CN104907570A - Preparation method of reduced iron powders for powder metallurgy - Google Patents
Preparation method of reduced iron powders for powder metallurgy Download PDFInfo
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Abstract
The invention belongs to the field of powder metallurgy, and in particular relates to a preparation method of reduced iron powders for powder metallurgy. The preparation method comprises the following steps: (1) crushing metallic iron containing raw materials, and then carrying out wet ore grinding and low intensity magnetic separation sequentially, so as to obtain iron powders subjected to primary impurity removing; (2) decarbonising and roasting the iron powders subjected to primary impurity removing; (3) carrying out mineral separation to the product of the decarbonising and roasting process to remove impurity, washing with acid, filtering, drying and blending, so as to obtain the reduced iron powders for the powder metallurgy. Compared with raw materials including iron scales and high pure iron ore concentrates in the prior art, the raw materials adopted in the method are wide in source and lower in cost. A novel way is provided for preparation of the reduced iron powders for the powder metallurgy.
Description
Technical field
The invention belongs to field of powder metallurgy, particularly, the present invention relates to a kind of preparation method of powder used in metallurgy reduced iron powder.
Background technology
Iron powder is one of maximum powder metallurgy raw material of consumption.Due to iron powder total output 70% ~ 80% for powder metallurgy, the therefore production status of iron powder and scale, the kind of iron powder, quality and cost, have material impact to the development of powder metallurgy industry.
The preparation of reduced iron powder utilizes gas or solid fuel as reducing agent, iron ore fine ore, the contour pure iron oxidizing thing of low carbon boil steel scale of steel rolling are reduced in the solid state the technical process of the quite high iron product of a kind of degree of metallization, all iron content of reduced iron powder is more than more than 98.5%.The reduced iron powder of external 80 ~ 90% is all that raw material is produced with ultrapure iron concentrate powder, and the primary raw material 95% of China's production iron powder is the low-carbon (LC) iron scale based on steel rolling mill's boiling steel, but fewer and feweri for the iron scale resource of reduced iron powder.Therefore the production of China's reduced iron powder only has Ling Pixin road.
Since domestic 20th century the mid-80s, the initial trial research that high-purity refined iron-mineral powder produces reduced iron powder has been carried out to the fine iron breeze of Shanxi Zuoquan, south, Benxi sweet smell, achieve good achievement, but in iron ore concentrate purification, due to technology imperfection, cause reduced iron powder impurity content high, be difficult to the requirement reaching TFe grade >71.5%, greatly hinder iron powder widening in purposes.
Application number is that the patent of CN201010613426.6 proposes a kind of method adopting ultrapure iron concentrate direct-reduction to produce powder used in metallurgy reduced iron powder.The product of this method has the advantages such as purity is high, phosphorus content is low, briquettability is good, but technique is very high to the purity requirement of raw material ultrapure iron concentrate, and therefore, this technology is very large by raw material restriction, is difficult to extensive universal.
Application number be CN201010501580.4 patent propose technical scheme be acid regeneration iron powder, iron scale and coke powder mix according to a certain ratio compressing after, in sealed crucible, be incubated 8h under 1300 DEG C of conditions, after cooling, obtain sponge iron.This invention adopts acid regeneration iron powder to replace part iron scale to obtain iron sponge powder, and saved cost, but it is low also to there is ferrous metal rate, TFe content is lower than 98.5%, and acid regeneration iron powder does not have the problems such as generality.
In sum, along with the minimizing of steel scale of steel rolling resource, be that raw material is prepared high-quality reduced iron powder and be there is there is lack of raw materials problem with steel scale of steel rolling.Because China's iron ore deposit exists poor, thin, assorted, be difficult to obtain ultrapure iron concentrate, thus cause being that raw material is prepared reduced iron powder to there is raw material grade equally low with ultrapure iron concentrate, be difficult to the problems such as ultrapureization.Therefore, find that a kind of flow process is short, technique is simple, significant to the high-quality iron powder preparation technology that raw material is scalable.
Summary of the invention
The present invention is directed to and existingly prepare the problems such as powder used in metallurgy reduced iron powder cost of material is high, energy consumption is high with iron scale and high-purity refined iron-mineral, there is provided that a kind of raw material sources are extensive, energy consumption is low, process conditions simple powder used in metallurgy reduced iron powder preparation method, the preparation for powder used in metallurgy reduced iron powder provides an effective approach.
The preparation method of powder used in metallurgy reduced iron powder of the present invention is with multiple cheap ferrous material for raw material, obtains a reduced iron powder, then high-temperature oxydation decarburization through direct-reduction, and pickling impurity removal, passivation are dried to powder used in metallurgy reduced iron powder.
The preparation method of a kind of powder used in metallurgy reduced iron powder of the present invention comprises the following steps:
(1) containing metal iron raw material is carried out ore grinding and magnetic separation successively after pulverizing, obtain a removal of impurities iron powder;
(2) the removal of impurities iron powder that step (1) obtains is carried out decarburization roasting in inert atmosphere or weak oxide atmosphere, obtain decarburization product of roasting;
(3) decarbonized iron powder is obtained after the decarburization product of roasting that step (2) obtains being carried out ore grinding and gravity treatment;
(4) decarbonized iron powder that step (3) obtains is carried out pickling impurity removal, obtain pickling iron powder;
(5) pickling iron powder washing step (4) obtained, to neutral, then carried out successively filtering, dry, sieve division and combination is criticized, obtain final iron powder.
Preparation in accordance with the present invention, the described containing metal iron raw material of step (1) is low-grade iron powder, slag or carry out the product after reduction roasting by iron oxide-containing materials.The metal Ferrum content preferably 10 ~ 98wt% of described containing metal iron raw material, phosphorus content is not more than 0.3wt%; Wherein, when metal Ferrum content is between 70 ~ 98wt%, step (1) can be saved directly prepare from step (2), directly in inert atmosphere or weak oxide atmosphere, carry out decarburization roasting by containing metal iron raw material, and the process carrying out step (3)-(5) further successively obtains high-grade iron powder.
According to preparation method of the present invention, the containing oxygen iron raw material meeting above-mentioned condition comprises iron ore concentrate or contains iron oxide waste residue.Such as, iron ore concentrate can be one or more in magnetite concentrate, vanadium titano-magnetite concentrate, hematite concentrate, paigeite concentrate, siderite concentrate and acid regeneration iron ore concentrate etc.; Can be one or more in gas mud, iron and steel flue dust and pyrite cinder etc. containing iron oxide waste residue.
According to preparation method of the present invention, described the reduction roasting that containing oxygen iron raw material carries out in reduction roasting step is comprised gas-based reduction or coal base reduction etc., as long as iron oxide reduction can be become metallic iron, reduction temperature can between 1000 DEG C to 1300 DEG C.The reduction degree of iron is more high better, and reduction degree should be not less than 60%.
According to method of the present invention, the ore grinding described in step (1) and magnetic separation are wet grinding and wet magnetic separation, and magnetic field intensity is preferably 60 ~ 300mT.
According to preparation method of the present invention, the inert atmosphere described in step (2) is nitrogen; Described weak oxide atmosphere is nitrogen, with one or more the mixed mists in carbon dioxide, steam and oxygen three kinds of oxygen-containing gas.Wherein, when using weak oxide atmosphere, shared by nitrogen, volume ratio is not less than 75%.
According to preparation method of the present invention, the decarburization sintering temperature described in step (2) is 850 ~ 1100 DEG C; Decarburization roasting time 0.5 ~ 4h.
According to preparation method of the present invention, the pH of the Acidwash solution of step (4) described pickling between 0.5 ~ 5, without H
2during S gas overflowing, (odorless egg odor) is pickling terminal.
According to preparation method of the present invention, the Acidwash solution that the acid cleaning process described in step (4) adopts comprises one or more in hydrochloric acid, sulfuric acid and salpeter solution.
According to preparation method of the present invention, be filtered into fast filtering described in step (5), described drying is low-temperature vacuum drying.
The present invention proposes a kind of preparation method of powder used in metallurgy reduced iron powder, as compared to the existing technique being raw material with iron scale and high-purity refined iron-mineral, there is obvious superiority:
(1) with traditional handicraft with iron scale with ultrapure iron concentrate for raw material is compared, the present invention is with the material of containing metal iron for raw material, and raw material sources are extensive, cheap.
(2) the present invention adopts wet type ore dressing removal of impurities, reduces the requirement to material reduction degree, and the low reduction apparatus of energy consumption can be adopted to replace traditional high energy consumption tunnel cave.
(3) the present invention selects non-hydrogen reduction decarburization, and pickling impurity removal, the impurity content of product is lower.
(4) must be less than compared with in the of 0.03% with traditional handicraft phosphorus content, the present invention also has certain adaptability to the raw material that phosphorus content exceeds standard.
Detailed description of the invention
Openly in this description to obtain arbitrary feature, unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.Unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.Describedly be only used to help and understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
Raw material is Liaoning boracic magnetite concentrate, its TFe content is 53.01%, P content is 0.04%, iron ore concentrate and 20% coal are mixed, cool after being incubated 5h in Muffle furnace at the temperature of 1000 DEG C, roasted product obtains a removal of impurities iron powder after broken, ore grinding and 300mT magnetic separation; Removal of impurities iron powder roasting 1h under 850 DEG C of nitrogen atmospheres in tube furnace, roasted product obtains decarbonized iron powder after ore grinding and gravity treatment; After decarbonized iron powder washs in the hydrochloric acid solution of pH=5, with clear water quick wash to neutral, after the vacuum drying of cryogenic inert atmosphere, obtain pickling iron powder; Pickling iron powder obtains final iron powder after screening conjunction is criticized, and index is in table 1 and table 2.
Embodiment 2
Raw material Hebei vanadium titano-magnetite concentrate, TFe content is 63.14%, P content is 0.017%, after iron ore concentrate briquetting, imbed and be equipped with in the crucible of coal, reduce with coal gas, cool be incubated 0.5h at the temperature of 1300 DEG C in Muffle furnace after, roasted product obtains a removal of impurities iron powder after broken, ore grinding and 200mT magnetic separation; Removal of impurities iron powder in tube furnace 1100 DEG C, roasting 0.5h under the atmosphere of 98% volume nitrogen and 2% volume oxygen, roasted product obtains decarbonized iron powder after ore grinding and gravity treatment; Decarbonized iron powder is in the hydrochloric acid solution of 0.5 after washing at pH, with clear water quick wash to neutral, obtains pickling iron powder after the vacuum drying of cryogenic inert atmosphere; Pickling iron powder obtains final iron powder after screening conjunction is criticized, and index is in table 1 and table 2.
Embodiment 3
Raw material is sulfate slag, and TFe content is 61.54%, P content is 0.021%; Sulfate slag and 25% coal are mixed, cool after being incubated 1.5h in Muffle furnace at the temperature of 1200 DEG C, roasted product obtains a removal of impurities iron powder after broken, ore grinding and 60mT magnetic separation; Removal of impurities iron powder roasting 3h under 950 DEG C of nitrogen atmospheres in tube furnace, roasted product obtains decarbonized iron powder after ore grinding and gravity treatment; After decarbonized iron powder washs in the salpeter solution of pH=1, with clear water quick wash to neutral, after the drying of cryogenic inert atmosphere, obtain pickling iron powder; Pickling iron powder is obtained after the vacuum drying of cryogenic inert atmosphere; Pickling iron powder obtains final iron powder after screening conjunction is criticized, and index is in table 1 and table 2.
Embodiment 4
Raw material is iron and steel flue dust, TFe content is 28.54%, P content is 0.28%, owing to carrying a large amount of carbon in iron and steel flue dust, so directly iron and steel flue dust is directly heated to 1200 DEG C in tube furnace, after insulation 2h, roasted product obtains a removal of impurities iron powder after fragmentation, ore grinding and 100mT magnetic separation; Removal of impurities iron powder in tube furnace 1150 DEG C, roasting 4h under 80% volume nitrogen and 20% volumes carbon dioxide atmosphere, roasted product obtains decarbonized iron powder after ore grinding and gravity treatment; After decarbonized iron powder washs in the sulfuric acid solution of pH=0.5, with clear water quick wash to neutral, after the vacuum drying of cryogenic inert atmosphere, obtain pickling iron powder; Pickling iron powder obtains final iron powder after screening conjunction is criticized, and index is in table 1 and table 2.
Embodiment 5
Raw material is slag, and TFe content is 18.02%, P content is 0.35%, because the iron part in slag is metallic iron, so obtain a removal of impurities iron powder after directly slag being carried out fragmentation, ore grinding and 200mT magnetic separation; Removal of impurities iron powder roasting 4h under 1000 DEG C of nitrogen atmospheres in tube furnace, roasted product obtains decarbonized iron powder after ore grinding and gravity treatment; After decarbonized iron powder washs in the sulfuric acid solution of pH=3, with clear water quick wash to neutral, after the vacuum drying of cryogenic inert atmosphere, obtain pickling iron powder; Pickling iron powder obtains final iron powder after screening conjunction is criticized, and index is in table 1 and table 2.
Embodiment 6
Raw material is low-grade iron powder, and metal Ferrum content is 81.02%, P content is 0.28%, and iron powder is roasting 4h under 1050 DEG C of nitrogen atmospheres in tube furnace directly, and roasted product obtains decarbonized iron powder after ore grinding and gravity treatment; After decarbonized iron powder washs in the sulfuric acid solution of pH=3, with clear water quick wash to neutral, after the vacuum drying of cryogenic inert atmosphere, obtain pickling iron powder; Pickling iron powder obtains final iron powder after screening conjunction is criticized, and index is in table 1 and table 2.
Table 1 powder used in metallurgy reduced iron powder chemical composition/% (mass fraction)
Table 2 powder used in metallurgy reduced iron powder physical technology performance
Certainly; the present invention can also have various embodiments; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art can openly make various corresponding change and distortion according to of the present invention, but these change accordingly and are out of shape the protection domain that all should belong to claim of the present invention.
Claims (12)
1. a preparation method for powder used in metallurgy reduced iron powder, comprises the following steps:
(1) containing metal iron raw material is carried out ore grinding and magnetic separation successively after pulverizing, obtain a removal of impurities iron powder;
(2) the removal of impurities iron powder that step (1) obtains is carried out decarburization roasting in inert atmosphere or weak oxide atmosphere, obtain decarburization product of roasting;
(3) decarbonized iron powder is obtained after the decarburization product of roasting that step (2) obtains being carried out ore grinding and gravity treatment;
(4) decarbonized iron powder that step (3) obtains is carried out pickling impurity removal, obtain pickling iron powder;
(5) pickling iron powder washing step (4) obtained, to neutral, then carried out successively filtering, dry, sieve division and combination is criticized, obtain final iron powder.
2. preparation method according to claim 1, is characterized in that, the described containing metal iron raw material of step (1) is low-grade iron powder, slag or carry out the product after reduction roasting by iron oxide-containing materials.
3. preparation method according to claim 1, is characterized in that, the metal Ferrum content of described containing metal iron raw material is 10-98wt%, and phosphorus content is not more than 0.3wt%.
4. preparation method according to claim 3, is characterized in that, the content of described containing metal iron feed metal iron is 70 ~ 98wt%, and described containing metal iron raw material, without step (1), is directly prepared from step (2).
5. preparation method according to claim 2, is characterized in that, described iron oxide-containing materials mainly comprises iron ore concentrate or contains iron oxide waste residue.
6. preparation method according to claim 2, is characterized in that, described reduction roasting comprises gas-based reduction or coal base reduction, and reduction temperature is between 1000 ~ 1300 DEG C.
7. preparation method according to claim 1, is characterized in that, the ore grinding described in step (1) and magnetic separation are wet grinding and wet magnetic separation, and wherein, the magnetic field intensity of described wet magnetic separation is 60 ~ 300mT.
8., according to the arbitrary described preparation method of claim 1-4, it is characterized in that, the inert atmosphere described in step (2) is nitrogen; Described weak oxide atmosphere is one or more the mixed mists in nitrogen and carbon dioxide, steam and oxygen three kinds of oxygen-containing gas.
9., according to the arbitrary described preparation method of claim 1-4, it is characterized in that, the decarburization sintering temperature described in step (2) is 850 ~ 1100 DEG C, decarburization roasting time 0.5 ~ 4h.
10., according to the arbitrary described preparation method of claim 1-4, it is characterized in that, the pH of the Acidwash solution of step (4) described pickling between 0.5 ~ 5, without H
2it is pickling terminal during S gas overflowing.
11. preparation methods according to claim 10, is characterized in that, the Acidwash solution that the acid cleaning process described in step (4) adopts comprises one or more in hydrochloric acid, sulfuric acid and salpeter solution.
12., according to the arbitrary described preparation method of claim 1-4, is characterized in that, described in step (5) be filtered into fast filtering, described drying is low-temperature vacuum drying.
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| CN106854407A (en) * | 2017-01-09 | 2017-06-16 | 娄底市湖泉亿达工贸有限公司 | A kind of method of comprehensive utilization of converter slag |
| CN110170646A (en) * | 2019-07-01 | 2019-08-27 | 重庆有研重冶新材料有限公司 | Superfine iron powder and its production method |
| US20220041449A1 (en) * | 2018-12-21 | 2022-02-10 | Höganäs Ab (Publ) | Pure iron containing compound |
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