CN104319053B - Device and method for preparing iron nitride magnetic liquid by barometric-pressure dielectric barrier discharge - Google Patents

Device and method for preparing iron nitride magnetic liquid by barometric-pressure dielectric barrier discharge Download PDF

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CN104319053B
CN104319053B CN201410525493.0A CN201410525493A CN104319053B CN 104319053 B CN104319053 B CN 104319053B CN 201410525493 A CN201410525493 A CN 201410525493A CN 104319053 B CN104319053 B CN 104319053B
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pipeline
magnetic
flow controller
mass flow
stop valve
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CN104319053A (en
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李艳琴
刘志升
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Dalian University
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Dalian University
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Abstract

The invention discloses a device and a method for preparing iron nitride magnetic liquid by barometric-pressure dielectric barrier discharge and belongs to the technical field of chemical equipment. According to the device for preparing the iron nitride magnetic liquid by the barometric-pressure dielectric barrier discharge, a pipeline III is communicated with one end of a mass flow controller I; the other end of the mass flow controller I is communicated with one end of a check valve I; a pipeline IV is communicated with one end of a mass flow controller II; the other end of the mass flow controller II is communicated with one end of a check valve II; a pipeline V is communicated with one end of a mass flow controller III; the other end of the mass flow controller III is communicated with one end of a check valve III; the other end of the check valve I is communicated with a pipeline I; the other end of the check valve II is communicated with the pipeline I; the tail end of the pipeline I enters a constant-temperature bath and the other end of the check valve III is communicated with a pipeline II; the tail end of the pipeline II is arranged in the constant-temperature bath; the constant-temperature bath is provided with a temperature controller and temperature of the constant-temperature bath is adjusted.

Description

Atmospheric dielectric barrier discharge prepares the apparatus and method of magnetic liquid of nitriding iron
Technical field
The present invention relates to atmospheric dielectric barrier discharge prepares the apparatus and method of magnetic liquid of nitriding iron, belong to chemical industry and set Standby technical field.
Background technology
Magnetic liquid is a kind of soft magnetism Intelligent liquid composite of superparamagnetic, by magnetic-particle, surfactant and load Liquid three part forms.Magnetic-particle is broadly divided into three major types: metal system, iron oxide, iron nitride-based.Metal system magnetic-particle master Fe, co, ni to be had and its alloy, it is easily oxidized, poor chemical stability, limits the development of metal system magnetic liquid.Oxygen Change ferrum system magnetic-particle and be mainly fe3o4, but its saturation magnetization relatively low it is impossible to prepare the magnetic liquid of high saturation and magnetic intensity Body.Iron nitride-based magnetic-particle is mainly ε-fe3N, its saturation magnetization is higher, is to prepare high saturation and magnetic intensity magnetic liquid The ideal material of body.
At present, the technology of preparing of magnetic liquid of nitriding iron mainly has gas-liquid phase method and Plasma Cvd.Iron and steel grinds Xu Jiaoren of Jiu Zong institute et al. (application number: 98101595.6, the manufacture method of iron nitride magnetic fluid) adopt gas-liquid phase legal system For magnetic liquid of nitriding iron, " high saturation and magnetic intensity nitrogenizes the article that its calendar year 2001 delivers in " Metallic Functional Materials " periodical The development of ferromagnetic fluid " shows, preparation time is up to 30 hours, and need by add in precipitant or stove coagulation method Lai Improve the saturation magnetization of magnetic liquid of nitriding iron, through loaded down with trivial details techniques such as precipitation process, solid-liquid separation, ultrasound wave dispersions. Huang Wei et al. (application number: 200510064275.2, the method preparing magnetic liquid of nitriding iron using concentrating agent of low volatilization point) Magnetic liquid of nitriding iron is prepared for using above-mentioned gas-liquid phase subtraction unit, preparation time does not still shorten, but this invention will be low Volatilization point concentrating agents are added in carrier fluid and the mixed liquor of surfactant, and the saturated magnetization that improve magnetic liquid of nitriding iron is strong Degree.Li Xuehui et al. (application number: 200310105229.3, the method and device of preparing nitrided iron magnetic liquid by plasma) adopt It is prepared for magnetic liquid of nitriding iron with plasma method, will shorten in the response time about 2 hours, but the method is in gas-liquid two Magnetic liquid of nitriding iron has been synthesized, course of reaction is extremely complex, to gas-liquid two-phase body discharge mechanism in phase body discharge plasma And magnetic liquid of nitriding iron synthesis mechanism studied the development further it is suppressed that magnetic liquid of nitriding iron preparation method.
Content of the invention
Above-mentioned in order to overcome the shortcomings of, the present invention provides atmospheric dielectric barrier discharge to prepare the dress of magnetic liquid of nitriding iron Put and method.
The technical scheme that the present invention takes is as follows:
Atmospheric pressure matter barrier discharge prepares the device of magnetic liquid of nitriding iron, pipeline tee joint mass flow controller one One end;The other end of mass flow controller one connects one end of stop valve one;Pipeline four connects mass flow controller two One end, the other end of mass flow controller two connects one end of stop valve two;Pipeline five connects mass flow controller three One end, the other end of mass flow controller three connects one end of stop valve three;The other end of stop valve one is connected with pipeline one, The other end of stop valve two is connected with pipeline one;The end of pipeline one enters in constant temperature bath, the other end connection of stop valve three Pipeline two, the end of pipeline two is in constant temperature bath;Constant temperature bath has temperature controller, regulating thermostatic bath temperature, and connection on pipeline one cuts Only one end of valve four, the other end of stop valve four connects the air inlet of discharge cavity bottom;Have on the outer wall of dielectric barrier and connect Ground electrode, the inside of dielectric barrier has high-field electrode, is connected with high frequency high between the upper end of high-field electrode and ground electrode Pressure alternating current power supply, is discharge air-gap between high-field electrode and the inwall of dielectric barrier, and micropore is installed in the upper end of dielectric barrier Plate, the top of microwell plate is reaction chamber, has microwell plate, a part for the bottom of inlet is anti-between reaction chamber and discharge cavity Answer intracavity, the upper end of inlet has check valve, the top connection flow meter of check valve, and the top of flow meter connects storage room, The lower exhaust port of chiller, in reaction intracavity, the outside wall surface of the bottom of reaction chamber has muff.
The method that atmospheric dielectric barrier discharge prepares magnetic liquid of nitriding iron, comprises the steps:
The first step, the preparatory stage: prepare surfactant and carrier fluid mixed liquor, supersound process 15 minutes, note in mass ratio Enter storage room, adjust the air of dilution ar flow displacement reaction intracavity;
Second step, the stage of reaction: liquid iron pentacarbonyl is heated to 30 DEG C, adjusts and carry ar flow, iron pentacarbonyl is steamed Vapour is carried along into discharge cavity, applied voltage, generates atmospheric pressure ar/nh3/fe(co)5Coaxial unit plasma, etc. In gas ions, the active group reaction of fe and n generates ε-fe3N magnetic-particle, the ε-fe being coated by surfactant3N magnetic-particle It is dispersed in carrier fluid, form magnetic liquid of nitriding iron;
3rd step, cooling stage: after preparation experiment terminates, the magnetic liquid for avoiding hotter is oxidized in atmosphere, continues Continuous logical dilution ar protection magnetic liquid, when reaction cavity temperature is reduced to room temperature, opens reaction chamber and collects magnetic liquid of nitriding iron.
Beneficial effects of the present invention: propose the device preparing magnetic liquid of nitriding iron using atmospheric dielectric barrier discharge And method, the manufacturing cycle of magnetic liquid of nitriding iron shorten to about 2 hours by the method from 30 hours, prepared magnetic liquid Good fluidity, saturation magnetization is up to 56.17 mt.The method greatlys save cost, is before one kind has industrial applications The magnetic liquid of nitriding iron technology of preparing of scape.
Brief description
Fig. 1 is assembly of the invention structure diagram.
Fig. 2 is ε-fe3The X-ray diffraction pattern of n magnetic-particle.
Fig. 3 is ε-fe3The transmission electron microscope photo of n magnetic-particle.
Fig. 4 is ε-fe3N magnetic particle diameter column scattergram.
The hysteresis curve of Fig. 5 magnetic liquid of nitriding iron.
In figure: 1. liquid iron pentacarbonyl, 2. constant temperature bath, 3. temperature controller, 41. mass flow controllers one, 42. mass flows Controller two, 43. mass flow controllers three, 51. stop valves one, 52. stop valves two, 53. stop valves three, 6. muff, 7. High frequency and high voltage power supply, 8. check valve, 9. flow meter, 10. storage room, 11. chillers, 12. air vents, 13. inlets, 14. reaction chambers, 15. carrier fluids and surfactant mixed liquor, 16. microwell plates, 17. discharge cavities, 18. high-field electrodes, 19. ground connection electricity Pole, 20. plasmas, 21. discharge air-gaps, 22. dielectric barriers, 23. air inlets, 24. stop valves four, 25. pipelines one, 26. Pipeline two, 27. pipelines three, 28. pipelines four, 29. pipelines five.
Specific embodiment
The present invention will be further described below in conjunction with the accompanying drawings:
As shown in Figure 1: atmospheric pressure matter barrier discharge prepares the device of magnetic liquid of nitriding iron, pipeline 3 27 connects quality stream One end of amount controller 1;The other end of mass flow controller 1 connects one end of stop valve 1;Pipeline 4 28 is even One end of logical mass flow controller 2 42, the other end of mass flow controller 2 42 connects one end of stop valve 2 52;Pipe Road 5 29 connects one end of mass flow controller 3 43, and the other end of mass flow controller 3 43 connects stop valve 3 53 One end;The other end of stop valve 1 is connected with pipeline 1, and the other end of stop valve 2 52 is connected with pipeline 1;Pipeline one 25 end enters in constant temperature bath 2, the other end connecting pipeline 2 26 of stop valve 3 53, and the end of pipeline 2 26 is in constant temperature bath In 2;Constant temperature bath 2 has temperature controller 3, regulating thermostatic bath temperature, and pipeline 1 connects one end of stop valve 4 24, stop valve four 24 other end connects the air inlet 23 of discharge cavity 17 bottom;Ground electrode 19, medium are had on the outer wall of dielectric barrier 22 The inside on barrier layer 22 has high-field electrode 18, is connected with high-frequency and high-voltage and hands between the upper end of high-field electrode 18 and ground electrode 19 Stream power supply 7, is discharge air-gap 21 between the inwall of high-field electrode 18 and dielectric barrier 22, and the upper end of dielectric barrier 22 is installed Microwell plate 16, the top of microwell plate 16 is reaction chamber 14, has microwell plate 16, inlet 13 between reaction chamber 14 and discharge cavity 17 Bottom a part in reaction chamber 14, the upper end of inlet 13 has check valve 8, the top connection flow meter of check valve 8 9, the top of flow meter 9 connection storage room 10, the lower exhaust port 12 of chiller 11 in reaction chamber 14, under reaction chamber 14 Muff 6 is had on the outside wall surface in portion.
The method that atmospheric dielectric barrier discharge prepares magnetic liquid of nitriding iron, comprises the steps:
The first step, the preparatory stage: prepare surfactant and carrier fluid mixed liquor, supersound process 15 minutes, note in mass ratio Enter storage room 10, adjust the air of dilution ar flow displacement reaction intracavity;
Second step, the stage of reaction: liquid iron pentacarbonyl is heated to 30 DEG C, adjusts and carry ar flow, iron pentacarbonyl is steamed Vapour is carried along into discharge cavity 17, applied voltage, generates atmospheric pressure ar/nh3/fe(co)5Coaxial unit plasma 20, the active group reaction of fe and n in plasma generates ε-fe3N magnetic-particle, the ε-fe being coated by surfactant3N magnetic Property even particulate dispersion in carrier fluid, formed magnetic liquid of nitriding iron;
3rd step, cooling stage: after preparation experiment terminates, the magnetic liquid for avoiding hotter is oxidized in atmosphere, continues Continuous logical dilution ar protection magnetic liquid, when temperature is reduced to room temperature in reaction chamber 14, opens reaction chamber 14 and collects iron nitride magnetic Liquid.
Atmospheric pressure matter barrier discharge as shown in Figure 1 prepares the device of magnetic liquid of nitriding iron, mainly by air distribution system, Atmospheric pressure coaxial unit plasma reactor, magnetic liquid of nitriding iron preparation system three part composition.Distribution system Tong You tri- road gas composition, pipeline 3 27 leads to ammonia (nh3), pipeline 4 28 leads to argon (ar), and pipeline 5 29 leads to argon (ar), with Portable belt iron pentacarbonyl (fe (co)5) enter discharge cavity;Ammonia (nh3) as reacting gas, a road argon (ar) is as nh3's Diluent gas;Another road ar is passed through iron pentacarbonyl (fe (co)5) in, carry iron pentacarbonyl steam and enter discharge cavity.By liquid five Carbonyl iron 1 is placed in constant temperature bath 2, using temperature controller 3 regulation and control heating-up temperature be 30 DEG C, with ar in the way of bubbling by iron pentacarbonyl Steam carries entrance discharge cavity 17 from bottom to top.Magnetic liquid of nitriding iron preparation system is mainly by muff 6, storage room 10, cold But device 11 and reaction chamber 14 4 part composition, install microwell plate 16 in reaction chamber 14 and discharge cavity 17 junction.For avoiding carrying Liquid and surfactant mixed liquor 15 are discharged with tail gas, are furnished with chiller 11 at air vent 12.Atmospheric pressure coaxial dielectric hinders Gear discharging plasma reactor adopts coaxial circles tubular electrode structure, and, as dielectric barrier 22, pipe is outer all for quartz glass tube Even winding copper wire is as ground electrode 19.High-field electrode 18 is the rustless steel of diameter 1.5mm;Ground electrode 19 adopts diameter In quartz glass tube outer surface, discharge air-gap is 2.75mm to the copper wire uniform winding of 1.0mm, and actual discharge length is 50mm;Stone English glass tubing as dielectric barrier 22, its internal diameter 7.0mm, external diameter 10.0mm, thickness 1.5mm.Iron pentacarbonyl steam, nh3With The mixed gas of ar enter discharge cavity 17 from bottom to top, produce electric discharge in the presence of high frequency and high voltage power supply 7, form air Pressure coaxial unit plasma 21, the active group reaction of fe and n in plasma generates ε-fe3N magnetic-particle, After being coated by surfactant, form magnetic liquid of nitriding iron.Hinder in conjunction with the atmospheric pressure coaxial dielectric that accompanying drawing 1 provides to the present invention The preparation method that magnetic liquid of nitriding iron is prepared in gear electric discharge is described as follows:
The first step, the preparatory stage: 2:11 in mass ratio prepares surfactant (pbsi-941) and carrier fluid (7# white oil) mixes Close liquid, supersound process 15 minutes, inject storage room 10.Good seal experimental provision is installed, opens mass flow controller 4, adjust Dilution ar flow is 900 ml/min, the air of displacement reaction intracavity.Open check valve 8 and preset mixed liquor is injected into reaction Chamber 14, due to microwell plate 16 effect and larger ar flow, mixed liquor rests on reaction chamber all the time, does not enter discharge cavity 17.
Second step, the stage of reaction: liquid iron pentacarbonyl 1 is heated to 30 DEG C, adjusts and carry ar flow, make fe (co)5Point Press as 5.17 × 102Pa, by fe (co)5Steam is carried along into discharge cavity 17, applied voltage, generates atmospheric pressure ar/nh3/fe (co)5Coaxial unit plasma.Adjust nh3Flow is 30 ml/min, makes the active group of fe and n keep one Desired value, generates the ε-fe of single thing phase3N magnetic-particle, the ε-fe of generation3N magnetic-particle with air-flow pass through microwell plate 16 under And on enter in surfactant and the mixed liquor of carrier fluid, due to the stirring action of microwell plate and larger air-flow, lived by surface Property agent cladding ε-fe3N magnetic-particle is dispersed in carrier fluid.Meanwhile, adjust temperature controller 3, make reaction temperature be maintained at 180 DEG C, this reaction temperature contributes to surfactant more preferable coated magnetic granule, also will not be to the mixing of carrier fluid and surfactant Liquid has a negative impact, and generates the higher magnetic liquid of nitriding iron of stability.For avoiding mixed liquor to discharge with tail gas, testing Cooling circulating water continuous service in journey.When the mixed liquor observing reaction intracavity becomes sticky black liquor, stopped reaction, Experimentation runs 2 hours.
3rd step, cooling stage: after preparation experiment terminates, the magnetic liquid for avoiding hotter is oxidized in atmosphere, continues Continuous logical dilution ar protection magnetic liquid, when temperature is reduced to room temperature in reaction chamber 14, opens reaction chamber 14 and collects magnetic liquid.
Below accompanying drawings other in brief description are explained.
ε-fe in magnetic liquid of nitriding iron prepared by the present invention for the Fig. 23The x-ray diffraction collection of illustrative plates of n magnetic-particle, three Strong diffraction maximum occurs in (111), (113), in (211) peak position, other several weaker diffraction maximums occur in (002), (112), (201), (202), in (222) peak position, substantially identical with the standard card (icdd/jcpds pdf 49-1663) of jade6.0, sentence The main component determining magnetic-particle is ε-fe3N, prepared is magnetic liquid of nitriding iron.
ε-fe in magnetic liquid of nitriding iron prepared by the present invention for the Fig. 33The transmission electron microscope of n magnetic-particle shines Piece, in photo, the director circle ball of black is magnetic-particle, and the gray layer of director circle outer surface of ball is the monolayer surface activity of cladding Agent, prevents magnetic-particle oxidized or clusters.Magnetic particle diameter is about 10 ~ 15 nm, less than single-domain critical size, magnetic Property granule be in single domain structure, magnetic-particle can be considered magnetic dipole, and the magnetic moment direction of magnetic dipole is by magnetocrystalline anisotropy In the direction of easy axis determining, the direction of easy axis of each magnetic dipole is different, and magnetic moment direction is also different, no externally-applied magnetic field effect When, the magnetic moment direction of each magnetic dipole is disorderly and unsystematic, cancel each other, and magnetic liquid does not show macroscopic magnetization.Fig. 4 is institute of the present invention ε-fe in the magnetic liquid of nitriding iron of preparation3N magnetic particle diameter column scattergram, carries out gauss plan using origin software Close, the average diameter that can obtain magnetic-particle is 11 nm.
Fig. 5 is the hysteresis curve of the magnetic liquid of nitriding iron prepared by the present invention, and hysteresis curve is in " s " type curve substantially, Remanent magnetism and coercivity all very littles, illustrate that prepared magnetic liquid of nitriding iron is superparamagnetism.
Method as described in specific embodiment, the raw material of prepared magnetic liquid of nitriding iron, technological parameter and performance such as table 1 With shown in table 2.
Table 1 magnetic liquid of nitriding iron preparing raw material and technological parameter
The performance indications of table 2 magnetic liquid of nitriding iron
.
Using the present invention preparation magnetic liquid of nitriding iron compared with prior art, greatly shorten preparation time, and The saturation magnetization of magnetic liquid of nitriding iron is also higher.Li Xuehui et al. (application number: 200310105229.3, plasma Prepare the method and device of magnetic liquid of nitriding iron) use the magnetic liquid of nitriding iron of plasma method preparation (in patent of invention Sample number into spectrum be 4 magnetic liquid) density bekg/m3When, its saturation magnetization is only 72.4 mt.This Invention is only using the magnetic liquid of nitriding iron of atmospheric pressure coaxial unit one step preparation, densitykg/m3 When, its saturation magnetization has reached 56.17 mt, illustrates using the magnetic liquid of nitriding iron magnetic prepared by the present invention Particulates' properties are fine.The density of magnetic liquid is mainly determined by the magnetic-particle quantity incorporating in carrier fluid, and Li Xuehui et al. is made Although standby magnetic liquid of nitriding iron density reacheskg/m3, but saturation magnetization is relatively low, illustrates made Standby magnetic-particle poor-performing.Huang Wei et al. (application number: 200510064275.2, prepare nitrogen using concentrating agent of low volatilization point Change ferromagnetic fluid method) using gas-liquid phase method preparation magnetic liquid of nitriding iron (lot number 9 magnetic in patent of invention Liquid) using after concentrating agents, the density of magnetic liquid of nitriding iron iskg/m3When, its saturation magnetization reaches 142.5 mt, but the method response time be up to 30 hours, relatively costly, be unsuitable for developing industry metaplasia and produce.To the present invention Prepared magnetic liquid of nitriding iron concentrates after removing part carrier fluid, and the density of magnetic liquid reacheskg/m3 When, its saturation magnetization has brought up to 139.4 mt, and its saturation magnetization has reached domestic level, and mobility is relatively Good.

Claims (1)

1. atmospheric pressure matter barrier discharge prepare magnetic liquid of nitriding iron device it is characterised in that: pipeline three (27) connection quality One end of flow controller one (41);The other end of mass flow controller one (41) connects one end of stop valve one (51);Pipe Road four (28) connects one end of mass flow controller two (42), the other end connection stop valve of mass flow controller two (42) Two (52) one end;Pipeline five (29) connects one end of mass flow controller three (43), mass flow controller three (43) The other end connects one end of stop valve three (53);The other end of stop valve one (51) is connected with pipeline one (25), stop valve two (52) the other end is connected with pipeline one (25);The end of pipeline one (25) enters in constant temperature bath (2), stop valve three (53) Other end connecting pipeline two (26), the end of pipeline two (26) is in constant temperature bath (2);Constant temperature bath (2) has temperature controller (3), adjusts Section constant temperature bath temperature, the upper one end connecting stop valve four (24) of pipeline one (25), the other end connection electric discharge of stop valve four (24) The air inlet (23) of chamber (17) bottom;Ground electrode (19), dielectric barrier (22) are had on the outer wall of dielectric barrier (22) Inside there is high-field electrode (18), be connected with high-frequency and high-voltage between the upper end of high-field electrode (18) and ground electrode (19) and exchange Power supply (7), is discharge air-gap (21) between the inwall of high-field electrode (18) and dielectric barrier (22), dielectric barrier (22) Microwell plate (16) is installed in upper end, and the top of microwell plate (16) is reaction chamber (14), has between reaction chamber (14) and discharge cavity (17) There is microwell plate (16), in reaction chamber (14), the upper end of inlet (13) has unidirectional a part for the bottom of inlet (13) Valve (8), top connection flow meter (9) of check valve (8), top connection storage room (10) of flow meter (9), chiller (11) Lower exhaust port (12) in reaction chamber (14), the outside wall surface of bottom of reaction chamber (14) has muff (6).
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CN109803480A (en) * 2019-03-20 2019-05-24 重庆中涪科瑞工业技术研究院有限公司 A kind of glow plasma generating means applied to macromolecule material surface modification
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05286704A (en) * 1992-04-10 1993-11-02 Natl Res Inst For Metals Device for producing magnetic fluid or grain
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
CN102063992A (en) * 2010-11-27 2011-05-18 大连大学 Magnetic liquid and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05286704A (en) * 1992-04-10 1993-11-02 Natl Res Inst For Metals Device for producing magnetic fluid or grain
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
CN102063992A (en) * 2010-11-27 2011-05-18 大连大学 Magnetic liquid and preparation method thereof

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