CN1261949C - Method and apparatus for preparing nitrided iron magnetic liquid by plasma - Google Patents
Method and apparatus for preparing nitrided iron magnetic liquid by plasma Download PDFInfo
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- CN1261949C CN1261949C CN 200310105229 CN200310105229A CN1261949C CN 1261949 C CN1261949 C CN 1261949C CN 200310105229 CN200310105229 CN 200310105229 CN 200310105229 A CN200310105229 A CN 200310105229A CN 1261949 C CN1261949 C CN 1261949C
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Abstract
The present invention belongs to a preparation method and a device for magnetic liquid. The present invention has a method for preparing nitridation ferromagnetic liquid by plasma that a first step, preparing preprocessed liquid and pouring in a reactor; a second step, replacing air in the reactor with inert gas; a third step, injecting carbonyl iron into the reactor; a fourth step, putting diluent gas and free ammonia in the reactor; a fifth step, reacting: preheating the reactor so as to keep temperature in a cavity at the temperature of 80 to 90 DEG C, and simultaneously starting up direct current high voltage and alternating current pulse high voltage; blocking the free ammonia and discharging so as to carry out ionization, regulating reaction temperature at the temperature of 100 to 140 DEG C, and running for 80 to 120 minutes; in the entire reaction process, a cooling device is run; a sixth step, cooling temperature in the reaction cavity which needs to be sealed to less than 40 DEG C and collecting black magnetic liquid. The present invention is a fund subsidizing project of national natural science, and plasma technique which is applied to preparing nanometer magnetic liquid is create in the country. The present invention has the advantages of simple steps, short flow paths and low cost; products are shaped in a one-step mode can be directly applied without processing.
Description
(1) technical field
The invention belongs to the preparation method and the equipment of magnetic liquid, especially adopt physical means to handle method and isolated plant thereof that chemical synthesis prepares magnetic liquid of nitriding iron.
(2) background technology
Magnetic liquid of nitriding iron is a kind of nano-functional material, is to be dispersed in the carrier fluid and the magnetic colloid solution that forms had both had ferromagnetic magnetic by the nanoscale single domain magnetic particle that surfactant coats, and has the flowability of liquid again.When no the action of a magnetic field, itself does not show magnetic, and nanoscale single domain magnetic particle is done Brownian movement as pollen in the water; Under the effect of outfield force, nanometer single domain magnetic particle does not condense yet and does not precipitate, and moves along magnetic direction is whole.
People such as Japan metal research institute two-story valley merit announce to make magnetic liquid of nitriding iron in the 6th the international magnetic liquid meeting that Paris, FRA is held, what adopt is the gas phase liquid phase method, though magnetic saturation intensity is a ferrite is 5 times of magnetic liquid, but preparation condition strictness, technical process is longer, general Fe (CO)
5Total reaction was wanted about 10 hours; 93 years disclosed preparation magnetic liquid of nitriding iron patents (No5180512) of the U.S., the preparation method who provides will be through repeatedly heating up, be incubated, lower the temperature, circulation recirculation, complex process, requirements of process tens hours; The Guo Guang of BeiJing, China university of chemical technology gives birth to " the solution-air chemical reaction the prepares magnetic liquid of nitriding iron " preparation time that waits the people to deliver in 2000 on " Journal of Inorganic Materials " also be about 10 hours; " development of high saturation and magnetic intensity magnetic liquid of nitriding iron " that Beijing Iron and Steel Research Geueral Inst teaches people such as benevolence to deliver on " Metallic Functional Materials " calendar year 2001 slowly is though prepare magnetic saturation intensity near international parameter, requirements of process 30 several hrs.
The retrieval domestic and foreign literature is the result show, the technology of preparation magnetic liquid is a lot, but the strictness of ubiquity preparation condition, complex process, technological process is tediously long to wait deficiency, thereby causes the with high costs of magnetic liquid, influences the Application and Development of magnetic liquid.
(3) summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, the method that provides a kind of plasma to prepare magnetic liquid of nitriding iron adopts physical means to handle the chemical synthesis problem, and technological process is simplified, and the reaction time shortens, and technology is simple, and production cost is low.The present invention also aims to provide a kind of device that plasma prepares magnetic liquid of nitriding iron that is used for, simple and reasonable, safety is easy to operate.
The technical scheme that the present invention is adopted for achieving the above object is: plasma prepares the method for magnetic liquid of nitriding iron, and concrete processing step is as follows:
The first step, preparation prefabricated solution: took by weighing surfactant, carrier fluid and anhydrous sodium sulfate in 1: 2～4: 1 by mass ratio, mixed preparing prefabricated solution and airtight leaving standstill more than 17 hours are poured in the reactor then.
Second step, displaced air: start aspiration pump, regulate controlling valve and bleed, charge in the reactor air in the metathesis reactor simultaneously with inert gas.
The 3rd step, injection carbonyl iron: take by weighing carbonyl iron by prefabricated solution and carbonyl iron mass ratio 1: 4～6, and in the injecting reactor.
The 4th step, input gas: carrier gas and ammonia are by in flow-rate ratio 1: 1～3 input reactors.
The 5th step, reaction: pre-thermal reactor, make reactor temperature be in 80～90 ℃, start high direct voltage, start the alternating-current pulse high pressure simultaneously, ammonia is intercepted discharge carry out ionization, reaction temperature is regulated and control at 100～140 ℃, operation 80～120min, in the entire reaction course, the cooling device operation on the reactor seal cover.
The 6th step, collection product: when reactor temperature to be sealed is cooled to below 40 ℃, collect black magnetic liquid.
Plasma prepares the device of magnetic liquid of nitriding iron, comprise and substitute exhaust equipment and reactor, the outside of reactor and bottom coat attemperating unit, reactor center is equipped with gas inlet pipe, the inner direct current negative electrode of placing of gas inlet pipe, outside tight fit is equipped with the direct current positive electrode, be with the insulated barriers pipe outward, pore sieve sheet is equipped with in the bottom of insulated barriers pipe, the DC electrode outer, coaxial is placed one group of ac electrode, the interior electrode of ac electrode and external electrode constitute the inside and outside wall of reactor, temperature sensor and multistage barrier flaps are housed in the reactor, multistage barrier flaps is fixed on the gas inlet pipe, and cooling device and sealing sprue are housed on the reactor seal cover, cooling device with substitute exhaust equipment and join.
Described direct current negative electricity is screw-type very, and positive electricity is very telescopic; The sleeve of the interior electrode of ac electrode and the very coaxial placement of dispatch from foreign news agency; Cooling device is a secondary cooling device from coarse to fine; Multistage barrier flaps is a tilting refluxing multi-stage barrier flaps.
Advantage of the present invention is: utilize the preparation facilities of development voluntarily, adopt physical means to handle the chemical synthesis problem---utilize plasma method to prepare nano-magnetic fluid.Start high direct voltage, DC electrode intercepts discharge to ammonia, and ion, atom, excited atom and the free radical of excitation ammonia molecular breakdown, ionization ammonification are with the carrying out of accelerated reaction; Then, ac electrode provides electron energy with more abundant ionization ammonia, improves activation effect and promotes and decompose and reconfigure; And enter reaction chamber by pore sieve sheet and reconfigure generation nanoscale iron nitride magnetic particulate with the iron nucleus that carbonyl iron decomposes, monolayer coating through surfactant is dispersed in the carrier fluid, all can prepare nano-magnetic fluid under the reactant conditions of differential responses temperature and various dose.Reaction process is simplified, and the reaction time foreshortened to about 2 hours, and technology is simple, the equipment advantages of simple, safety is easy to operate, does not need the vacuum reaction environment, and the magnetic liquid of preparation " flowability " is better, " stability " is higher, and magnetic saturation intensity reaches domestic like product index, and cost is low.
The present invention is national natural science fund subsidy project (50077002), compares with domestic and international prior art, and it is domestic initiation that plasma technique is applied to prepare nano-magnetic fluid; Step is simple, and flow process shortens, and cost reduces; The product one-shot forming need not to handle and can directly use.A large amount of experiments and data declaration plasma method are a kind of new methods that preparation iron nitride magnetic fluid shortens reaction process.
(4) description of drawings
Accompanying drawing is the present device structural representation.
(5) embodiment
Embodiment 1
Below in conjunction with accompanying drawing present device is further described, plasma prepares the device of magnetic liquid of nitriding iron, comprise and substitute exhaust equipment and reactor, the outside of reactor and bottom coat attemperating unit 4, according to the internal-response state of reactor, instant regulation and control are to guarantee suitable reaction temperature; Reactor center is equipped with gas inlet pipe 5, the gas inlet pipe 5 inner screw-type direct current negative electrodes 8 of placing, outside tight fit is equipped with telescopic direct current positive electrode 9, be with insulated barriers pipe 10 outward, millimeter level pore sieve sheet 15 is equipped with in the outside of insulated barriers pipe 10, entire electrode adopts high direct voltage 19 power supplies, forms high direct voltage column casing formula and intercepts sparking electrode, and main purpose is the activation ammonia; The DC electrode outer, coaxial is placed two sleeves and is constituted ac electrode, adopt 20 power supplies of alternating-current pulse high pressure, main purpose is to be further activation, disassociation, reconfiguring provides electron energy, the interior electrode 1 of ac electrode and external electrode 2 constitute the inside and outside wall of reactor, temperature sensor 7 and inclination refluxing multi-stage barrier flaps 6 are housed in the reactor, temperature sensor 7 connects display 18, multistage barrier flaps 6 is fixed on the gas inlet pipe 5, cooling device and sealing sprue 13 are housed on the reactor seal cover 3, cooling device is that bubble formula condenser 11 and spiral condenser 12 from coarse to fine constitutes, condenser is substituted the aspiration pump that does not show in gas port 14 map interlinkings, regulate controlling valve 16 control flowmeters 17, control gaseous is bled, ventilation, air in the displacement sealing system makes the rapid cooling for reflux of carbonyl iron.
Adopt the said equipment to prepare the method for magnetic liquid of nitriding iron, its concrete processing step is as follows:
The first step, preparation prefabricated solution: the self-control surfactant: with polyethylene polyamine and unrighted acid is raw material, adopts solvent method to synthesize amide surfactants.Reactant ratio is 4: 1; Temperature range is at 140～180 ℃; 8～10 hours reaction time got surfactant, and is stand-by.
Take by weighing self-control surfactant, carrier fluid (can be aviation kerosine, white oil, guide rail wet goods), anhydrous sodium sulfate in 1: 2～4: 1 by mass ratio, be hybridly prepared into " prefabricated solution ", pour reactor into after airtight static 17～19 hours.Surfactant also can be selected polybutylene-based succimide TEPA for use, and by the product that Japanese LUBRIZOL company produces, commodity be called lubrizol-941, abbreviation PBSI.
Second step, displaced air: start aspiration pump, reconcile controlling valve and bleed, charge in the reactor with inert gas, the air in the displacement sealing system, inert gas can be argon gas, nitrogen etc., this process 2～3 times repeatedly.
The 3rd step, inject carbonyl iron: take by weighing carbonyl iron by prefabricated solution and carbonyl iron mass ratio 1: 4～6, with carbonyl iron by sealing in the sprue injecting reactor.
The 4th step, input gas: adjusting controlling valve, is that 1: 1.5 ratio is imported gas inlet pipe from source of the gas with gas in the flow-rate ratio of carrier gas and ammonia.
The 5th step, reaction: the pre-thermal reactor 20～30min of attemperating unit, make reactor temperature reach 80～90 ℃, start high direct voltage, ammonia is intercepted discharge, start the alternating-current pulse high pressure simultaneously, provide electron energy with abundant ionization ammonia, improve activation effect and promote and decompose and reconfigure.Reaction operation 80～90min, in the whole service process, system all is in the mobile state of cooling of frozen water, and reaction temperature is regulated and control at 100～120 ℃.
The 6th step, collection product: when the temperature sealing is cooled to below 40 ℃ in the question response device, collect black magnetic liquid.
Press that embodiment 1 described method prepared nano-magnetic fluid under the differential responses condition is raw materials used, activation parameter, technological parameter; Following each table of characteristic, granularmetric composition and the distribution thereof of the nano-magnetic fluid of preparation:
Table 1 is raw materials used
| Sample number into spectrum | Base stock | Carrier fluid | Surfactant | Carrier gas |
| 1 | Fe(CO) 5 NH 3 | Aviation kerosine | PBSI (Japan) | Argon gas |
| 2 | Fe(CO) 5 NH3 | Aviation kerosine | PBSI (Japan) | Nitrogen |
| 3 | Fe(CO) 5 NH 3 | Rail oil | Self-control | Argon gas |
| 4 | Fe(CO) 5 NH 3 | White oil | Self-control | Argon gas |
Table 2 activation parameter
| Sample number into spectrum | High direct voltage (KV) | Ac high-voltage (KV) | Frequency (KHz) | Help thermal power (W) |
| 1 | 40 | 15 | 62 | 170～200 |
| 2 | 50 | 18 | 62 | 170～200 |
| 3 | 60 | 20 | 62 | 170～200 |
| 4 | 70 | 25 | 62 | 170～200 |
Table 3 technological parameter
| Lot number | Reaction temperature (℃) | Reaction time (min) | Carrier gas/ammonia flow ratio |
| 1 | 100 | 100 | 1∶1 |
| 2 | 110 | 110 | 1∶1.5 |
| 3 | 120 | 120 | 1∶1.5 |
| 4 | 130 | 140 | 1∶2 |
Granularmetric composition of table 4 products obtained therefrom and distribution thereof
| Sample number into spectrum | Granularmetric composition (%) | Particle mean size (nm) | |||||
| 1-5 | 5-10 | 10-18 | 18-36 | 36-60 | 60-69 | ||
| 1 | 0.73 | 7.98 | 4.85 | 1.01 | 0.03 | 0.00 | 13.7 |
| 2 | 0.34 | 3.53 | 5.85 | 1.42 | 0.36 | 0.00 | 15.3 |
| 3 | 0.34 | 6.27 | 4.21 | 1.64 | 0.17 | 0.00 | 17.1 |
| 4 | 3.07 | 10.03 | 2.52 | 0.96 | 0 | 0 | 11.7 |
The characteristic of the magnetic liquid of table 5 preparation
| Sample number into spectrum | Magnetic average particle size (nm) | Density (g/cm3) | Magnetic saturation intensity (Gs) | Remarks |
| 1 | 13.7 | 1.5085 | 367.9 | Before concentrating |
| 2 | 15.3 | 1.143 | 485.6 | Before concentrating |
| 3 | 17.1 | 1.162 | 538.7 | Before concentrating |
| 4 | 11.7 | 1.6186 | 724.4 | Before concentrating |
Claims (6)
1, plasma prepares the method for magnetic liquid of nitriding iron, it is characterized in that: concrete processing step is as follows:
The first step, preparation prefabricated solution: took by weighing amide surfactants, carrier fluid and anhydrous sodium sulfate in 1: 2～4: 1 by mass ratio, mixed preparing prefabricated solution and airtight leaving standstill more than 17 hours, pour into then in the reactor, described carrier fluid is aviation kerosine, white oil or rail oil;
Second step, displaced air: start aspiration pump, regulate controlling valve and bleed, charge in the reactor air in the metathesis reactor with inert gas;
The 3rd step, injection carbonyl iron: take by weighing carbonyl iron by prefabricated solution and carbonyl iron mass ratio 1: 4～6, and in the injecting reactor;
The 4th step, input gas: inert gas and ammonia are by in flow-rate ratio 1: 1～3 input reactors;
The 5th step, reaction: pre-thermal reactor, make reactor temperature be in 80～90 ℃, start high direct voltage, start the alternating-current pulse high pressure simultaneously, ammonia is intercepted discharge carry out ionization, reaction temperature is regulated and control at 100～140 ℃, operation 80～120min, in the entire reaction course, the cooling device operation on the reactor seal cover;
The 6th step, collection product: when reactor temperature to be sealed is cooled to below 40 ℃, collect black magnetic liquid.
2, the used plasma of claim 1 method prepares the device of magnetic liquid of nitriding iron, comprise and substitute exhaust equipment and reactor, it is characterized in that: the outside of reactor and bottom coat attemperating unit (4), reactor center is equipped with gas inlet pipe (5), the inner direct current negative electrode (8) of placing of gas inlet pipe (5), outside tight fit is equipped with direct current positive electrode (9), be with insulated barriers pipe (10) outward, pore sieve sheet (15) is equipped with in the bottom of insulated barriers pipe (10), the DC electrode outer, coaxial is placed one group of ac electrode, the interior electrode (2) of ac electrode and external electrode (1) constitute the inside and outside wall of reactor, temperature sensor (7) and multistage barrier flaps (6) are housed in the reactor, multistage barrier flaps (6) is fixed on the gas inlet pipe (5), cooling device and sealing sprue (13) are housed on the reactor seal cover (3), cooling device with substitute exhaust equipment and join.
3, plasma according to claim 2 prepares the device of magnetic liquid of nitriding iron, it is characterized in that: direct current negative electrode (8) is a screw-type, and positive electrode (9) is telescopic.
4, plasma according to claim 2 prepares the device of magnetic liquid of nitriding iron, it is characterized in that: the interior electrode (2) and the external electrode (1) of ac electrode are the sleeve of coaxial placement.
5, plasma according to claim 2 prepares the device of magnetic liquid of nitriding iron, it is characterized in that: cooling device is a secondary cooling device from coarse to fine.
6, plasma according to claim 2 prepares the device of magnetic liquid of nitriding iron, it is characterized in that: multistage barrier flaps (6) is a tilting refluxing multi-stage barrier flaps.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310105229 CN1261949C (en) | 2003-11-28 | 2003-11-28 | Method and apparatus for preparing nitrided iron magnetic liquid by plasma |
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|---|---|---|---|
| CN 200310105229 CN1261949C (en) | 2003-11-28 | 2003-11-28 | Method and apparatus for preparing nitrided iron magnetic liquid by plasma |
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| CN100358061C (en) * | 2005-04-14 | 2007-12-26 | 钢铁研究总院 | Method for preparing magnetic liquid of nitriding iron by using concentrating agent of low volatilization point |
| CN101531949B (en) * | 2009-04-08 | 2011-12-07 | 大连大学 | Method and device for synthesizing nano magnetic lubricating oil with under synergic action of alternative electric field and temperature field |
| CN101607701B (en) * | 2009-07-24 | 2011-01-05 | 东北大学 | Method and device for preparing iron nitride material by double promotion of nanocrystallization and strong magnetic field |
| CN101891163A (en) * | 2010-07-07 | 2010-11-24 | 北京科技大学 | Method for preparing superfine spherical iron nitride powder |
| CN102063992B (en) * | 2010-11-27 | 2012-05-30 | 大连大学 | Magnetic liquid and preparation method thereof |
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| CN104851548B (en) * | 2015-04-18 | 2017-02-01 | 北京工业大学 | Method for preparing ferrum-nitrogen compound magnetic fluid with high-frequency plasma |
| CN110400689B (en) * | 2019-07-29 | 2020-07-10 | 浙江鑫盛永磁科技有限公司 | Magnetic fluid extraction equipment |
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