Method for comprehensive utilization of calcified vanadium tailings

Abstract

The application discloses a method for comprehensively utilizing calcified vanadium extraction tailings, which comprises the following steps: grinding and classifying the vanadium extraction tailings, obtaining first classified minerals on the screen and second classified minerals under the screen after the classification; performing weak magnetic separation on the second classified minerals to obtain first tailings and first concentrates; performing strong magnetic separation on the first tailings to obtain second tailings and second concentrates; performing concentration on the second tailings to obtain concentrated ore slurry; adding the concentrated ore slurry and flotation reagents into a flotation tank to perform multiple times of flotation, so as to finally obtain third concentrates and third flotation tailings; and combining the first concentrates, the second concentrates and the third concentrates into final concentrate products, and taking the third flotation tailings as final tailing products. The method can obtain final concentrates with high TFe and V2O5 contents and low S content and tailing products with low TFe and V2O5 contents and high S content, so that the effect of enriching Fe and V and significantly reducing S is achieved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of metal smelting, and particularly relates to a method for comprehensively utilizing calcified vanadium extraction tailings. BACKGROUND

[0002] In the research and development process of vanadium-titanium magnetite, the process of vanadium-titanium magnetite concentrate blast furnace smelting-vanadium extraction from molten iron-vanadium slag production of vanadium oxide is a process mainly for ironmaking and auxiliary for vanadium extraction, and is currently the most main and economically most reasonable process for recovering vanadium from vanadium-titanium magnetite concentrate. The process is developed after the breakthrough of the technology of smelting vanadium-titanium magnetite in a blast furnace. For the vanadium-titanium magnetite resources in Panxi and Chengde regions of China, large steel and vanadium product production bases have been established in the above two regions, and both of them use the blast furnace-converter combined process to produce general steel and vanadium slag. The vanadium slag produced by steelmaking usually uses sodium calcination and calcification roasting leaching process to extract vanadium oxide, and the leaching residue is the tailings after vanadium extraction. Generally, 10 tons of tailings after vanadium extraction are produced for every 1 ton of V2O5. The main phases of the tailings after vanadium extraction are decomposed and oxidized from the spinel phase and olivine phase of the original slag into hematite, lamellar titanite and augite phase. The main elements are Fe, Si, Ti, Mn, Al, Ca, Mg, V, Cr and Na. Comprehensive utilization of the tailings after vanadium extraction can not only recover the valuable metals therein and avoid resource waste, but also increase the economic benefits of enterprises and reduce environmental pollution. The most harmful elements to human health in the tailings after vanadium extraction are soluble toxic Cr 6+ , V 5+ , etc. If directly stacked, not only the site is occupied, but also a 200mm thick concrete slag discharge field needs to be poured, otherwise the surrounding ecological environment will be seriously affected. During the storage period, the slag discharge field still needs to be regularly maintained to prevent waste water from being discharged and landslides, and the long-term management cost is huge. For a long time, many scholars have conducted researches on the comprehensive utilization of the tailings after vanadium extraction from various aspects, mainly focusing on extracting residual vanadium, iron, titanium and gallium from the tailings after vanadium extraction, and preparing vanadium-titanium black ceramic building materials, far infrared coating and converter slagging agent.

[0003] The tailings after vanadium extraction by calcification of vanadium-titanium magnetite contain TFe 30%±, TiO2 9%±, V2O5 1.5%±, S 6%±, CaO 12%±, MgO 2%± and SiO2 15%±. Due to the high S content, low TFe and V content, the comprehensive utilization way is limited and the cost of secondary recovery of V is relatively high.

[0004] Therefore, there is a need for improvement in the method for comprehensively utilizing the tailings after vanadium extraction by calcification in the prior art. SUMMARY

[0005] Therefore, the embodiment of the present application aims to provide a method for comprehensive utilization of calcified vanadium extraction tailings, which can significantly improve the grade of valuable components such as TFe and V2O5 in the calcified vanadium extraction tailings, and lay a foundation for further economic utilization.

[0006] Based on the above purpose, the embodiment of the present application provides a method for comprehensive utilization of calcified vanadium extraction tailings, which comprises the following steps:

[0007] Grinding and grading treatment is performed on the vanadium extraction tailings, and after grading, a first graded mineral is obtained on the screen, and a second graded mineral is obtained under the screen;

[0008] Weak magnetic separation treatment is performed on the second graded mineral to obtain a first tailing and a first concentrate;

[0009] Strong magnetic separation treatment is performed on the first tailing to obtain a second tailing and a second concentrate;

[0010] Concentration treatment is performed on the second tailing to obtain a concentrated slurry, and the concentrated slurry and a flotation reagent are added into a flotation tank for flotation, and the froth is scraped out as a first flotation tailing, and the flotation reagent is added twice, and the froth is scraped out as a first middling and a second middling, respectively, and is left in the flotation tank as a third concentrate, the first flotation tailing is added into the flotation tank, soluble starch is added, and the froth is scraped out as a second flotation tailing, and is left in the flotation tank as a third middling, the second flotation tailing is added into the flotation tank, soluble starch is added, and the froth is scraped out as a third flotation tailing, and is left in the flotation tank as a fourth middling;

[0011] Among them, the first concentrate, the second concentrate and the third concentrate are combined as a final concentrate product, and the third flotation tailing is a final tailing product.

[0012] In some embodiments, the weak magnetic separation includes one-stage roughing and one-stage cleaning to obtain a first roughing tailing, a first cleaning tailing and a first concentrate, wherein the first roughing tailing and the first cleaning tailing are combined as the first tailing.

[0013] In some embodiments, the magnetic field strength of the weak magnetic separation treatment is 2500 Oe-3500 Oe.

[0014] In some embodiments, the strong magnetic separation includes one-stage roughing and one-stage cleaning to obtain a second roughing tailing, a second cleaning tailing and a second concentrate, wherein the second roughing tailing and the second cleaning tailing are combined as the second tailing.

[0015] In some embodiments, the magnetic field strength of the strong magnetic separation treatment is 15000 Oe-21000 Oe.

[0016] In some embodiments, the grinding treatment grinds the vanadium extraction tailings to-0.038 mm accounting for 85%-90%, and the grinding concentration is 60%-80%.

[0017] In some embodiments, the classification process adopts ultrasonic vibration screen for screening classification, the ultrasonic frequency is 38KHz, the screen hole diameter is 0.038mm, and the feed concentration is 20% to 40%.

[0018] In some embodiments, the feed concentration in the concentration process is 1% to 5%, the concentration of the concentrated slurry of the underflow is 25% to 35%, and the solid content of the overflow is ≤2g / L.

[0019] In some embodiments, the flotation reagent includes sulfuric acid, soluble starch and petroleum sulfonic acid sodium.

[0020] In some embodiments, the first classified mineral further returns to the grinding process.

[0021] The present application has at least the following beneficial technical effects:

[0022] The method of the present application adopts fine grinding-weak magnetic separation to select strong magnetic minerals, the tailings of weak magnetic separation are subjected to strong magnetic separation to select weak magnetic minerals, the tailings of strong magnetic separation are subjected to flotation to remove high-S minerals, thereby obtaining a final concentrate with high TFe and V2O5 contents and low S content and a tailing product with low TFe and V2O5 contents and high S content, achieving the effect of Fe and V enrichment and significant reduction of S, and laying a foundation for further economic utilization of the tailings of the calcification vanadium extraction of vanadium-titanium magnetite. BRIEF DESCRIPTION OF DRAWINGS

[0023] In order to more clearly illustrate the technical solutions of the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and those skilled in the art can also obtain other embodiments according to these drawings without creative labor.

[0024] Figure 1 The schematic diagram of the method for comprehensive utilization of calcification vanadium extraction tailings provided by the present application;

[0025] Figure 2 The schematic diagram of the specific embodiment of the process parameter and flow provided by the present application. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical scheme and advantages of the present application more clear, the following will further describe the embodiments of the present application in combination with specific embodiments and with reference to the drawings.

[0027] The terms "comprise", "comprising", "include", "including", "have", "having" and any variations thereof in the Specification and in the Claims of the present application, as well as in the above Description of the Drawings, are intended to cover a non-exclusive inclusion; the terms "first", "second", and the like in the Specification and in the Claims of the present application, or in the above Description of the Drawings, are used to distinguish between similar objects, not to describe a particular sequential order. The meaning of "a", "an" and "the" include singular and plural references unless expressly limited to one.

[0028] Further, reference being made herein to "embodiments" means that certain features, structures or characteristics described in connection with an embodiment can be included in at least one embodiment of the present application. The occurrence of the phrase "in one embodiment" or other variations thereof in various places throughout the specification does not necessarily refer to the same embodiment, nor does it necessarily refer to a particular combination of features unless otherwise specifically stated. It is expressly understood that the embodiments described herein can be combined with each other in their entirety or with each other in part, unless otherwise specifically noted.

[0029] As Figure 1 is a schematic diagram of an embodiment of the method for comprehensive utilization of vanadium extraction tailings provided by the present application, the method of the present application comprises:

[0030] S1 grinding treatment-S2 classification treatment-S3 low intensity magnetic separation treatment-S4 high intensity magnetic separation treatment-S5 thickening treatment-S6 flotation treatment.

[0031] Further, the method of the present application specifically comprises the following steps:

[0032] Grinding treatment is performed on the vanadium extraction tailings, and the vanadium extraction tailings are ground to 85% to 90% of -0.038 mm by using a vertical stirring ball mill, and the grinding product is fed into a classification operation after being added with water;

[0033] Classification treatment is performed on the vanadium extraction tailings after the grinding treatment, and a first classified mineral is obtained on the screen, and a second classified mineral is obtained under the screen;

[0034] The second classified mineral is subjected to low intensity magnetic separation treatment to obtain a first tailing and a first concentrate;

[0035] The first tailing is subjected to high intensity magnetic separation treatment to obtain a second tailing and a second concentrate;

[0036] The second tailing is subjected to thickening treatment to obtain thickened slurry, and the thickened slurry and a flotation reagent are added into a flotation tank for flotation, and the froth scraped out is a first flotation tailing, and the flotation reagent is added twice, and the froth scraped out is a first middling and a second middling, respectively, and the residue in the flotation tank is a third concentrate, and the first flotation tailing is added into the flotation tank, and soluble starch is added, and the froth scraped out is a second flotation tailing, and the residue in the flotation tank is a third middling, and the second flotation tailing is added into the flotation tank, and soluble starch is added, and the froth scraped out is a third flotation tailing, and the residue in the flotation tank is a fourth middling;

[0037] The first concentrate, the second concentrate and the third concentrate are combined as a final concentrate product, and the third flotation tailings are a final tailings product.

[0038] Further, the classification treatment adopts ultrasonic rotary vibration screen for screening classification, the ultrasonic frequency is 38KHz, the screen hole diameter is 0.038mm, the feed concentration is 20% to 40%, the oversize product is fed into grinding, and the undersize product is fed into weak magnetic separation.

[0039] Further, the weak magnetic separation treatment selects strong magnetic minerals, the weak magnetic separation feed concentration is 15% to 35%, the fineness is-0.038mm, the magnetic field strength is 2500Oe to 3500Oe, and the magnetic separation process is one-stage roughing and one-stage cleaning to obtain first roughing tailings, first cleaning tailings and a first concentrate, wherein the first roughing tailings and the first cleaning tailings are combined as first tailings.

[0040] Further, the strong magnetic separation treatment selects weak magnetic minerals, the strong magnetic separation feed concentration is 15% to 30%, the magnetic field strength is 15000Oe to 21000Oe, and the strong magnetic separation process is one-stage roughing and one-stage cleaning to obtain second roughing tailings, second cleaning tailings and a second concentrate, wherein the second roughing tailings and the second cleaning tailings are combined as second tailings.

[0041] Further, the thickening operation has a feed concentration of 1% to 5%, the underflow thickened slurry has a concentration of 25% to 35%, the overflow has a solid content of ≤2g / L, and the underflow is fed into flotation.

[0042] Further, the thickened slurry and flotation reagents are added into a flotation tank, wherein the flotation reagents include sulfuric acid, soluble starch and petroleum sulfonic acid sodium, the flotation machine is opened for stirring, the stirring speed is 1790rad / min, each time the air is filled and the bubbles are scraped for 6min.

[0043] The specific implementation manner of the present application will be further described below according to specific embodiments.

[0044] The raw ore sample of the calcified vanadium extraction tailing contains V205 1.70%, TFe 25.25%, SiO2 12.32%, CaO 11.22%, MgO 1.35%, Al2O3 1.28%, TiO2 7.50%, MnO 7.43%, S 5.75%, and 0-0.074 mm accounts for 76.42% in the sample. The ore is the tailing of the acid leaching after the calcification roasting of the steelmaking vanadium slag, and the particle size is fine, and the powder particles are seriously adhered to the iron; the oxidized iron accounts for 40.49% in the sample, the iron-platinite accounts for 18.55%, the quartz accounts for 18.86%, the iron olivine accounts for 5.83%, the augite accounts for 6.64%, the anorthite accounts for 1.53%, the wolframite accounts for 2.17%, the calcium manganese vanadate mixture accounts for 2.17%, and the calcium sulfate accounts for 2.86%; under the electron microscope, the mineral crystal particle size is fine, and the structure is microcrystalline-honeycomb-amorphous; the mineral is embedded with fine particle size, and the wrapping and cementation are common.

[0045] The specific test process is as follows:

[0046] (1) The calcified vanadium extraction tailing is added into the LJM-50L vertical spiral stirring mill, water is added to adjust the pulp concentration to 70%, and the grinding is performed to 0-0.038 mm accounts for 87.63%;

[0047] (2) The ground ore is added to the KM-800-4S ultrasonic vibration screen for screening, and the oversize product is returned to the LJM-50L vertical spiral stirring mill;

[0048] (3) The undersize product is fed into the XCRS-ф400×300 drum-type magnetic separator, and the magnetic field strength is 3000 Oe;

[0049] (4) The concentrate product is fed into the GMT-6 high-efficiency pulse demagnetizer for demagnetization;

[0050] (5) The demagnetized product is fed into the XCRS-ф400×300 drum-type magnetic separator, and the magnetic field strength is 3000 Oe, to obtain the concentrate product 1;

[0051] (6) The tailing product of the XCRS-ф400×300 drum-type magnetic separator and the XCRS-ф400×300 drum-type magnetic separator is fed into the XCSQ-50×70 wet high-intensity magnetic separator;

[0052] (7) The magnetic field strength of the XCSQ-50×70 wet high-intensity magnetic separator is 18000 Oe, the concentrate product is fed into the XCSQ-50×70 wet high-intensity magnetic separator, and the tailing product is fed into the PGKY-1 type sedimentation thickener;

[0053] (8) The magnetic field strength of the XCSQ-50×70 wet high-intensity magnetic separator is 16000 Oe, the concentrate product is the concentrate, and the tailing product is fed into the PGKY-1 type sedimentation thickener;

[0054] (9) The underflow of the thickening device is fed into the XFD IV-1.5L single-tank flotation machine, the mass concentration of the ore slurry is adjusted to 30-40%, the flotation machine is opened for stirring, the stirring speed is 1790 rad / min, sulfuric acid is added and stirred for 2 min, soluble starch is added and stirred for 2 min, petroleum sodium sulfonate is added and stirred for 2 min, air is filled, and froth is scraped for 6 min, and S-containing tailings 2 is scraped out;

[0055] (10) Sulfuric acid is continuously added in the single-tank flotation machine and stirred for 2 min, soluble starch is added and stirred for 2 min, petroleum sodium sulfonate is added and stirred for 2 min, air is filled, and froth is scraped for 4 min, and S-containing middlings 1 is scraped out;

[0056] (11) Soluble starch is continuously added in the single-tank flotation machine and stirred for 2 min, petroleum sodium sulfonate is added and stirred for 2 min, air is filled, and froth is scraped for 3 min, and S-containing middlings 2 is scraped out, and the product in the tank is concentrate 3;

[0057] (12) Tailings 2 is added into the XFD IV-1.0L single-tank flotation machine, the liquid level of the ore slurry is adjusted to the standard height, the flotation machine is opened for stirring, the stirring speed is 1790 rad / min, soluble starch is added and stirred for 2 min, air is filled, and froth is scraped for 5 min, and S-containing tailings 3 is scraped out, and the product in the tank is middlings 3;

[0058] (13) Tailings 3 is added into the XFD IV-1.0L single-tank flotation machine, the liquid level of the ore slurry is adjusted to the standard height, the flotation machine is opened for stirring, the stirring speed is 1790 rad / min, soluble starch is added and stirred for 2 min, air is filled, and froth is scraped for 4 min, and S-containing tailings 4 is scraped out, and the product in the tank is middlings 4;

[0059] (14) Middlings 1 and middlings 3 are returned to the operation of (9), middlings 2 is returned to the operation of (10), and middlings 4 is returned to the operation of (12), so as to realize the closed circuit flotation. The tailings after the calciumization vanadium extraction are subjected to the combined process of grinding-classification-weak magnetic separation-strong magnetic separation-flotation, so as to obtain the final concentrate composed of concentrate 1, concentrate 2 and concentrate 3 and the final tailings (tailings 4), which lays a foundation for the economic utilization of the tailings after the calciumization vanadium extraction of the vanadium-titanium magnetite.

[0060] The results show that, in the example, the raw ore of the tailings after the calciumization vanadium extraction is ground to-0.038 mm, the above-mentioned equipment and process flow (weak magnetic separation: one-stage roughing and one-stage cleaning, strong magnetic separation: one-stage roughing and one-stage cleaning, flotation: one-stage roughing, two-stage cleaning, two-stage scavenging, and closed circuit process with the middlings returned in sequence) are adopted, Figure 2The yield of the total vanadium-iron concentrate with V2O52.83%, TFe 40.95%, S 0.25%, V2O5and TFe recovery rate of 80.26% and 82.47% respectively, and the total tailings (tailings) yield of 50.51% with V2O50.59%, TFe 9.87%, S 11.37% can be obtained under the condition of the flotation reagent and the process parameters in the above-mentioned process.

[0061] The above is the exemplary embodiment disclosed by the present application, but it should be noted that various changes and modifications can be made without departing from the scope of the embodiments disclosed by the present application defined by the claims. The functions, steps and / or acts of the method claims described herein need not be performed in any particular order. Furthermore, although elements of the embodiments disclosed by the present application can be described or claimed in individual form, unless explicitly restricted otherwise, they can also be understood as plural.

[0062] It should be understood that, as used herein, the singular forms "a", "an" and "the" are intended to include plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises", "comprising", "includes" and / or "including", as used herein, specify the presence of stated features, integers, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof.

[0063] The above-mentioned embodiment number of the embodiments disclosed by the present application is only for description, not representing the advantages or disadvantages of the embodiments.

[0064] Those skilled in the art should understand that the above discussion of any embodiment is only exemplary, and is not intended to imply that the scope of the embodiments disclosed by the present application (including claims) is limited to these examples; under the idea of the embodiments disclosed by the present application, the above embodiments or technical features in different embodiments can also be combined, and there are many other changes of different aspects of the embodiments disclosed by the present application as above. In order to be brief, they are not provided in details. Therefore, any omission, modification, equivalent replacement, improvement, etc. made within the spirit and principles of the embodiments disclosed by the present application shall be included in the scope of protection of the embodiments disclosed by the present application.

Claims

1. A method for comprehensive utilization of calcified vanadium extraction tailings, characterized in that: include: The vanadium extraction tailings are ground and classified, and after classification, the first-class minerals are obtained on the sieve, and the second-class minerals are obtained under the sieve; performing a weak magnetic separation on the second classified mineral to obtain a first tailing and a first concentrate, wherein the weak magnetic separation includes a roughing stage and a concentrating stage to obtain a first rougher tailing, a first concentrating tailing, and a first concentrate, wherein the first rougher tailing and the first concentrating tailing are combined into the first tailing; Performing high-intensity magnetic separation on the first tailings to obtain second tailings and a second concentrate, wherein the high-intensity magnetic separation includes a roughing stage and a concentrating stage to obtain second rougher tailings, second concentrating tailings and a second concentrate, wherein the second rougher tailings and the second concentrating tailings are combined into the second tailings; The second tailings are concentrated to obtain concentrated slurry, the concentrated slurry and a flotation agent are added to a flotation cell for flotation, and foam is scraped off to obtain a first flotation tailing. The flotation agent is added twice more, and foam is scraped off to obtain a first middling ore and a second middling ore respectively, and the ore remaining in the flotation cell is a third concentrate. The first flotation tailings are added to the flotation cell, soluble starch is added, and foam is scraped off to obtain a second flotation tailing. The ore remaining in the flotation cell is a third middling ore. The second flotation tailings are added to the flotation cell, soluble starch is added, and foam is scraped off to obtain a third flotation tailing. The ore remaining in the flotation cell is a fourth middling ore. The first concentrate, the second concentrate and the third concentrate are combined into the final concentrate product, and the third flotation tailings are the final tailings product.

2. The method for comprehensive utilization of calcified vanadium extraction tailings according to claim 1, characterized in that: The magnetic field strength of the weak magnetic separation treatment is 2500Oe~3500Oe.

3. The method for comprehensive utilization of calcified vanadium extraction tailings according to claim 1, characterized in that: The magnetic field strength of the strong magnetic separation treatment is 15000Oe~21000Oe.

4. The method for comprehensive utilization of calcified vanadium extraction tailings according to claim 1, characterized in that: The grinding process grinds the vanadium extraction tailings to -0.038 mm, accounting for 85% to 90%, and the grinding concentration is 60% to 80%.

5. The method for comprehensive utilization of calcified vanadium extraction tailings according to claim 1, characterized in that: The classification process adopts ultrasonic rotary vibrating screen for screening and classification, with ultrasonic frequency of 38KHz, screen hole diameter of 0.038mm and feed concentration of 20% to 40%.

6. The method for comprehensive utilization of calcified vanadium extraction tailings according to claim 1, characterized in that: In the concentration treatment, the feed concentration is 1% to 5%, the bottom flow concentrated pulp concentration is 25% to 35%, and the overflow solid content is ≤ 2g / L.

7. The method for comprehensive utilization of calcified vanadium extraction tailings according to claim 1, characterized in that: The flotation reagents include sulfuric acid, soluble starch and sodium petroleum sulfonate.

8. The method for comprehensive utilization of calcified vanadium extraction tailings according to claim 1, characterized in that: The first classified minerals are further fed back to the grinding process.

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