CN115212999A - A kind of method for comprehensive utilization of calcification to extract vanadium tailings - Google Patents

Abstract

The invention discloses a method for comprehensively utilizing calcification vanadium extraction tailings, which comprises the following steps: grinding and classifying vanadium extraction tailings; The second grade minerals are subjected to weak magnetic separation treatment to obtain the first tailings and the first concentrate; the first tailings are subjected to strong magnetic separation treatment to obtain the second tailings and the second concentrate; the second tailings are subjected to concentration treatment In order to obtain concentrated ore pulp, the concentrated ore pulp and flotation agent are added into the flotation cell for multiple flotation, so as to finally obtain the third concentrate and the third flotation tailings, the first concentrate, the second concentrate, the third The concentrates are combined into the final concentrate product and the third flotation tailings are the final tailings product. By using the method of the present invention, the final concentrate with high content of TFe and V ₂ O ₅ and low content of S and tailings products with low content of TFe and V ₂ O ₅ and high content of S can be obtained, and the enrichment of Fe and V is achieved and the S content is significant. reduced effect.

Description

A kind of method for comprehensive utilization of calcification to extract vanadium tailings

technical field

The invention relates to the technical field of metal smelting, in particular to a method for comprehensively utilizing calcification to extract vanadium tailings.

Background technique

In the process of research and development of vanadium titanomagnetite, the formed vanadium titanomagnetite concentrate blast furnace smelting - hot metal extraction of vanadium - vanadium slag to produce vanadium oxide process is based on iron smelting as the main process to extract vanadium as a supplement, and it is also the current vanadium smelting process. The most important and economically reasonable process for recovering vanadium from titanomagnetite concentrates. The process was developed after a breakthrough in blast furnace smelting vanadium titanomagnetite technology. Aiming at the vanadium-titanium-magnetite resources in Panxi and Chengde in my country, large-scale steel and vanadium production bases have been established in the above two regions, and both blast furnace-converter dual process is used to produce common steel and vanadium slag. Vanadium slag produced by steelmaking is usually extracted from vanadium _oxide by _{sodiumization} and calcification roasting and leaching process. The main phases of the vanadium extraction tailings are decomposed and oxidized from the spinel phase and olivine phase of the raw slag to hematite, ferrobrookite and pyroxene phases. The main elements are: Fe, Si, Ti, Mn, Al, Ca, Mg, V, Cr, Na. Comprehensive utilization of vanadium extraction tailings can not only recover valuable metals and avoid waste of resources, but also increase economic benefits for enterprises and reduce environmental pollution. The soluble and toxic Cr ⁶⁺ and V ⁵⁺ in the vanadium extraction tailings are the most harmful to human health. If they are stacked directly, they will not only occupy the site, but also need to pour a 200mm thick concrete slag dump, otherwise it will seriously affect the surrounding ecology. surroundings. During the storage period, it is still necessary to carry out regular maintenance on the slag discharge yard to prevent the discharge of waste water and landslides, and the long-term treatment costs are huge. For a long time, many scholars have carried out various researches on the comprehensive utilization of vanadium extraction tailings, mainly focusing on extracting residual vanadium, iron, titanium and gallium from vanadium extraction tailings, preparing vanadium-titanium black porcelain building materials and far-infrared coatings , converter slag making agent, etc.

The tailings after vanadium calcification extraction with vanadium titanomagnetite contain TFe 30%±, TiO ₂ 9%±, V ₂ O ₅ 1.5%±, S6%±, CaO 12%±, MgO 2%±, SiO ₂ 15 %±, because of its high S content and low TFe and V content, it limits its comprehensive utilization and causes the cost of secondary recovery of V to be high.

Therefore, there is a need for an improved method for comprehensively utilizing calcification to extract vanadium tailings in the prior art.

SUMMARY OF THE INVENTION

In view of this, the purpose of the embodiment of the present invention is to propose a kind of method for comprehensive utilization of calcification vanadium extraction tailings, and adopting this method can realize that the grades of valuable components such as _TFe and _V2O5 in the calcification vanadium extraction tailings can be significantly improved. , laying the foundation for further economic utilization.

Based on the above purpose, the embodiment of the present invention provides a method for comprehensively utilizing calcification to extract vanadium tailings, and the method comprises the following steps:

Grinding and grading the vanadium extraction tailings, after grading, the first graded minerals are obtained on the screen, and the second graded minerals are obtained under the screen;

performing weak magnetic separation treatment on the second graded minerals to obtain the first tailings and the first concentrate;

The first tailings are subjected to intensive magnetic separation treatment to obtain the second tailings and the second concentrate;

Concentrate the second tailings to obtain concentrated pulp, add the concentrated pulp and flotation reagents into the flotation tank for flotation, scrape out the foam as the first flotation tailings, add flotation reagents twice, and scrape them separately. The froth is the first medium ore and the second medium ore, and the third concentrate is left in the flotation tank. The first flotation tailings are added to the flotation tank, soluble starch is added, and the froth is scraped out for the second flotation. The tailings are left in the flotation tank as the third medium ore, the second flotation tailings are added into the flotation tank, soluble starch is added, and the foam is scraped out as the third flotation tailings, which are left in the flotation tank as the third flotation tailings. Fourth China Mine;

Among them, the first concentrate, the second concentrate and the third concentrate are combined into the final concentrate product, and the third flotation tailing is the final tailing product.

In some embodiments, the weak magnetic separation comprises one stage of roughing and one stage of beneficiation to obtain first rougher tailings, first beneficiary tailings and first concentrate, wherein the first rougher tailings and the first Selected tailings are consolidated into the first tailings.

In some embodiments, the magnetic field strength of the weak magnetic separation process is 2500Oe˜3500Oe.

In some embodiments, the strong magnetic separation includes one stage of roughing and one stage of beneficiation to obtain a second rougher tailings, a second beneficiary tailings, and a second concentrate, wherein the second rougher tailings and the second Selected tailings are consolidated into second tailings.

In some embodiments, the magnetic field strength of the strong magnetic separation process is 15000Oe-21000Oe.

In some embodiments, in the grinding treatment, the vanadium extraction tailings are ground to -0.038 mm, accounting for 85% to 90%, and the grinding concentration is 60% to 80%.

In some embodiments, the classification treatment adopts ultrasonic rotary vibrating screen for screening and classification, the ultrasonic frequency is 38KHz, the diameter of the sieve hole is 0.038mm, and the ore feeding concentration is 20% to 40%.

In some embodiments, in the concentration treatment, the concentration of feed ore is 1% to 5%, the concentration of concentrated ore pulp in the underflow is 25% to 35%, and the solid content of the overflow is ≤ 2g/L.

In some embodiments, the flotation reagent includes sulfuric acid, soluble starch, and sodium petroleum sulfonate.

In some embodiments, the first classified mineral is further returned to the grinding process.

The present invention has at least the following beneficial technical effects:

The method of the invention adopts fine grinding - weak magnetic separation to select strong magnetic minerals - weak magnetic separation of tailings to select weak magnetic minerals - strong magnetic separation of tailings to remove minerals with high S content by flotation, thereby obtaining TFe , the final concentrate with high V ₂ O ₅ content and low S content and the tailings product with low TFe and V ₂ O ₅ content and high S content to achieve the effect of Fe, V enrichment and S significantly reduced, in order to utilize vanadium and titanium The foundation for further economic utilization of tailings from magnetite calcification to extract vanadium is laid.

Description of drawings

In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. For those of ordinary skill in the art, other embodiments can also be obtained according to these drawings without creative efforts.

Fig. 1 is the schematic diagram of the method embodiment of the comprehensive utilization of calcification to extract vanadium tailings provided by the invention;

FIG. 2 is a schematic diagram of a specific embodiment of marking process parameters and processes provided by the present invention.

Detailed ways

In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the embodiments of the present invention will be further described in detail below with reference to the specific embodiments and the accompanying drawings.

The terms "comprising" and "having" and any variations thereof in the description and claims of the present invention and the above description of the drawings are intended to cover non-exclusive inclusions; The terms "first", "second", etc. are used to distinguish different objects, rather than to describe a specific order. "Plurality" means two or more, unless expressly specifically limited otherwise.

Furthermore, reference herein to an "embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the present invention. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor a separate or alternative embodiment that is mutually exclusive of other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.

As shown in Figure 1, it is the schematic diagram of the method embodiment of the comprehensive utilization of calcification to extract vanadium tailings provided by the present invention, and the method of the present invention comprises:

S1 grinding treatment - S2 classification treatment - S3 weak magnetic separation treatment - S4 strong magnetic separation treatment - S5 concentration treatment - S6 flotation treatment.

Further, the method of the present invention specifically comprises the following steps:

The vanadium extraction tailings are subjected to grinding treatment, and the vanadium extraction tailings are ground to -0.038mm by vertical stirring ball mill, accounting for 85% to 90%, and the grinding products are added with water and fed into the grading operation;

The vanadium extraction tailings after the grinding treatment are classified, and after classification, the first classified minerals are obtained on the screen, and the second classified minerals are obtained under the screen;

performing weak magnetic separation treatment on the second graded minerals to obtain the first tailings and the first concentrate;

The first tailings are subjected to intensive magnetic separation treatment to obtain the second tailings and the second concentrate;

Concentrate the second tailings to obtain concentrated pulp, add the concentrated pulp and flotation reagents into the flotation tank for flotation, scrape out the foam as the first flotation tailings, add flotation reagents twice, and scrape them separately. The froth is the first medium ore and the second medium ore, and the third concentrate is left in the flotation tank. The first flotation tailings are added to the flotation tank, soluble starch is added, and the froth is scraped out for the second flotation. The tailings are left in the flotation tank as the third medium ore, the second flotation tailings are added into the flotation tank, soluble starch is added, and the foam is scraped out as the third flotation tailings, which are left in the flotation tank as the third flotation tailings. Fourth China Mine;

Among them, the first concentrate, the second concentrate and the third concentrate are combined into the final concentrate product, and the third flotation tailing is the final tailing product.

Further, the grading treatment adopts ultrasonic rotary vibrating screen for screening and classification. The ultrasonic frequency is 38KHz, the sieve diameter is 0.038mm, and the ore feeding concentration is 20% to 40%. .

Further, the weak magnetic separation process selects strong magnetic minerals, the weak magnetic separation feed concentration is 15% to 35%, the fineness is -0.038mm, and the magnetic field strength is 2500Oe to 3500Oe. The magnetic separation process is one stage of roughing and one stage of selection. To obtain the first rougher tailings, the first beneficiary tailings and the first concentrate, wherein the first rougher tailings and the first beneficiary tailings are combined into the first tailings.

Further, the strong magnetic separation process selects weakly magnetic minerals, the strong magnetic separation feed concentration is 15% to 30%, the magnetic field intensity is 15000Oe to 21000Oe, and the strong magnetic separation process is one stage of roughing and one stage of selection, so as to obtain the second roughing process. The tailings, the second beneficiary tailings and the second concentrate, wherein the second rougher tailings and the second beneficiary tailings are combined into the second tailings.

Further, the concentration of the ore feeding in the concentration operation is 1% to 5%, the concentration of the underflow concentrated pulp is 25% to 35%, the solid content of the overflow is ≤2g/L, and the underflow is fed into the flotation.

Further, add the concentrated pulp and flotation reagents into the flotation cell, wherein the flotation reagents include sulfuric acid, soluble starch and sodium petroleum sulfonate, turn on the flotation machine for stirring, and the stirring speed is 1790rad/min. Soak for 6 minutes.

The specific embodiments of the present invention are further described below according to specific embodiments.

The calcification vanadium extraction tailings raw ore sample contains V ₂ O ₅ 1.70%, TFe 25.25%, SiO ₂ 12.32%, CaO 11.22%, MgO 1.35%, Al ₂ O ₃ 1.28%, TiO ₂ 7.50%, MnO 7.43%, S 5.75%, 0-0.074mm in the sample accounts for 76.42%, the ore belongs to the acid leaching tailings of steel-making vanadium slag after calcification and roasting, the particle size is fine, and the powder particles are seriously adhered to iron; iron oxide accounts for 40.49% in the sample , 18.55% iron brookite, 18.86% quartz, 5.83% fayalite, 6.64% pyroxene, 1.53% plagioclase, 2.17% sphene, 2.17% calcium and manganese vanadate mixture, sulfuric acid Calcium accounts for 2.86%; under the electron microscope, the mineral crystal size is relatively fine, showing a microcrystalline-honeycomb-amorphous-structure, the mineral grains are finely embedded, and encapsulation and cementation are common.

The specific test process is as follows:

(1) Add the calcified vanadium extraction tailings to LJM-50L vertical spiral stirring mill, add water to adjust the slurry concentration to 70%, and grind to 0～0.038mm, accounting for 87.63%;

(2) The ground ore is added to the KM-800-4S ultrasonic vibrating screen for screening, and the products on the screen are returned to the LJM-50L vertical spiral stirring mill;

(3) The products under the sieve are fed into the XCRS-ф400×300 drum magnetic separator, and the magnetic field strength is 3000Oe;

(4) The concentrate product is fed into a GMT-6 high-efficiency pulse demagnetizer for demagnetization;

(5) The demagnetized product is fed into the XCRS-ф400×300 drum-type magnetic separator, and the magnetic field intensity is 3000Oe, and the concentrate product 1 is obtained;

(6) The tailings of XCRS-ф400×300 drum magnetic separator and XCRS-ф400×300 drum magnetic separator are fed into XCSQ-50×70 wet magnetic separator;

(7) The magnetic field strength of the XCSQ-50×70 wet magnetic separator is 18000Oe, and the concentrate products are fed into the XCSQ-50×70 wet magnetic separator; the tailings products are fed into the PGKY-1 sedimentation and concentration device;

(8) The magnetic field strength of XCSQ-50×70 wet magnetic separator is 16000Oe, the concentrate product is concentrate, and the tailings product is fed into PGKY-1 type sedimentation and concentration device;

(9) The bottom flow of the sedimentation and concentration device is fed into the XFDIV-1.5L single-cell flotation machine, and the mass concentration of the pulp is adjusted to 30-40%, and the flotation machine is turned on for stirring. The stirring speed is 1790rad/min, and sulfuric acid is added and stirred for 2min. Then add soluble starch and stir for 2 minutes, add sodium petroleum sulfonate and stir for 2 minutes, inflate, and scrape bubbles for 6 minutes to scrape out S-containing tailings 2;

(10) Continue to add sulfuric acid in the single-tank flotation machine and stir for 2 minutes, then add soluble starch and stir for 2 minutes, add sodium petroleum sulfonate and stir for 2 minutes, inflate, and scrape bubbles for 4 minutes, and scrape out S-containing ore 1;

(11) Continue to add soluble starch in the single-tank flotation machine and stir for 2min, add sodium petroleum sulfonate and stir for 2min, inflate, and scrape foam for 3min, scrape out S-containing ore 2, and the product in the tank is concentrate 3;

(12) Add the tailings 2 to the XFDⅣ-1.0L single-tank flotation machine, adjust the slurry level to the standard height, and turn on the flotation machine for stirring. The stirring speed is 1790rad/min. Add soluble starch and stir for 2 minutes, aerate, And scrape bubbles for 5min, scrape out S-containing tailings 3, and the product in the tank is medium ore 3;

(13) Add the tailings 3 to the XFDⅣ-1.0L single-tank flotation machine, adjust the slurry level to the standard height, and turn on the flotation machine for stirring. And scrape bubbles for 4min, scrape out S-containing tailings 4, the product in the tank is medium ore 4;

(14) The medium mine 1 and the medium mine 3 are returned to the operation (9), the medium mine 2 is returned to the operation (10), and the medium mine 4 is returned to the operation (12) to realize the flotation closed circuit. The calcification vanadium extraction tailings undergo a combined process of grinding-classification-weak magnetic separation-strong magnetic separation-flotation to obtain the final concentrate and final tailings (tailings 4) composed of concentrate 1, concentrate 2 and concentrate 3. ), laying the foundation for the economic utilization of tailings from vanadium titanomagnetite calcification to extract vanadium.

The results show that in the example, the calcification vanadium extraction tailings are ground to -0.038mm, and the above equipment and process flow are used (weak magnetic separation: one stage of roughing, one stage of selection, strong magnetic separation: one stage of roughing, one stage of selection, flotation : a closed-circuit process of one-stage roughing, two-stage selection, two-stage scavenging, and return of medium ore in turn), the flotation reagent conditions and process parameters in Figure 2 can obtain a yield of 49.49%, including V ₂ O ₅ 2.83% , TFe40.95%, S 0.25%, V ₂ O ₅ and TFe recoveries are 80.26% and 82.47% of the total vanadium iron concentrate, the concentrate grade is 15.7 percentage points higher than the original ore TFe, and the V ₂ O ₅ grade is 1.13 higher percent; total tailings (tailings) yield 50.51%, containing V ₂ O ₅ 0.59%, TFe 9.87%, S 11.37%.

The above are exemplary embodiments of the present disclosure, but it should be noted that various changes and modifications may be made without departing from the scope of the disclosure of the embodiments of the present invention as defined in the claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements disclosed in the embodiments of the present invention may be described or claimed in the singular, unless explicitly limited to the singular, the plural may also be construed.

It should be understood that, as used herein, the singular form "a" is intended to include the plural form as well, unless the context clearly supports an exception. It will also be understood that "and/or" as used herein is meant to include any and all possible combinations of one or more of the associated listed items.

The above-mentioned embodiments of the present invention disclose the serial numbers of the embodiments only for description, and do not represent the advantages and disadvantages of the embodiments.

Those of ordinary skill in the art should understand that the discussion of any of the above embodiments is only exemplary, and is not intended to imply that the scope (including the claims) disclosed by the embodiments of the present invention is limited to these examples; under the idea of the embodiments of the present invention , the technical features in the above embodiments or different embodiments can also be combined, and there are many other changes in different aspects of the above embodiments of the present invention, which are not provided in detail for the sake of brevity. Therefore, any omission, modification, equivalent replacement, improvement, etc. made within the spirit and principle of the embodiments of the present invention should be included within the protection scope of the embodiments of the present invention.

Claims (10)

1. a method for comprehensive utilization of calcification to carry vanadium tailings, is characterized in that, comprises: Grinding and grading the vanadium extraction tailings, after grading, the first graded minerals are obtained on the screen, and the second graded minerals are obtained under the screen; performing weak magnetic separation treatment on the second classified minerals to obtain first tailings and first concentrate; subjecting the first tailings to intensive magnetic separation to obtain second tailings and a second concentrate; The second tailings are concentrated to obtain concentrated pulp, the concentrated pulp and flotation reagents are added to the flotation tank for flotation, the foam is scraped out to be the first flotation tailings, and the first flotation tailings are added twice. The flotation agent, scraped out the foam respectively, is the first medium ore and the second medium ore, and the third concentrate is left in the flotation tank, and the first flotation tailings are added into the flotation tank, Add soluble starch, scrape out the foam as the second flotation tailings, stay in the flotation tank as the third medium ore, add the second flotation tailings into the flotation tank, add soluble starch, The foam scraped out is the third flotation tailings, and the fourth medium ore is left in the flotation tank; Wherein, the first concentrate, the second concentrate, and the third concentrate are combined into the final concentrate product, and the third flotation tailing is the final tailing product. 2. the method for comprehensively utilizing calcification to extract vanadium tailings according to claim 1, is characterized in that, described weak magnetic separation comprises a section of roughing and a section of beneficiation, to obtain the first roughing tailings, the first beneficiation Tailings and a first concentrate, wherein the first rougher tailings and the first beneficiary tailings are combined into the first tailings. 3 . The method for comprehensively utilizing calcification to extract vanadium tailings according to claim 2 , wherein the magnetic field intensity of the weak magnetic separation treatment is 2500Oe～3500Oe. 4 . 4. the method for comprehensively utilizing calcification to extract vanadium tailings according to claim 1, is characterized in that, described strong magnetic separation comprises a section of roughing and a section of beneficiation, to obtain the second roughing tailings, the second beneficiation Tailings and a second concentrate, wherein the second rougher tailings and the second beneficiary tailings are combined into the second tailings. 5 . The method for comprehensively utilizing calcification to extract vanadium tailings according to claim 4 , wherein the magnetic field intensity of the strong magnetic separation treatment is 15000Oe～21000Oe. 6 . 6. The method for comprehensively utilizing calcification vanadium extraction tailings according to claim 1, characterized in that, in the grinding treatment, the vanadium extraction tailings are ground to -0.038 mm, accounting for 85% to 90%, and the grinding concentration is 85% to 90%. 60% to 80%. 7. the method for comprehensive utilization of calcification to extract vanadium tailings according to claim 1, is characterized in that, described classification treatment adopts ultrasonic vibrating screen to carry out sieving classification, ultrasonic frequency 38KHz, sieve diameter 0.038mm, ore feeding concentration 20% to 40%. 8 . The method for comprehensively utilizing calcification to extract vanadium tailings according to claim 1 , wherein in the concentration treatment, the concentration of feeding ore is 1% to 5%, the concentration of concentrated ore pulp of underflow is 25% to 35%, and the overflow Solid content≤2g/L. 9 . The method for comprehensively utilizing calcification to extract vanadium tailings according to claim 1 , wherein the flotation agent comprises sulfuric acid, soluble starch and sodium petroleum sulfonate. 10 . 10 . The method for comprehensively utilizing calcification to extract vanadium tailings according to claim 1 , wherein the first graded minerals are further returned to the grinding treatment. 11 .

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