CN102963872B - Device and method for preparing nitrided iron micro powders - Google Patents
Device and method for preparing nitrided iron micro powders Download PDFInfo
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- CN102963872B CN102963872B CN201110257858.2A CN201110257858A CN102963872B CN 102963872 B CN102963872 B CN 102963872B CN 201110257858 A CN201110257858 A CN 201110257858A CN 102963872 B CN102963872 B CN 102963872B
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Abstract
The invention relates to a device and a method for preparing nitrided iron micro powders, the particle degree of the prepared nitrided iron micro powders is controllable, the particle size distribution is uniform, the nitridation degree is high, the sphericility is good, the spheroidization rate is high, the temperature is low and the energy consumption is less, a magnetorheological fluid prepared by the nitrided iron micro powders has high saturation magnetization strength and yield stress. A technical scheme employs a carbonyl iron liquid as a reaction initial material, and the nitrided iron micro powders can be prepared by two steps of an ammonolysis reaction and a thermal decomposition reaction. The carbonyl iron liquid and ammonia gas are added in a helix tube type ammonification furnace for the ammonolysis reaction to generate an ammonolysis carbonyl iron complex; the generated ammonolysis carbonyl iron complex is pumped in a gasifier, then entered in a thermal decomposition furnace along a tube under the pressure effect to generate the nitrided iron micro powders, the granularity of the nitrided iron micro powders are regulated and controlled by regulating and controlling the flow of the nitrided iron micro powders, the pyrolysis temperature and the gasification temperature, the generation ratio of the ammonolysis carbonyl iron complex can be controlled by regulating and controlling the carbonyl iron flow, the ammonia gas flow and the ammonolysis temperature, thereby the nitrided iron micro powders components can be controlled.
Description
Technical field
The present invention relates to technical field of magnetic materials, relate in particular to preparation method and the device of iron nitride material.
Background technology
Nitrided iron (Fe
xn) magnetic is the novel magnetic material that development in recent years is got up, not only magnetic performance is good for it, but also there is anti-oxidant and wear resistance preferably, be the very potential magneticsubstance of new generation of one, in chemical industry and national defence high-tech research field, there is all more important using values.Especially at novel intelligent material---traditional magnetic that magnetic flow liquid compares in producing has application prospect widely.
The kind of nitrided iron has many, up to now, thinks known mainly containing: ζ-Fe
2n, ε-Fe
3n, γ '-Fe
4n and Fe
16n
2deng, be found in the earliest in the hardened layer of steel surface nitriding processing.The preparation method of current nitrided iron iron powder mainly comprises Fe (CO)
5nitriding, alpha-feooh reduction nitridation method, halogen molysite and reduction of ferrous oxide nitriding and high-purity α-Fe nitriding etc.
It is Fe by reduction of ferrous oxide nitriding production principal phase that Chinese patent CN1670870A discloses one
16n
2the method of fe nitride magnetic powder.The method is using the pyrrhosiderite containing solid solution Al as ferric oxide, then in 300～600 DEG C of temperature ranges, pass into hydrogen reducing, then at not higher than the temperature of 200 DEG C, in containing nitrogen gas stream (being typically ammonia), keep can obtaining mainly by Fe for several hours
16n
2the nitrogenize iron powder of phase composite.
Chinese patent CN101607701A discloses a kind of method of preparing nitrided iron by the high-purity α-Fe of nitrogenize.The method packs pure nanometer α-Fe powder or the pure α-Fe of nanometer film in high-intensity magnetic field gas nitriding furnace into, passes into hydrogen, and control air speed is 0.5-5h
-1, at 300-450 DEG C, be incubated 10～90 minutes, then stop heating, naturally cool to 60～100 DEG C. at this temperature, apply the magnetic field of 6～20T by field generator for magnetic, pass into ammonia simultaneously, control air speed is 0.5-5h
-1, reactor temperature is increased to 120～250 DEG C and be incubated 8～30 hours, then naturally cool to room temperature, or iron nitride powder or film product.
Chinese patent CN1117020A discloses a kind of synthetic ultra-fine method of nitrided iron of laser Gaseous.The method is with Fe (CO)
5for source of iron, pass through the source of iron of heating taking ammonia as reaction gas, enter continuous CO 2 laser gas-phase reaction chamber, carbon dioxide laser brings out ammonia and Fe (CO)
5gas phase pyrolysis, at Ar or N
2next step synthesis of superfine ferric nitride powder of atmosphere.
The problems such as aforesaid method ubiquity preparation cost is higher, and powder sphericity is not high, granularity control difficulty, this makes magnetic poor stability in the time forming magnetic fluid or magnetic flow liquid, affects the Application and Development of nitrided iron powder.
Summary of the invention
The object of this invention is to provide a kind of device and method of preparing nitrided iron micro powders, the nitrided iron Powder Particle Size of preparing is controlled, size distribution is even, nitridation is high, good sphericity, nodularization rate are high and make that temperature is lower, less energy consumption, and the magnetic flow liquid of preparing with it has higher saturation magnetization and yielding stress.
Technical scheme of the present invention adopts iron carbonyl liquid as the initial thing of reaction, and two-step approach is prepared nitrided iron magnetic flow liquid.Prepare nitrogenize iron powder by aminating reaction and pyrolysis two steps.First iron carbonyl liquid and ammonia are joined in helix tube type ammonification stove, carry out " solution-air " two-phase aminating reaction, generate ammonification iron carbonyl complex compound; The ammonification iron carbonyl complex compound generating is pumped in gasifier, gasify, then enter pyrolysis oven along pipeline voluntarily under pressure, there is pyrolysis, generate nitrogenize iron powder, regulate and control the granularity of nitrided iron micro powders by regulation and control ammonification iron carbonyl complex compound flow, pyrolysis temperature, gasification temperature, control the generation ratio of ammonification iron carbonyl complex compound by regulation and control iron carbonyl flow, ammonia flow, ammonification temperature, reach thus the object of controlling nitrided iron meal component.
Description 1 is as follows to the detailed description of the invention:
The structural representation that accompanying drawing 1 is nitrogenize iron powder preparation facilities of the present invention.
As shown in Figure 1, nitrided iron micro powders preparation facilities of the present invention is made up of tubular type ammonification furnace system I, ammonification intermediate gasification system II, pyrolysis system III, powder gathering system IV system.
Tubular type aminating reaction system I, is made up of thermostatical oil bath (1), tubular reactor (2), agitator (3), well heater (4), gas-liquid separator (5) and ammonification PID temperature controller (6).The interior filling heat-conductive oil of thermostatical oil bath (1), well heater is inserted in thermal oil, PID temperature controller (6) is controlled the temperature of thermostatical oil bath (1), agitator (3) makes uniformity of temperature profile in oil bath pan by stirring thermal oil, and guarantee tubular reactor (2) and heat-conduction oil heat exchange are carried out smoothly.Tubular reactor (2) front end will react initial thing ammonia by stainless-steel pipe and iron carbonyl liquid imports, and rear end is connected with gas-liquid separator (5) by stainless steel tube.
Ammonification intermediate gasification system II, is made up of thermostatical oil bath (7), well heater (8), micropump (9), gasifier (10), agitator (11), gasification PID temperature controller (12), reversing valve (13).The interior filling heat-conductive oil of thermostatical oil bath (7), well heater (8) is inserted in thermal oil, gasification PID temperature controller (12) is controlled the temperature of thermostatical oil bath (7), agitator (11) makes uniformity of temperature profile in oil bath by stirring thermal oil, and guarantee gasifier (10) and heat-conduction oil heat exchange are carried out smoothly.Micropump (9) pumps into the ammonification iron carbonyl complex compound liquid in gas-liquid separator (5) in gasifier (10).Reversing valve (13) can make ammonification iron carbonyl complex compound liquid and Ar protection gas alternately enter in gasifier (10);
Pyrolysis system III, is made up of reversing valve (14), heater strip (15), pyrolysis oven (16) and thermolysis PID temperature controller (17).Ammonification iron carbonyl complex compound gas in gasifier described in claim 3 (10), under pressure, be transported in pyrolysis oven (16) by pipeline, by the ammonification iron carbonyl complex compound gas in heater strip (15) heating pyrolysis oven (16), thermolysis PID temperature controller (17) is controlled pyrolysis oven (16) heat temperature raising speed and thermolysis thermostat temperature.Reversing valve (14) can make ammonification iron carbonyl complex compound gas and Ar protection gas alternately enter in pyrolysis oven (16);
Powder gathering system IV, by powder cooling room (18), jointing clip (19), powder receiving flask (20) composition.Before and after powder cooling room (18) is characterized in that, symmetry has been installed glass peep hole (21), the symmetrical operation gloves (22) of having installed, the condition of production that the effect of peep hole (21) is to observe iron nitride powder, the effect of operation gloves (22) is to clean the iron nitride powder of assembling on cooling locular wall.
Complete assembly and connecting tube all adopt 304 stainless steels to make;
The method of preparing nitrided iron micro mist of the present invention comprises following processing step:
Implementation process is carried out in nitrided iron micro mist manufacturing installation of the present invention.
(1) the first step, start agitator (3), well heater (4) and ammonification PID temperature controller (6), temperature in thermostatical oil bath (1) is risen to 75～95 DEG C, the rotating speed of agitator (3) is 50～200r/min, keep constant temperature after 3 minutes, ammonia and iron carbonyl liquid are passed in tubular reactor (2) and carry out aminating reaction.Input speed in iron carbonyl liquid input tubular reactor (2) is 10mL～1L/h, and it is 100mL～10L/min that ammonia passes into speed;
(2) second step, completes described in the first step after operation, and by reversing valve (13), to input Ar shielding gas in gasifier (10), the input speed of Ar gas is 10～100mL/min; Start agitator (11), well heater (8) and gasification PID temperature controller (12), temperature in thermostatical oil bath (7) is risen to 90～140 DEG C, and the rotating speed of agitator (11) is 50～200r/min;
(3) the 3rd steps complete described in second step after operation, in pyrolysis oven (16), input Ar shielding gas by reversing valve (14), the input speed of Ar gas is 10～100mL/min, start thermolysis PID temperature controller (17) and heater strip (15), control 3～5 DEG C/min of temperature rise rate, make pyrolysis oven (16) internal temperature rise to 180～360 DEG C; ;
(4) the 4th steps, after 60 minutes, stop input Ar shielding gas in gasifier (10) by reversing valve (13), start micropump (9) the ammonification iron carbonyl complex compound liquid pump of the interior collection storage of gas-liquid separator (5) is entered in gasifier (10); The input speed that ammonification iron carbonyl complex compound liquid pumps in gasifier (10) is 5mL～1L/h; The 5th step; stop input Ar shielding gas in pyrolysis oven (16) by reversing valve (14); ammonification iron carbonyl complex compound gas in gasifier (10) in importing pyrolysis oven (16), reversing valve (14) is carried out to pyrolysis; temperature of reaction is controlled at 180～360 DEG C of scopes; thermal decomposition time is 3～20 hours; in pyrolysis process, can pass through the condition of production of peep hole (21) observation iron nitride powder.
(5) the 5th steps are swept to powder collection bottle (20) by operation gloves (22) by the nitrogenize iron powder of preparation in powder cooling room (18).The nitrided iron powder making can, with ball mill or shredder processing, make it to disperse, and finally makes nitrided iron micro mist.
The present invention manufactures in the implementation process of metal magnetic flow liquid, in tubular type aminating reaction system, carries out following aminating reaction.
Ammonification iron carbonyl complex compound gas-liquid after reaction is carried out, after gas-liquid separator condensation is collected, pumped into from gasifier top by micropump, in gasifier, be converted into the gas of ammonification iron carbonyl complex compound, enter under pressure pyrolysis oven, carry out rapidly pyrolysis.Pyrolysis formula is as follows:
Reaction generates nitrided iron (as nitrided iron) magnetic particle, and emits carbon monoxide, ammonia, hydrogen.
Iron carbonyl liquid enters flow in pyrolysis oven and has determined the concentration of oily carrier fluid and iron carbonyl liquid mixed solution in pyrolysis oven, the add-on of the height of this concentration, the height of pyrolysis temperature, tensio-active agent has determined the size of the iron nitride magnetic particulate of thermolysis generation, and the length of thermal decomposition time has determined the percentage composition of iron nitride magnetic particulate in oily carrier fluid.
Adopt device and method of the present invention can obtain the magnetic flow liquid that contains submicron order iron nitride magnetic particulate, its particle diameter can reach 0.5～8 μ m.
Brief description of the drawings
Fig. 1 nitrided iron micro powders preparation facilities schematic diagram
In figure: (1) thermostatical oil bath, (2) tubular reactor, (3) agitator, (4) well heater, (5) gas-liquid separator, (6) ammonification PID temperature controller, (7) thermostatical oil bath, (8) well heater, (9) micropump, (10) gasifier, (11) agitator, (12) gasification PID temperature controller, (13) reversing valve, (14) reversing valve, (15) heater strip, (16) pyrolysis oven, (17) pyrolysis PID temperature controller, (18) powder cooling room, (19) jointing clip, (20) powder receiving flask, (21) glass peep hole, (22) operation gloves.
Embodiment
The method of preparing iron nitride material is as follows:
Ammonia and iron carbonyl liquid are passed into and in tubular reactor, carry out aminating reaction.Input speed in iron carbonyl liquid input tubular reactor (2) is 240mL/h, and it is 3.5L/min that ammonia passes into speed, and controlling constant temperature oil bath pot temperature is 85 DEG C, maintains this process 4 hours, then stops.The ammonification iron carbonyl complex compound micropump that collection in gas-liquid separator is deposited pumps into gasifier gasification with the speed of 360mL/h, ammonification iron carbonyl complex compound after gasification enters pyrolysis oven along pipeline, carry out thermolysis, prepare nitrided iron micro powders, in reaction process, control pyrolysis oven temperature-stable at 240 DEG C, until the ammonification carbonylcomplex that reaction generates is used up.The powder ball milling that reaction makes disperses for 3 hours.After testing, gained iron nitride powder gross weight 200g, wherein ε-Fe
3n content is 40%, γ '-Fe
4n content is 35%, ζ-Fe
2n content is 25%, the Fe of minute quantity
3o
4; Powder size is 2～4 μ m.
Claims (6)
1. prepare the device of nitrided iron micro powders for one kind, it is characterized in that by tubular type ammonification furnace system I: thermostatical oil bath (1), tubular reactor (2), the first agitator (3), primary heater (4), gas-liquid separator (5) and ammonification PID temperature controller (6), ammonification intermediate gasification system II: thermostatical oil bath (7), secondary heater (8), micropump (9), gasifier (10), the second agitator (11), gasification PID temperature controller (12), the first reversing valve (13), pyrolysis system III: the second reversing valve (14), heater strip (15), pyrolysis oven (16), with thermolysis PID temperature controller (17), powder gathering system IV: powder cooling room (18), jointing clip (19), powder receiving flask (20) composition, utilize the granularity of nitrided iron micro powders of this device preparation at 0.5～8 μ m.
2. the device of preparing nitrided iron micro powders according to claim 1, it is characterized in that, the interior filling heat-conductive oil of thermostatical oil bath (1), well heater is inserted in thermal oil, ammonification PID temperature controller (6) is controlled the temperature of thermostatical oil bath (1), the first agitator (3) makes uniformity of temperature profile in oil bath pan by stirring thermal oil, guarantee tubular reactor (2) and heat-conduction oil heat exchange are carried out smoothly, tubular reactor (2) front end will react initial thing ammonia by stainless-steel pipe and iron carbonyl liquid imports, rear end is connected with gas-liquid separator (5) by stainless steel tube.
3. the device of preparing nitrided iron micro powders according to claim 1, it is characterized in that, the interior filling heat-conductive oil of thermostatical oil bath (7), secondary heater (8) is inserted in thermal oil, gasification PID temperature controller (12) is controlled the temperature of thermostatical oil bath (7), the second agitator (11) makes uniformity of temperature profile in oil bath by stirring thermal oil, guarantee gasifier (10) and heat-conduction oil heat exchange are carried out smoothly, micropump (9) pumps into the ammonification iron carbonyl complex compound liquid in gas-liquid separator (5) in gasifier (10), the first reversing valve (13) can make ammonification iron carbonyl complex compound liquid and Ar protection gas alternately enter in gasifier (10).
4. the device of preparing nitrided iron micro powders according to claim 1, it is characterized in that, ammonification iron carbonyl complex compound gas in gasifier (10), under pressure, be transported in pyrolysis oven (16) by pipeline, by the ammonification iron carbonyl complex compound gas in heater strip (15) heating pyrolysis oven (16), thermolysis PID temperature controller (17) is controlled pyrolysis oven (16) heat temperature raising speed and thermolysis thermostat temperature, the second reversing valve (14) can make ammonification iron carbonyl complex compound gas and Ar protection gas alternately enter in pyrolysis oven (16).
5. the device of preparing nitrided iron micro powders according to claim 1, it is characterized in that, before and after powder cooling room (18), symmetry has been installed glass peep hole (21), the symmetrical operation gloves (22) of having installed, the condition of production that the effect of glass peep hole (21) is to observe iron nitride powder, the effect of operation gloves (22) is to clean the iron nitride powder of assembling on cooling locular wall.
6. the device of preparing nitrided iron micro powders according to claim 1, is characterized in that complete assembly and connecting tube all adopt 304 stainless steels to make.
7. the device of preparing nitrided iron micro powders according to claim 1 is prepared the method for nitrided iron micro mist, it is characterized in that processing step is as follows: the first step, start the first agitator (3), primary heater (4), with ammonification PID temperature controller (6), temperature in thermostatical oil bath (1) is risen to 75～95 DEG C, the rotating speed of the first agitator (3) is 50～200r/min, keep constant temperature after 3 minutes, ammonia and iron carbonyl liquid are passed in tubular reactor (2) and carry out aminating reaction, input speed in iron carbonyl liquid input tubular reactor (2) is 10mL～1L/h, it is 100mL～10L/min that ammonia passes into speed, second step, completes described in the first step after operation, and by the first reversing valve (13), to input Ar shielding gas in gasifier (10), the input speed of Ar gas is 10～100mL/min, start the second agitator (11), secondary heater (8) and gasification PID temperature controller (12), temperature in thermostatical oil bath (7) is risen to 90～140 DEG C, and the rotating speed of the second agitator (11) is 50～200r/min, the 3rd step, complete described in second step after operation, in pyrolysis oven (16), input Ar shielding gas by the second reversing valve (14), the input speed of Ar gas is 10～100mL/min, start thermolysis PID temperature controller (17) and heater strip (15), control 3～5 DEG C/min of temperature rise rate, make pyrolysis oven (16) internal temperature rise to 180～360 DEG C, the 4th step, after 60 minutes, stop inputting Ar shielding gas in gasifier (10) by the first reversing valve (13), start micropump (9) the ammonification iron carbonyl complex compound liquid of the interior collection storage of gas-liquid separator (5) is pumped in gasifier (10), the input speed that ammonification iron carbonyl complex compound liquid pumps in gasifier (10) is 5mL～1L/h, the 5th step, stop inputting Ar shielding gas in pyrolysis oven (16) by the second reversing valve (14), ammonification iron carbonyl complex compound gas in gasifier (10) in importing pyrolysis oven (16), the second reversing valve (14) is carried out to pyrolysis, temperature of reaction is controlled at 180～360 DEG C of scopes, thermal decomposition time is 3～20 hours, in pyrolysis process, can pass through the condition of production of peep hole (21) observation iron nitride powder, the 6th step is swept to powder collection bottle (20) by operation gloves (22) by the nitrogenize iron powder of preparation in powder cooling room (18), and the nitrided iron powder making can, with ball mill or shredder processing, make it to disperse.
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| CN103273074B (en) * | 2013-03-27 | 2014-12-10 | 深圳市中金岭南科技有限公司 | Process method of continuously producing ultra-fine nickel powder |
| CN103349993B (en) * | 2013-07-17 | 2015-04-15 | 北京航空航天大学 | Method for synthesizing magnetically separable iron nitride-based magnetic nanophotocatalyst |
| CN113059182A (en) * | 2020-01-02 | 2021-07-02 | 吉林卓创新材料有限公司 | Preparation method of carbonyl iron powder special for magnetic grinding fluid |
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| CN101891163A (en) * | 2010-07-07 | 2010-11-24 | 北京科技大学 | Method for preparing superfine spherical iron nitride powder |
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