CN101531949B - Method and device for synthesizing nano magnetic lubricating oil with under synergic action of alternative electric field and temperature field - Google Patents
Method and device for synthesizing nano magnetic lubricating oil with under synergic action of alternative electric field and temperature field Download PDFInfo
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- CN101531949B CN101531949B CN2009100111268A CN200910011126A CN101531949B CN 101531949 B CN101531949 B CN 101531949B CN 2009100111268 A CN2009100111268 A CN 2009100111268A CN 200910011126 A CN200910011126 A CN 200910011126A CN 101531949 B CN101531949 B CN 101531949B
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Abstract
The invention relates to the field of lubricating oil, in particular to a method and a device for synthesizing nano magnetic lubricating oil with under the synergic action of an alternative electric field and a temperature field. The device comprises a heat booster, a stirrer, an electrode, a quartz umbrella, an internal cooling device, a feeding device, a cooling device, an electrode interface, a water inlet-outlet interface, a driving device, a digital control motor, a first air inlet-outlet interface, a first lifting device, a fine-tuning device, a supporting plate adjuster, a reaction kettle, a sensor, a second air inlet-outlet interface and a second lifting device. The method for synthesizing the nano magnetic lubricating oil by applying the device comprises the following: a stage of ultrasonic processing, a stage of feeding materials to the reaction kettle, a stage of the synergic action of the alternating electric field and the temperature field, a stage of circulation, and a stage of closed-down, cooling and bottling. The method and the device have quite broad application prospects.
Description
Technical field
The present invention relates to the lubricating oil field, be specifically related to one and adopt alternating electric field/temperature field synergy to prepare the method and the device of nano magnetic lubricating oil.
Background technology
In the market the lubricating oil of Xiao Shouing drip when being subjected to gravity, magnetic force, centrifugal action, all can occur, splash, phenomenon such as leakage, loss, poorness, cause environmental pollution and economic waste, for solving " maintenance of lubricating oil " problem, people such as Qiao Hongbin research is used as nano metal powder, nanometer sulfide, nano rare earth compound, the nano-oxide of lubricating oil additive, make lubricating oil have nanometer, improve the antiwear and friction reduction property of lubricating oil; Bi Yanjun invents " a kind of magnetic lubricating oil ", is to add neutral sulfocompound in existing lubricating oil, make lubricating oil be magnetic, but these two kinds of lubricating oil can not have nanometer performance and magnetic property simultaneously.We adopt the synergistic method in alternating electric field/temperature field to develop " nano magnetic lubricating oil " on home-made contrivance, and it is to coat the nano magnetic lubricating oil made from proper lubrication oil thorough mixing again by the magnetic-particle with nanometer scale through polar tensio-active agent unimolecular layer is arranged.
Summary of the invention
The purpose of this invention is to provide a kind of have simultaneously nanometer performance and magnetic property, under gravity, magnetic force, centrifugal action, do not separate and do whole moving, have and utilize external magnetic field to keep the preparation method and the device of the ability lubricating oil of lubricating oil at the lubricated position of needs.
Technical solution of the present invention is: the synthesizing nano magnetic lubricating oil device is worked in coordination with in alternating electric field/temperature field, comprises helping thermic devices 1, agitator 2, electrode 3, quartzy umbrella 4, interior device for cooling 5, material injecting device 6, refrigerating unit 7, electrode interface 8, Inlet and outlet water interface 9, transmission mechanism 10, numerical-control motor 11, the first turnover gas interface 12, first lifting device 13, micromatic setting 14, supporting plate setting device 15, reactor 16, transmitter 17, the second turnover gas interface 18 and second lifting device 19.Reactive material is sent into reactor 16 from material injecting device 6, help thermic devices 1 to be positioned at reactor 16 bottoms, agitator 2 and quartzy umbrella 4, electrode 3, transmitter 17 is positioned at reactor 16, numerical-control motor 11 drives agitator 2 by transmission mechanism 10 and quartzy umbrella 4 evenly stirs reactant to set numerical value, the temperature of transmitter 17 detection reaction stills 16 internal reaction things, and be connected with temperature controller, device for cooling 5 in top in reactor 16 was provided with, with regulation and control reactor 16 temperature inside, refrigerating unit 7 communicates with reactor 16, refrigerating unit 7 tops connect the first turnover gas interface 12, device for cooling 5 and refrigerating unit 7 in Inlet and outlet water interface 9 connects, feed frozen water and cool off reactant rapidly, electrode 3 is connected with the pulse power by electrode interface 8, give for reactor 16, the scission of link step by step of material molecule in the reactor 16 is provided and reconfigures needed activation energy, the numerical-control motor 11 and first lifting device 13, transmission mechanism 10, micromatic setting 14, the supporting plate setting device 15 and second lifting device 19 interconnect, the second turnover gas interface 18 connects agitator 2, by the numerical control mass-flow gas meter, gas mixer connects the second turnover gas interface 18, guarantees the ratio of the required ionized gas of synthesizing nano magnetic particle in the reactor 16.
The method that adopts the collaborative synthesizing nano magnetic lubricating oil device in alternating electric field/temperature field to prepare nano magnetic lubricating oil is as follows:
A, supersound process stage:
Press 1: 9 weighing tensio-active agent of mass ratio and lubricating base oils white oil, thorough mixing also carries out the 10min supersound process at SCQ-600 dual-frequency ultrasonic wave cleanser, and ultrasonic frequency is controlled at 21000Hz, and power is controlled at 500W.
B, past reactor material feeding stage:
Ultrasonic good solution is injected in the reactor 16 from material injecting device 6, is the mass ratio benchmark with the tensio-active agent, draws weighing iron carbonyl solution by 1: 10 needle tubing and also injects in the reactors 16 from material injecting device 6 rapidly; From the second turnover gas interface, 18 input flow rates than 1: 4 nitrogen and ammonia in reactor 16.
C, alternating electric field, temperature field synergy stage:
Connection helps thermic devices 1, reactor 16 is preheated, the variation of detection reaction still 16 inner sensors 17 displays temperature fields in real time, when showing 118 ℃, close and help thermic devices 1, device for cooling 5 in opening makes that iron carbonyl falls after rise rapidly to reactor 16 in the refrigerating unit 7, and full cycle needs time 4～6min; Connection helps thermic devices 1, device for cooling 5 in closing, 8 places connect the alternating-current pulse high-voltage power supply at electrode interface, in the alternating electric field zone, i.e. and agitator 2 and electrode 3 gaps, ammonia, iron carbonyl liquid are carried out discharge activation, its pulse-repetition regulation and control 63.5KHz, electric pressure controlling be to 10kV, working current 200mA, the speed of adjusting agitator 2 in the reactor 16 is 330rad/min, begins second circulation.What adopt in this circulation is the method that alternating electric field/temperature field combines, under airshed and discharge parameter the same terms, reactor temperature is fast changing, the time and heat up rapidly, the time and smooth change, the time and descend rapidly, reflect moment disassociation, the scission of link of gas, liquid molecule in the reactor, the fierce degree of complex reaction.
D, cycle stage:
Repeat second circulation later on, totally ten times, approximately move 120min, be in the frozen water state of cooling in the process of the collaborative synthesizing nano magnetic lubricating oil in whole alternating electric field/temperature field always.
E, shutdown cooling bottling stage:
After adopting the collaborative activation in alternating electric field/temperature field synthesizing nano magnetic lubricating oil, close the alternating-current pulse power supply, help thermic devices 1, nitrogen, ammonia, when question response still 16 is cooled to 37～40 ℃, open reactor 16, pour the black nano magnetic lubricating oil into vial and be built in refrigerating chamber.
The invention has the beneficial effects as follows, the lubricating oil of using the present invention's preparation is to be coated through polar tensio-active agent unimolecular layer is arranged by the magnetic-particle with nanometer scale, the liquid that mixes of a kind of special superparamagnetism solid-liquid made from suitable lubricating base oils thorough mixing again, be a kind of to magnetic-field-sensitive, controlled by magnetic field, be in and have the novel nano magnetic lubricating oil that keeps lubricating oil ability in the magnetic field, this kind lubricating oil has nanometer performance and magnetic property simultaneously, at gravity, magnetic force, do not separate under the centrifugal action and do whole moving, solved gear, the maintenance problem of privileged sites such as piston and vertical rail thereof lubricating oil, its application prospect is very wide.
Description of drawings
Fig. 1 is the collaborative synthesizing nano magnetic lubricating oil device synoptic diagram in alternating electric field/temperature field;
Among the figure: 1, help thermic devices, 2, agitator, 3, electrode, 4, quartzy umbrella, 5, interior device for cooling, 6, material injecting device, 7, refrigerating unit, 8, electrode interface, 9, the Inlet and outlet water interface, 10, transmission mechanism, 11, numerical-control motor, 12, the first turnover gas interface, 13, first lifting device, 14, micromatic setting, 15, the supporting plate setting device, 16, reactor, 17, transmitter, 18, the second turnover gas interface, 19 second lifting devices.
Fig. 2 is that the structure of the magnetic lubricating oil of embodiment 1 preparation is formed and size-grade distribution.
Fig. 3 is the TEM of the magnetic lubricating oil of embodiment 1 preparation;
Wherein: figure a is 300K TEM doubly, and figure b is 250K TEM doubly.
Fig. 4 is the magnetic hysteresis loop of the magnetic lubricating oil of embodiment 1 preparation.
Embodiment
As shown in Figure 1, the collaborative synthesizing nano magnetic lubricating oil device in alternating electric field/temperature field comprises and helps thermic devices 1, agitator 2, electrode 3, quartzy umbrella 4, interior device for cooling 5, material injecting device 6, refrigerating unit 7, electrode interface 8, Inlet and outlet water interface 9, transmission mechanism 10, numerical-control motor 11, the first turnover gas interface 12, first lifting device 13, micromatic setting 14, supporting plate setting device 15, reactor 16, transmitter 17, the second turnover gas interface 18 and second lifting device 19.Reactive material is sent into reactor 16 from material injecting device 6, help thermic devices 1 to be positioned at reactor 16 bottoms, agitator 2 and quartzy umbrella 4, electrode 3, transmitter 17 is positioned at reactor 16, numerical-control motor 11 drives agitator 2 by transmission mechanism 10 and quartzy umbrella 4 evenly stirs reactant to set numerical value, the temperature of transmitter 17 detection reaction stills 16 internal reaction things, and be connected with temperature controller, device for cooling 5 in top in reactor 16 was provided with, with regulation and control reactor 16 temperature inside, refrigerating unit 7 communicates with reactor 16, refrigerating unit 7 tops connect the second turnover gas interface 18, device for cooling 5 and refrigerating unit 7 in Inlet and outlet water interface 9 connects, feed frozen water and cool off reactant rapidly, electrode 3 is connected with the pulse power by electrode interface 8, give for reactor 16, the scission of link step by step of material molecule in the reactor 16 is provided and reconfigures needed activation energy, the numerical-control motor 11 and first lifting device 13, transmission mechanism 10, micromatic setting 14, the supporting plate setting device 15 and second lifting device 19 interconnect, the first turnover gas interface 12 connects agitator 2, by the numerical control mass-flow gas meter, gas mixer connects the first turnover gas interface 12, guarantees the ratio of the required ionized gas of synthesizing nano magnetic particle in the reactor 16.
The scheme that adopts the collaborative synthesizing nano magnetic lubricating oil device in alternating electric field/temperature field to prepare nano magnetic lubricating oil is as follows:
A, supersound process stage:
Press that mass ratio weighing in 1: 9 Japan produces tensio-active agent 8 grams and lubricating base oils white oil 72 restrains, shake to make its thorough mixing and carry out the 10min supersound process at SCQ-600 dual-frequency ultrasonic wave cleanser, ultrasonic frequency is controlled at 21000Hz, and power is controlled at 500W.
B, past reactor material feeding stage:
Ultrasonic good solution is injected in the reactor 16 from material injecting device 6, is the mass ratio benchmark with the tensio-active agent, draws weighing iron carbonyl solution by 1: 10 needle tubing and also injects in the reactors 16 from material injecting device 6 rapidly; By throughput ratio is that nitrogen flow is 60sccm at 1: 4, and ammonia flow is 240sccm from the second turnover gas interface 18 input nitrogen and ammonia in reactor 16.
C, alternating electric field, temperature field synergy stage:
Connection helps thermic devices 1, reactor 16 is preheated, the variation of detection reaction still 16 inner sensors 17 displays temperature fields in real time, when showing 118 ℃, close and help thermic devices 1, device for cooling 5 in opening makes that iron carbonyl falls after rise rapidly to reactor 16 in the refrigerating unit 7, and full cycle needs time 5min; Connection helps thermic devices 1, device for cooling 5 in closing, 8 places connect the alternating-current pulse high-voltage power supply at electrode interface, in the alternating electric field zone, i.e. and agitator 2 and electrode 3 gaps, ammonia, iron carbonyl liquid are carried out discharge activation, its pulse-repetition regulation and control 63.5KHz, electric pressure controlling be to 10kV, working current 200mA, the speed of adjusting agitator 2 in the reactor 16 is 330rad/min, begins second circulation.
D, circulation previous step are rapid:
Repeat second circulation later on, totally ten times, approximately move 120min, be in the frozen water state of cooling in the process of the collaborative synthesizing nano magnetic lubricating oil in whole alternating electric field/temperature field always.
E, shutdown cooling bottling stage:
After adopting the collaborative activation in alternating electric field/temperature field synthesizing nano magnetic lubricating oil, close the alternating-current pulse power supply, help thermic devices, nitrogen, ammonia, when question response still 16 is cooled to 37～40 ℃, open reactor 16, pour the black nano magnetic lubricating oil into vial and be built in refrigerating chamber.
F, data analysis:
Adopt X ray small angle scattering method, at the Japan's little angle of 3014 optical diffraction spectrograph ratky of science goniometer, Co target and voltage 30KV, under the electric current 30mA experiment condition, the structure of the magnetic lubricating oil of embodiment 1 preparation is formed and size-grade distribution is tested, test result as shown in Figure 2, magnetic lubricating oil to embodiment 1 preparation is made of magnetic-particle really, and wherein size range is wider, and the particle diameter overwhelming majority is less than 18nm.
Adopt JEM-2000EX type transmission electron microscope, its resolving power is 0.1nm, and magnification is 250K-300K times, pattern to the magnetic lubricating oil of embodiment 1 preparation is tested, test result as shown in Figure 3, a figure is a 300K times of Electronic Speculum picture among Fig. 3, b figure is a 250K times of transmission electron microscope picture.As seen from Figure 3, the magnetic-particle majority that constitutes magnetic lubricating oil is about 10nm, with employing X ray small angle scattering method test result basically identical, illustrates that the magnetic lubricating oil of preparation has nanostructure.
Adopt LDJ-9500 type vibrating sample magnetometer, DT-100 balance to measure the magnetic hysteresis loop of magnetic lubricating oil.Test result as shown in Figure 4, Fig. 4 shows that the magnetic history of magnetic lubricating oil is a reversible, both coercive force, magnetic hysteresis loss approached zero, magnetic hysteresis loop is a zeroaxial S type curve, almost there is not hysteresis, both formed between these nano magnetic particles of magnetic lubricating oil and do not interacted, in lubricating base oils, freely drifted, had superparamagnetism.
Claims (2)
1. the synthesizing nano magnetic lubricating oil device is worked in coordination with in alternating electric field/temperature field, it is characterized in that this device comprises and helps thermic devices (1), agitator (2), electrode (3), quartzy umbrella (4), interior device for cooling (5), material injecting device (6), refrigerating unit (7), electrode interface (8), Inlet and outlet water interface (9), transmission mechanism (10), numerical-control motor (11), the first turnover gas interface (12), first lifting device (13), micromatic setting (14), supporting plate setting device (15), reactor (16), transmitter (17), second turnover gas interface (18) and second lifting device (19); Reactive material is sent into reactor (16) from material injecting device (6), help thermic devices (1) to be positioned at reactor (16) bottom, agitator (2) and quartzy umbrella (4), electrode (3), transmitter (17) is positioned at reactor (16), numerical-control motor (11) drives agitator (2) by transmission mechanism (10) and quartzy umbrella (4) evenly stirs reactant to set numerical value, transmitter (17) is connected with temperature controller, top in reactor (16) is provided with interior device for cooling (5), refrigerating unit (7) communicates with reactor (16), refrigerating unit (7) top connects the first turnover gas interface (12), device for cooling (5) and refrigerating unit (7) fed frozen water in Inlet and outlet water interface (9) connected, electrode (3) is connected with the pulse power by electrode interface (8), numerical-control motor (11) and first lifting device (13), transmission mechanism (10) connects, first lifting device (13) is provided with micromatic setting (14), micromatic setting (14), supporting plate setting device (15) and second lifting device (19) interconnect, and the second turnover gas interface (18) connects agitator (2).
2. the method that adopts the collaborative synthesizing nano magnetic lubricating oil device in the described alternating electric field/temperature field of claim 1 to prepare nano magnetic lubricating oil is as follows:
A, supersound process stage:
Press 1: 9 weighing tensio-active agent of mass ratio and lubricating base oils white oil, thorough mixing also carries out the 10min supersound process at SCQ-600 dual-frequency ultrasonic wave cleanser, and ultrasonic frequency is controlled at 21000Hz, and power is controlled at 500W;
B, past reactor material feeding stage:
Ultrasonic good solution is injected in the reactor (16) from material injecting device (6), is the mass ratio benchmark with the tensio-active agent, draws weighing iron carbonyl solution by 1: 10 needle tubing and also injects in the reactor (16) from material injecting device (6) rapidly; From second turnover gas interface (18) input flow rate than 1: 4 nitrogen and ammonia in reactor (16);
C, alternating electric field, temperature field synergy stage:
Connection helps thermic devices (1), reactor (16) is preheated, the variation of detection reaction still (16) inner sensor 17 displays temperature fields in real time, when showing 118 ℃, close and help thermic devices (1), device for cooling (5) in opening falls to reactor (16) the middle iron carbonyl of refrigerating unit (7) rapidly after rise, and full cycle needs time 4～6min; Connection helps thermic devices (1), close interior device for cooling (5), locate to connect the alternating-current pulse high-voltage power supply at electrode interface (8), in the alternating electric field zone, i.e. agitator (2) and electrode (3) gap, ammonia, iron carbonyl liquid are carried out discharge activation, its pulse-repetition regulation and control 63.5KHz, electric pressure controlling be to 10kV, working current 200mA, the speed of adjusting the interior agitator of reactor (16) (2) is 330rad/min, begins second circulation;
D, cycle stage:
Repeat second circulation later on, totally 10 times, approximately move 120min, be in the frozen water state of cooling in the process of the collaborative synthesizing nano magnetic lubricating oil in whole alternating electric field/temperature field always;
E, shutdown cooling bottling stage:
After adopting the collaborative activation in alternating electric field/temperature field synthesizing nano magnetic lubricating oil, close the alternating-current pulse power supply, help thermic devices (1), nitrogen, ammonia, when question response still (16) is cooled to 37～40 ℃, open reactor (16), pour the black nano magnetic lubricating oil into vial and be built in refrigerating chamber.
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| CN2009100111268A CN101531949B (en) | 2009-04-08 | 2009-04-08 | Method and device for synthesizing nano magnetic lubricating oil with under synergic action of alternative electric field and temperature field |
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| RU2483101C2 (en) * | 2010-01-29 | 2013-05-27 | Александр Николаевич Мартьянов | Method of producing lubricant composition |
| CN102198380B (en) * | 2011-04-29 | 2015-02-04 | 无锡虹业自动化工程有限公司 | High-precision intelligent extraction batching robot |
| CN105749827B (en) * | 2016-02-26 | 2019-04-26 | 东北大学 | A kind of device and method using high-intensity magnetic field liquid phase synthesis low-dimension nano material |
| CN110564487B (en) * | 2019-08-29 | 2021-09-28 | 杭州电子科技大学 | Method for preparing green nano cutting fluid by combining cycloidal ultrasonic stirring with alternating electric field |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5180512A (en) * | 1990-04-12 | 1993-01-19 | National Research Institute For Metals | Method of manufacturing fine-particle colloid or magnetic fluid |
| CN1547223A (en) * | 2003-11-28 | 2004-11-17 | 大连大学 | Method and apparatus for preparing nitrided iron magnetic liquid by plasma |
| CN201389453Y (en) * | 2009-04-08 | 2010-01-27 | 大连大学 | Apparatus for synthesizing nano magnetic lubricant by adopting cooperation of alternating electric field and temperature field |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5180512A (en) * | 1990-04-12 | 1993-01-19 | National Research Institute For Metals | Method of manufacturing fine-particle colloid or magnetic fluid |
| CN1547223A (en) * | 2003-11-28 | 2004-11-17 | 大连大学 | Method and apparatus for preparing nitrided iron magnetic liquid by plasma |
| CN201389453Y (en) * | 2009-04-08 | 2010-01-27 | 大连大学 | Apparatus for synthesizing nano magnetic lubricant by adopting cooperation of alternating electric field and temperature field |
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