CN100410170C - Method for preparing iron carbide using iron ore concentrate powder - Google Patents
Method for preparing iron carbide using iron ore concentrate powder Download PDFInfo
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- CN100410170C CN100410170C CNB2005101205955A CN200510120595A CN100410170C CN 100410170 C CN100410170 C CN 100410170C CN B2005101205955 A CNB2005101205955 A CN B2005101205955A CN 200510120595 A CN200510120595 A CN 200510120595A CN 100410170 C CN100410170 C CN 100410170C
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- iron
- mixed gas
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- iron carbide
- iron ore
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Abstract
The present invention belongs to a method for preparing Fe3C, particularly to a method for preparing Fe3C by using iron ore concentrate powder. The present invention has the technical scheme that vanadium containing oxide which is used as an additive is added into the iron ore concentrate powder, and the addition quantity of the vanadium containing oxide accounts for 1 to 5% of the weight of the iron ore concentrate powder; a proper quantity of water is added to manufacture pellets after the vanadium containing oxide and the iron ore concentrate powder are evenly mixed, and then, the pellets are dried; then, the dried pellets are put into a furnace with the temperature of 800 to 900DEG C, sintered for 10 to 20 minutes, taken out and cooled to reach the room temperature; finally, the dried pellets react with a mixed gas under the condition of the temperature of 700 to 800DEG C, the reaction time is of 30 to 50 minutes when the mixed gas is CH4-H2, and the reaction time is of 90 to 180 minutes when the mixed gas is CO-H2 or H2-CO-CO2; the pellets are rapidly cooled to reach the room temperature by an inert gas after the reaction. The present invention has the characteristics of high reaction speed, high conversion rate, high stability, and no sulfur containing impurity increase.
Description
One, technical field
The invention belongs to iron carbide (Fe
3C) preparation method relates in particular to a kind of method for preparing iron carbide with fine iron breeze.
Two, technical background
Iron carbide with its distinctive physical properties, chemical property and working condition, is subjected to extensive concern as a kind of direct-reduced iron product that occur the seventies: 1, receive metallurgist's concern with its outstanding advantage, and can be as the surrogate of steel scrap; 2, as steelmaking feed, compare with the blast furnace production technique of iron, the production temperature of iron carbide is lower, and the byproduct of its production process mainly is a water, the main products iron carbide is solid-state, stable, is easy to transportation and storage, therefore, the Production Flow Chart of iron carbide is as the alternative flow process of the technical process of traditional blast furnace ironmaking, in energy consumption, environmental protection with very big advantage is arranged economically; 3, the electromagnetic performance of iron carbide uniqueness can be used as information material and electromagnetic shielding material; 4, iron carbide can be used as hydrogen storage material.
For above-mentioned reasons, people are devoted to the research of iron carbide preparation always.The main preparation principle of iron carbide is under certain conditions, with containing the reducing gas of carburizing gas (as H
2-CH
4) react with iron ore, make iron carbide.
1, utilizes CH
4-H
2It is mixed gas production iron carbide.Studies show that in 650 ~ 950 ℃ temperature range, optimum operation condition is: CH
4: H
2Ratio be 40: 60,750 ℃ of temperature, most with this understanding iron ores all were transformed into iron carbide (Fe in 45 minutes
3C) [middle river is big, and mountain, village force is clear, little wild sun one, ほ か. synthetic To of セ メ Application ィ ト and Pot The iron Mining stone proterties shadow Ring. material と プ ロ セ ス, 1994,7:85], [middle river is big, and mountain, village force is clear, little wild sun one, ほ か. synthetic To of セ メ Application ィ ト and Pot The ガ ス form と temperature shadow Ring. material と プ ロ セ ス, 1995,8:109], [middle river is big, mountain, village force is clear, the positive .CH in little open country
4-H
2Mixing ガ ス To ょ Ru ァ ィ ァ Application カ one バ ィ De System makes. iron と Steel, 1996,82 (4): 261]; Another research then shows [Ni Hongwei, grey big strong, Jiang Junpu. temperature of reaction, atmosphere are to the influence of iron carbide preparation process. steel research .1999, No.6:22-25]: powdered iron ore and H2-CH4 mixed gas reaction, when temperature is 700 ℃, the gas percentage composition is 50～80%H
2+ 20～50%CH
4The time, iron carbide early generates, and can keep conversion rate faster in early stage, but in the later stage of reaction, iron carbide transforms slower, and the decomposition reaction of iron carbide easily takes place; When temperature is 500 ℃, 600 ℃, the mixed gas percentage composition is 30～50%H
2+ 50～70%CH
4The time, can obtain higher iron carbide transformation efficiency, later but iron carbide begins to transform, and transform slowly.
2, utilize CO-H
2The mixed gas reducing iron ore.Studies show that [horse is strong for Wang Guanghui, Jiang Maofa. about the research of iron carbide. and steel-making .1997, Vol (12): 22-23]: CO-H
2Be that gas is difficult to directly obtain iron carbide from reduction of iron ore, add an amount of sulfurous gas (as H
2S) after, though can make iron carbide in 550～950 ℃ of scopes, the transformation efficiency of iron carbide is low, and brings sulfur impurity in the product into.
3, utilize the H2-CO-CO2 mixed gas to prepare iron carbide.In the time of 550～700 ℃, H
2-CO-CO
2Gas mixture can from iron ore, make iron carbide [Wang Guanghui, Jiang Maofa. utilize the experimental study of COREX tail gas reducing iron ore production iron carbide. iron and steel .1998, Vol.33, No.1:18-21], at 700 ℃, reducing gas composition 20%H
2+ 60%CO+20%CO
2Reaction is 4 hours under the condition, and the iron carbide transformation efficiency reaches as high as 94.02%.According to said method, though obtained comparatively ideal iron carbide transformation efficiency, transform too slow.
Although can obtain the transformation efficiency of higher iron carbide in laboratory scale, the slow and not high pressing issues that still need solve of productive rate of the conversion rate of iron carbide.CIRCOFER by the exploitation of German LURGI) technology (also iron carbide technology), fine iron breeze is participated in reaction at circulating fluidized bed earlier after preheating, and the products obtained therefrom degree of metalization can reach 80%, and through the subordinate phase reaction, degree of metalization can reach more than 93% again.This technology is produced equipment of direct reduction factory's operation under Trinidad and Tobago U.S. knob Ke (NUCOR) company in 1994 of 500,000 tons per year, but it is a lot of because of going wrong in the production process, it is stable that production can't reach, stopped industrialness production [metal Leader, the world, November 23 calendar year 2001: world's direct-reduced iron production new technology summary] in 1999.Nineteen ninety-five Grabke Hans Jurgen etc. find the stable influential [Grabke of sulphur to iron carbide, Hans Jurgen et al.:Effect of sulfur on the stability of cementite, SteelResearch, 66 (1995): 254].Thereafter, the clear second-class discovery H of the woods of Nagoya Institute of Technology
2-CH
4Add micro-H in the mixed gas
2S can suppress separating out of uncombined carbon, improves productive rate [the Hayashi etal.:Iron Carbide Synthesis by Reaction of Iron Ore with H of iron carbide
2-CH
4Gas MixturesContaining Traces of Sulfur, ISIJ Int., 37 (1997) 16,345], but sulphur do can make poisoning of catalyst in the reducing gas technological process at the reformation Sweet natural gas, also can bring sulfur impurity into to product, its application is restricted.
Three, summary of the invention
The purpose of this invention is to provide that a kind of speed of response is fast, transformation efficiency is high, good stability, do not increase sulfur-containing impurities prepare the method for iron carbide with fine iron breeze
For achieving the above object, the technical solution adopted in the present invention is, will contain barium oxide and add in the fine iron breeze as additive, contains barium oxide or is V
2O
5, or be V
2O
3, or be V
2O
5, V
2O
3Mixture, its add-on is 1%～5% of a fine iron breeze weight; Join suitable quantity of water behind the mixing and make pelletizing,, then the pelletizing of oven dry is put into temperature and be 800～900 ℃ stove sintering 10～20 minutes, take out and be cooled to room temperature again with pelletizing oven dry; At last temperature be under 700～800 ℃ of conditions with mixed gas reaction, mixed gas is CH
4-H
2Shi Fanying 30～50 minutes, mixed gas are CO-H
2Or H
2-CO-CO
2Shi Fanying 90～180 minutes, the reaction back is quickly cooled to room temperature with rare gas element.
Described V
2O
5, V
2O
3Mixture any for both than mixing.
The weight percentage of described fine iron breeze is: all iron content is not less than 64%, and sulphur content is less than 0.04%, TiO
2Be less than 0.5%; The granularity of fine iron breeze is below 80 orders.
Described mixed gas or be CH
4-H
2, or be CO-H
2, or be H
2-CO-CO
2Mixed gas CH
4-H
2Volumn concentration be 60～80%H
2+ 20～40%CH
4, mixed gas CO-H
2Volumn concentration be 60～85%CO+15～40%H
2, mixed gas H
2-CO-CO
2Volumn concentration be 10～30%H
2+ 50～70%CO+10～20%CO
2
Owing to adopt above-mentioned technology, the present invention has that speed of response is fast, transformation efficiency is high, good stability, do not increase the sulfur-containing impurities characteristics.
Four, description of drawings
Fig. 1 is the present invention and non-additive contrast synoptic diagram;
Fig. 1 is with TiO
2Be additive and non-additive contrast synoptic diagram.
Five, embodiment
1 one kinds of embodiment prepare the method for iron carbide with fine iron breeze, and it is as shown in the table for its fine ore chemical ingredients.Granularity is the following fine iron breezes of 80 orders, allocates industrial V into by 2%～4% of fine iron breeze weight
2O
5Be additive, both are mixed; Add and dry an amount of water is made the pelletizing of diameter 8mm～10mm with pelletizer after.Again pelletizing is put into 800～900 ℃ High Temperature Furnaces Heating Apparatus sintering and take out after 10～15 minutes and be cooled to room temperature, pelletizing preparation is so far finished.
The iron ore concentrate chemical ingredients
| Form | T.Fe | FeO | SiO 2 | CaO | MgO | S |
| Weight % | 67.05 | 0.81 | 1.89 | 0.89 | 0.11 | 0.033 |
Iron carbide preparation method: after the temperature of reaction vessel was raised to 700～800 ℃, logical nitrogen was driven the air in the container in reaction vessel, and pelletizing is inserted in the reaction vessel, treat temperature-stable after, feed reactant gases (70%H
2+ 30%CH
4), react after 30～35 minutes, change logical nitrogen and be quickly cooled to room temperature.
Products obtained therefrom is solemn Regensburg ear spectrum analysis, Fe in the product
3The turnover ratio of C is 96.0%.
Embodiment 2
The powdered iron ore raw material is identical with embodiment 1 with preparation process, and additive is that weight percentage is 60%V
2O
5+ 40%V
2O
3Mixture, addition is 2.0%～4.5% of a powdered iron ore weight.Reactant gases is H
2-CO-CO
2, its volumn concentration is 10～30%H
2+ 50～70%CO+10～20%CO
2After being 120～150 minutes with the pelletizing reaction times, feeding nitrogen and be quickly cooled to room temperature.
Products obtained therefrom is solemn Regensburg ear spectrum analysis, the Fe in the product
3The C turnover ratio is 95.0%.
Embodiment 3
Present embodiment is a reference examples.
The powdered iron ore raw material is identical with embodiment 1 with preparation process, adds V respectively
2O
5, TiO
2, another does not add any additives.V
2O
5, TiO
2Add-on respectively be 1～2% of powdered iron ore weight.The result as shown in Figure 1 and Figure 2.The rate of weight loss ascent stage is the reduction of iron ore among the figure, as seen uses additive V from Fig. 1, Fig. 2
2O
5Or TiO
2With not doping this elementary reaction speed all there is not obvious influence.Product began weightening finish after weightlessness reached maximum value among Fig. 1, Fig. 2, and this stage is the carbonation stage of iron.Learn with not adding any additives from Fig. 1 and to compare, add 1% V
2O
5Back carbonization speed can improve greatly, and Dui Zhao Fig. 2 adds 2% TiO with it
2The carbonization speed of iron is descended.In the identical reaction times (30 minutes), add 1% V
2O
5, additive-free, add 2% TiO
2Iron carbide transformation efficiency in the product is respectively 96%, 84.8%, 73.2%.Only add 1% V
2O
5The transformation efficiency of iron carbide is improved more than 10%, and speed of reaction also is improved.
Claims (4)
1. one kind prepares the method for iron carbide with fine iron breeze, it is characterized in that containing barium oxide and adds in the fine iron breeze as additive, contains barium oxide or is V
2O
5, or be V
2O
3, or be V
2O
5, V
2O
3Mixture, its add-on is 1%～5% of a fine iron breeze weight; Join suitable quantity of water behind the mixing and make pelletizing,, then the pelletizing of oven dry is put into temperature and be 800～900 ℃ stove sintering 10～20 minutes, take out and be cooled to room temperature again with pelletizing oven dry; At last temperature be under 700～800 ℃ of conditions with mixed gas reaction, mixed gas is CH
4-H
2Shi Fanying 30～50 minutes, mixed gas are CO-H
2Or H
2-CO-CO
2Shi Fanying 90～180 minutes, the reaction back is quickly cooled to room temperature with rare gas element.
2. according to claim 1ly prepare the method for iron carbide, it is characterized in that described V with fine iron breeze
2O
5, V
2O
3Mixture any for both than mixing.
3. according to claim 1ly prepare the method for iron carbide with fine iron breeze, it is characterized in that the weight percentage of described fine iron breeze is: all iron content is not less than 64%, and sulphur content is less than 0.04%, TiO
2Be less than 0.5%; The granularity of fine iron breeze is below 80 orders.
4. according to claim 1ly prepare the method for iron carbide, it is characterized in that described mixed gas or be CH with fine iron breeze
4-H
2, or be CO-H
2, or be H
2-CO-CO
2Mixed gas CH
4-H
2Volumn concentration be 60～80%H
2+ 20～40%CH
4, mixed gas CO-H
2Volumn concentration be 60～85%CO+15～40%H
2, mixed gas H
2-CO-CO
2Volumn concentration be 10～30%H
2+ 50～70%CO+10～20%CO
2
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| CN100410170C true CN100410170C (en) | 2008-08-13 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010261101A (en) * | 2009-04-07 | 2010-11-18 | Mitsutaka Hino | Method for producing metallic iron |
| CN107082428B (en) * | 2017-04-28 | 2019-03-26 | 苏州大学 | A method of cementite is prepared using more metal sulfate slags |
| CN107082429A (en) * | 2017-04-28 | 2017-08-22 | 苏州大学 | A kind of method that utilization Dust of Iron And Steel Works prepares cementite |
| CN107058720B (en) * | 2017-04-28 | 2018-12-14 | 苏州大学 | A method of cementite is prepared using low-grade complex iron ore |
| CN108677022A (en) * | 2018-06-19 | 2018-10-19 | 苏州大学 | A kind of method that sintering dust separation ash prepares removing harmful element during cementite |
| CN109652604A (en) * | 2019-01-30 | 2019-04-19 | 上海大学 | A method of cementite is prepared using ferriferous oxide two-step method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1640110A1 (en) * | 1987-03-25 | 1991-04-07 | Украинский научно-исследовательский институт специальных сталей, сплавов и ферросплавов | Method of separation of titanium carbides from complex alloyed carbide steels |
| US5234674A (en) * | 1991-06-27 | 1993-08-10 | Teledyne Industries, Inc. | Process for the preparation of metal carbides |
| CN1083024A (en) * | 1992-07-20 | 1994-03-02 | 中国科学院合肥智能机械研究所 | A kind of carbon steel preparation of nanomaterials |
| CN1249004A (en) * | 1997-02-28 | 2000-03-29 | 川崎重工业株式会社 | Production method of iron carbide |
| JP2002274829A (en) * | 2001-03-21 | 2002-09-25 | Daido Steel Co Ltd | Cementite or cementite-based compound and method of producing the same |
-
2005
- 2005-12-31 CN CNB2005101205955A patent/CN100410170C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1640110A1 (en) * | 1987-03-25 | 1991-04-07 | Украинский научно-исследовательский институт специальных сталей, сплавов и ферросплавов | Method of separation of titanium carbides from complex alloyed carbide steels |
| US5234674A (en) * | 1991-06-27 | 1993-08-10 | Teledyne Industries, Inc. | Process for the preparation of metal carbides |
| CN1083024A (en) * | 1992-07-20 | 1994-03-02 | 中国科学院合肥智能机械研究所 | A kind of carbon steel preparation of nanomaterials |
| CN1249004A (en) * | 1997-02-28 | 2000-03-29 | 川崎重工业株式会社 | Production method of iron carbide |
| JP2002274829A (en) * | 2001-03-21 | 2002-09-25 | Daido Steel Co Ltd | Cementite or cementite-based compound and method of producing the same |
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| CN1807237A (en) | 2006-07-26 |
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