CN103509935A - Production process for improving iron content and reducing phosphorus content in low-grade high-phosphorus oolitic hematite - Google Patents
Production process for improving iron content and reducing phosphorus content in low-grade high-phosphorus oolitic hematite Download PDFInfo
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Abstract
The invention relates to a production process for improving iron content and reducing phosphorus content of low-grade high-phosphorus oolitic hematite, which comprises the following steps: (1), grinding the low-grade high-phosphorus oolitic hematite to fineness of more than or equal to 90 weight percent of minus 300 mesh mass ratio; (2), carrying out primary enrichment and iron content improvement by adopting a magnetic separation method so as to obtain rough concentrates of iron ores; (3), carrying out acid-leaching phosphorous removal on the rough concentrates of iron ores, which are obtained by magnetic separation, for 1 to 2 hours, filtering, returning filtrate to repeatedly utilize the filtrate for 1 to 3 times, then enabling the filtrate to enter the neutralizing treatment step, and enabling filter residues to be subjected to the step (4); (4), carrying out alkaline-leaching desilicication on iron ore concentrates obtained by acid leaching in the step (3) for 2 to 4 hours, filtering, returning filtrate to repeatedly utilize the filtrate for 1 to 3 times, then enabling the filtrate to enter the neutralizing treatment step, and obtaining filter residues which are iron ore concentrate products; (5), performing the acid-alkali neutralization reaction on the filtrate obtained in the step (3) and the filtrate obtained in the step (4) according to a stoichiometric ratio so as to obtain neutral waste liquor. The production process has a short flow and low energy consumption, is simple to operate and is low in cost; and in the process, the generated acid waste liquor and alkali waste liquor are neutralized, so that pollution to the environment is low.
Description
Technical field
The present invention relates to a kind of rhombohedral iron ore production technique, especially relate to a kind of low-grade high-phosphor oolitic hematite and carry iron and fall production of phosphorus.
Background technology
There are 3,000,000,000 tons of high-phosphor oolitic hematites in China, and this iron ore is containing P high (0.4～1.0%), grade lower (35～50%).Ferric oxide crystal grain disseminated grain size thin (1～3 μ m), sorts separated difficult, thereby does not obtain effectively exploitation utilization.Phosphorus in this iron ore is composed and is deposited with the form of collophanite, and mixed in together with the chamosite that is rich in ferric oxide, forms the alternate oolith structure of concentric layered shell polysaccharide, and oolitic hematite stone is one of iron ore type of the most difficult choosing of generally acknowledging both at home and abroad at present.
Phosphorus is very large on the impact of steel performance, phosphorus is the harmful element in most steel grades, is mainly manifested in: (1) phosphorus significantly expands Mushy Zone, when casting solidification, strong segregation phenomena can occur, dwindle phase region simultaneously, thereby encouraged the segregation in process of setting; (2) phosphorus velocity of diffusion in α and γ Solid solution is slower, causes the inhomogeneous of tissue.Because the solubleness of phosphorus in liquid phase is more much bigger than the solubleness in solid phase, therefore phosphorus is easily separated out on crystal boundary, so phosphorus can form the fragility texture of high phosphorus at intercrystalline, the fragility of infringement steel, particularly evident when low temperature (being commonly called as cold short), for the high steel of carbon containing, the damaging effect of phosphorus is more remarkable.
Due to the above-mentioned harm of phosphorus, therefore, in steelmaking process, should reduce as far as possible the phosphorus content in molten steel, if iron ore just can be removed phosphorus wherein before entering stove, will greatly reduce steel-making cost so.At present, the method for reducing phosphorus of high-phosphorus iron ore mainly contains beneficiation method, chemical process, smelting process and Biodephosphorization method.
Beneficiation method mainly comprises: calcining magnetic separation, high intensity magnetic separation, floatation process, the sorting of selectivity agglomerate, combined process flow.In recent years, both at home and abroad phosphorus theory is fallen in high-phosphorus iron ore and technique has been carried out a large amount of research and made some progress.But due to China's high-phosphorus iron ore mineral composition more complicated of " Ningxiang's formula " high-phosphor oolitic hematite particularly, phosphorus ore thing disseminated grain size is tiny, thereby utilizes beneficiating method dephosphorization still to have many problems.As the weak magnetic of use the last the one magnetic dephosphorization technologies such as Chen Youyi select dephosphorization research deeply to meishan iron mine stone, result shows: (1) dephosphorization rate is low; (2), due to fine grinding, treatment capacity while reducing ball milling platform, has increased product sedimentation, concentrated difficulty; Grinding fineness increases, and during ball milling platform, processing power reduces, and ore grinding cost is obviously increased; (3) loss amount of iron is large, and the rate of recovery of iron reduces.Because phosphorus ore thing granularity in high-phosphorus iron ore is tiny, embedding Bu Tezheng is complicated, and ore mineral forms complicated, adopts traditional beneficiation method to be difficult to reach gratifying effect.In order to obtain better dephosphorization effect, researchist has developed with interpolation dephosphorizing agent and has carried out direct-reduction roasting-magnetic selection method, and this method can effectively reduce the phosphorus content in iron ore concentrate, but the method need to be by whole ore roasting to 1000 ℃ left and right, energy consumption is very big, and burns in a large number coal contaminate environment.
Chemical process dephosphorization carries out acidleach dephosphorization with nitric acid, hydrochloric acid or sulfuric acid to ore exactly.The method is a kind of dephosphorizing method of relative efficiency, and phosphorus ore thing monomer dissociation completely in ore, as long as come out, just contact and can reach the object of falling phosphorus with leach liquor, yet chemical process dephosphorization acid consumption is large, cost is high, acid leaching solution is large to the corrosion of equipment, and a large amount of acid soak easily causes soluble iron mineral dissolution in ore, causes iron loss.Nanfang Metallurgy College utilizes dispergation to soak Kuang Fadui“ Ningxiang formula " delvauxite stone carries out anti-salt and protects iron and fall phosphorus research, result shows, can remove in ore 40～50% phosphorus, but the concentration of medium that this scheme is used is up to 3～5mol/L, cost is high, and dephosphorization rate is still lower.Generally speaking, although chemical method dephosphorization effect is better, still owe desirable, particularly cost is higher; In addition, also has a problem: the spent acid solution of generation can serious environment pollution.
Some Steel Plant adopts and smelts dephosphorization, comprises liquid iron pretreatment dephosphorizing and converter steelmaking dephosphorization.The ultimate principle of liquid iron pretreatment dephosphorizing is, hot metal in steelmaking, before entering converter or electric furnace, reacts with oxidisability and the basic slag of basic oxide or hyperoxia voltinism and the phosphorus in molten iron, and molten iron is carried out to pretreatment dephosphorizing.This method is effective, but cost is higher, and hot metal temperature drop is large, and the dephosphorization of high phosphorus hot metal is existed to certain difficulty.Dephosphorization of molten iron is requisite operation in converter steelmaking flow process, the steelworks having at present adopts double slag operation of converter and the low dephosphorization smelting control technique of drawing carburetting to combine of smelting endpoint, according to dephosphorisation reaction feature, require dephosphorization under the condition of low temperature, hyperoxia voltinism, high alkalinity, to carry out.
In recent years, utilize the research of microbiological treatment Mineral resources very active, Jin Jiuronglin aspect, just oneself is through finding that a variety of bacteriums, fungi, actinomycetes all have molten phosphorus effect.They mainly produce the pH value of sour reduction system by metabolism, make phosphorus mineral dissolution.Research shows, some bacteriums have the excessive characteristic of taking the photograph phosphorus, and this is also one of mechanism of Biodephosphorization.The He Liangju of Northeastern University etc. utilizes in meishan iron mine ore and contains part pyrite, first uses (Tf) bacterium oxidation pyrite to produce acid leaching solution, then with leach liquor, carries out leach liquor ore deposit dephosphorization.Dephosphorization rate can reach 76.89%, and iron loss rate is 3.87%, for high-phosphorus iron ore dephosphorization provides new way.But microbiological treatment ores efficient low, the time is long, equipment is huge etc. a series ofly in the industrial problem that is difficult to realize, needs to solve.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, provides a kind of rate of recovery higher, and production cost is lower, and dephosphorization efficiency is high, and the little low-grade high-phosphor oolitic hematite of environmental pollution is carried iron and fallen production of phosphorus.
The technical scheme that the present invention solves its technical problem employing is that a kind of low-grade high-phosphor oolitic hematite is carried iron and fallen production of phosphorus, comprises the following steps:
(1) fineness to-300 order mass ratio >=90wt% by low-grade high-phosphor oolitic hematite ore grinding;
(2) adopt magnetic selection method to carry out preliminary enrichment and carry iron, obtain iron ore rough concentrate;
The preferred one roughing once purging selection of described magnetic selection method primary cleaning, magnetic separation roughly select concentrate and scavenger concentrate merge carry out selected, the magneticstrength that magnetic separation is roughly selected, scanned is 0.80～0.95 tesla, time is respectively 2～6 minutes, 3～7 minutes, the selected magneticstrength of magnetic separation is 0.70～0.95 tesla, and the time is 3～7 minutes;
(3) iron ore rough concentrate magnetic separation being obtained carries out acidleach dephosphorization, and leaching time 1-2 hour filters, and filtrate enters neutralizing treatment step after returning and reusing 1～3 time, and filter residue enters step (4);
(4) iron ore concentrate after step (3) acidleach is carried out to alkali and soak desiliconization, the alkali time of soaking is 2～4 hours, filters, and filtrate enters neutralizing treatment step after returning and reusing 1～3 time, and filter residue is iron extract mine producation;
(5) filtrate that filtrate step (3) being obtained obtains with step (4) is carried out acid-base neutralisation according to stoichiometric ratio and is reacted, and forms neutral waste liquid.
In step (1), the preferred ball milling of described milling method; Preferably by low-grade high-phosphor oolitic hematite ore grinding to-300 orders >=95wt%.
In step (3), acidleach pharmacy optimization sulfuric acid or hydrochloric acid, acid concentration is massfraction 5%～30%(preferably 8%～15%); The mass ratio of iron ore Cu Jing Kuang ︰ acid solution is 1 preferred 1:0.9～1.5 of ︰ 0.8-2.5().
In step (4), alkali soaks the compound alkali lye of pharmacy optimization, compound alkali lye is preferably 15 wt%-30wt% of 5wt%～40wt%(by saturated ammoniacal liquor and mass concentration) sodium hydroxide solution according to preferred 1:1.5～2.5 of 1:0.8～3() composite the forming of mass ratio, the iron ore concentrate after acidleach: the mass ratio of alkali lye is preferred 1:0.8～1.6 of 1:0.6～2().
Integrated use ore dressing-chemical process of the present invention, creationary introducing alkaline purification desilication process, make whole operational path have the roasting of exempting from, sour consumption little, without features such as spent acid discharges, with respect to traditional technology, production cost is lower, and energy consumption is little, the rate of recovery and dephosphorization efficiency are high, and environmental pollution is little.
Flow process of the present invention is short, and energy consumption is low, simple to operate, and cost is low.
Phosphorus falls in the iron of carrying that the present invention is applicable to domestic and international low-grade high-phosphor oolitic hematite ore.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment comprises the following steps:
(1) adopt ball mill ore grinding to-300 order mass ratioes 100% in low-grade high-phosphor oolitic hematite (containing Fe 43.77%, P 1.05%) raw ore;
(2) adopt magnetic selection method to carry out the preliminary enrichment of magnetic separation and carry iron, magnetic separation process is one roughing once purging selection primary cleaning, and concentrate is roughly selected in magnetic separation and primary cleaning is carried out in scavenger concentrate merging; Roughly select, selected magneticstrength Wei0.9 tesla, the time is respectively 3 minutes, 5 minutes; Scanning magneticstrength is that 0.85 tesla's time was 3 minutes; Obtain the magnetic concentrate of Fe grade 52.31%;
(3) step (2) gained magnetic separation rough concentrate is carried out to acidleach, acidleach medicament is sulfuric acid, sulfuric acid concentration 10wt%, concentrate: acid solution solid-liquid mass ratio is 1:1, leaching time is 1 hour, filters, filtrate enters neutralizing treatment step after returning and reusing 2 times, and filter residue enters step (4);
(4) will be after step (3) acidleach filter residue carry out alkali and soak, it is compound alkali lye that alkali soaks medicament, the sodium hydroxide solution that compound alkali lye is 30wt% by saturated ammoniacal liquor and mass concentration forms according to the mass ratio of 1:2 is composite, iron ore concentrate after acidleach: the mass ratio of alkali lye is 1:1, the alkali time of soaking is 2 hours; Filter, filtrate enters neutralizing treatment step after returning and reusing 2 times, and filter residue is iron extract mine producation.
(5) filtrate that filtrate step (3) being obtained obtains with step (4) is carried out acid-base neutralisation according to stoichiometric ratio and is reacted, and obtains neutral waste liquid.
Through magnetic separation-acidic leaching with alkaline, soak process integration, obtain Fe grade 55.49%, P grade 0.09%, the iron ore concentrate of the Fe rate of recovery 58.16%, the grade of the present embodiment raw ore and product, productive rate, the rate of recovery the results are shown in Table 1.
The present embodiment comprises the following steps:
(1) adopt ball mill ore grinding to-300 order 95wt% in low-grade high-phosphor oolitic hematite (containing Fe 43.43%, P 0.95%) raw ore;
(2) adopt magnetic selection method to carry out the preliminary enrichment of magnetic separation and carry iron, magnetic separation process is one roughing once purging selection primary cleaning, and concentrate is roughly selected in magnetic separation and primary cleaning is carried out in scavenger concentrate merging; Roughly select, selected magneticstrength is 0.92 tesla, the time is respectively 4 minutes, 4 minutes; Scanning magneticstrength is 0.88 tesla, and the time is 5 minutes; Obtain the magnetic concentrate of Fe grade 52.60%;
(3) iron ore rough concentrate magnetic separation being obtained carries out acidleach, and acidleach medicament is hydrochloric acid, concentration of hydrochloric acid 15wt%, and iron ore rough concentrate: the mass ratio of acid solution is 1:1.4, leaching time is 2 hours; Filter, filtrate enters neutralizing treatment step after returning and reusing 1 time, and filter residue enters step (4);
(4) filter residue after acidleach being carried out to alkali soaks, it is compound alkali lye that alkali soaks medicament, compound alkali lye is that the solution of 20wt% sodium hydroxide forms according to the mass ratio of 1:1.5 is composite by saturated ammoniacal liquor and mass concentration, the iron ore concentrate after acidleach: the mass ratio of alkali lye is 1:1.5, and the alkali time of soaking is 2 hours; Filter, filtrate enters neutralizing treatment step after returning and reusing 1 time, and filter residue is iron extract mine producation.
Through magnetic separation-acidic leaching with alkaline, soak process integration, obtain Fe grade 55.33%, P grade 0.11%, the iron ore concentrate of the Fe rate of recovery 59.46%, in embodiment, the grade of raw ore and product, productive rate, the rate of recovery the results are shown in Table 2.
Embodiment 3
The present embodiment comprises the following steps:
(1) adopt ball mill ore grinding to-300 orders 100% in low-grade high-phosphor oolitic hematite (containing Fe 44.07%, P 1.02%) raw ore;
(2) adopt magnetic selection method to carry out the preliminary enrichment of magnetic separation and carry iron, magnetic separation process is one roughing once purging selection primary cleaning, and concentrate is roughly selected in magnetic separation and primary cleaning is carried out in scavenger concentrate merging; Roughly select, selected magneticstrength is 0.89 tesla, the time is respectively 6 minutes, 4 minutes; Scanning magneticstrength Wei0.9 tesla's time is 3 minutes; Obtain the magnetic concentrate of Fe grade 52.47%;
(3) iron ore rough concentrate magnetic separation being obtained carries out acidleach, and acidleach medicament is sulfuric acid, sulfuric acid concentration 10wt%, and concentrate: acid solution solid-liquid mass ratio is 1:1, leaching time is 1 hour; Filter, filtrate enters neutralizing treatment step after returning and reusing 3 times, and filter residue enters step (4);
(4) filter residue after step (3) acidleach being carried out to alkali soaks, it is compound alkali lye that alkali soaks medicament, compound alkali lye is formed according to the mass ratio of 1:2.5 is composite by saturated ammoniacal liquor and 15wt% sodium hydroxide solution, the iron ore concentrate after acidleach: alkali lye solid-liquid mass ratio is 1:0.9, and the alkali time of soaking is 3 hours; Filter, filtrate enters neutralizing treatment step after returning and reusing 3 times, and filter residue is iron extract mine producation
Through magnetic separation-acidic leaching with alkaline, soak process integration, obtain Fe grade 55.67%, P grade 0.11%, the iron ore concentrate of the Fe rate of recovery 59.66%, in embodiment, the grade of raw ore and product, productive rate, the rate of recovery the results are shown in Table 3.
Claims (10)
1. low-grade high-phosphor oolitic hematite is carried iron and is fallen a production of phosphorus, it is characterized in that, comprises the following steps:
(1) fineness to-300 order mass ratio >=90wt% by low-grade high-phosphor oolitic hematite ore grinding;
(2) adopt magnetic selection method to carry out preliminary enrichment and carry iron, obtain iron ore rough concentrate;
(3) iron ore rough concentrate magnetic separation being obtained carries out acidleach dephosphorization, and leaching time 1-2 hour filters, and filtrate enters neutralizing treatment step after returning and reusing 1～3 time, and filter residue enters step (4);
(4) iron ore concentrate after step (3) acidleach is carried out to alkali and soak desiliconization, the alkali time of soaking is 2～4 hours, filters, and filtrate enters neutralizing treatment step after returning and reusing 1～3 time, and filter residue is iron extract mine producation;
(5) filtrate that filtrate step (3) being obtained obtains with step (4) is carried out acid-base neutralisation according to stoichiometric ratio and is reacted, and forms neutral waste liquid.
2. low-grade high-phosphor oolitic hematite according to claim 1 is carried iron and is fallen production of phosphorus, it is characterized in that, in step (1), described milling method is ball milling.
3. low-grade high-phosphor oolitic hematite according to claim 1 and 2 is carried iron and is fallen production of phosphorus, it is characterized in that, in step (1), by low-grade high-phosphor oolitic hematite ore grinding to-300 order >=95%.
4. low-grade high-phosphor oolitic hematite according to claim 1 and 2 is carried iron and is fallen production of phosphorus, it is characterized in that, described magnetic selection method is one roughing once purging selection primary cleaning, magnetic separation roughly select concentrate and scavenger concentrate merge carry out selected, the magneticstrength that magnetic separation is roughly selected, scanned is 0.80～0.95 tesla, and the time is respectively 2～6 minutes, 3～7 minutes, the selected magneticstrength of magnetic separation is 0.70～0.95 tesla, and the time is 3～7 minutes.
5. low-grade high-phosphor oolitic hematite according to claim 1 and 2 is carried iron and is fallen production of phosphorus, it is characterized in that, in step (3), acidleach medicament is sulfuric acid or hydrochloric acid, and acid concentration is massfraction 5%～30%; The mass ratio of iron ore Cu Jing Kuang ︰ acid solution is 1 ︰ 0.8-2.5.
6. low-grade high-phosphor oolitic hematite according to claim 5 is carried iron and is fallen production of phosphorus, it is characterized in that, acid concentration is massfraction 8%～15%.
7. low-grade high-phosphor oolitic hematite according to claim 5 is carried iron and is fallen production of phosphorus, it is characterized in that, the mass ratio of iron ore Cu Jing Kuang ︰ acid solution is 1:0.9～1.5.
8. low-grade high-phosphor oolitic hematite according to claim 1 and 2 is carried iron and is fallen production of phosphorus, it is characterized in that, in step (4), it is compound alkali lye that alkali soaks medicament, the sodium hydroxide solution that described compound alkali lye is 5wt%～40wt% by saturated ammoniacal liquor and mass concentration forms according to the mass ratio of 1:0.8～3 is composite, the iron ore concentrate after acidleach: the mass ratio of alkali lye is 1:0.6～2.
9. low-grade high-phosphor oolitic hematite according to claim 8 is carried iron and is fallen production of phosphorus, it is characterized in that, the sodium hydroxide solution that compound alkali lye is 15wt%-30wt% by saturated ammoniacal liquor and mass concentration forms according to the mass ratio of 1:1.5～2.5 is composite.
10. low-grade high-phosphor oolitic hematite according to claim 8 is carried iron and is fallen production of phosphorus, it is characterized in that the iron ore concentrate after acidleach: the mass ratio of alkali lye is 1:0.8～1.6.
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| CN103882225A (en) * | 2014-04-04 | 2014-06-25 | 北京科技大学 | Method for removing phosphorus in high-phosphorus iron ore by virtue of acid leaching and recycling acid liquor |
| CN104404245A (en) * | 2014-11-19 | 2015-03-11 | 武汉钢铁(集团)公司 | Method for producing abrasion-resistant material by utilizing high-phosphorus oolitic hematite |
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| CN108993770A (en) * | 2018-07-27 | 2018-12-14 | 湖南农业大学 | A kind of ore-dressing technique of fine grain teeth cloth silicate-type iron oxide ore |
| CN109943716A (en) * | 2019-03-26 | 2019-06-28 | 昆明理工大学 | A kind of method that miscellaneous preparation high-quality iron ore concentrate drops in high-phosphor oolitic hematite chemistry |
| CN111876593A (en) * | 2020-09-01 | 2020-11-03 | 中南大学 | Method for separating iron and removing phosphorus from high-phosphorus oolitic hematite |
| CN113042201A (en) * | 2021-03-30 | 2021-06-29 | 酒泉钢铁(集团)有限责任公司 | Iron-extracting and phosphorus-removing process for high-phosphorus hematite |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882225A (en) * | 2014-04-04 | 2014-06-25 | 北京科技大学 | Method for removing phosphorus in high-phosphorus iron ore by virtue of acid leaching and recycling acid liquor |
| CN104404245A (en) * | 2014-11-19 | 2015-03-11 | 武汉钢铁(集团)公司 | Method for producing abrasion-resistant material by utilizing high-phosphorus oolitic hematite |
| CN104404245B (en) * | 2014-11-19 | 2016-10-05 | 武汉钢铁(集团)公司 | A kind of method utilizing high-phosphor oolitic hematite to produce high-abrasive material |
| CN104785347A (en) * | 2015-04-03 | 2015-07-22 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Separation method of high-silicon low-grade oxidized iron ore |
| CN104785347B (en) * | 2015-04-03 | 2018-04-03 | 甘肃酒钢集团宏兴钢铁股份有限公司 | A kind of method for separating of the low-grade ferric oxide ore of high silicon |
| CN108993770A (en) * | 2018-07-27 | 2018-12-14 | 湖南农业大学 | A kind of ore-dressing technique of fine grain teeth cloth silicate-type iron oxide ore |
| CN109943716A (en) * | 2019-03-26 | 2019-06-28 | 昆明理工大学 | A kind of method that miscellaneous preparation high-quality iron ore concentrate drops in high-phosphor oolitic hematite chemistry |
| CN111876593A (en) * | 2020-09-01 | 2020-11-03 | 中南大学 | Method for separating iron and removing phosphorus from high-phosphorus oolitic hematite |
| CN113042201A (en) * | 2021-03-30 | 2021-06-29 | 酒泉钢铁(集团)有限责任公司 | Iron-extracting and phosphorus-removing process for high-phosphorus hematite |
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