CN102732715B - Sodium-salt-modified paigeite and application thereof in reducing and sorting of hard-to-process iron-containing resource - Google Patents
Sodium-salt-modified paigeite and application thereof in reducing and sorting of hard-to-process iron-containing resource Download PDFInfo
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Abstract
The invention provides a sodium-salt-modified paigeite. A preparation method of the sodium-salt-modified paigeite comprises the steps that: paigeite is well mixed with sodium sulfate and sodium carbonate with a certain ratio; agglomeration is carried out; and dried agglomerates are subjected to reductive roasting, such that the sodium-salt-modified paigeite is obtained. The invention also provides an application method of the sodium-salt-modified paigeite in the reducing and sorting of hard-to-process iron-containing resources (including oolitic hematite, nickel laterite, and red mud). The application method comprises the steps that: the sodium-salt-modified paigeite is finely grinded, and is fully mixed with oolitic hematite, nickel laterite, or red mud; agglomeration is carried out; the agglomerate are dried by baking; the dried agglomerates are subjected to reductive roasting under a certain temperature with non-coking coal as a reducing agent; a reduction product is subjected to crushing and grinding; and the product is sorted by using a wet weak magnetic separation method, such that high-quality permalloy powder or metal iron powder can be obtained. During a direct reduction process of the hard-to-process iron-containing resource, with the sodium-salt-modified paigeite, the reduction temperature can be substantially reduced, the agglomeration and growth of metal iron grains can be promoted, and high-efficiency magnetic separation of the metal iron and gangue mineral can be further realized. Therefore, the sodium-salt-modified paigeite is suitable for industrialized applications.
Description
Technical field
The invention discloses a kind of sodium salt modification paigeite and the application in difficult iron-containing resource reduction and separation thereof.Belong to technical field of ferrous metallurgy.
Background technology
The boron resource of China approximately 60% is composed and is stored in paigeite (containing B
2o
3approximately 7%, full Fe approximately 30%), paigeite, because of its altogether/reason such as associated mineral is many, complex structure, by conventional beneficiation method separation difficulty, not yet forms plant-scale exploitation.
The processing and utilization key of paigeite is the separation of iron, boron, and treatment process mainly contains wet separation, pyrometallurgical smelting two class techniques.Method for wet separation is that paigeite is directly obtained to boric acid or borax with acid/alkaline purification, and leached mud obtains iron ore concentrate through magnetic separation again, and ferro-boron is separated.Although this technique can realize the comprehensive utilization of resource, because paigeite activity is low, need to carry out high-temperature activation pre-treatment, and the acid that later stage wet-leaching needs/alkali number consumes high (0.4 ton/1 ton raw ore), and production cost is high, also brings the problems such as acid corrosion equipment, contaminate environment simultaneously.The main direction of studying of pyrogenic process separating technology is mainly for blast furnace process, and paigeite is first thrown except the part SiO in raw ore through ore dressing
2, Al
2o
3, then by entering blast-furnace smelting after sintering for agglumeration, product is pig iron containing boron and boron-rich slag.The advantage of this technique is that technical process is short, equipment is simple, but commerical test research shows, when blast-furnace smelting paigeite is produced the pig iron containing boron of boracic approximately 1.0%, the decline of blast furnace production capacity, coke ratio high (about 1150kg/t), blast furnace lining corroding are serious, product sulfur-bearing is high, the more important thing is the B of boron-rich slag
2o
3active low, can not meet the requirement that carbon alkaline process borax is produced, if improve B by slow cooling
2o
3activity, realizes suitability for industrialized production technically and is all difficult economically, fails so far to realize suitability for industrialized production steady in a long-term.
For difficult iron-containing resources such as oolitic hematite, red soil nickel ore and red muds, the features such as because its valuable element content is low, mineral disseminated grain size is thin, complex structure, adopt conventional ore dressing, smelting technology to be difficult to efficiently be utilized.In recent years, direct-reduction-sorting process, because of advantages such as technique are simple, flow process is short, running cost is low, is widely used in the processing of Complex Iron Ore resource.But because follow-up physical separation flow process has higher requirements to the size of metallic iron crystal grain, thereby in Direct Reduction, must realize metallic iron crystal grain gathering, grow up, otherwise will cause the problems such as separating effect is poor, recovery rate of valuable metals is low, quality product is not high; If rely on merely rising reduction temperature, realize growing up of metallic iron crystal grain and will certainly increase the risk that material melting and reactor are adhered, totally unfavorable to production direct motion.Therefore,, at difficult iron-containing resource manufacture field, effectively reducing reduction temperature is the key point that direct-reduction-sorting process is applied.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and a kind of sodium salt modification paigeite and the application in difficult iron-containing resource reduction and separation thereof are provided, realizing the industrialization increment processing and utilization of paigeite inferior; The separating effect of metallic iron and gangue mineral while simultaneously improving the difficult iron-containing resource reduction and separations such as oolitic hematite, red soil nickel ore and red mud.
Sodium salt modification paigeite provided by the invention is to adopt following proposal to realize: by levigate paigeite, account for 40%～60% to-0.074mm, then mix with sodium sulfate and sodium carbonate, agglomeration, obtain paigeite agglomerate after dry, by after the reducing roasting of described paigeite agglomerate, obtain sodium salt modification paigeite; The per-cent that the addition of described sodium sulfate and sodium carbonate accounts for paigeite powder quality is: sodium sulfate 5%～40%, sodium carbonate 1～35%.
In sodium salt modification paigeite of the present invention, described reducing roasting temperature is 800～950 ℃, reducing roasting time 20～30min.
The application of sodium salt modification paigeite of the present invention in difficult iron-containing resource reduction and separation, be by sodium salt modification paigeite ore grinding to-after 0.074mm mass percent accounts for more than 70%, be added in difficult iron-containing resource mix, agglomeration, oven dry, then take mill coal as reductive agent reducing roasting, reduzate is after fragmentation, ore grinding, adopt the sorting of wet type low intensity magnetic separation method, obtain metal iron powder or ferronickel powder; Described difficult iron-containing resource is oolitic hematite, red soil nickel ore or red mud; It is 10%～40% that the addition of described sodium salt modification paigeite accounts for difficult iron-containing resource mass percent.
Sodium salt modification paigeite of the present invention selects in the application in smelting iron-containing resource reduction and separation in difficulty, and described reducing roasting temperature is 1000 ℃～1100 ℃, reducing roasting time 30～75min, and reduzate ore grinding to-200 order mass content account for more than 90%.
Action principle of the present invention is: make paigeite and Na
2sO
4or Na
2cO
3carry out low-temperature reduction roasting, magnetite part in paigeite is reduced into metallic iron, after fine grinding is processed, this part metallic iron subparticle is introduced the roasting of difficult iron-containing resource direct-reduction as crystal seed, for metallic iron crystal grain in difficult iron-containing resource provides growth site, reduce the nucleating potential barrier of iron crystal grain, promoted iron grain growth.Boron component in paigeite is in its low temperature sodium reduction pretreatment process, react with sodium salt and generate cenotype boric acid sodium salt, the alkalimetal ion that ionic radius is less and boron ion are in the direct-reduction roasting process of difficult iron-containing resource, not only can cause the lattice distortion of ferriferous oxide, the reduction of catalysis ferriferous oxide, but also can with difficult iron-containing resource in phosphorous, magnesium, silicon, the gangue mineral generation chemical reactions such as aluminium, destroy the original densification of difficult iron-containing resource ore, symbiotic structure, generate low melting component, for favourable mineralogy condition is created in metallic iron and gangue mineral separation.Thereby can significantly reduce reduction temperature, and shorten the recovery time, save energy consumption, reduce production costs, realize the high efficiency separation of metallic iron and gangue mineral.
Major advantage of the present invention is: after sodium salt modification paigeite, its magnetite part is reduced into metallic iron, for metallic iron crystal grain in difficult iron-containing resource reducing roasting process provides growth site; Boron component is reacted with sodium salt and is generated cenotype boric acid sodium salt, and reduction that can catalysis ferriferous oxide promotes the separation of metallic iron and gangue mineral.The present invention not only realizes efficient utilization of industrialization increment processing of paigeite inferior, but also valuable element iron, the rate of recovery of nickel and the decreasing ratio of harmful element while having improved oolitic hematite, red soil nickel ore and red mud reduction and separation support for the efficient utilization of difficult iron-containing resource provides new technology.Sodium salt modification paigeite prepares that desired raw material source is wide, technique is simple, environmental friendliness, can significantly reduce difficult iron-containing resource reduction temperature, shorten the recovery time, saves energy consumption, reduces production costs, and is suitable for industrial applications.
Embodiment
The main chemical compositions of paigeite, oolitic hematite, red soil nickel ore and red mud that the embodiment of the present invention adopts is respectively as shown in table 1, table 2, table 3, table 4.Before processing, respectively by red soil nickel ore, oolitic hematite and red mud in advance broken, ore grinding to-0.074mm quality percentage composition account for more than 80%.
Main chemical compositions/the % of table 1. paigeite
Main chemical compositions/the % of table 2. oolitic hematite
Main chemical compositions/the % of table 3. red soil nickel ore
Main chemical compositions/the % of table 4. red mud
Reference examples
Reference examples 1: after the agglomeration of oolitic hematite powder, being dried, with bituminous coal, make reductive agent, at the roasting temperature 60min of 1050 ℃, reduzate fragmentation, ore grinding to-0.074mm quality percentage composition is accounted for to 90%, magnetic separation under 1000Gs magneticstrength, iron grade 70.18% in metal iron powder, the phosphorus content 0.66% of obtaining, magnetic separation iron recovery 64.83%, phosphorus decreasing ratio 61.11%.
Reference examples 2: after the agglomeration of oolitic hematite powder, being dried, with coal, make reductive agent, at the roasting temperature 60min of 1350 ℃, by reduzate fragmentation, ore grinding, magnetic separation under 1000Gs magneticstrength, iron grade 86.28% in granulated iron, the phosphorus content 0.69% of obtaining, magnetic separation iron recovery 88.82%, phosphorus decreasing ratio 52.67%.
Reference examples 3: after the agglomeration of red soil nickel ore powder, being dried, with coal, make reductive agent, at the roasting temperature 60min of 1100 ℃, reduzate fragmentation, ore grinding to-0.074mm quality percentage composition is accounted for to 90%, magnetic separation under 1000Gs magneticstrength, iron grade 57.2% in ferronickel powder, the nickel grade 2.07% of obtaining, magnetic separation iron recovery 33.6%, nickel recovery 19.1%.
Reference examples 4: after the agglomeration of red soil nickel ore powder, being dried, with bituminous coal, make reductive agent, at the roasting temperature 60min of 1300 ℃, reduzate fragmentation, ore grinding to-0.074mm quality percentage composition is accounted for to 90%, magnetic separation under 1000Gs magneticstrength, iron grade 74.76% in ferronickel powder, the nickel grade 3.35% of obtaining, magnetic separation iron recovery 79.2%, nickel recovery 82.5%.
Reference examples 5: after the agglomeration of red mud powder, being dried, with bituminous coal, make reductive agent, at the roasting temperature 60min of 1050 ℃, reduzate fragmentation, ore grinding to-0.074mm quality percentage composition is accounted for to 90%, magnetic separation under 1000Gs magneticstrength, the iron grade 83.72% in metal iron powder that obtains, magnetic separation iron recovery 92.08%.
Reference examples 6: after the agglomeration of red mud powder, being dried, make reductive agent with coal, at the roasting temperature 60min of 1350 ℃, by reduzate fragmentation, ore grinding, magnetic separation under 1000Gs magneticstrength, the iron grade 88.57% in granulated iron product that obtains, magnetic separation iron recovery 94.35%.
Embodiment
Embodiment 1:
In accounting for 50% paigeite, broken, ore grinding to-0.074mm mass ratio allocates respectively sodium sulfate, sodium carbonate into by 30%, 1% mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 800 ℃, reduction agglomerate fragmentation, ore grinding to-0.074mm quality percentage composition accounts for 75%, makes sodium salt modification paigeite additive; By above-mentioned additive by mass percentage 30% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 90.67%, phosphorus content 0.16% in the metal iron powder obtaining, magnetic separation iron recovery 80.79%, phosphorus decreasing ratio 92.43%.
Embodiment 2:
In broken, ore grinding to-0.074mm mass ratio accounts for 60% paigeite, be 10%, 15% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 850 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 75%, make product and be modification paigeite additive to-0.074mm; By above-mentioned additive by mass percentage 30% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 90.15%, phosphorus grade 0.17% in the metal iron powder obtaining, magnetic separation iron recovery 83.59%, phosphorus decreasing ratio 90.41%.
Embodiment 3:
In broken, ore grinding to-0.074mm mass ratio accounts for 40% paigeite, be 25%, 15% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 900 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 75%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 30% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 93.38%, phosphorus grade 0.11% in the metal iron powder obtaining, magnetic separation iron recovery 87.98%, phosphorus decreasing ratio 93.27%.
Embodiment 4:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 25%, 10% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 900 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 75%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 40% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 90.75%, phosphorus grade 0.14% in the metal iron powder obtaining, magnetic separation iron recovery 81.5%, phosphorus decreasing ratio 91.02%.
Embodiment 5:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 40%, 15% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 900 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 75%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 30% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 92.75%, phosphorus grade 0.10% in the metal iron powder obtaining, magnetic separation iron recovery 85.64%, phosphorus decreasing ratio 93.50%.
Embodiment 6:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 25%, 20% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 900 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 75%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 30% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 91.91%, phosphorus grade 0.10% in the metal iron powder obtaining, magnetic separation iron recovery 88.26%, phosphorus decreasing ratio 94.13%.
Embodiment 7:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 25%, 5% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 20min at the temperature of 950 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 75%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 30% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 91.58%, phosphorus grade 0.105% in the metal iron powder obtaining, magnetic separation iron recovery 89.26%, phosphorus decreasing ratio 94.18%.
Embodiment 8:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 25%, 10% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 950 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 75%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 30% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 92.68%, phosphorus grade 0.09% in the metal iron powder obtaining, magnetic separation iron recovery 90.26%, phosphorus decreasing ratio 94.75%.
Embodiment 9:
In broken, ore grinding to-0.074mm mass ratio accounts for 60% paigeite, be 25%, 20% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 950 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 85%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 10% be added in oolitic hematite mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 1, iron grade 88.97%, phosphorus grade 0.21% in the metal iron powder obtaining, magnetic separation iron recovery 77.79%, phosphorus decreasing ratio 88.93%.
Embodiment 1-9 and reference examples 1,2 are compared, can find, adopt modification paigeite provided by the present invention, can be when significantly reducing oolitic hematite reduction temperature, significantly improve follow-up mill ore magnetic selection iron phosphorus separating effect, magnetic separation iron recovery and dephosphorization rate are high, and in iron powder, iron is of high grade and phosphorus content is low, meets steelmaking feed requirement.
Embodiment 10:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 30% to allocate sodium sulfate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 900 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 85%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 20% be added in red soil nickel ore mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 3, iron grade 79.2%, nickel grade 5.36% in the ferronickel powder obtaining, magnetic separation iron recovery 48.39%, nickel recovery 70.67%.
Embodiment 11:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 40% to allocate sodium sulfate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 950 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 85%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 40% be added in red soil nickel ore mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing with under conditional parameter identical in reference examples 3, iron grade 89.6%, nickel grade 5.73% in the ferronickel powder obtaining, magnetic separation iron recovery 50.1%, nickel recovery 83.95%.
Embodiment 10,11 and reference examples 3,4 are compared, can find, adopt modification paigeite provided by the present invention, can be when significantly reducing red soil nickel ore reduction temperature, follow-up mill ore magnetic selection nickel separating effect, nickel in magnetic separation nickel recovery and ferronickel powder, iron grade all obtain significantly and improve, and to stainless steel, refining is smelted very favourable.
Embodiment 12:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 10%, 5% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 20min at the temperature of 950 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 85%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 20% be added in red mud mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing, iron grade 90.3% in the metal iron powder obtaining, magnetic separation iron recovery 83.4% with under conditional parameter identical in reference examples 5.
Embodiment 13:
In broken, ore grinding to-0.074mm mass ratio accounts for 50% paigeite, be 5%, 10% to allocate respectively sodium sulfate, sodium carbonate in mass ratio, mix, agglomeration, dry after, take bituminous coal as reductive agent, reducing roasting 30min at the temperature of 950 ℃, obtained agglomerate fragmentation, ore grinding are accounted for to 85%, make product and be modification paigeite additive to-0.074mm.By above-mentioned additive by mass percentage 30% be added in red mud mix, agglomeration, dry agglomerate is carrying out reduction-grinding choosing, iron grade 91.6% in the metal iron powder obtaining, magnetic separation iron recovery 89.7% with under conditional parameter identical in reference examples 5.
Embodiment 12,13 and reference examples 5,6 are compared, can find, adopt modification paigeite provided by the present invention, can, when significantly reducing red mud reduction temperature, significantly improve iron grade, the iron recovery of follow-up mill ore magnetic selection gained iron powder.
Claims (3)
1. sodium salt modification paigeite, it is characterized in that: by levigate paigeite, account for 40% ~ 60% to-0.074mm mass percent, then mix with sodium sulfate and sodium carbonate, agglomeration, obtain paigeite agglomerate after dry, by after the reducing roasting of described paigeite agglomerate, obtain sodium salt modification paigeite; The per-cent that the addition of described sodium sulfate and sodium carbonate accounts for paigeite powder quality is: sodium sulfate 5% ~ 40%, sodium carbonate 1 ~ 35%; Described reducing roasting temperature is 800 ~ 950 ℃, reducing roasting time 20 ~ 30min.
2. the application of sodium salt modification paigeite according to claim 1 in difficult iron-containing resource reduction and separation, it is characterized in that: by sodium salt modification paigeite ore grinding to-after 0.074mm mass percent accounts for more than 70%, be added in difficult iron-containing resource mix, agglomeration, oven dry, then take mill coal as reductive agent, carry out reducing roasting, reduzate is after fragmentation, ore grinding, adopt the sorting of wet type low intensity magnetic separation method, obtain ferronickel powder or metal iron powder; Described difficult iron-containing resource is the one in red soil nickel ore or red mud; It is 10% ~ 40% that the addition of described sodium salt modification paigeite accounts for difficult iron-containing resource mass percent.
3. the application of sodium salt modification paigeite according to claim 2 in difficult iron-containing resource reduction and separation, it is characterized in that: described reducing roasting temperature is 1000 ~ 1100 ℃, reducing roasting time 30 ~ 75min, reduzate ore grinding to-200 order mass content account for more than 90%.
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| "EFFECTS OF SODIUM SALTS-MODIFIED PAIGEITE ON DEPHOSPHORIZATION OF HIGH-PHOSPHORUS OOLITIC HEMATITE DURING REDUCTION";Guanghui Li等;《3rd International Symposium on High-Temperature Metallurgical Processing》;20120430;第483-490页 * |
| Guanghui Li等."EFFECTS OF SODIUM SALTS-MODIFIED PAIGEITE ON DEPHOSPHORIZATION OF HIGH-PHOSPHORUS OOLITIC HEMATITE DURING REDUCTION".《3rd International Symposium on High-Temperature Metallurgical Processing》.2012,第483-490页. |
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