A reagent and method for removing potassium feldspar in collophanite by step flotation to reduce potassium content

Abstract

The present application belongs to the field of phosphate rock flotation, and particularly relates to a medicament and method for removing potassium feldspar in collophanite by step-by-step flotation to reduce potassium content. The present application realizes the removal of potassium feldspar in collophanite by two-stage grinding and fine column machine combined step-by-step flotation, that is, for fine particle mineral particles, a dispersing agent is first used to fully disperse the mineral, then a selective stronger collector is added, and at the same time, a filling type micro-bubble countercurrent contact flotation column is used to reduce the bubble size, improve the collision probability of micro-fine particle potassium feldspar and bubbles, and realize high-efficiency flotation of micro-fine particle potassium feldspar. The two-stage grinding avoids the over-grinding to cause the deterioration of the froth phenomenon. For the roughing concentrate slurry, a modified compound collector is added to improve the flotation froth stability and enhance the collecting performance. The added ultrasonic device can efficiently break the froth and facilitate the transfer of the slurry. The present application can realize the sufficient removal of potassium feldspar in collophanite, and the flotation process is stable, simple and efficient in the recovery of phosphate rock resources.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of phosphate rock flotation, and particularly relates to a reagent and method for removing potassium feldspar in collophanite by step-by-step flotation to reduce potassium content. BACKGROUND

[0002] Phosphate rock is an important non-metallic mineral resource which is non-renewable and irreplaceable, and is widely used in agriculture, medicine, food, national defense, sugar production, new energy and other fields.

[0003] The mineral dissemination size of medium and low grade collophanite is fine, and the paragenetic relationship is complex, so fine grinding is often needed to realize the monomer liberation of useful minerals and gangue minerals. A large amount of fine particles are easily produced in the grinding process, which will have adverse effects on subsequent flotation, such as large amount of reagent adsorption, serious mechanical entrainment, small collision probability of mineral particles and reagents, and also cause the phenomenon of sticky and over-stable flotation froth and easy tank overflow. The traditional process generally uses methods such as screening, hydrocyclone or magnetic separation to separate the fine and coarse particle levels and then carries out flotation, but this process flow is complex, and a large amount of manpower and material resources need to be invested in industrial application, and the flotation cost is high. Potassium feldspar is a potassium-containing aluminosilicate mineral, and in the production process of phosphoric acid, K + The reaction generates K2SiF6 which is precipitated in the form of crystalline material on the filtration vacuum system and acid conveying pipeline of the phosphoric acid device, which is easy to cause pipeline and equipment scaling and blockage, and is not conducive to the production of phosphoric acid. In the traditional process, a single cationic amine collector is usually used for the removal of potassium feldspar, but the amine collector has strong collecting property but poor selectivity. SUMMARY

[0004] In view of the above problems of the prior art, the purpose of the present application is to provide a reagent and method for removing potassium feldspar in phosphate rock by step-by-step flotation to reduce potassium content, which utilizes the difference in the properties of coarse and fine particles of minerals to remove potassium feldspar in steps, and has the advantages of flexible process, low reagent consumption, high recovery rate and the like.

[0005] To solve the above technical problems, the present application adopts the following technical scheme:

[0006] A reagent for removing potassium feldspar in phosphate rock by step-by-step flotation to reduce potassium content, the reagent comprising a collector I and a collector II.

[0007] The collector I is composed of amine reagent, foaming agent, surfactant and low-viscosity hydrocarbon oil in a mass ratio of 43-62:13-27:9-18:7-13, and has strong selectivity and weak collecting ability. The collector I is used for potassium removal roughing in a flotation column, and the addition amount is 50 g / t-100 g / t. The collector I is used for removing fine particles in the flotation column.

[0008] The collector II is composed of amine reagent, surfactant and high viscosity hydrocarbon oil with a mass ratio of 53-76:14-22:12-25, the collector II has weak selectivity and strong collecting ability, and is used in the flotation machine for removing potassium in the rough fraction.

[0009] The collector used in the present application is compounded according to the differences of specific surface area, volume ratio and surface energy of coarse and fine particle size of gangue minerals in collophanite, the collector I is used for fine particle minerals, has relatively strong selectivity and weak collecting ability, and needs to be added with a dispersant for dispersion and inhibition, and then the collector I is removed by using the adsorption difference between useful minerals and gangue minerals in collophanite, the collector II has strong collecting ability and relatively weak selectivity, and has better effect on coarse particle minerals, the present application mixes the components of the collector I and the collector II in a certain ratio to achieve better effect, and makes the interaction between reagents play the maximum role, and has good selectivity and collecting performance.

[0010] In the preferred embodiment of the present application, in the collector I, the amine reagent is one of quaternary ammonium salt and condensed amine, the foaming agent is one of pinol oil, methyl isobutyl carbinol, fatty hydrocarbon ester and phenolic alcohol compound, the surfactant is one of Tween 20, Tween 80, Span 80, sodium dodecyl sulfate, sodium fatty acid and sodium dodecyl benzene sulfonate, and the low viscosity hydrocarbon oil is one of lamp kerosene, aviation kerosene, machine oil and paraffin base oil.

[0011] Further preferably, in the collector I, the amine reagent is quaternary ammonium salt or condensed amine, the foaming agent is methyl isobutyl carbinol or pinol oil, and the surfactant is Tween 80, sodium dodecyl sulfate or sodium dodecyl benzene sulfonate.

[0012] In the preferred embodiment of the present application, in the collector II, the amine reagent is one of amine oxide, ether amine and polyamine, the surfactant is one of Tween 80, Span 80, polyoxyethylene ether, ethylene oxide and polyhydric alcohol fatty acid ester, and the high viscosity hydrocarbon oil is one of poly-alpha olefin, light diesel oil, heavy oil and hydrogenated isomerization oil.

[0013] Further preferably, in the collector II, the amine reagent is ether amine or polyamine, the foaming agent is methyl isobutyl carbinol or pinol oil, and the surfactant is Span 80, polyoxyethylene ether or polyhydric alcohol fatty acid ester.

[0014] Another object of the present application is to provide a method for removing potassium feldspar in collophanite by step-by-step flotation to reduce potassium content, and the method uses the reagent described in any one of the above, and the method comprises the following steps:

[0015] The collophanite raw ore is ground, and then water is added to obtain a first slurry, and then a dispersant and a collector I are added to the first slurry, and then the first slurry is subjected to roughing potassium removal in a flotation column to obtain a roughing concentrate slurry and a roughing tailing.

[0016] The roughing concentrate slurry is concentrated, and then second grinding is performed, and then water is added to obtain a second slurry, and then a dispersant and a collector I are added to the second slurry, and then the second slurry is subjected to roughing potassium removal in a flotation column to obtain a first cleaning concentrate and a first cleaning tailing.

[0017] The first cleaning concentrate is subjected to secondary cleaning potassium removal in a flotation machine to obtain a secondary cleaning concentrate and a secondary cleaning tailing.

[0018] The secondary cleaning tailing, the roughing tailing and the first cleaning tailing are combined, and then ultrasonic treatment is performed to eliminate surface foam, and then the combined tailing is subjected to primary scavenging potassium removal to obtain a primary scavenging concentrate and a primary scavenging tailing.

[0019] The primary scavenging tailing is subjected to secondary scavenging potassium removal in a flotation machine to obtain a secondary scavenging concentrate and a secondary scavenging tailing, and the secondary scavenging tailing is a potassium removal tailing product.

[0020] The secondary cleaning concentrate, the primary scavenging concentrate and the secondary scavenging concentrate are combined, and then a pH adjuster and a collector III are added to the combined concentrate to obtain a phosphorus concentrate product and a magnesium removal tailing product.

[0021] In a preferred embodiment of the present application, in the collector III, the fatty acid is one of sodium oleate, oxidized paraffin soap and naphthenic acid, and the surfactant is one of Tween 20, Tween 80, Span 80, cetyltrimethylammonium bromide and sodium dodecyl benzene sulfonate.

[0022] Further preferably, in the collector III, the fatty acid is sodium oleate or naphthenic acid, and the surfactant is cetyltrimethylammonium bromide or sodium dodecyl benzene sulfonate.

[0023] Further preferably, the dispersant is sodium hexametaphosphate or sodium carbonate, and the pH adjuster is phosphoric acid.

[0024] In a preferred embodiment of the present application, the dispersant is one of sodium hexametaphosphate, sodium silicate, sodium carbonate and sodium tripolyphosphate; the collector III is composed of a fatty acid and a surfactant in a mass ratio of 6-12:1; and the pH adjuster is one or both of phosphoric acid and sulfuric acid.

[0025] In the preferred embodiment of the present application, the adding amount of the dispersant in the first slurry and the second slurry is 50 g / t-200 g / t, the adding amount of the collector I in the first slurry and the second slurry is 50 g / t-100 g / t, the adding amount of the collector II is 300 g / t-450 g / t, the adding amount of the collector III is 350 g / t-450 g / t, the adding amount of the pH regulator is 6 kg / t-8 kg / t, the mass concentration of the pH regulator is 10%, and the pH range after adjustment is 3.5-5.5.

[0026] In the preferred embodiment of the present application, the mass percentage concentration of the slurry in the two times of potassium removal roughing is 20%-30%, the mass fraction of the ground collophanite crude ore with a particle size less than 74 μm is 65%-85%, and the mass fraction of the second stage ground collophanite crude ore with a particle size less than 74 μm is 75%-95%.

[0027] In the preferred embodiment of the present application, the flotation column is a filling type micro-bubble reverse flow contact type flotation column, and the flotation machine is an XFD flotation machine.

[0028] In the preferred embodiment of the present application, the ultrasonic treatment adopts an ultrasonic generator and an ultrasonic transducer.

[0029] In the preferred embodiment of the present application, the collophanite is medium-grade collophanite, the P2O5 grade of the collophanite is 25%-30%, the K2O grade is 1%-3%, the SiO2 grade is 12%-23%, and the MgO grade is 1%-3%.

[0030] Compared with the prior art, the present application has the beneficial effects that:

[0031] 0、The collector used in the application is compounded according to the differences of specific surface area, volume and surface energy of coarse and fine particle size of gangue minerals in collophanite, collector I and collector II are added into the flotation column and the flotation machine respectively for roughing and cleaning of potassium removal, collector I is composed of amine reagent, foaming agent, surfactant and hydrocarbon oil with a mass ratio of 43-62:13-27:9-18:7-13, collector I is for fine particle minerals, has relatively strong selectivity and relatively weak collecting ability, and the dosage is small, 50 g / t-100 g / t, a dispersant needs to be added for dispersion and inhibition, then the useful minerals and gangue minerals in collophanite are removed by using the adsorption difference between them, collector II is composed of amine reagent, surfactant and hydrocarbon oil with a mass ratio of 53-76:14-22:12-25, collector II has strong collecting ability and relatively weak selectivity, and is used for cleaning of potassium removal in the flotation machine, the addition amount is 300 g / t-450 g / t, and the effect on coarse particle minerals is better, the components of collector I and collector II are mixed in a certain proportion in the application, better effect is achieved, the interaction between the reagents is maximized, and the application has good selectivity and collecting performance.

[0032] 1、The application realizes accurate removal of potassium feldspar and improves the recovery rate of useful minerals by adjusting the different properties of collectors for column-machine combined flotation according to the different properties of volume, specific surface area and surface energy of coarse and fine particle size; two-stage grinding is adopted, which can realize sufficient dissociation of apatite and potassium feldspar and avoid over-grinding, thereby reducing the pressure of flotation foam and stabilizing the process; the added ultrasonic device can effectively eliminate the foam generated in the reverse flotation and potassium removal process, and is convenient for subsequent potassium removal cleaning.

[0033] 2、The application realizes the removal of potassium feldspar in collophanite by two-stage grinding and fine column-machine combined step-by-step flotation, that is, the dispersant is added to make the mineral fully dispersed, and then the collector with strong selectivity is added, and at the same time, the filling type micro-bubble countercurrent contact flotation column is used to reduce the bubble size and improve the collision probability of micro-fine potassium feldspar and bubbles, thereby realizing high-efficiency flotation of micro-fine potassium feldspar; the two-stage grinding avoids the over-grinding to cause the deterioration of foam; the improved compounded collector is added to the rough concentrate slurry, thereby improving the stability of flotation foam and enhancing the collecting performance; the added ultrasonic device can efficiently break the foam and facilitate the transfer of slurry; in summary, the application can realize the sufficient removal of potassium feldspar in collophanite, the flotation process is stable, simple and convenient, and the phosphorite resources can be efficiently recovered. BRIEF DESCRIPTION OF DRAWINGS

[0034] Figure 1 The process flow chart for removing potassium feldspar in collophanite by step-by-step flotation in the application. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present application will be clearly and completely described in connection with the preferred embodiments and the accompanying drawings, and obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application.

[0036] It should be noted that all the professional terms used in the present application are only for the purpose of describing the specific embodiments, and are not intended to limit the protection scope of the present application. Unless otherwise specified, the various raw materials, reagents, instruments and equipment used in the following embodiments of the present application can be purchased from the market or prepared by the existing method.

[0037] The purpose of the present application is to provide a reagent and method for removing potassium feldspar in collophanite by step flotation to reduce potassium content. First, two-stage grinding is used to avoid over-grinding of ultra-fine particles and reduce the pressure of flotation foam; second, innovative collectors with different properties are used for column-machine combined flotation to remove fine and coarse particles in steps, achieve accurate flotation, reduce reagent consumption and flotation cost; at the same time, the foam generated during the reverse flotation process is eliminated by an ultrasonic device, which facilitates subsequent cleaning and improves the recovery rate of useful minerals.

[0038] Embodiment 1

[0039] For a potassium-aluminum-silicon collophanite in Hubei, the P2O5 grade of the raw ore is 26.83%, the K2O grade is 2.10%, and the MgO grade is 1.42%. The following process is used for treatment:

[0040] (1) The blocky collophanite is crushed to less than 1 mm, ground, and sampled. The grinding fineness is -0.074 mm, accounting for 76.12%. Water is added to adjust the pulp concentration to 25%. Sodium carbonate, a dispersant, is added to the slurry tank at a dosage of 0.06 kg / t, and stirred for 2 min. Collector I is added at a dosage of 0.085 kg / t, and stirred for 1 min before being pumped to the filling type micro-bubble reverse flow contact flotation column for reverse flotation and roughing to obtain a rough concentrate slurry and a rough tailing. The collector I used is a mixture of quaternary ammonium salt, methyl isobutyl carbinol, sodium fatty acid, and machine oil at a mass ratio of 61:17:10:12.

[0041] (2) The rough concentrate slurry is concentrated and subjected to two-stage grinding, with the mass fraction of particles less than 74 μm being 85.54%. Water is added to adjust the pulp mass percentage concentration to 25%, and the slurry and flotation operations in step (1) are repeated for potassium removal and cleaning to obtain a primary cleaning concentrate slurry and a primary cleaning tailing.

[0042] (3) The primary concentration concentrate slurry is added into the flotation machine, collector II is added, the dosage is 0.35 kg / t, stirring for 1 min, and the potassium removal secondary concentration is carried out by reverse flotation to obtain the secondary concentration concentrate and the secondary concentration tailings. The collector II used is a mixture of dodecylamine, Span 80 and light diesel oil with a mass ratio of 70:16:14.

[0043] (4) The secondary concentration tailings obtained above are combined with the roughing tailings and the primary concentration tailings, and ultrasonic equipment is used for ultrasonic treatment for 5 times, 4 seconds each time, and 3 seconds interval. After the surface foam is removed, the potassium removal primary scavenging is carried out to obtain the primary scavenging concentrate and the primary scavenging tailings.

[0044] (5) The primary scavenging tailings are put into the flotation machine for potassium removal secondary scavenging to obtain the secondary scavenging concentrate and the secondary scavenging tailings, which is the final potassium removal tailings product.

[0045] (6) The secondary concentration concentrate, the primary scavenging concentrate and the secondary scavenging concentrate are combined, 10wt% phosphoric acid is added as a pH adjuster, stirring for 1 min, and then collector III is added for reverse flotation to remove magnesium to obtain the phosphate concentrate and the magnesium removal tailings. The collector III used is a mixture of naphthenic acid and cetyltrimethylammonium bromide with a mass ratio of 11:1.

[0046] In example 1, the final P2O5 grade is 32.47%, the K2O grade is 0.79%, the MgO grade is 0.73%, the phosphate concentrate recovery rate is 82.11%, and the separation index is relatively ideal.

[0047] Example 2

[0048] For a potassium-aluminum-silicon colloidal phosphate ore in Hubei, the raw ore P2O5 grade is 26.87%, the K2O grade is 1.57%, and the MgO grade is 1.87%. The ore is processed according to the following process method:

[0049] (1) The blocky colloidal phosphate ore is crushed to below 1 mm, ground and sampled, the grinding fineness is-0.074 mm, accounting for 78.65%, the slurry concentration is adjusted to 20% by adding water, and dispersant sodium hexametaphosphate is added to the slurry, the dosage is 0.06 kg / t, and stirring for 2 min. Collector I is added, the dosage is 0.085 kg / t, and stirring for 1 min, and then the slurry is pumped into the filling type micro-bubble reverse flow contact flotation column for reverse flotation potassium removal roughing to obtain the roughing concentrate slurry and the roughing tailings. The collector I used is a mixture of condensed amine, pine oil, Tween 80 and aviation kerosene with a mass ratio of 57:19:13:11.

[0050] (2) The rough concentrate slurry is concentrated and then ground for a second time until the mass fraction of particles smaller than 74 μm is 83.78%, and then water is added to adjust the mass percentage of the slurry to 25%, and the slurry is subjected to the slurry adjusting and flotation operations of step (1) to perform potassium removal cleaning to obtain a primary cleaning concentrate slurry and a primary cleaning tailing.

[0051] (3) The primary cleaning concentrate slurry is added to a flotation machine, collector II is added in an amount of 0.40 kg / t, and stirring is performed for 1 min to perform reverse flotation potassium removal secondary cleaning to obtain a secondary cleaning concentrate and a secondary cleaning tailing. The collector II used is a mixture of isodecyl oxypropyl propylenediamine, Span 80, and poly-alpha-olefin in a mass ratio of 75:13:11.

[0052] (4) The secondary cleaning tailing obtained above is combined with the rough cleaning tailing and the primary cleaning tailing, and ultrasonic equipment is used to perform ultrasonic treatment for 5 times, 4 seconds each time with an interval of 3 seconds, and then the surface foam is removed to perform potassium removal primary scavenging to obtain a primary scavenging concentrate and a primary scavenging tailing.

[0053] (5) The primary scavenging tailing is added to a flotation machine to perform potassium removal secondary scavenging to obtain a secondary scavenging concentrate and a secondary scavenging tailing, which is the final potassium removal tailing product.

[0054] (6) The secondary cleaning concentrate, the primary scavenging concentrate, and the secondary scavenging concentrate are combined, 10 wt% phosphoric acid is added as a pH adjusting agent, stirring is performed for 1 min, and then collector III is added to perform reverse flotation magnesium removal to obtain a phosphorus concentrate and a magnesium removal tailing. The collector III used is a mixture of sodium oleate and dodecyl benzene sulfonic acid in a mass ratio of 9:1.

[0055] In Example 2, the final P2O5 grade is 30.59%, the K2O grade is 0.98%, the MgO grade is 0.94%, the phosphorus concentrate recovery rate is 88.37%, and the separation index is relatively ideal.

[0056] Example 3

[0057] For a potassium-aluminum-silicon-containing collophanite in Hubei, the raw ore has a P2O5 grade of 26.83%, a K2O grade of 2.10%, and a MgO grade of 1.42%, and is processed according to the following process method:

[0058] (1) The lump collophanite is crushed to below 1 mm, and then ground and sampled. The grinding fineness is -0.074 mm, accounting for 65%, and the pulp concentration is adjusted to 20% by adding water. Sodium carbonate, a dispersant, is added to the pulp conditioning tank in an amount of 0.05 kg / t, and stirred for 2 min. Collector I is added in an amount of 0.050 kg / t, and stirred for 1 min before being pumped into the filling type micro-bubble countercurrent contact flotation column for reverse flotation potassium roughing to obtain a roughing concentrate and a roughing tailing. The collector I used is a mixture of quaternary ammonium salt, methyl isobutyl carbinol, fatty acid sodium and machine oil in a mass ratio of 43:13:9:7.

[0059] (2) The roughing concentrate is concentrated and then subjected to secondary grinding until the mass fraction of particles less than 74 μm is 75%. The pulp is adjusted to a mass percentage concentration of 25% by adding water. The conditioning and flotation operations in step (1) are repeated to perform potassium removal cleaning to obtain a cleaning concentrate and a cleaning tailing.

[0060] (3) The cleaning concentrate is added into a flotation machine, and collector II is added in an amount of 0.30 kg / t, and stirred for 1 min to perform reverse flotation potassium removal cleaning to obtain a cleaning concentrate and a cleaning tailing. The collector II used is a mixture of dodecylamine, Span 80 and light diesel oil in a mass ratio of 53:14:12.

[0061] (4) The cleaning tailing, the roughing tailing and the cleaning tailing are combined, and subjected to ultrasonic treatment for 5 times, each for 4 seconds and with an interval of 3 seconds. After the surface foam is eliminated, the combined tailings are subjected to potassium removal scavenging to obtain a scavenging concentrate and a scavenging tailing.

[0062] (5) The scavenging tailing is subjected to potassium removal scavenging to obtain a scavenging concentrate and a scavenging tailing, which is the final potassium removal tailing product.

[0063] (6) The cleaning concentrate, the scavenging concentrate and the scavenging concentrate are combined, 10 wt% phosphoric acid is added as a pH adjuster, and stirred for 1 min. Collector III is then added to perform reverse flotation magnesium removal to obtain a phosphate concentrate and a magnesium removal tailing. The collector III used is a mixture of naphthenic acid and cetyltrimethylammonium bromide in a mass ratio of 6:1.

[0064] Example 4

[0065] A certain potassium-aluminum-silicon collophanite in Hubei has a P2O5 grade of 26.83%, a K2O grade of 2.10%, and a MgO grade of 1.42%. The ore is processed according to the following process:

[0066] (1) The lump collophanite is crushed to below 1 mm, and then ground and sampled. The grinding fineness is -0.074 mm, accounting for 85%, the pulp concentration is adjusted to 30% by adding water, and then the dispersing agent sodium carbonate is added into the pulp conditioning barrel at a dosage of 0.2 kg / t, and stirred for 2 min. Then the collector I is added at a dosage of 0.1 kg / t, and stirred for 1 min, and then pumped into the filling type micro-bubble reverse flow contact flotation column for reverse flotation potassium roughing to obtain a roughing concentrate and a roughing tailing. The collector I is a mixture of quaternary ammonium salt, methyl isobutyl carbinol, fatty acid sodium and machine oil at a mass ratio of 62:27:18:13.

[0067] (2) The roughing concentrate is concentrated and then subjected to secondary grinding to obtain a mass fraction of less than 74 μm particles of 95%, and then the pulp is adjusted to a mass percentage concentration of 25% by adding water, and then the pulp conditioning and flotation operations in step (1) are repeated to obtain a primary cleaning concentrate and a primary cleaning tailing.

[0068] (3) The primary cleaning concentrate is added into a flotation machine, and the collector II is added at a dosage of 0.45 kg / t, and stirred for 1 min, and then subjected to reverse flotation potassium secondary cleaning to obtain a secondary cleaning concentrate and a secondary cleaning tailing. The collector II is a mixture of dodecylamine, Span 80 and light diesel oil at a mass ratio of 76:22:25.

[0069] (4) The secondary cleaning tailing obtained above is combined with the roughing tailing and the primary cleaning tailing, and subjected to ultrasonic treatment for 5 times, each for 4 seconds and with an interval of 3 seconds, and then subjected to potassium removal once cleaning after the surface foam is eliminated to obtain a once cleaning concentrate and a once cleaning tailing.

[0070] (5) The once cleaning tailing is subjected to potassium removal twice cleaning to obtain a twice cleaning concentrate and a twice cleaning tailing, and the twice cleaning tailing is the final potassium removal tailing product.

[0071] (6) The secondary cleaning concentrate, the once cleaning concentrate and the twice cleaning concentrate are combined, 10 wt% phosphoric acid is added as a pH adjusting agent, and stirred for 1 min, and then the collector III is added for reverse flotation magnesium removal to obtain a phosphate concentrate and a magnesium removal tailing. The collector III is a mixture of naphthenic acid and cetyltrimethylammonium bromide at a mass ratio of 12:1.

[0072] Comparative Example 1

[0073] The one-stage grinding is adopted to obtain a mass fraction of less than 74 μm particles of 76.12%, and the secondary grinding is not performed, and the other steps are the same as those in Example 1. The final P2O5 grade is 28.47%, the K2O grade is 1.15%, and the MgO grade is 0.66%.

[0074] The results show that secondary grinding can realize more complete removal of potassium feldspar, and it is observed that the amount of foam produced by the roughing of the first stage of grinding is too large, which increases the pressure of the subsequent scavenging; in the process of the potassium removal cleaning, the flotation efficiency is obviously reduced, and the concentrate quality is decreased.

[0075] Comparative Example 2

[0076] The dodecylamine, Span 80 and diesel oil in the collector II are mixed in a certain proportion, and the remaining steps are the same as those in Example 2, and finally the P2O5 grade of the phosphate concentrate is 29.24%, the K2O grade is 1.28%, and the MgO grade is 1.04%.

[0077] The results show that the components of the collector need to be mixed in a certain proportion to play a better effect, so that the mutual effect of the reagents can be maximized, and the selectivity and collecting performance are good.

[0078] Comparative Example 3

[0079] The collector II in step (5) is replaced by the collector I, and the remaining step conditions are the same as those in Example 2, and finally the P2O5 grade of the phosphate concentrate is 29.84%, the K2O grade is 1.17%, and the MgO grade is 0.99%.

[0080] The results show that the collector used in the present application is compounded according to the differences in specific surface area, volume and surface energy of the coarse and fine particle size of gangue minerals, the collector I is for fine minerals, has strong selectivity and relatively weak collecting ability, and needs to add a dispersant to play a dispersion inhibition role, and then the useful minerals and gangue minerals are removed by using the adsorption difference between them; the collector II has strong collecting ability and relatively weak selectivity, and has better effect on coarse minerals.

[0081] Comparative Example 4

[0082] The filling type micro-bubble countercurrent contact type flotation column in steps (2) and (4) is replaced by an XFD flotation machine, and the remaining step conditions are the same as those in Example 1, and finally the P2O5 grade of the phosphate concentrate is 30.08%, the K2O grade is 1.03%, and the MgO grade is 0.94%.

[0083] The results show that for the slurry containing fine minerals, the traditional XFD flotation machine is used, the fine minerals are covered without selectivity and are seriously mechanically entrained, which easily causes the tailings yield to be too large, the grade to be increased, and better indexes to be unable to be obtained. In the present application, different types of flotation machines are used in the potassium removal roughing and cleaning according to the differences in volume, surface area and contact mode of coarse and fine particles, different sizes of bubbles are produced, the minerals and reagents are fully contacted, and the problem is effectively solved.

[0084] In summary, the present application grinds the collophanite raw ore, then adds water to make slurry, sequentially adds dispersant, collector I, and pumps to the flotation column for roughing to remove potassium, the roughing concentrate slurry is subjected to secondary grinding, then repeated roughing operation, the obtained slurry is added with collector II for secondary cleaning to remove potassium, then pH regulator and collector III are sequentially added for reverse flotation to remove magnesium, and finally the phosphorus concentrate product and the magnesium-removed tailing product are obtained; the froth product in the reverse flotation process is subjected to ultrasonic defoaming to remove potassium, and then the potassium-removed tailing product is obtained. The present application uses collectors with different properties for column-machine combined flotation, and removes potassium in different steps for coarse and fine particles, and breaks the froth by ultrasonic equipment, which effectively improves the separation in the flotation process, simplifies the process flow, and achieves the purpose of removing potassium feldspar in collophanite to reduce potassium content.

[0085] It should be noted that when the present application involves a numerical range, both endpoints of each numerical range and any number between the two endpoints can be selected. Since the same steps and examples are used, the preferred embodiments are described in the present application to prevent redundancy. Although the preferred embodiments of the present application have been described, those skilled in the art can make additional changes and modifications to the embodiments once they understand the basic inventive concept. Therefore, the appended claims are intended to include the preferred embodiments and all changes and modifications falling within the scope of the present application.

[0086] Obviously, those skilled in the art can make various modifications and variations to the present application without departing from the spirit and scope of the present application. Thus, if these modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application also intends to include these modifications and variations.

Claims

1. A method for reducing the potassium content of potassium feldspar in collophanite by stepwise flotation, characterized in that, The flotation reagent comprises collector I and collector II; The collector I is composed of amine reagent, foaming agent, surfactant and hydrocarbon oil with a mass ratio of 43-62:13-27:9-18:7-13, and is used for adding into the flotation column for roughing of potassium removal, and the adding amount is 50 g / t-100 g / t; The collector II is composed of amine reagent, surfactant and hydrocarbon oil with a mass ratio of 53-76:14-22:12-25, and is used for adding into the flotation machine for cleaning of potassium removal, and the adding amount is 300 g / t-450 g / t; The method comprises the following steps: After grinding the collophanite raw ore, water is added to obtain a first ore slurry, and a dispersing agent and the collector I are added into the first ore slurry in sequence to mix, and roughing of potassium removal is carried out in a flotation column to obtain a roughing concentrate and a roughing tailing; The roughing concentrate is concentrated and then subjected to secondary grinding, water is added to obtain a second ore slurry, and then the dispersing agent and the collector I are added into the second ore slurry to carry out roughing of potassium removal, and a primary cleaning concentrate and a primary cleaning tailing are obtained; The primary cleaning concentrate is added into a flotation machine, the collector II is added to mix to carry out secondary cleaning of potassium removal, and a secondary cleaning concentrate and a secondary cleaning tailing are obtained; The secondary cleaning tailing, the roughing tailing and the primary cleaning tailing are combined, ultrasonic treatment is carried out to eliminate surface foam, and primary scavenging of potassium removal is carried out to obtain a primary scavenging concentrate and a primary scavenging tailing; The primary scavenging tailing is added into a flotation machine to carry out secondary scavenging of potassium removal, and a secondary scavenging concentrate and a secondary scavenging tailing are obtained, and the secondary scavenging tailing is the product of potassium removal tailing.

2. The method for removing potassium feldspar in collophanite by step flotation to reduce potassium content according to claim 1, characterized in that, In the collector I, the amine reagent is one of quaternary ammonium salt and condensed amine, the foaming agent is one of pinol oil, methyl isobutyl carbinol, fatty hydrocarbon ester and phenolic alcohol compound, the surfactant is one of Tween 20, Tween 80, Span 80, sodium dodecyl sulfate, sodium fatty acid and sodium dodecyl benzene sulfonate, and the hydrocarbon oil is one of lamp kerosene, aviation kerosene, machine oil and paraffin base oil.

3. The method for stepwise flotation removal of potassium feldspar to reduce the potassium content in collophanite according to claim 1, characterized in that, In the collector II, the amine reagent is one of amine oxide, ether amine and polyamine, the surfactant is one of Tween 80, Span 80, polyoxyethylene ether, ethylene oxide and polyhydric alcohol fatty acid ester, and the hydrocarbon oil is one of poly-alpha olefin, light diesel oil, heavy petroleum and hydrogenated isomerization oil.

4. The method for stepwise flotation removal of potassium feldspar to reduce the potassium content in collophanite according to claim 1, characterized in that, The dispersing agent is one of sodium hexametaphosphate, sodium silicate, sodium carbonate and sodium tripolyphosphate.

5. The method for stepwise flotation removal of potassium feldspar to reduce the potassium content in collophanite according to claim 1, characterized in that, The adding amount of the dispersing agent in the first ore slurry and the second ore slurry is 50 g / t-200 g / t, the adding amount of the collector I in the first ore slurry and the second ore slurry is 50 g / t-100 g / t, and the adding amount of the collector II is 300 g / t-450 g / t.

6. The method for stepwise flotation removal of potassium feldspar to reduce the potassium content in collophanite according to claim 1, characterized in that, In the two roughing of potassium removal, the mass percentage concentration of the ore slurry is 20%-30%, the collophanite raw ore is ground to a particle size of less than 74 μm, and the mass fraction of the particle is 65%-85%, and the secondary grinding is carried out to a particle size of less than 74 μm, and the mass fraction of the particle is 75%-95%.

7. The method for stepwise flotation removal of potassium feldspar to reduce the potassium content in collophanite according to claim 1, characterized in that, The flotation column is a filling type micro-bubble countercurrent contact type flotation column, and the flotation machine is an XFD flotation machine.

8. The method of stepwise flotation for removal of potassium feldspar from collophanite to reduce the potassium content according to claim 1, characterized in that, The ultrasonic treatment employs an ultrasonic generator and an ultrasonic transducer.

9. The method of stepwise flotation for removal of potassium feldspar from collophanite to reduce the potassium content according to claim 1, characterized in that, The collophanite is medium-grade collophanite, the P2O5 grade of the collophanite is 25-30%, the K2O grade is 1-3%, the SiO2 grade is 12-23%, and the MgO grade is 1-3%.

Images