CN105126993A - Comprehensive recovery process for associated tantalum-niobium ore - Google Patents
Comprehensive recovery process for associated tantalum-niobium ore Download PDFInfo
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Abstract
The invention provides a comprehensive recovery process of associated tantalum-niobium ore, which is mainly characterized in that the raw ore is classified after coarse grinding, coarse-grained tantalum-niobium ore and mica ore rich in rare metal are recovered from coarse-grained products on a screen by adopting a high-gradient magnetic separation-heavy liquid separation method, fine-grained tantalum-niobium ore and feldspar ore rich in rare metal are recovered from undersize products by adopting a flotation method after sulfide ore flotation and impurity removal, and bisphosphonic acid, benzohydroxamic acid and soybean oleic acid which are combined collectors having strong selectivity and collecting capability on the tantalum-niobium ore are added during tantalum-niobium flotation for flotation of tantalum-niobium ore. The process not only obtains the tantalum-niobium mineral with better index, but also comprehensively recovers other associated rare metals in the mineral.
Description
Technical field
The invention belongs to technical field of beneficiation, be specifically related to the technique of tantalum niobium element in a kind of synthetical recovery association tantalum niobium concentrate and association rare metal.
Background technology
Tantalum and niobium belong to high-melting-point rare metal, and being widely used in the fields such as Aero-Space, military project, semiconductor, is the indispensable metal material of high-tech industry.China tantalum niobium mineral resources are abundanter, but single mineral deposit is few, mostly is accompanying mineral deposit, and the rare metals such as normal association rubidium, beryllium, comprehensive utilization value is large.
The character feature that the ore dressing of tantalum niobium concentrate thing is normally different according to tantalum niobium concentrate thing, adopts the method for gravity treatment, magnetic separation, flotation to reclaim.Such as, to only tantalum niobium concentrate thing density is large, and the ore that tantalum niobium concentrate thing disseminated grain size is thicker, usually adopt the sorting process based on gravity treatment; Large to there being multi mineral density, and the ore that tantalum niobium concentrate thing disseminated grain size is thicker, the sorting process adopting gravity treatment to combine with magnetic separation, electric separation more; Large to there being multi mineral density, and the ore that tantalum niobium concentrate thing disseminated grain size is thinner, adopt the sorting process based on flotation more.But uneven for disseminated grain size, distribution dispersion, complicated components be rich in the association tantalum niobium concentrate thing of other rare metal, said method exists that the tantalum niobium rate of recovery is low, tantalum-niobium concentrate grade is low, other valuable metal can not obtain the defect rationally recycled.
Summary of the invention
The present invention is directed to defect of the prior art, uneven for tantalum niobium concentrate thing disseminated grain size, recovery difficult is comparatively large, and the mineral that associated metal value is high, propose a kind of ore-dressing technique of complicated association tantalum niobium concentrate synthetical recovery.
The present invention is achieved by the following technical solutions:
A comprehensive recycling process for association tantalum niobium concentrate, comprises the steps:
1) ore grinding: wet-milling after association tantalum niobium concentrate and crushing raw ore is accounted for 35% ~ 45% to fineness-0.074mm, ore milling concentration is 50% ~ 60%;
2) sieve: sieved by the ore pulp after wet-milling, screen size is 0.1mm ~ 0.3mm, obtain the coarse grain product on sieving and the fine particle product under sieve;
3) coarse grain product magnetic separation: described coarse grain product feeds high gradient magnetic separator and carries out high intensity magnetic separation separation, and magnetic field intensity is 1.2T ~ 1.6T, the magnetic product obtained and non-magnetic product; Magnetic product is the bulk concentrate of tantalum niobium and magnetic mica.
4) heavy-fluid is selected: gained magnetic product is carried out the selected separation of heavy-fluid, and the heavy-fluid density selected is 2.9g/cm
3~ 5g/cm
3, obtain the mica concentrate that heavy product-coarse grain tantalum-niobium concentrate and the little product of proportion are rich in rare metal;
5) fine particle product and non-magnetic product mixing ore grinding: fine particle product described in screening gained and magnetic separation gained non-magnetic product are regrinded, account for more than 60% to fineness for-0.074mm, ore milling concentration is preferably 60% ~ 70%;
6) to regrind flotation of ore pulp: by step 5) gained regrinds after ore pulp is sized mixing and carries out sulfide flotation, obtains sulphide ore and sulfide flotation mine tailing; Sulfide flotation mine tailing carries out tantalum niobium concentrate flotation and obtains particulate tantalum-niobium concentrate and tantalum niobium flotation tailing; Tantalum niobium flotation tailing carries out feldspar ore flotation acquisition and is rich in the feldspar concentrate of rare metal and final flow process mine tailing.
More specifically, step 6) after ore pulp adjustment pulp density 30% ~ 35% of regrinding in ore pulp ore dressing of regrinding, in ore pulp quality, add collecting agent butyl xanthate 50 ~ 100g/t, infusion 2
#oil 10 ~ 60g/t, carries out sulfide flotation; Sulfide flotation mine tailing ore pulp is adjusted to pH values of pulp=4 ~ 5, in ore pulp quality, adds combined capturing and collecting agent 30 ~ 100g/t, carry out tantalum niobium concentrate roughly select, scan, selected, component and the quality proportioning thereof of described combined capturing and collecting agent are: two banks 2 ~ 3.5 parts
Benzyl hydroximic acid 1 ~ 2.5 part
Soybean oleic acid 1 ~ 2 part;
It is 25% ~ 33% adjustment pH=2 ~ 3 that tantalum niobium flotation tailing is adjusted to pulp density, in ore pulp quality, adds activator hydrofluoric acid 300 ~ 1000g/t, collecting agent lauryl amine 60 ~ 120g/t, carry out feldspar ore roughly select, scan, selected.
Beneficial effect of the present invention:
Sieve classification is carried out after raw ore corase grind, thickness grade mineral adopt different ore-dressing techniques to reclaim, and have both reduced the follow-up cost regrinded, and play the effect early reclaiming and early utilize, additionally reduce mineral circulation loss on stream, be conducive to the overall recovery improving tantalum niobium concentrate thing; The method that coarse grain tantalum niobium concentrate thing adopts magnetic separation-heavy-fluid to be separated reclaims, and heavy-fluid separation method is applicable to be separated the mineral that a small amount of granularity is greater than 0.1mm, has separative efficiency high, the advantage that heavy-fluid can be reused; Add combined capturing and collecting agent during the flotation of fine tantalite-columbite thing and replace conventional collecting agent, two banks energy and Fe in acid medium
2+, Fe
3+plasma forms indissoluble salt and collecting tantalum niobium concentrate thing, has selective preferably, the oximido energy that benzyl hydroximic acid has and Ta
5+, Nb
5+, Fe
2+form the better chelate of stability of indissoluble and all comparatively strong to the selective of tantalum niobium concentrate thing and collecting ability Deng metal ion, soybean oleic acid collecting ability is strong, controls the floatation indicators that certain consumption can improve tantalum niobium concentrate thing.The invention solves the problem that the uneven tantalum niobium concentrate thing floatation process of disseminated grain size is complicated, recovery rate in ore-dressing is low, associated metal utilization rate is low.The method has the advantage that technique is simple, production cost is low, mineral processing index is good, comprehensive resource utilization rate is high.
Accompanying drawing explanation
The comprehensive recycling process flow chart of Fig. 1 a kind of association tantalum niobium concentrate of the present invention.
Detailed description of the invention
Embodiment one
Gansu association tantalum niobium concentrate Ta
2o
5grade 29.6g/t, Nb
2o
5grade 104g/t, tantalum niobium mainly exists with the form of niobium-tantalum ore, and ildefonsite disseminated grain size is uneven, and coarse grain is greater than 0.15mm, and particulate, less than 0.037mm, except tantalum niobium, goes back association rare metal rubidium in ore, Rb
2o grade is 0.14%, and the essential mineral in ore is biotite, potassic feldspar, quartz, and also containing a small amount of sulfide, biotite granularity is comparatively thick, much in 0.15mm, and rubidium is composed to be existed in biotite and feldspar.
This ore carries out tantalum niobium, the recovery process of rare metal is:
1) ore grinding: after raw ore wet-milling is accounted for 45% to fineness-0.074mm, ore milling concentration is 55%;
2) sieve: adopt 75 object sieves to carry out sieve classification to the ore pulp after wet-milling;
3) coarse grain product magnetic separation: on sieve, coarse grain product feeds magnetic field intensity is that the high gradient magnetic separator of 1.3T carries out strong magnetic ore separation, obtains magnetic product and non-magnetic product.
4) heavy-fluid is selected: magnetic product feeds in the separatory funnel that heavy-fluid diiodomethane is housed and carries out heavy-liquid concentration, obtains (Ta, Nb)
2o
5grade is 10.27%, (Ta, Nb)
2o
5the rate of recovery is the coarse grain tantalum-niobium concentrate of 19.71% and contains Rb
2o grade is the biotite concentrate of 0.81%.
5) fine particle product and non-magnetic product mixing ore grinding: under the non-magnetic product that high-gradient magnetic separation obtains and the sieve that sieve classification obtains, fine particle product feeds ball mill and regrinds, and is milled to fineness and accounts for 65% for-0.074mm.
6) to regrind flotation of ore pulp: regulate pulp density to 33% of regrinding, in ore pulp quality, add butyl xanthate 80g/t, 2
#oil 15g/t carries out sulfide flotation removal of impurities, in sulfide flotation mine tailing ore pulp, add sulfuric acid be adjusted to pH values of pulp=4, in ore pulp quality, and add the combined capturing and collecting agent of 40g/t, its component and mass ratio are the collector for columbite-tantalite two banks of 2:2.25:1, benzyl hydroximic acid, soybean oleic acid carry out the flotation of tantalum niobium, through one roughing, once purging selection, twice selected acquisition (Ta, Nb)
2o
5grade is 9.22%, (Ta, Nb)
2o
5the rate of recovery is 49.57% fine-graded tantalum-niobium concentrate, tantalum niobium flotation tailing is after 26% through the concentrated pulp density that is adjusted to, add sulfuric acid and be adjusted to pH values of pulp=2.5, in ore pulp quality, and successively add activator hydrofluoric acid 400g/t, collecting agent lauryl amine 100g/t, carries out feldspar flotation, obtains containing Rb through one roughing, once purging selection, primary cleaning
2o grade is feldspar concentrate and the mine tailing of 0.28%.
Embodiment two
Essential mineral in Jiangxi association tantalum niobium concentrate ore has zinnwaldite, albite, quartz and a small amount of sulfide, and tantalum niobium concentrate owner will exist with the form of niobium manganotantalite, Ta
2o
5grade 87.23g/t, Nb
2o
5grade 97.58g/t, tantalum niobium disseminated grain size thickness great disparity, coarse grain is greater than 0.2mm, and particulate is less than 0.037mm, and also with rare metal lithium in ore, lithium is composed to be existed in zinnwaldite, Li
2o grade is 0.087%.
This ore carries out tantalum niobium, the recovery process of rare metal is:
1) ore grinding: raw ore wet-milling is accounted for 40% to fineness-0.074mm, ore milling concentration is 60%;
2) sieve: adopt 120 object sieves to carry out sieve classification to the ore pulp after wet-milling;
3) coarse grain product magnetic separation: on sieve, coarse grain product feeds magnetic field intensity is that the high gradient magnetic separator of 1.5T carries out strong magnetic ore separation, obtains magnetic product and non-magnetic product.
4) heavy-fluid is selected: magnetic product feeds in the separatory funnel that heavy-fluid diiodomethane is housed and carries out heavy-liquid concentration, obtains (Ta, Nb)
2o
5grade is 15.05%, (Ta, Nb)
2o
5the rate of recovery is the coarse grain tantalum-niobium concentrate of 20.56% and contains Li
2o grade is the zinnwaldite concentrate of 3.98%.
5) fine particle product and non-magnetic product mixing ore grinding: under the non-magnetic product that high-gradient magnetic separation obtains and the sieve that sieve classification obtains, fine particle product feeds two sections of ball mills and regrinds, and is milled to fineness and accounts for 70% for-0.074mm;
6) to regrind flotation of ore pulp: regulate pulp density to 33% of regrinding, in ore pulp quality, add butyl xanthate 100g/t, 2
#oil 30g/t carries out sulfide flotation removal of impurities, in sulfide flotation mine tailing ore pulp, add sulfuric acid be adjusted to pH values of pulp=4, in ore pulp quality, and add the combined capturing and collecting agent of 100g/t, its component and mass ratio are the collector for columbite-tantalite two banks of 2.5:2.4:1.5, benzyl hydroximic acid, soybean oleic acid carry out the flotation of tantalum niobium, through one roughing, once purging selection, twice selected acquisition (Ta, Nb)
2o
5grade is 11.28%, (Ta, Nb)
2o
5the rate of recovery is the fine fraction tantalum-niobium concentrate of 52.97%.Tantalum niobium flotation tailing is after 30% through the concentrated mass concentration that is adjusted to, and adds sulfuric acid and is adjusted to pH values of pulp=3, in ore pulp quality, and successively add activator hydrofluoric acid 500g/t, collecting agent lauryl amine 60g/t, carries out feldspar flotation, obtains containing Rb through one roughing, once purging selection, primary cleaning
2o grade is feldspar concentrate and the mine tailing of 0.27%.
Embodiment three
Essential mineral in Inner Mongol association tantalum niobium concentrate ore has biotite, zinnwaldite, potassic feldspar, quartz, and tantalum niobium concentrate owner will exist with the form of niobium-tantalum ore, Ta
2o
5grade 70.77g/t, Nb
2o
5grade 135.37g/t, tantalum niobium disseminated grain size thickness great disparity, coarse grain is greater than 0.15mm, and particulate is less than 0.037mm, and also with rare metal lithium, rubidium in ore, lithium is composed to be existed in zinnwaldite, and rubidium is composed to be existed in biotite and potassic feldspar, Rb
2o grade 0.12%, Li
2o grade 0.041%.
This ore carries out tantalum niobium, the recovery process of rare metal is:
1) ore grinding: after raw ore wet-milling is accounted for 45% to fineness-0.074mm, ore milling concentration is 50%; 2) sieve: adopt 140 object sieves to carry out sieve classification to the ore pulp after wet-milling;
3) coarse grain product magnetic separation: on sieve, coarse grain product feeds magnetic field intensity is that the high gradient magnetic separator of 1.6T carries out strong magnetic ore separation, obtains magnetic product and non-magnetic product.
4) heavy-fluid is selected: magnetic product feeds in the separatory funnel that heavy-fluid diiodomethane is housed and carries out heavy-liquid concentration, obtains (Ta, Nb)
2o
5grade is 13.20%, (Ta, Nb)
2o
5the rate of recovery is the coarse grain tantalum-niobium concentrate of 21.89% and contains Rb
2o grade is 0.73%, Li
2o is the mica concentrate (mixture of biotite and zinnwaldite) of 2.75%.
5) fine particle product and non-magnetic product mixing ore grinding: under the non-magnetic product that high-gradient magnetic separation obtains and the sieve that sieve classification obtains, fine particle product feeds ball mill and regrinds, and is milled to fineness and accounts for 60% for-0.074mm.
6) to regrind flotation of ore pulp: regulate pulp density to 35% of regrinding, in ore pulp quality, add butyl xanthate 100g/t, 2
#oil 60g/t carries out sulfide flotation removal of impurities, in sulfide flotation mine tailing ore pulp, add sulfuric acid be adjusted to pH values of pulp=4.5, in ore pulp quality, and add the combined capturing and collecting agent of 50g/t, described combined capturing and collecting agent mass ratio is the collector for columbite-tantalite two banks of 2.5:2.5:2, benzyl hydroximic acid, soybean oleic acid carry out the flotation of tantalum niobium, through one roughing, once purging selection, twice selected acquisition (Ta, Nb)
2o
5grade is 11.13%, (Ta, Nb)
2o
5the rate of recovery is 51.24% fine-graded tantalum-niobium concentrate, tantalum niobium flotation tailing is after 26% through the concentrated mass concentration that is adjusted to, add sulfuric acid and be adjusted to pH values of pulp=2.5, in ore pulp quality, and successively add activator hydrofluoric acid 500g/t, collecting agent lauryl amine 120g/t, carries out feldspar flotation, obtains containing Rb through one roughing, once purging selection, primary cleaning
2o grade is feldspar concentrate and the mine tailing of 0.21%.
Claims (2)
1. a comprehensive recycling process for association tantalum niobium concentrate, comprises the steps:
1) ore grinding: wet-milling after association tantalum niobium concentrate crushing raw ore is accounted for 35% ~ 45% to fineness-0.074mm, and ore milling concentration is 50% ~ 60%;
2) sieve: sieved by the ore pulp after wet-milling, screen size is 0.1mm ~ 0.3mm, obtain the coarse grain product on sieving and the fine particle product under sieve;
3) coarse grain product magnetic separation: described coarse grain product feeds high gradient magnetic separator and carries out high intensity magnetic separation separation, and magnetic field intensity is 1.2T ~ 1.6T, the magnetic product obtained and non-magnetic product; Magnetic product is the bulk concentrate of tantalum niobium and magnetic mica.
4) heavy-fluid is selected: described magnetic product is carried out the selected separation of heavy-fluid, and the heavy-fluid density selected is 2.9g/cm
3~ 5g/cm
3, obtain the mica concentrate of heavy product-coarse grain tantalum-niobium concentrate and the little product of proportion-be rich in rare metal;
5) fine particle product and non-magnetic product mixing ore grinding: non-magnetic product described in fine particle product described in screening gained and magnetic separation gained is regrinded to fineness and account for more than 60% for-0.074mm;
6) to regrind flotation of ore pulp: by step 5) gained regrinds after ore pulp is sized mixing and carries out sulfide flotation, obtains sulphide ore and sulfide flotation mine tailing; Described sulfide flotation mine tailing carries out tantalum niobium concentrate flotation and obtains particulate tantalum-niobium concentrate and tantalum niobium flotation tailing; Described tantalum niobium flotation tailing carries out feldspar ore flotation acquisition and is rich in the feldspar concentrate of rare metal and final flow process mine tailing.
2. the comprehensive recycling process of a kind of association tantalum niobium concentrate as claimed in claim 1, is characterized in that: described step 6) regrind and to regrind after ore pulp adjustment pulp density 30% ~ 35% described in ore pulp ore dressing, add collecting agent butyl xanthate 50 ~ 100g/t, infusion 2
#oil 10 ~ 60g/t, carries out sulfide flotation; Sulfide flotation mine tailing ore pulp is adjusted to pH values of pulp=4 ~ 5, adds combined capturing and collecting agent 30 ~ 100g/t, carry out tantalum niobium concentrate roughly select, scan, selected, component and the quality proportioning thereof of described combined capturing and collecting agent are: two banks 2 ~ 3.5 parts
Benzyl hydroximic acid 1 ~ 2.5 part
Soybean oleic acid 1 ~ 2 part;
It is 25% ~ 33% adjustment pH=2 ~ 3 that tantalum niobium flotation tailing is adjusted to pulp density, adds activator hydrofluoric acid 300 ~ 1000g/t, collecting agent lauryl amine 60 ~ 120g/t, carry out feldspar ore roughly select, scan, selected.
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