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CN103014216A - Reduction method of iron compound in iron-containing material - Google Patents

Reduction method of iron compound in iron-containing material Download PDF

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Publication number
CN103014216A
CN103014216A CN2013100055974A CN201310005597A CN103014216A CN 103014216 A CN103014216 A CN 103014216A CN 2013100055974 A CN2013100055974 A CN 2013100055974A CN 201310005597 A CN201310005597 A CN 201310005597A CN 103014216 A CN103014216 A CN 103014216A
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iron
solution
slurries
ferrous material
tfe
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CN103014216B (en
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李小斌
刘楠
余顺文
彭志宏
刘桂华
周秋生
齐天贵
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Central South University
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Abstract

The invention discloses a reduction method of iron compound in an iron-containing material. Under the alkali hydrothermal condition, high-valence iron in the iron-containing material is reduced by using a reducing agent for facilitating the comprehensive utilization of iron in the iron-containing polymetallic ore or metallurgical waste residue. The reduction method has the advantages of extensive applicability, cheap and available reducing agent and the like, and is easily combined with the metallurgical process.

Description

The method of reducing of iron cpd in a kind of ferrous material
Technical field
The present invention relates to the method for reducing of iron cpd in a kind of ferrous material, belong to metallurgical technology field.
Background technology
In iron content polymetallic ore or metallurgical slag comprehensive utilization process, need will be wherein the non-magnetic iron things such as rhombohedral iron ore, pyrrhosiderite be reduced to magnetite or metallic iron so that the separation and concentration of iron wherein.Therefore, the reduction of iron mineral has important effect aspect the comprehensive utilization of ferrous material.
In the main employing of metallurgical technology field iron mineral reduction pyrogenic process process, and there are the problems such as process more complicated, energy consumption height in the pyrogenic process process to the comprehensive utilization of iron in the ferrous material.Although the wet reducing process easily combines with metallurgical process, flow process is simple, energy consumption is low, has no the research report of this aspect.
And can be in field of material preparation, the relevant report of reduced iron compound in the hydrothermal system to be arranged for what use for reference.Chinese patent CN 101885512A has proposed a kind of in 120～180 ℃ hydrothermal system, adopts reduced iron powder with colloid Fe (OH) 3Reduction is to prepare the method for superfine Fe 3 O 4 particle; Chinese patent CN101323466A proposed a kind of in Organic Alcohol solution with the mixture of iron trichloride and sodium hydroxide through hydrothermal treatment consists to prepare the method for nano ferriferrous oxide.(Journal of CrystalGrowth, 2005) such as Ni Xiaoming have proposed a kind of under the alkaline water heat condition, adopt hydrazine hydrate with Fe (OH) 3, Fe 2O 3Be reduced to nanometer Fe or Fe 3O 4Method; Glavee etc. have proposed a kind of borohydride reduction molysite compound that utilizes to prepare the method for nanometer metallic iron under hydrothermal condition.But hydrazine hydrate in the aforesaid method, hydroborate cost are high, and its process to as if pure iron cpd, need specially preparation.Therefore, in processing iron content polymetallic ore or metallurgical slag comprehensive utilization iron process, aforesaid method is difficult to direct application.
Summary of the invention
The method of reducing that the purpose of this invention is to provide iron cpd in a kind of ferrous material, the economic comprehensive utilization that realizes iron in iron content polymetallic ore or the metallurgical slag.
In order to achieve the above object, the inventive method comprises the steps:
1) ferrous material, reductive agent are joined in the alkaline solution, be mixed with slurries, wherein alkaline solution is sodium hydroxide solution, sodium carbonate solution or sodium aluminate solution, and alkali concn is with Na 2O counts 10～300g/L, the amount of allocating into of ferrous material is counted 50～500g/L by the volume of alkaline solution, reductive agent is one or more the mixture in alcohols, carbohydrate, aldehydes, alkanes, activated carbon, graphite, coal, coal tar, the wheat bran, and the reductive agent consumption is counted 0.2～200g/L by the volume of alkaline solution;
2) prepared slurries are at 90～350 ℃ of lower hydrothermal treatment consists 20～600min.
Preferably, in the aforesaid method, reductive agent is one or more the mixture in methyl alcohol, glycerol, glucose, starch, formaldehyde, kerosene, coal, coal tar, the wheat bran.
The present invention has following advantage: 1) suitability is wide, not only can be used for the conversion of iron mineral in the ferrous material, and can be used for the preparation of iron content functional materials; 2) reductive agent is cheap and easy to get; 3) easily combine with metallurgical process, simple.
Description of drawings
The XRD figure of used ferric oxide spectrum among Fig. 1 embodiment 12;
The XRD figure of hydrothermal treatment consists slag spectrum among Fig. 2 embodiment 12.
Embodiment
The following examples are in order more clearly to describe characteristics of the present invention, choose bauxite in the aluminum oxide production process and red mud as exemplary ferrous material, but this do not consist of any restriction to applicable object of the present invention.
Embodiment 1
With diaspore type bauxite (main component: Al 2O 356.63%, SiO 29.85%, Fe 2O 318.56%, TiO 22.36%), lime, sodium aluminate solution (100mL) and formaldehyde are mixed with raw pulp.Wherein, sodium aluminate solution consists of: Na 2O k220.34g/L, Al 2O 3120.58g/L; Press the sodium aluminate solution volumeter, ore proportioning quantity is that 255g/L, formaldehyde addition are 5g/L; The liming amount is 7% of dry ore weight.Prepared raw pulp is at 260 ℃ of lower stripping 60min, and gained stripping slurries obtain dissolution fluid and stripping slag through solid-liquid separation.The stripping slag is to carry out magnetic separation under the 120kA/m in field intensity, and full iron (TFe) quality percentage composition and the iron recovery of gained iron ore concentrate are respectively 56.30% and 48.74%; And do not add formaldehyde, when other condition is identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 30.52% and 17.37%.
Embodiment 2
With high ferro trihydrate aluminium stone ore (Fe 2O 342%, Al 2O 330%), sodium aluminate solution (100mL) and methanol mixed are mixed with raw pulp.Wherein, sodium aluminate solution consists of: Na 2O k160.23g/L, Al 2O 382.72g/L; Press the sodium aluminate solution volumeter, ore proportioning quantity is that 200g/L, methyl alcohol addition are 5g/L; Prepared raw pulp is at 90 ℃ of lower stripping 120min, and gained stripping slurries obtain dissolution fluid and stripping slag through solid-liquid separation.The stripping slag is to carry out magnetic separation under the 120kA/m in field intensity, and full iron (TFe) quality percentage composition and the iron recovery of gained iron ore concentrate are respectively 55.12% and 35.32%; And do not add methyl alcohol, when other condition is identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 41.50% and 7.67%.
Embodiment 3
With red mud (Fe 2O 354%, Al 2O 314%), glycerol, sodium hydroxide solution (100mL) are hybridly prepared into slurries.Wherein concentration of sodium hydroxide solution is that 10g/L is (with Na 2The O meter, lower same); Press the sodium hydroxide solution volumeter, the red mud dosage is that 50g/L, glycerol addition are 0.2g/L.The slurries of preparing are processed 20min under 350 ℃ hydrothermal condition.Slag after the above-mentioned hydrothermal treatment consists carries out magnetic separation in field intensity is the magnetic separation tube of 120kA/m, full iron (TFe) the quality percentage composition of gained magnetic concentrate is 58.42%, the rate of recovery of iron is 55.31%.And do not add glycerol, when other treatment condition are identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 42.50% and 16.87%.
Embodiment 4
With red mud (Fe 2O 354%, Al 2O 314%), glucose, sodium carbonate solution (100mL) are hybridly prepared into slurries.Wherein sodium carbonate solution concentration is that 50g/L is (with Na 2The O meter, lower same); Press the sodium carbonate solution volumeter, the red mud dosage is that 300g/L, glucose addition are 5g/L.The slurries of preparing are processed 600min under 280 ℃ hydrothermal condition.Slag after the above-mentioned hydrothermal treatment consists carries out magnetic separation in field intensity is the magnetic separation tube of 120kA/m, full iron (TFe) the quality percentage composition of gained magnetic concentrate is 62.42%, the rate of recovery of iron is 75.68%.And do not add glucose, when other treatment condition are identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 41.35% and 18.87%.
Embodiment 5
With red mud (Fe 2O 354%, Al 2O 314%), starch, onium hydroxide solution (100mL) are hybridly prepared into slurries.Wherein concentration of sodium hydroxide solution is that 150g/L is (with Na 2The O meter, lower same); Press the sodium hydroxide solution volumeter, the red mud dosage is that 500g/L, starch addition are 10g/L.The slurries of preparing are processed 180min under 260 ℃ hydrothermal condition.Slag after the above-mentioned hydrothermal treatment consists carries out magnetic separation in field intensity is the magnetic separation tube of 120kA/m, full iron (TFe) the quality percentage composition of gained magnetic concentrate is 60.42%, the rate of recovery of iron is 70.24%.And do not add starch, when other treatment condition are identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 42.4% and 15.87%.
Embodiment 6
With red mud (Fe 2O 354%, Al 2O 314%), coal dust, onium hydroxide solution (100mL) are hybridly prepared into slurries.Wherein concentration of sodium hydroxide solution is that 300g/L is (with Na 2The O meter, lower same); Press the sodium hydroxide solution volumeter, the red mud dosage is that 300g/L, coal dust addition are 200g/L.The slurries of preparing are processed 180min under 350 ℃ hydrothermal condition.Slag after the above-mentioned hydrothermal treatment consists carries out magnetic separation in field intensity is the magnetic separation tube of 120kA/m, full iron (TFe) the quality percentage composition of gained magnetic concentrate is 57.32%, the rate of recovery of iron is 55.02%.And do not add coal dust, when other treatment condition are identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 43.65% and 20.87%.
Embodiment 7
With red mud (Fe 2O 354%, Al 2O 314%), wheat bran, onium hydroxide solution (100mL) are hybridly prepared into slurries.Wherein concentration of sodium hydroxide solution is that 50g/L is (with Na 2The O meter, lower same); Press the sodium hydroxide solution volumeter, the red mud dosage is that 300g/L, wheat bran addition are 50g/L.The slurries of preparing are processed 180min under 200 ℃ hydrothermal condition.Slag after the above-mentioned hydrothermal treatment consists carries out magnetic separation in field intensity is the magnetic separation tube of 120kA/m, full iron (TFe) the quality percentage composition of gained magnetic concentrate is 56.32%, the rate of recovery of iron is 53.12%.And do not add wheat bran, when other treatment condition are identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 40.25% and 15.62%.
Embodiment 8
With high ferro trihydrate aluminium stone ore (Fe 2O 342%, Al 2O 330%), sodium aluminate solution (100mL) and kerosene are hybridly prepared into raw pulp.Wherein, sodium aluminate solution consists of: Na 2O k160.23g/L, Al 2O 382.72g/L; Press the sodium aluminate solution volumeter, ore proportioning quantity is that 280g/L, kerosene addition are 5g/L; Prepared raw pulp is at 145 ℃ of lower stripping 90min.Above-mentioned stripping slag is to carry out magnetic separation under the 120kA/m condition in field intensity, and full iron (TFe) quality percentage composition and the iron recovery of gained iron ore concentrate are respectively 57.42% and 45.32%; And do not add kerosene, when other condition is identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 41.92% and 10.82%.
Embodiment 9
With diaspore type bauxite (main component: Al 2O 356.63%, SiO 29.85%, Fe 2O 318.56%, TiO 22.36%), lime, sodium aluminate solution (100mL) and coal tar are mixed with raw pulp.Sodium aluminate solution consists of: Na 2O k220.34g/L, Al 2O 3120.58g/L; Press the sodium aluminate solution volumeter, ore proportioning quantity is that 255g/L, coal tar addition are 30g/L; The liming amount is 7% of dry ore weight.Prepared raw pulp is at 260 ℃ of lower stripping 120min.Above-mentioned stripping slag is to carry out magnetic separation under the 120kA/m in field intensity, and full iron (TFe) quality percentage composition and the iron recovery of gained iron ore concentrate are respectively 58.35% and 54.39%; And do not add coal tar, when other condition is identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 31.02% and 17.57%.
Embodiment 10
With diaspore type bauxite (main component: Al 2O 356.63%, SiO 29.85%, Fe 2O 318.56%, TiO 22.36%), lime, sodium aluminate solution (100mL), methyl alcohol, starch are mixed with raw pulp.Wherein, sodium aluminate solution consists of: Na 2O k220.34g/L, Al 2O 3120.58g/L; Press the sodium aluminate solution volumeter, ore proportioning quantity is that 255g/L, methyl alcohol addition are that 0.5g/L, starch addition are 2g/L; The liming amount is 7% of dry ore weight.Prepared raw pulp is at 260 ℃ of lower stripping 120min.Above-mentioned stripping slag is to carry out magnetic separation under the 120kA/m in field intensity, and full iron (TFe) quality percentage composition and the iron recovery of gained iron ore concentrate are respectively 55.75% and 50.87%; And the contrast and experiment of not adding methyl alcohol and starch reductive agent is with embodiment 9.
Embodiment 11
With red mud (Fe 2O 354%, Al 2O 314%), formaldehyde, starch, coal tar, onium hydroxide solution (100mL) are hybridly prepared into slurries.Wherein, concentration of sodium hydroxide solution is that 100g/L is (with Na 2The O meter, lower same); Press the sodium hydroxide solution volumeter, the red mud dosage is that 300g/L, formaldehyde addition are that 0.2g/L, starch addition are that 2g/L, coal tar addition are 2g/L.The slurries of preparing are processed 300min under 240 ℃ hydrothermal condition.Slag after the above-mentioned hydrothermal treatment consists carries out magnetic separation in field intensity is the magnetic separation tube of 120kA/m, full iron (TFe) the quality percentage composition of gained magnetic concentrate is 57.42%, the rate of recovery of iron is 62.25%.And do not add formaldehyde, coal tar and starch reductive agent, when other treatment condition are identical, full iron (TFe) quality percentage composition and the iron recovery of magnetic concentrate are respectively 41.25% and 16.32%.
Embodiment 12
With analytical pure Fe 2O 3, sodium hydroxide solution, formaldehyde and glucose is hybridly prepared into slurries.Wherein, concentration of sodium hydroxide solution is that 150g/L is (with Na 2The O meter); Press the sodium hydroxide solution volumeter, analytical pure Fe 2O 3Dosage is that 200g/L, formaldehyde addition are that 0.5g/L, glucose dosage are 5g/L.The slurries of preparing are processed 180min under 280 ℃ hydrothermal condition.The X-ray diffracting spectrum (XRD) of material respectively as depicted in figs. 1 and 2 before and after the hydrothermal treatment consists.Fe among diffraction peak and the Jade5.0 among Fig. 1 2O 3Standard diagram (PDF24-0072#) conform to diffraction peak and Fe among Fig. 2 3O 4Standard diagram (PDF 07-0322#) conform to, illustrate that in the hydrothermal treatment consists process of above-mentioned interpolation reductive agent, reduzate is Z 250.

Claims (2)

1. the method for reducing of iron cpd in the ferrous material is characterized in that, may further comprise the steps:
1) ferrous material, reductive agent are joined in the alkaline solution, be mixed with slurries, wherein alkaline solution is sodium hydroxide solution, sodium carbonate solution or sodium aluminate solution, and alkali concn is with Na 2O counts 10～300g/L, the amount of allocating into of ferrous material is counted 50～500g/L by the volume of alkaline solution, reductive agent is one or more the mixture in alcohols, carbohydrate, aldehydes, alkanes, activated carbon, graphite, coal, coal tar, the wheat bran, and the reductive agent consumption is counted 0.2～200g/L by the volume of alkaline solution;
2) prepared slurries are at 90～350 ℃ of lower hydrothermal treatment consists 20～600min.
2. the method for reducing of iron cpd in according to claim 1 a kind of ferrous material is characterized in that, described additive is one or more the mixture in methyl alcohol, glycerol, glucose, starch, formaldehyde, kerosene, coal, coal tar, the wheat bran.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103521205A (en) * 2013-10-10 2014-01-22 上海大学 Method of preparing core-shell structure TiO2 material with high photocatalytic activity
CN103755005A (en) * 2014-01-02 2014-04-30 上海大学 Ferric ion reduction method
CN104327885A (en) * 2014-10-10 2015-02-04 昆明理工大学 Hogwash oil mixed oil fuel reducing agent applied to metallurgy pyrometallurgical process
CN105238924A (en) * 2015-10-23 2016-01-13 辽宁科技大学 Method for extracting aluminum and iron from high-iron diasporic bauxite
CN105710383A (en) * 2016-04-30 2016-06-29 安徽农业大学 Method for preparing Cu powder by reducing CuO by adopting glycerinum
CN105801077A (en) * 2016-02-17 2016-07-27 中国科学院地球化学研究所 Preparation method of red mud/carbon-based magnetic composite material
CN106319226A (en) * 2016-08-22 2017-01-11 中国铝业股份有限公司 Method for comprehensively recycling aluminium oxide, sodium oxide and ferric oxide from red mud

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US4154608A (en) * 1978-07-19 1979-05-15 Uop Inc. Production of high purity iron powder
US5055136A (en) * 1988-06-24 1991-10-08 Bayer Aktiengesellschaft Heat-stable iron oxide black pigments, processes for their production and their use
CN101070193A (en) * 2007-06-19 2007-11-14 南开大学 Method for preparing magnetite Fe3O4 nano particles material
CN101914650A (en) * 2010-06-29 2010-12-15 同济大学 Method for reducing oxidation state iron into simple substance iron by using glycerol

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4154608A (en) * 1978-07-19 1979-05-15 Uop Inc. Production of high purity iron powder
US5055136A (en) * 1988-06-24 1991-10-08 Bayer Aktiengesellschaft Heat-stable iron oxide black pigments, processes for their production and their use
CN101070193A (en) * 2007-06-19 2007-11-14 南开大学 Method for preparing magnetite Fe3O4 nano particles material
CN101914650A (en) * 2010-06-29 2010-12-15 同济大学 Method for reducing oxidation state iron into simple substance iron by using glycerol

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103521205A (en) * 2013-10-10 2014-01-22 上海大学 Method of preparing core-shell structure TiO2 material with high photocatalytic activity
CN103755005A (en) * 2014-01-02 2014-04-30 上海大学 Ferric ion reduction method
CN103755005B (en) * 2014-01-02 2016-12-07 上海大学 Ferric ion reduction method
CN104327885A (en) * 2014-10-10 2015-02-04 昆明理工大学 Hogwash oil mixed oil fuel reducing agent applied to metallurgy pyrometallurgical process
CN105238924A (en) * 2015-10-23 2016-01-13 辽宁科技大学 Method for extracting aluminum and iron from high-iron diasporic bauxite
CN105801077A (en) * 2016-02-17 2016-07-27 中国科学院地球化学研究所 Preparation method of red mud/carbon-based magnetic composite material
CN105710383A (en) * 2016-04-30 2016-06-29 安徽农业大学 Method for preparing Cu powder by reducing CuO by adopting glycerinum
CN106319226A (en) * 2016-08-22 2017-01-11 中国铝业股份有限公司 Method for comprehensively recycling aluminium oxide, sodium oxide and ferric oxide from red mud

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