Nanometer Copper is easily oxidized, easy pollution products in collection process;
4, prepared powder is crystal structure, active low.
5, be not easy in the long stable dispersion of lubricating oil as lube oil additive.
Summary of the invention
The object of this invention is 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, active high.
The technical solution adopted in the present invention is:
As the preparation method of the copper nanoparticle of lube oil additive, it is characterized in that:
Realized by following steps:
Step one: take the cupric sulfate pentahydrate of 12.5 g and the ethylenediamine tetra-acetic acid of 3.65 g, join in the lump in 300 ml distilled water and obtain solution A, stir;
The inferior sodium phosphate taking 12.71 g joins in 200 ml distilled water and obtains solution B, stirs;
Step 2: carry out heating water bath to solution A and B, after being warming up to 60 ~ 70 oC, stirs solution A with the rotating speed of 650 ~ 750 r/min, solution B is poured in solution A, and isothermal reaction 1 ~ 1.5 h, obtains copper powder;
Step 3: wash copper powder with distilled water, then with the rotating speed collected by centrifugation of 1100 ~ 1800 r/min, be placed in and store liquid ultrasonic disperse 15 ~ 30 min;
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars vacuum freeze drying in freeze dryer, water vessel temperature-55 ~-60 oC, vacuum 0.01 ~ 0.018 mbar, freeze-drying time 15 ~ 24 h, obtain the freeze-drying copper nanoparticle of black, vacuum seal is preserved.
In step one, add surfactant in addition in solution B, surfactant is the polyvinylpyrrolidone of 0.12 g or the stearic acid of 0.32 g.
In step 3, store the alcohol water mixed solution that liquid is 40 ~ 50 ml, be mixed to get with the volume ratio of 1:4 by ethanol and distilled water.
In step 4, freezing processing method is selected from:
(1) load container with the degree of depth of 5.5 ~ 7.5 mm, freeze-drying machine partition board directly freezes, and solidification point is-40 oC;
(2) load container with the degree of depth of 8 ~ 10 mm, on freeze-drying machine partition board, when water vessel temperature drops to-55 oC, vacuumize quick freezing;
(3) Quick freezing in liquid nitrogen is joined.
As described in the copper nanoparticle that obtains of the preparation method of copper nanoparticle being used as lube oil additive.
The present invention has the following advantages:
1, product grain fine uniform, hard aggregation-free;
2, process is simple, and product easily collecting is preserved, and ensures products pure degree;
3, prepared powder granule is the copper nanoparticle without metallic luster, active high.
4, be easy to and surface modifier generation physics, chemisorbed, improve it in the long stable dispersion of lubricating oil.
Accompanying drawing explanation
Fig. 1 is the XRD figure of Cu nano particle.
Fig. 2 is the TEM photo of sample.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be described in detail.
The preparation method being used as the copper nanoparticle of lube oil additive that the present invention relates to, is realized by following steps:
Step one: take the cupric sulfate pentahydrate of 12.5 g and the ethylenediamine tetra-acetic acid of 3.65 g, join in the lump in 300 ml distilled water and obtain solution A, stir;
The inferior sodium phosphate taking 12.71 g joins in 200 ml distilled water and obtains solution B, stirs;
Step 2: carry out heating water bath to solution A and B, after being warming up to 60 ~ 70 oC, stirs solution A with the rotating speed of 650 ~ 750 r/min, solution B is poured in solution A, and isothermal reaction 1 ~ 1.5 h, obtains copper powder;
Step 3: wash copper powder with distilled water, then with the rotating speed collected by centrifugation of 1100 ~ 1800 r/min, be placed in and store liquid ultrasonic disperse 15 ~ 30 min;
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars vacuum freeze drying in freeze dryer, water vessel temperature-55 ~-60 oC, vacuum 0.01 ~ 0.018 mbar, freeze-drying time 15 ~ 24 h, obtain the freeze-drying copper nanoparticle of black, vacuum seal is preserved.
In step one, add surfactant in addition in solution B, surfactant is the polyvinylpyrrolidone of 0.12 g or the stearic acid of 0.32 g.
In step 3, store the alcohol water mixed solution that liquid is 40 ~ 50 ml, be mixed to get with the volume ratio of 1:4 by ethanol and distilled water.
In step 4, freezing processing method is selected from:
(1) load container with the degree of depth of 5.5 ~ 7.5 mm, freeze-drying machine partition board directly freezes, and solidification point is-40 oC;
(2) load container with the degree of depth of 8 ~ 10 mm, on freeze-drying machine partition board, when water vessel temperature drops to-55 oC, vacuumize quick freezing;
(3) Quick freezing in liquid nitrogen is joined.
The present invention uses desivac to prepare copper nanoparticle, and desivac course of reaction is carried out be in the state freezed at solution under, makes solvent directly distil under vacuum, and solute retains.In the latter stage of drying process, between particle, the surface tension of aqueous water can make to produce larger gravitation between powder granule, thus cause powder generation hard aggregation, and the prerequisite of desivac makes solute dispersed in the solution, solute is fixed on and freezes in solvent, along with the distillation freezing water, ethanol molecule, solute is separated out gradually, the gravitation produced when overcoming aqueous water volatilization, cause grain diameter to be difficult to control, what therefore obtain after vacuum freeze-drying is hard aggregation-free, even particle size and tiny, active high Nanometer Copper powder.
The freeze-drying copper nanoparticle that the present invention obtains has larger surface-active, is uniformly dispersed, make it carrying out finishing as being easy to during lube oil additive, improve adsorption rate, the adsorption effect between copper nanoparticle and surface modifier, thus reach copper nanoparticle long stably dispersing in lubricating oil, for Nanometer Copper to provide next step thinking as lube oil additive, there is more excellent prospects for commercial application.
Embodiment 1:
Step one: take the cupric sulfate pentahydrate of 12.5 g and the ethylenediamine tetra-acetic acid of 3.65 g, join in the lump in 300 ml distilled water and obtain solution A, stir;
The inferior sodium phosphate taking 12.71 g joins in 200 ml distilled water and obtains solution B, stirs;
Step 2: heating water bath is carried out to solution A and B, after being warming up to 60 oC, stirring, solution B poured in solution A with the rotating speed of 750 r/min to solution A, isothermal reaction 1h, obtains copper powder;
Step 3: wash copper powder with distilled water, then with the rotating speed collected by centrifugation of 1800 r/min, be placed in and store liquid ultrasonic disperse 15min;
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars vacuum freeze drying in freeze dryer, water vessel temperature-60 oC, vacuum 0.01mbar, freeze-drying time 24 h, obtains the freeze-drying copper nanoparticle of black, and vacuum seal is preserved.
In step 3, store the alcohol water mixed solution that liquid is 40 ml, be mixed to get with the volume ratio of 1:4 by ethanol and distilled water.
In step 4, freezing processing method is: load container with the degree of depth of 7.5 mm, freeze-drying machine partition board directly freezes, and solidification point is-40 oC.
Embodiment 2:
Step one: take the cupric sulfate pentahydrate of 12.5 g and the ethylenediamine tetra-acetic acid of 3.65 g, join in the lump in 300 ml distilled water and obtain solution A, stir;
The inferior sodium phosphate taking 12.71 g joins in 200 ml distilled water and obtains solution B, stirs;
Step 2: heating water bath is carried out to solution A and B, after being warming up to 65 oC, stirring, solution B poured in solution A with the rotating speed of 700 r/min to solution A, isothermal reaction 1h, obtains copper powder;
Step 3: wash copper powder with distilled water, then with the rotating speed collected by centrifugation of 11500 r/min, be placed in and store liquid ultrasonic disperse 20min;
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars vacuum freeze drying in freeze dryer, water vessel temperature-58 oC, vacuum 0.014 mbar, freeze-drying time 20 h, obtains the freeze-drying copper nanoparticle of black, and vacuum seal is preserved.
In step one, add surfactant in addition in solution B, surfactant is the polyvinylpyrrolidone of 0.12 g.
In step 3, store the alcohol water mixed solution that liquid is 45 ml, be mixed to get with the volume ratio of 1:4 by ethanol and distilled water.
In step 4, freezing processing method is: load container with the degree of depth of 8 ~ 10 mm, on freeze-drying machine partition board, when water vessel temperature drops to-55 oC, vacuumize quick freezing.
Embodiment 3:
Step one: take the cupric sulfate pentahydrate of 12.5 g and the ethylenediamine tetra-acetic acid of 3.65 g, join in the lump in 300 ml distilled water and obtain solution A, stir;
The inferior sodium phosphate taking 12.71 g joins in 200 ml distilled water and obtains solution B, stirs;
Step 2: carry out heating water bath to solution A and B, after being warming up to 65 oC, stirring solution A with the rotating speed of 700 r/min, solution B is poured in solution A, and isothermal reaction 1 h, obtains copper powder;
Step 3: wash copper powder with distilled water, then with the rotating speed collected by centrifugation of 1500 r/min, be placed in and store liquid ultrasonic disperse 20 min;
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars vacuum freeze drying in freeze dryer, water vessel temperature-58 oC, vacuum 0.014mbar, freeze-drying time 20 h, obtains the freeze-drying copper nanoparticle of black, and vacuum seal is preserved.
In step one, add surfactant in addition in solution B, surfactant is the stearic acid of 0.32 g.
In step 3, store the alcohol water mixed solution that liquid is 45 ml, be mixed to get with the volume ratio of 1:4 by ethanol and distilled water.
In step 4, freezing processing method is: join Quick freezing in liquid nitrogen.
Embodiment 4:
Step one: take the cupric sulfate pentahydrate of 12.5 g and the ethylenediamine tetra-acetic acid of 3.65 g, join in the lump in 300 ml distilled water and obtain solution A, stir;
The inferior sodium phosphate taking 12.71 g joins in 200 ml distilled water and obtains solution B, stirs;
Step 2: carry out heating water bath to solution A and B, after being warming up to 70 oC, stirring solution A with the rotating speed of 650r/min, solution B is poured in solution A, and isothermal reaction 1.5 h, obtains copper powder;
Step 3: wash copper powder with distilled water, then with the rotating speed collected by centrifugation of 1100 r/min, be placed in and store liquid ultrasonic disperse 30 min;
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars vacuum freeze drying in freeze dryer, water vessel temperature-55oC, vacuum 0.018 mbar, freeze-drying time 15h, obtains the freeze-drying copper nanoparticle of black, and vacuum seal is preserved.
In step one, add surfactant in addition in solution B, surfactant is the polyvinylpyrrolidone of 0.12 g.
In step 3, store the alcohol water mixed solution that liquid is 50 ml, be mixed to get with the volume ratio of 1:4 by ethanol and distilled water.
In step 4, freezing processing method is: join Quick freezing in liquid nitrogen.
Utilize X-ray diffractometer and transmission electron microscope to carry out purity, droplet measurement to product grain, the sweep limits of XRD is 10o ~ 80o, and the sweep speed of its angle of diffraction 2 θ is 4o/min; The multiplication factor 100,000,140,000 times (see accompanying drawing 1-2) of TEM.
Can find out 4 sample particle particle diameter fine uniform from Fig. 2, do not have hard aggregation between particle, good dispersion, pattern is similar to orbicule.Be below purity and the particle size of sample:
Content of the present invention is not limited to cited by embodiment, and the conversion of those of ordinary skill in the art by reading description of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.
Claims (5)
1. be used as the preparation method of the copper nanoparticle of lube oil additive, it is characterized in that:
Realized by following steps:
Step one: take the cupric sulfate pentahydrate of 12.5 g and the ethylenediamine tetra-acetic acid of 3.65 g, join in the lump in 300 ml distilled water and obtain solution A, stir;
The inferior sodium phosphate taking 12.71 g joins in 200 ml distilled water and obtains solution B, stirs;
Step 2: carry out heating water bath to solution A and B, after being warming up to 60 ~ 70 oC, stirs solution A with the rotating speed of 650 ~ 750 r/min, solution B is poured in solution A, and isothermal reaction 1 ~ 1.5 h, obtains copper powder;
Step 3: wash copper powder with distilled water, then with the rotating speed collected by centrifugation of 1100 ~ 1800 r/min, be placed in and store liquid ultrasonic disperse 15 ~ 30 min;
Step 4: copper powder is carried out freezing processing together with storage liquid and obtains scars, by scars vacuum freeze drying in freeze dryer, water vessel temperature-55 ~-60 oC, vacuum 0.01 ~ 0.018 mbar, freeze-drying time 15 ~ 24 h, obtain the freeze-drying copper nanoparticle of black, vacuum seal is preserved.
2. the preparation method being used as the copper nanoparticle of lube oil additive according to claim 1, is characterized in that:
In step one, add surfactant in addition in solution B, surfactant is the polyvinylpyrrolidone of 0.12 g or the stearic acid of 0.32 g.
3. the preparation method being used as the copper nanoparticle of lube oil additive according to claim 2, is characterized in that:
In step 3, store the alcohol water mixed solution that liquid is 40 ~ 50 ml, be mixed to get with the volume ratio of 1:4 by ethanol and distilled water.
4. the preparation method being used as the copper nanoparticle of lube oil additive according to claim 3, is characterized in that:
In step 4, freezing processing method is selected from:
(1) load container with the degree of depth of 5.5 ~ 7.5 mm, freeze-drying machine partition board directly freezes, and solidification point is-40 oC;
(2) load container with the degree of depth of 8 ~ 10 mm, on freeze-drying machine partition board, when water vessel temperature drops to-55 oC, vacuumize quick freezing;
(3) Quick freezing in liquid nitrogen is joined.
5. the copper nanoparticle that the preparation method being used as the copper nanoparticle of lube oil additive as claimed in claim 4 obtains.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107335810A (en) * | 2017-05-30 | 2017-11-10 | 胡建锋 | A kind of preparation method of lyophilized copper nanoparticle |
| CN111112639A (en) * | 2020-01-02 | 2020-05-08 | 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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Cited By (3)
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| CN107335810A (en) * | 2017-05-30 | 2017-11-10 | 胡建锋 | A kind of preparation method of lyophilized copper nanoparticle |
| CN111112639A (en) * | 2020-01-02 | 2020-05-08 | 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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Effective date of registration: 20210128 Address after: No.03, 23 / F, building a, Huixin IBC, No.1 zhangbayi Road, Zhangba Street office, high tech Zone, Xi'an City, Shaanxi Province, 710076 Patentee after: XI'AN ZEGU NEW MATERIAL TECHNOLOGY Co.,Ltd. Address before: 710032 No. 2 Xuefu Middle Road, Weiyang District, Xi'an City, Shaanxi Province Patentee before: XI'AN TECHNOLOGICAL University |