CN113458406A - Method for quickly producing superfine iron powder - Google Patents
Method for quickly producing superfine iron powder Download PDFInfo
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Abstract
The invention utilizes a two-stage steel belt furnace to produce superfine iron powder, and oxygen is introduced into the first stage to oxidize magnetite so as to change the magnetite into Fe2O3The second stage is to introduce hydrogen to make Fe2O3The core point is the treatment of gas type, pressure and flow direction at the interface between the two sections of furnaces, the treatment of gas pressure and flow direction at the interface is particularly important because the first section is filled with oxygen and the second section is filled with hydrogen, otherwise, the contact of hydrogen and oxygen at high temperature can occur to cause ignition and even explosion, and in addition, the temperature control of reduction is lower, about 570 ℃, so that Fe is reduced2O3The direct reduction to Fe does not pass through the FeO stage because it is more difficult to reduce to Fe if FeO is present, so although the reduction rate is relatively slow at low temperatures, it does not pass through the FeO stage, but is relatively slow compared to Fe3O4The reduction at higher temperatures is also faster, making it less expensive to produce.
Description
Technical Field
The invention belongs to a powder preparation technology in the field of powder metallurgy, and particularly relates to a rapid preparation technology of superfine iron powder.
Background
The superfine iron powder is an important raw material in the powder metallurgy industry, has the average particle size of 1-10 microns, and is widely applied to various fields of automobile industry, household appliance industry, superhard materials, electromagnetism, biology, medicine, optics and the like. Compared with common iron powder (200 meshes (75 mu m)), the ultrafine iron powder has larger specific surface area and activity, special electric, magnetic, optical and catalytic, adsorption and chemical reactivity and the like. With the development of powder metallurgy products in the directions of high density, high strength, complex shape and the like, the dosage of the superfine iron powder is larger and larger. For example, adding a certain amount of superfine iron powder into a powder metallurgy product can obviously improve the density of the product, thereby improving the strength of the product and reducing the sintering temperature of the product. In recent years, the 3D printing technology and the development of superhard materials have been vigorous, so that the market of ultrafine iron powder is further expanded.
Due to the special properties and wide application of the superfine iron powder, people have conducted a great deal of research on the preparation method of the superfine iron powder. The preparation method mainly at home and abroad comprises the following steps: reduction, carbonyl, vacuum evaporation, sputtering, and high-energy ball milling. But the existing methods for industrially producing the superfine iron powder on a large scale only comprise a carbonyl method and an oxalic acid precipitation method.
The carbonyl method first requires the carbonylation of Fe and CO under certain conditions to produce carbonyl iron (Fe (CO))5) Then, the pyrolysis is carried out under certain temperature and pressure conditions, so as to form the superfine iron powder. The method has the advantages that the produced superfine iron powder has high purity, fine and uniform granularity and good fluidity; the disadvantages are CO and Fe (CO)5The method has the advantages that the carbonyl iron powder is flammable, explosive and toxic, the production process has great pollution to the environment, the production cost is high, the price of the carbonyl iron powder is high, and the factors hinder the popularization and application of the carbonyl iron powder.
The oxalic acid method is to use ferric sulfate as raw material, replace sulfate radical with oxalic acid to obtain pure ferric oxalate, then heat to decompose and reduce with hydrogen to obtain superfine iron powder. The product can meet the requirement of particle size of several microns, but the preparation cost is high. The raw material cost of the ferrous oxalate oxalic acid of each ton of the superfine iron powder is 15000-.
Disclosure of Invention
The invention is mainly realized by the following technical scheme:
firstly, the raw material adopts the large-quantity cheap ultra-pure iron concentrate powder on the current market, and the technical indexes are as follows:
chemical components:
| composition (I) | TFe | MnO | TiO2 | SiO2 | Al2O3 | Hydrochloric acid insoluble substance |
| Content (wt.) | >71.5 | 0.07 | 0.13 | 0.11 | 0.13 | 0.13 |
The iron ore concentrate powder has granularity smaller than-700 mesh and water content smaller than 0.3%.
Original workerThe technological process includes oxidizing iron ore concentrate powder with oxygen in the same steel belt furnace to convert the iron ore concentrate powder into Fe3O4Becomes Fe2O3Meanwhile, according to the study of document 2, in this process, due to the change of the crystal structure, Fe is newly generated2O3Internal voids are formed inside the crystal structure, and the structure is favorable for the reduction of the oxide by hydrogen, so that the reduction speed is accelerated. The specific furnace type structure is shown in the figure. The length of the oxidation section is generally between 6 and 8m, the specific length is determined according to the production capacity, the temperature is between 350 and 450 ℃, the flow of oxygen is excessive when the pressure of a 1# regulating valve is set to be 1.5 to 2KPa, the parameters also need to be adjusted according to the production capacity and the length of the oxidation section, the oxygen is discharged from the tail end of the oxidation section through a furnace end, the pressure at an oxygen inlet is 5 to 7KPa, and the pressure at an outlet is about 1.5 to 2 KPa.
The oxidizing section is connected with the reducing section through a flange, the length of the flange is 1.5-2m, and nitrogen is introduced into the flange section so as to divide the atmosphere of the oxidizing section and the atmosphere of the reducing section, so that the oxygen and the hydrogen are prevented from being mixed at high temperature to cause explosion. The inlet pressure of nitrogen is 5-7KPa, when guaranteeing 2# governing valve pressure setting for 2-2.5 KPa, the export pressure keeps about 2-2.5 KPa, can make nitrogen separate oxygen and hydrogen like this, further ensures safety.
The material enters a hydrogen reduction section after passing through an intermediate flange section, the temperature of the section is set to 570 ℃, hydrogen enters a furnace body from a cooling section, the hydrogen is discharged out of the furnace body from the beginning outlet of the reduction section and is subjected to ignition treatment, the pressure at a hydrogen inlet is kept at 5-7KPa, the hydrogen flow is excessive when the pressure of a 3# regulating valve is set to be 1.5-2 KPa, and the pressure at the outlet is kept at about 1.5-2 KPa; the ratio of the lengths of the oxidation zone and the reduction zone should be in the range of 1: 3, cooling and discharging through a cooling section after reduction, and then crushing, detecting and packaging to obtain the finished product of the superfine iron powder.
The technology uses the super-pure iron concentrate powder as raw material, and uses the method of firstly oxidizing and then reducing to produce superfine iron powder on the same steel-band furnaceThe method has the advantages of low reduction temperature, short reduction time, low overall production cost of the superfine iron powder, no influence on the environment, and no discharge of three wastes such as waste water, waste gas and waste materials. The method of document 1 (a low-cost low-temperature direct reduction for preparing superfine iron powder CN 107186216 a) proposes a method of oxidation before reduction, but the present patent and document 1 have many differences in raw material treatment, reduction equipment, and reduction process parameter selection, which mainly appear as follows: firstly, in the aspect of processing raw materials, the raw material magnetite is firstly refined in the document 1, but the patent technology does not refine the raw materials, but directly utilizes the structural change of the magnetite in the oxidation process to form the superfine porous raw material, which is clearly explained in the document 2 (page P5 for researching the rule of the influence of the hematite ratio of the university of Zhongnan on the preparation of oxidized pellets), namely, the oxidation of the magnetite into hematite is an exothermic reaction, so that the magnetite can be fully oxidized in the roasting process; and the new Fe is generated along with the change of the crystal structure2O3Has strong migration capability. Hematite in a crystalline state has many pores in its particles, and is easily reduced and crushed. Secondly, in document 1, a pusher furnace is used, and oxidation and reduction are not performed in the same equipment, so that temperature reduction is required after oxidation, otherwise, reloading is difficult, while continuous oxidation and reduction are performed in the same equipment, and temperature reduction is not performed after oxidation, and the oxidized material directly enters a reduction section for reduction through a transition section, so that the requirement on the equipment is high, and the equipment structure and corresponding atmosphere control are also a core content of the patent. Thirdly, the reduction temperature in document 1 is about 800 degrees, mainly considering that the reduction speed is higher at higher temperature, while the reduction temperature is controlled to be about 570 degrees, which is obviously lower than that in document 1, the main reason is that although the increase of the reduction temperature is beneficial to the acceleration of the reduction speed, the reduction process at different temperatures is different, and the reduction of iron ore is the initial process of steel production, so a great deal of research is carried out on the reduction process, and the research result shows that at lower temperature, namely below 570 degrees, the reduction process is from iron oxide to iron, no matter the raw material is Fe2O3Or is Fe3O4Namely:
the reaction process of reducing iron oxide by hydrogen at the temperature of below 570 ℃ is as follows:
3 Fe2O3+H2==2 Fe3O4+H2O
0.25 Fe3O4+H2==0.75Fe+H2
the reaction process of reducing iron oxide by hydrogen at the temperature of more than 570 ℃ is as follows:
3 Fe2O3+H2==2 Fe3O4+H2O
Fe3O4+H2==3FeO+H2O
FeO+H2==Fe+H2O
that is, the technology in document 1 has FeO during the reduction process due to the higher reduction temperature, and due to the unique structure of FeO, it takes a longer time for the FeO to be reduced to Fe, so that the reduction time is shortened due to the increased temperature, and the produced FeO needs a longer reduction time to be offset; the process directly adopts lower reduction temperature, namely, the temperature is controlled below 570 ℃, so that FeO phase does not appear in the reduction process, and Fe directly2O3To Fe3O4And the stage is directly followed by metallic Fe, so that although the reduction speed is slow due to low temperature, the total reduction time is basically equal to the reduction time of 800 ℃ because the difficult reduction stage of FeO phase is not passed, and the energy consumption is obviously reduced due to low reduction temperature. For the above reasons, the technical process is still clearly distinguished from the technical process in document 1.
The invention has the following beneficial effects:
1. the raw materials are not crushed and refined any more, the particle size of the ultra-pure iron concentrate powder is relatively fine, generally is-700 meshes, and the aim of further refining is achieved by utilizing the phase change of the raw materials in the oxidation process, so that the preparation cost of the ultra-fine iron powder is reduced;
2. in the same steel strip furnace, oxidation is carried out firstly, and then reduction is carried out, so that the heat energy is utilized to the maximum extent;
3. the temperature of reduction is set at around 570 ℃ so that no FeO phase occurs during reduction, and although the increase in temperature is kinetically advantageous in accelerating the reduction rate, after the temperature is higher than 570 ℃, thermodynamically the FeO phase occurs during reduction, while the FeO phase belongs to a recognized hard-to-reduce phase, so in this patent technique, the reduction temperature is set at a lower temperature to avoid the occurrence of the FeO phase.
Drawings
FIG. 1 is a SEM morphology photograph of an ultrafine iron powder of example 1;
FIG. 2 is a SEM morphology photograph of the superfine iron powder of example 2;
FIG. 3 is a process flow diagram.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and together with the description, serve to explain the principles of the invention.
Example 1
Step 1, adding ultrapure iron concentrate powder into a two-section type steel strip furnace, wherein the thickness of a material layer is 30mm, the strip speed of the steel strip furnace is 130mm/min, the oxidation temperature is 350 ℃, the oxidation time is 60min, a thin film regulating valve is arranged at an oxygen inlet, a 1-2# pressure gauge is arranged at an oxygen outlet and is interlocked with a 1# regulating valve at the air inlet, and the pressure of the 1# regulating valve is set to be 1.5 kpa.
And 2, reducing the temperature of a reduction section at 570 ℃, reducing the time at 180min, arranging a film regulating valve at a hydrogen inlet, arranging a 3-2# pressure gauge at a hydrogen outlet to be interlocked with a 3# regulating valve at the hydrogen inlet, and setting the 3# regulating valve at 1.5 kpa.
And 3, installing a film regulating valve at the nitrogen inlet of the transition section, arranging a 2-2# pressure gauge at the nitrogen outlet to be interlocked with the 2# valve for regulating the air inlet, and setting the pressure of the 2# regulating valve to be 2 kpa.
And 4, crushing, screening, detecting and analyzing the reduced iron powder.
The ingredients of the iron ore concentrate powder before reduction are shown in Table 1
TABLE 1 analysis results of the components and particle size of iron ore concentrate powder
| TFe (all iron) | AIC (acid insoluble) | D50 (Primary particle size) |
| 71.70 | 0.18 | 19.3 |
The SEM pictures and components of the reduced superfine iron powder are shown in the attached figure 1 and the table 2.
Table 2 analysis results of components of reduced iron powder
| TFe (all iron) | AIC (acid insoluble) | O (oxygen content) D50 (primary particle size) |
| 98.60 | 0.16 | 0.458.4 |
Example 2
Step 1, adding ultrapure iron concentrate powder into a two-section type steel strip furnace, wherein the thickness of a material layer is 30mm, the strip speed of the steel strip furnace is 130mm/min, the oxidation temperature is 350 ℃, the oxidation time is 60min, an oxygen inlet is provided with a thin film regulating valve, an oxygen outlet is provided with a 1-2# pressure gauge and is interlocked with a 1# regulating valve of the air inlet, and the pressure of the 1# regulating valve is set to be 2 kpa.
And 2, reducing the temperature of a reduction section at 570 ℃, reducing the time at 180min, arranging a film regulating valve at a hydrogen inlet, arranging a 3-2# pressure gauge at a hydrogen outlet to be interlocked with a 3# regulating valve at the hydrogen inlet, and setting the 3# regulating valve at 2 kpa.
And 3, installing a film regulating valve at the nitrogen inlet of the transition section of the embodiment, arranging a 2-2# pressure gauge at the nitrogen outlet to be interlocked with the 2# regulating valve at the air inlet, and setting the pressure of the 2# regulating valve to be 2.5 kpa.
And 4, crushing, screening, detecting and analyzing the reduced iron powder.
The ingredients of the iron ore concentrate powder before reduction are shown in Table 3
TABLE 3 analysis results of the components and particle size of iron ore concentrate powder
| TFe (all iron) | AIC (acid insoluble) | D50 (Primary particle size) |
| 71.70 | 0.18 | 19.4 |
The SEM pictures and components of the reduced superfine iron powder are shown in figure 2 and table 4.
Table 4 analysis results of components of reduced iron powder
| TFe (all iron) | AIC (acid insoluble) | O (oxygen content) D50 (primary particle size) |
| 98.80 | 0.14 | 0.36 7.3 |
Claims (6)
1. A method for rapidly producing superfine iron powder is characterized in that: using a two-stage steel belt furnace, and adopting oxygen to carry out Fe treatment on a magnetite raw material at a certain temperature in the first stage3O4Is oxidized into Fe2O3Meanwhile, the oxidation section is also a preheating section and then enters a reduction section through a transition section, and Fe is reduced by hydrogen at a lower temperature in the reduction section2O3Directly reducing the iron powder into Fe without passing through the FeO stage, cooling, discharging, crushing and grading to obtain the finished product of the superfine iron powder.
2. The method for rapidly manufacturing an ultra fine iron powder as claimed in claim 1, wherein: to accelerate the reduction rate, magnetite Fe is first introduced3O4Oxidation is carried out to generate Fe2O3In order to accelerate the oxidation process, oxygen is introduced into the oxidation process; the oxidation temperature is 350-450 ℃, a 1# regulating valve is arranged at an oxygen inlet, a 1-1# pressure gauge and a 1-2# pressure gauge are arranged at an oxygen inlet and outlet, the 1-2# pressure gauge is interlocked with the 1# regulating valve, and the length of the oxidation section is matched with that of the reduction sectionThe ratio is 1: 3.
3. the method for rapidly manufacturing an ultra fine iron powder as claimed in claim 1, wherein: the inlet of oxygen is arranged at the furnace end, the outlet is arranged at the tail end of the oxidation section, the pressure of the oxygen inlet is kept at 5-7KPa, the pressure of a 1# regulating valve is set to be 1.5-2 KPa, and the pressure of the oxygen outlet is kept at about 1.5-2 KPa.
4. The method for rapidly manufacturing an ultra fine iron powder as claimed in claim 1, wherein: the transition section in the middle of the oxidation section and the reduction section is in flange connection, and double-layer glass fiber yarns are arranged at two ends of the transition section, so that the mixing of oxygen and hydrogen is prevented, nitrogen is introduced above the transition section and flows out from the lower part of the transition section, a 2# regulating valve is arranged at a nitrogen inlet, a 2-1# pressure gauge and a 2-2# pressure gauge are arranged at the nitrogen inlet and outlet, the inlet pressure of the nitrogen is kept to be 5-7KPa, the pressure of the 2# regulating valve is kept to be 2-2.5 KPa, the 2-2# pressure gauge is interlocked with the 2# regulating valve, the outlet pressure of the nitrogen is kept to be about 2-2.5 KPa, so that the nitrogen can separate the oxygen from the hydrogen, and the safety is further ensured.
5. The method for rapidly manufacturing an ultra fine iron powder as claimed in claim 1, wherein: in the reduction stage, the reduction temperature is controlled to be about 570 ℃ to ensure Fe2O3The reducing time is prolonged because FeO is difficult to reduce if FeO occurs, so that the reducing time is shortened, in the reducing section, hydrogen is introduced from a cooling section at the tail of the furnace, flows out from an inlet of the reducing section and is ignited, the hydrogen which is not consumed in the reducing section is combusted to prevent the hydrogen from leaking into a factory building, a 3# regulating valve is arranged at a hydrogen inlet, a 3-1# pressure gauge and a 3-2# pressure gauge are arranged at a hydrogen inlet and a hydrogen outlet, the 3-2# pressure gauge is arranged before ignition and is interlocked with the 3# regulating valve, the pressure at the hydrogen inlet is kept at 5-7KPa, the 3# regulating valve is set at 1.5-2 KPa, and the pressure at the outlet is kept at about 1.5-2 KPa.
6. The method for rapidly manufacturing an ultra fine iron powder as claimed in claim 1, wherein: and crushing, screening and detecting the reduced superfine iron powder to obtain a finished product of the superfine iron powder, and packaging and warehousing.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115072675A (en) * | 2022-06-14 | 2022-09-20 | 中南大学 | Method for preparing superfine iron nitride powder by hydrogen reduction method |
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