Maintaining the main method of beneficiation of tungsten ores and the use of auxiliary dehydration processes in the technological scheme of approx. Methods for processing tungsten concentrates Production structure of the tungsten ore enrichment factory

Main enrichment

For some beneficiation factories, in pre-beneficiation, first Xinhai will use moving screen jigger, and then enter into finishing operations.

Gravity enrichment

For wolframite gravity technology, Xinhai usually uses a gravity process that includes multi-stage jigging, multi-stage table and middling product regrinding. That is, after fine crushing, worthy ores, which, through the classification of a vibrating screen, carry out multi-stage jigging and produce coarse sand from jigging and from gravity. Then ballast jigging products large class will enter the mill for additional grinding. And the fine-grade jigging ballast products will enter the sorting of a multi-stage table through classification, then coarse sand is produced from gravity and from the table, then the tailings from the table will enter the tailings hopper, the middling products from the table are then returned to the stage of the additional grinding cycle, and the gravity coarse sand from the jigging and table will enter into finishing operations.

Cleaning

In the wolframite finishing operation, a combined flotation and gravity enrichment technology or a combined flotation technology - gravity and magnetic enrichment is usually used. At the same time, returns the accompanying item.

The finishing operation usually uses a combined method of flotation and enrichment table and washing of sulfur pyrites through flotation. At the same time, we can enter into the flotation separation of sulfur pyrites. After this, wolframite concentrates are produced, if wolframite concentrates contain scheelite and cassiterite, then wolframite concentrates, scheelite concentrates and cassiterite concentrates are produced through a combined flotation and gravity enrichment technology or a combined gravitational and magnetic flotation technology enrichment.

Fine sludge treatment

The processing method for fine sludge in Xinhai is usually as follows: firstly, desulfurization is carried out, then, according to the properties of the fine sludge and material, gravity, flotation, magnetic and electrical enrichment technology is used, or a combined beneficiation technology of several technologies is used to return tungsten ore, and at the same time time will carry out the utilization of associated ore minerals.

Practical examples

The Xinhai wolframite object was taken as an example; the size distribution of the ore of this mine was inhomogeneous, and the ore was very heavily sludged. The initial technological scheme used by the beneficiation plant, which includes pre-concentration crushing, gravity and refining, due to a number of technological defects, resulted in huge losses of small-grade tungsten ores, high beneficiation costs, such as the poor state of comprehensive beneficiation indicators. In order to improve the wolframite sorting status, this beneficiation plant authorized Xinhai to carry out technical reconstruction tasks. After careful research on the properties of ore and beneficiation technology of this factory, Xinhai optimized the technology for beneficiation of wolframite of this factory and added fine sludge processing technology. and ultimately obtain ideal enrichment rates. The enrichment indicator of the factory before and after the transformation is as follows:

After the transformation, the extraction of tungsten ore increased significantly. And mitigated the effects of fine sludge on the wolframite sorting process, achieved good recovery rate, effectively improved the economic efficiency of the factory.

IRKUTSK STATE TECHNICAL UNIVERSITY

As a manuscript

Artemova Olesya Stanislavovna

DEVELOPMENT OF TECHNOLOGY FOR EXTRACTING TUNGSTEN FROM STANDING TAILS OF THE DZHIDINSK VMK

Specialty 25.00.13- Mineral processing

dissertations for competition scientific degree candidate of technical sciences

Irkutsk 2004

The work was carried out at Irkutsk State Technical University.

Scientific supervisor: Doctor of Technical Sciences,

Professor K.V. Fedotov

Official opponents: Doctor of Technical Sciences,

Professor Yu.P. Morozov

Candidate of Technical Sciences A.Ya. Mashovich

Leading organization: St. Petersburg State

Mining Institute (Technical University)

The defense will take place on December 22, 2004 at /O* hours at a meeting of the dissertation council D 212.073.02 of the Irkutsk State Technical University at the address: 664074, Irkutsk, st. Lermontova, 83, room. K-301

Scientific secretary of the dissertation council, professor

GENERAL DESCRIPTION OF WORK

Relevance of the work. Tungsten alloys are widely used in mechanical engineering, mining, metalworking industry, and in the production of electric lighting equipment. The main consumer of tungsten is metallurgy.

An increase in tungsten production is possible due to the involvement in processing of ores that are complex in composition, difficult to enrich, poor in the content of valuable components and off-balance ores, through the widespread use of gravity enrichment methods.

Involvement in the processing of stale ore dressing tailings Dzhidinsky VMC will solve the current problem of the raw material base, increase the production of in-demand tungsten concentrate and improve environmental situation in the Transbaikal region.

Purpose of the work: to scientifically substantiate, develop and test rational technological methods and modes of enrichment of stale tungsten-containing tailings from the Dzhidinsky VMC.

The idea of ​​the work: to study the relationship between the structural, material and phase compositions of the stale tailings of the Dzhida VMC with their technological properties, which makes it possible to create a technology for processing technogenic raw materials.

The following tasks were solved in the work: to assess the distribution of tungsten throughout the entire space of the main technogenic formation of the Dzhida VMC; study the material composition of the stale tailings of the Dzhizhinsky VMC; study the contrast of stale tailings in the original size in terms of W and 8 (II) content; to study the gravitational enrichment of stale tailings of the Dzhida VMC in various sizes; determine the feasibility of using magnetic enrichment to improve the quality of crude tungsten-containing concentrates; to optimize the technological scheme for the enrichment of technogenic raw materials of the general waste treatment plant of the Dzhida VMC; conduct pilot tests of the developed scheme for extracting W from the stale tailings of the DVMK.

Research methods: spectral, optical, optical-geometric, chemical, mineralogical, phase, gravitational and magnetic methods for analyzing the material composition and technological properties of initial mineral raw materials and enrichment products.

The reliability and validity of scientific statements and conclusions are ensured by a representative volume of laboratory research; confirmed by satisfactory convergence of calculated and experimentally obtained enrichment results, compliance with the results of laboratory and pilot tests.

NATIONAL I LIBRARY I SPEC gLYL!

Scientific novelty:

1. It has been established that technogenic tungsten-containing raw materials of the Dzhida VMC in any size are effectively enriched by the gravitational method.

2. Using generalized gravity concentration curves, the limiting technological indicators for processing stale tailings from the Dzhida VMC of various sizes using the gravity method were determined and the conditions for obtaining waste tailings with minimal tungsten losses were identified.

3. New patterns of separation processes have been established that determine the gravitational enrichment of tungsten-containing technogenic raw materials in a particle size of +0.1 mm.

4. For the stale tailings of the Dzhida VMC, a reliable and significant correlation between the contents of WO3 and S(II) was revealed.

Practical significance: a technology has been developed for the enrichment of stale tailings from the Dzhidinsky VMC, which ensures the effective extraction of tungsten and makes it possible to obtain a standard tungsten concentrate.

Approbation of the work: the main content of the dissertation work and its individual provisions were presented at the annual scientific and technical conferences of the Irkutsk State Technical University (Irkutsk, 2001-2004), the All-Russian school-seminar of young scientists “Leonov Readings - 2004” (Irkutsk , 2004), scientific symposium “Miner’s Week - 2001” (Moscow, 2001), All-Russian scientific and practical conference “New technologies in metallurgy, chemistry, enrichment and ecology” (St. Petersburg, 2004 .), Plaksinsky readings - 2004. The dissertation work was presented in full at the Department of Mineral Processing and Environmental Engineering at ISTU, 2004 and at the Department of Mineral Processing at SPGGI (TU), 2004.

Publications. 8 printed publications have been published on the topic of the dissertation work.

Structure and scope of work. The dissertation consists of an introduction, 3 chapters, a conclusion, 104 bibliographic sources and contains 139 pages, including 14 figures, 27 tables and 3 appendices.

The author expresses deep gratitude to the scientific supervisor, Doctor of Technical Sciences, Prof. K.V. Fedotov for professional and friendly leadership; prof. HE. Belkova - for valuable advice and useful critical comments expressed during the discussion of the dissertation work; G.A. Badenikova - for consulting on the calculation of the technological scheme. The author sincerely thanks the department staff for their comprehensive assistance and support provided during the preparation of the dissertation.

The objective prerequisites for the involvement of man-made formations in production turnover are:

The inevitability of preserving natural resource potential. This is achieved by reducing the extraction of primary mineral resources and reducing the amount of damage caused to the environment;

The need to replace primary resources with secondary ones. Determined by the needs of production for material and raw materials, including those industries whose natural resource base is practically exhausted;

The possibility of using technogenic waste is ensured by the introduction of scientific and technological progress.

Production of products from technogenic deposits, as a rule, is several times cheaper than from raw materials specially mined for this purpose, and is characterized by a quick return on investment.

Ore processing waste storage facilities are objects of increased environmental hazard due to their negative impact on the air basin, underground and surface water, soil cover over vast areas.

Payments for pollution are a form of compensation for economic damage from emissions and discharges of pollutants into the environment natural environment, as well as for the disposal of waste on the territory of the Russian Federation.

The Dzhida ore field belongs to the high-temperature deep hydrothermal quartz-wolframite (or quartz-gübnerite) type of deposits, playing vital role in tungsten mining. The main ore mineral is wolframite, the composition of which ranges from ferberite to pobnerite with all intermediate members of the series. Scheelite is a less common tungstate.

Wolframite ores are enriched mainly by gravity; Gravity methods of wet enrichment are usually used on jigging machines, hydrocyclones and concentration tables. To obtain quality concentrates, magnetic separation is used.

Until 1976, ores at the Dzhida VMC factory were processed according to a two-stage gravity scheme, including heavy-medium concentration in hydrocyclones, two-stage concentration of narrowly classified ore materials on three-deck tables of the SK-22 type, additional grinding and enrichment of industrial products in a separate cycle. The sludge was enriched according to a separate gravitational scheme using domestic and foreign sludge concentration tables.

From 1974 to 1996 Only tungsten ore enrichment tailings were stored. In 1985-86, ores were processed using a gravity-flotation technological scheme. Therefore, gravity enrichment tailings and sulfide flotogravity product were dumped into the main tailings pond. Since the mid-80s, due to the increased flow of ore supplied from the Inkursky mine, the specific gravity large waste

classes, up to 1-3 mm. After the Dzhidinsky GOK was shut down in 1996, the settling pond self-destructed due to evaporation and filtration.

In 2000, the “emergency discharge tailings storage facility” (EDT) was identified as an independent object due to its rather significant difference from the main tailings storage facility in terms of the conditions of occurrence, the scale of reserves, the quality and degree of safety of technogenic sands. Another secondary tailings storage facility is alluvial technogenic sediments (ATS), which include redeposited molybdenum ore flotation tailings in the area of ​​the river valley. Modoncul.

The basic standards for payment for waste disposal within the established limits for the Dzhida VMC are 90,620,000 rubles. Annual environmental damage from land degradation due to the disposal of stale ore processing tailings is estimated at 20,990,200 rubles.

Thus, the involvement of stale ore dressing tailings of the Dzhida VMC in the processing will allow: 1) to solve the problem of the enterprise’s raw material base; 2) increase the production of the sought-after "-concentrate" and 3) improve the environmental situation in the Trans-Baikal region.

Material composition and technological properties of technogenic mineral formation of the Dzhida VMC

Geological sampling of the stale tailings of the Dzhida VMC was carried out. During the inspection of the secondary tailings dump (emergency discharge tailings dump (EDT)), 13 samples were taken. 5 samples were taken from the ATO deposit area. The sampling area of ​​the main tailings dump (MTD) was 1015 thousand m2 (101.5 hectares), 385 private samples were taken. The weight of the selected samples is 5 tons. All selected samples were analyzed for the content of "03 and 8 (I).

OTO, CHAT and ATO were statistically compared in terms of "03" content using the Student's t test. With a confidence level of 95%, it was established: 1) the absence of a significant statistical difference in "03" content between private samples of side tailings; 2) the average results of testing the general waste dumps in terms of content "03 in 1999 and 2000 refer to the same general population; 3) the average results of testing the main and side tailings dumps in terms of content "03 significantly differ from each other and the mineral raw materials of all tailings dumps cannot be processed according to the same technology.

The subject of our research is general relativity.

The material composition of the mineral raw materials of the OTO of the Dzhida VMC was established based on the analysis of ordinary and group technological samples, as well as the products of their processing. Random samples were analyzed for the content of "03 and 8(11). Group samples were used for mineralogical, chemical, phase and sieve analyses.

According to the spectral semi-quantitative analysis of a representative analytical sample, the main useful component - "and minor ones - Pb, Iu, Cu, Au and Content "03 in the form of scheelite were identified

quite stable in all size classes of various sand varieties and averages 0.042-0.044%. The content of WO3 in the form of hübnerite varies in various classes size. High contents of WO3 in the form of hübnerite were observed in particles of +1 mm size (from 0.067 to 0.145%) and especially in the -0.08+0 mm class (from 0.210 to 0.273%). This feature is typical for light and dark sands and is preserved for the average sample.

The results of spectral, chemical, mineralogical and phase analyzes confirm that the properties of hübnerite, as the main mineral form of \UOz, will determine the technology of enrichment of mineral raw materials of the OTO of the Dzhida VMC.

The granulometric characteristics of OTO raw materials with the distribution of tungsten by size class are shown in Fig. 1.2.

It can be seen that the bulk of the OTO sample material (~58%) has a particle size of -1+0.25 mm, 17% each falls on the large (-3+1 mm) and small (-0.25+0.1 mm) classes . The share of material with a particle size of -0.1 mm is about 8%, of which half (4.13%) is of the slurry class -0.044+0 mm.

Tungsten is characterized by a slight fluctuation (0.04-0.05%) in the content in size classes from -3 +1 mm to -0.25+0.1 mm and a sharp increase (up to 0.38%) in the size class -0 .1+0.044 mm. In the slurry class -0.044+0 mm, the tungsten content is reduced to 0.19%. That is, 25.28% of tungsten is concentrated in the -0.1+0.044 mm class with an output of this class of about 4% and 37.58% in the -0.1+0 mm class with an output of this class of 8.37%.

As a result of the analysis of data on the dissemination of hübnerite and scheelite in the OTO mineral raw material of the original size and crushed to - 0.5 mm (see Table 1).

Table 1 - Distribution of grains and intergrowths of pobnerite and scheelite by size class of initial and crushed mineral raw materials _

Size classes, mm Distribution, %

Huebnerite Scheelite

Free grains | Splices Free grains | Splices

OTO material in original size (- 5 +0 mm)

3+1 36,1 63,9 37,2 62,8

1+0,5 53,6 46,4 56,8 43,2

0,5+0,25 79,2 20,8 79,2 20,8

0,25+0,125 88,1 11,9 90,1 9,9

0,125+0,063 93,6 6,4 93,0 7,0

0,063+0 96,0 4,0 97,0 3,0

Amount 62.8 37.2 64.5 35.5

OTO material, crushed to - 0.5 +0 mm

0,5+0,25 71,5 28,5 67,1 32,9

0,25+0,125 75,3 24,7 77,9 22,1

0,125+0,063 89,8 10,2 86,1 13,9

0,063+0 90,4 9,6 99,3 6,7

Amount 80.1 19.9 78.5 21.5

It was concluded that it is necessary to classify deslimed mineral raw materials OTO according to a particle size of 0.1 mm and separate enrichment of the resulting classes. From the large class it is necessary: ​​1) to separate free grains into a rough concentrate, 2) tailings containing intergrowths are subjected to additional grinding, desliming, combining with the desliming class -0.1+0 mm of the original mineral raw material and gravity enrichment to extract fine grains of scheelite and pobnerite into industrial products.

To assess the contrast of OTO mineral raw materials, a technological sample was used, which is a combination of 385 individual samples. The results of fractionation of individual samples according to the content of WO3 and sulfide sulfur are shown in Fig. 3, 4.

0 Y OS 0.2 "l M o l O 2 SS * _ " 8

S(kk|Yupytetr "oknsmm" fr**m.% Contained gulfkshoy

Rice. 3 Conditional contrast curves of the original Fig. 4 Conditional contrast curves of the original

mineral raw materials OTO by content Ch/O) mineral raw materials OTO by content 8 (II)

It was found that the contrast indices for the content of WO3 and S (II) are equal to 0.44 and 0.48, respectively. Taking into account the classification of ores by contrast, the studied mineral raw materials in terms of WO3 and S (II) content belong to the category of non-contrast ores. Radiometric enrichment is not

suitable for extracting tungsten from small-sized stale tailings of the Dzhida VMC.

The results of the correlation analysis, with the help of which a mathematical relationship was revealed between the concentrations of \\Sos and 8 (II) (Stoz = 0»0232 + 0.038C5(u)And r = 0.827; the correlation is valid and reliable), confirm the conclusions about the inappropriateness of using radiometric separation.

The results of the analysis of the separation of OTO mineral grains in heavy liquids prepared on the basis of selenium bromide were used to calculate and construct gravity enrichment curves (Fig. 5), from the form of which, especially the curve, it follows that the OTO of the Dzhida VMC in any size is suitable for mineral raw materials gravity enrichment method.

Taking into account the shortcomings in the use of gravity concentration curves, especially the curve for determining the metal content in floating fractions with a given yield or recovery, generalized gravity concentration curves were constructed (Figure 6), the results of the analysis of which are given in Table. 2.

Table 2 - Forecast technological indicators of enrichment different classes size of stale tailings from the Dzhida VMC using the gravity method_

g Size class, mm Maximum losses \U with tailings, % Tailings yield, % XV content, %

in the tails at the end

3+1 0,0400 25 82,5 0,207 0,1

3+0,5 0,0400 25 84 0,19 0,18

3+0,25 0,0440 25 90 0,15 0,28

3+0,1 0,0416 25 84,5 0,07 0,175

3+0,044 0,0483 25 87 0,064 0,27

1+0,5 0,04 25 84,5 0,16 0,2

1+0,044 0,0500 25 87 0,038 0,29

0,5+0,25 0,05 25 92,5 0,04 0,45

0,5+0,044 0,0552 25 88 0,025 0,365

0,25+0,1 0,03 25 79 0,0108 0,1

0,25+0,044 0,0633 15 78 0,02 0,3

0,1+0,044 0,193 7 82,5 0,018 1,017

In terms of gravity washability, the classes -0.25+0.044 and -0.1+0.044 mm are significantly different from materials of other sizes. The best technological indicators of gravitational enrichment of mineral raw materials are predicted for the size class -0.1+0.044 mm: ^ |*0M4=82.5%, =0.018% and e* =7%.

The results of electromagnetic fractionation of heavy fractions (HF), gravitational analysis using the Sochnev S-5 universal magnet and magnetic separation of HF showed that the total yield of highly magnetic and non-magnetic fractions is 21.47% and the losses in them are 4.5%. Minimum losses "with a non-magnetic fraction and the maximum content" in the combined weakly magnetic product are predicted provided that the separation power in a strong magnetic field has a particle size of -0.1+0 mm.

Rice. 5 Gravity enrichment curves for stale tailings of the Dzhida VMC

e) class -0.1+0.044 mm

Rice. 6 Generalized gravity concentration curves for various size classes of mineral raw materials GTO

Development of a technological scheme for the enrichment of stale ore dressing tailings of the Dzhidinsky VM K

Technological testing results in various ways gravitational enrichment of stale tailings from the OTO of the Dzhida VMC are presented in Table. 3.

Table 3 - Results of testing gravity devices

Comparable technological indicators were obtained for the extraction of WO3 into rough concentrate during the enrichment of unclassified stale tailings using both screw separation and centrifugal separation. Minimal losses of WO3 with tailings were detected during enrichment in a centrifugal concentrator of class -0.1+0 mm.

In table Figure 4 shows the granulometric composition of the rough W-concentrate with a particle size of -0.1+0 mm.

Table 4 - Granulometric composition of rough W-concentrate

Size class, mm Yield of classes, % Content Distribution of AUOz

Absolute Relative, %

1+0,071 13,97 0,11 1,5345 2,046

0,071+0,044 33,64 0,13 4,332 5,831

0,044+0,020 29,26 2,14 62,6164 83,488

0,020+0 23,13 0,28 6,4764 8,635

Total 100.00 0.75 75.0005 100.0

In the concentrate, the main amount of WO3 is in the class -0.044+0.020 mm.

According to mineralogical analysis, compared to the source material, the concentrate contains a higher mass fraction of pobnerite (1.7%) and ore sulfide minerals, especially pyrite (16.33%). The content of rock-forming materials is 76.9%. The quality of rough W-concentrate can be increased by the sequential use of magnetic and centrifugal separation.

The results of testing gravitational devices for extracting >V03 from the tailings of the primary gravitational enrichment of mineral raw materials OTO in a particle size of +0.1 mm (Table 5) have proven that the most effective device is the KKEL80No concentrator

Table 5 - Results of testing gravity devices

Product G,% ßwo>, % rßwo> st">, %

screw separator

Concentrate 19.25 0.12 2.3345 29.55

Tails 80.75 0.07 5.5656 70.45

Initial sample 100.00 0.079 7.9001 100.00

wing gateway

Concentrate 15.75 0.17 2.6750 33.90

Tails 84.25 0.06 5.2880 66.10

Initial sample 100.00 0.08 7.9630 100.00

concentration table

Concentrate 23.73 0.15 3.56 44.50

Tails 76.27 0.06 4.44 55.50

Initial sample 100.00 0.08 8.00 100.00

centrifugal concentrator KC-MD3

Concentrate 39.25 0.175 6.885 85.00

Tails 60.75 0.020 1.215 15.00

Initial sample 100.00 0.081 8.100 100.00

When optimizing the technological scheme for the beneficiation of mineral raw materials of the OTO of the Dzhida VMC, the following were taken into account: 1) technological schemes for processing finely disseminated wolframite ores from domestic and foreign enrichment plants; 2) specifications modern equipment used and its dimensions; 3) the possibility of using the same equipment for simultaneous implementation of two operations, for example, separation of minerals by size and dehydration; 4) economic costs for the hardware design of the technological scheme; 5) the results presented in Chapter 2; 6) GOST requirements for quality tungsten concentrates.

During semi-industrial testing of the developed technology (Figure 7-8 and Table 6), 15 tons of initial mineral raw materials were processed in 24 hours.

results spectral analysis A representative sample of the resulting concentrate confirms that the W-concentrate III of magnetic separation is standard and corresponds to the KVG (T) grade of GOST 213-73.

Fig. 8 Results of technological testing of the scheme for finishing rough concentrates and middling products from the stale tailings of the Dzhida VMC

Table 6 - Results of testing the technological scheme

Product

Conditioned concentrate 0.14 62.700 8.778 49.875

Dump tailings 99.86 0.088 8.822 50.125

Initial ore 100.00 0.176 17.600 100.000

CONCLUSION

The work provides a solution to a pressing scientific and production problem: scientifically substantiated, developed and, to a certain extent, implemented effective technological methods for extracting tungsten from the stale ore dressing tailings of the Dzhida VMC.

The main results of the research, development and their practical implementation are as follows:

The main useful component is tungsten, the content of which stale tailings are a non-contrasting ore, represented mainly by hübnerite, which determines the technological properties of technogenic raw materials. Tungsten is unevenly distributed among size classes and its main amount is concentrated in the size

It has been proven that the only effective method enrichment of W-containing stale tailings of the Dzhida VMC is gravitational. Based on the analysis of generalized gravity enrichment curves for stale W-containing tailings, it was established that dump tailings with minimal tungsten losses are a distinctive feature of the enrichment of technogenic raw materials in a size of -0.1+Ohm. New patterns of separation processes have been established that determine the technological indicators of gravitational enrichment of stale tailings from the Dzhida VMC in a size of +0.1 mm.

It has been proven that among the gravitational devices used in the mining industry for the beneficiation of W-containing ores, the screw separator and the centrifugal concentrator KKEL80N are suitable for maximum extraction of tungsten from the technogenic raw materials of the Dzhida VMC into rough W-concentrates. The effectiveness of using the KKEL80K concentrator has also been confirmed for additional extraction of tungsten from tailings of primary enrichment of technogenic W-containing raw materials in size - 0.1 mm.

3. An optimized technological scheme for the extraction of tungsten from the stale ore dressing tailings of the Dzhidinsky VMC made it possible to obtain a standard W-concentrate, solve the problem of depletion of mineral resources of the Dzhidinsky VMC and reduce negative impact production activities of the enterprise on the environment.

Preferred use of gravity equipment. During semi-industrial testing of the developed technology for extracting tungsten from the stale tailings of the Dzhida VMC, a standard “-concentrate” was obtained with a “03 content of 62.7% with an extraction of 49.9%. The payback period for the processing plant for processing stale tailings from the Dzhida VMC in order to extract tungsten was 0.55 years.

The main provisions of the dissertation work were published in the following works:

1. Fedotov K.V., Artemova O.S., Polinskina I.V. Assessment of the possibility of processing stale tailings of the Dzhida VMC, Ore dressing: Sat. scientific works - Irkutsk: ISTU Publishing House, 2002. - 204 pp., pp. 74-78.

2. Fedotov K.V., Senchenko A.E., Artemova O.S., Polinkina I.V. The use of a centrifugal separator with continuous unloading of concentrate for the extraction of tungsten and gold from the tailings of the Dzhida VMC, Environmental problems and new technologies for complex processing of mineral raw materials: Proceedings of the International Meeting “Plaksin Readings - 2002”. - M.: P99, Publishing House PKTs "Altex", 2002 - 130 p., P.96-97.

3. Zelinskaya E.V., Artemova O.S. The possibility of regulating the selectivity of the action of the collector during the flotation of tungsten-containing ores from stale tailings, Directed changes in the physico-chemical properties of minerals in mineral processing processes (Plaksin Readings), materials of the international meeting. - M.: Altex, 2003. -145 p., pp. 67-68.

4. Fedotov K.V., Artemova O.S. Problems of processing stale tungsten-containing products Modern methods processing of mineral raw materials: Conference materials. Irkutsk: Irk. State Those. Univ., 2004 - 86 s.

5. Artemova O. S., Gaiduk A. A. Extraction of tungsten from stale tailings of the Dzhida tungsten-molybdenum plant. Prospects for the development of technology, ecology and automation of chemical, food and metallurgical industries: Materials of a scientific and practical conference. - Irkutsk: ISTU Publishing House. - 2004 - 100 p.

6. Artemova O.S. Assessment of the uneven distribution of tungsten in the Dzhida tailings dump. Modern methods for assessing the technological properties of mineral raw materials noble metals and diamonds and advanced technologies for their processing (Plaksin Readings): Materials of the international meeting. Irkutsk, September 13-17, 2004 - M.: Altex, 2004. - 232 s.

7. Artemova O.S., Fedotov K.V., Belkova O.N. Prospects for the use of the technogenic deposit of the Dzhidinsky VMC. All-Russian scientific and practical conference “New technologies in metallurgy, chemistry, enrichment and ecology”, St. Petersburg, 2004.

Signed for publication on November 12, 2004. Format 60x84 1/16. Printing paper. Offset printing. Conditional oven l. Academician-ed.l. 125. Circulation 400 copies. Law 460.

ID No. 06506 dated December 26, 2001 Irkutsk State Technical University 664074, Irkutsk, st. Lermontova, 83

RNB Russian Fund

1. IMPORTANCE OF TECHNOGENIC MINERAL RAW MATERIALS

1.1. Mineral resources of the ore industry in the Russian Federation and the tungsten sub-industry

1.2. Technogenic mineral formations. Classification. Need for use

1.3. Technogenic mineral formation of the Dzhida VMC

1.4. Goals and objectives of the study. Research methods. Provisions for defense

2. RESEARCH OF THE SUBSTANTIAL COMPOSITION AND TECHNOLOGICAL PROPERTIES OF STELLED TAILINGS OF THE DZHIDINSK VMK

2.1. Geological testing and evaluation of tungsten distribution

2.2. Material composition of mineral raw materials

2.3. Technological properties of mineral raw materials

2.3.1. Grading

2.3.2. Study of the possibility of radiometric separation of mineral raw materials in the original size

2.3.3. Gravity analysis

2.3.4. Magnetic analysis

3. DEVELOPMENT OF A TECHNOLOGICAL SCHEME FOR THE EXTRACTION OF TUNGSTEN FROM STANDING TAILS OF THE DZHIDINSK VMK

3.1. Technological testing of various gravity devices for the enrichment of stale tailings of various sizes

3.2. Optimization of the general waste processing scheme

3.3. Pilot testing of the developed technological scheme for the enrichment of general waste and an industrial plant

Introduction Dissertation on geosciences, on the topic "Development of technology for extracting tungsten from the stale tailings of the Dzhida VMC"

The sciences of mineral processing are, first of all, aimed at developing the theoretical foundations of mineral separation processes and the creation of processing apparatus, at revealing the relationship between the distribution patterns of components and separation conditions in processing products in order to increase the selectivity and speed of separation, its efficiency and economy, and environmental safety.

Despite significant mineral reserves and a decline in last years resource consumption, depletion of mineral resources is one of the most important problems in Russia. Poor use of resource-saving technologies contributes to large losses of minerals during the extraction and enrichment of raw materials.

An analysis of the development of equipment and technology for mineral processing over the past 10-15 years indicates significant achievements in the domestic fundamental science in the field of knowledge of the main phenomena and patterns in the separation of mineral complexes, which makes it possible to create highly efficient processes and technologies for primary processing ores of complex material composition and, as a result, provide the metallurgical industry with the necessary range and quality of concentrates. At the same time, in our country in comparison with developed foreign countries There is still a significant lag in the development of the machine-building base for the production of main and auxiliary enrichment equipment, in its quality, metal intensity, energy intensity and wear resistance.

In addition, due to the departmental affiliation of mining and processing enterprises, complex raw materials were processed only taking into account the necessary industry needs for a specific metal, which led to the irrational use of natural mineral resources and increased costs for waste storage. Currently, more than 12 billion tons of waste have been accumulated, the content of valuable components in which in some cases exceeds their content in natural deposits.

In addition to the above negative trends, since the 90s, the environmental situation at mining and processing enterprises has sharply worsened (in a number of regions, threatening the existence of not only biota, but also humans), there has been a progressive decline in the production of non-ferrous and ferrous metal ores, mining and chemical raw materials, deterioration in the quality of processed ores and, as a consequence, the involvement in the processing of difficult-to-process ores of complex material composition, characterized by a low content of valuable components, fine dissemination and similar technological properties of minerals. Thus, over the past 20 years, the content of non-ferrous metals in ores has decreased by 1.3-1.5 times, iron by 1.25 times, gold by 1.2 times, the share of difficult ores and coal has increased from 15% to 40% of total mass raw materials supplied for enrichment.

The human impact on the natural environment in the process of economic activity is now becoming global in nature. In terms of the scale of extracted and transported rocks, transformation of the relief, impact on the redistribution and dynamics of surface and groundwater, activation of geochemical transfer, etc. this activity is comparable to geological processes.

The unprecedented scale of extracted mineral resources leads to their rapid depletion, accumulation of large amounts of waste on the Earth’s surface, in the atmosphere and hydrosphere, and gradual degradation natural landscapes, reduction in biodiversity, reduction in the natural potential of territories and their life-supporting functions.

Ore processing waste storage facilities are objects of increased environmental hazard due to their negative impact on the air basin, ground and surface water, and soil cover over vast areas. Along with this, tailings dumps are little-studied technogenic deposits, the use of which will make it possible to obtain additional sources of ore and mineral raw materials while significantly reducing the scale of disturbance of the geological environment in the region.

Production of products from technogenic deposits, as a rule, is several times cheaper than from raw materials specially mined for this purpose, and is characterized by a quick return on investment. However, the complex chemical, mineralogical and granulometric composition of tailings, as well as the wide range of minerals they contain (from main and associated components to the simplest building materials) make it difficult to calculate the total economic effect of their processing and determine an individual approach to the assessment of each tailings.

Consequently, at the moment a number of insoluble contradictions have emerged between the change in the nature of the mineral resource base, i.e. the need to involve difficult-to-process ores and technogenic deposits in the processing, the environmentally aggravated situation in mining regions and the state of technology, technology and organization of primary processing of mineral raw materials.

The issues of using waste from the enrichment of polymetallic, gold-containing and rare metals have both economic and environmental aspects.

In achieving the current level of development of the theory and practice of processing tailings from the enrichment of non-ferrous, rare and precious metal ores, V.A. made a great contribution. Chanturia, V.Z. Kozin, V.M. Avdokhin, S.B. Leonov, J.I.A. Barsky, A.A. Abramov, V.I. Karmazin, S.I. Mitrofanov and others.

Important integral part general strategy of the ore industry, incl. tungsten, is the increased use of ore processing waste as additional sources of ore and mineral raw materials, with a significant reduction in the scale of disturbance of the geological environment in the region and the negative impact on all components environment.

In the field of using ore processing waste, the most important thing is a detailed mineralogical and technological study of each specific, individual technogenic deposit, the results of which will make it possible to develop an effective and environmentally friendly technology for the industrial development of an additional source of ore and mineral raw materials.

The problems considered in the dissertation work were solved in accordance with scientific direction Department of Mineral Processing and Engineering Ecology of Irkutsk State Technical University on the topic “Fundamental and technological research in the field of processing of mineral and technogenic raw materials for the purpose of their integrated use, taking into account environmental problems in complex industrial systems" and paper topic No. 118 "Study of the beneficiation of stale tailings of the Dzhida VMC."

The purpose of the work is to scientifically substantiate, develop and test rational technological methods for the enrichment of stale tungsten-containing tailings from the Dzhida VMC.

The following tasks were solved in the work:

Assess the distribution of tungsten throughout the entire space of the main technogenic formation of the Dzhida VMC;

To study the material composition of the stale tailings of the Dzhizhinsky MMC;

Investigate the contrast of stale tailings in the original size according to the content of W and S (II); to study the gravitational enrichment of stale tailings of the Dzhida VMC in various sizes;

To determine the feasibility of using magnetic enrichment to improve the quality of rough tungsten-containing concentrates;

Optimize the technological scheme for the enrichment of technogenic raw materials of the OTO of the Dzhida VMC; conduct pilot tests of the developed scheme for extracting W from the stale tailings of DVMC;

To develop a circuit diagram of devices for the industrial processing of stale tailings from the Dzhida VMC.

To carry out the research, a representative technological sample of stale tailings from the Dzhida VMC was used.

When solving the formulated problems, the following research methods were used: spectral, optical, chemical, mineralogical, phase, gravitational and magnetic methods for analyzing the material composition and technological properties of the initial mineral raw materials and enrichment products.

The following basic scientific provisions are submitted for defense: The patterns of distribution of initial technogenic mineral raw materials and tungsten by size classes have been established. The need for primary (preliminary) classification by size of 3 mm has been proven.

The quantitative characteristics of the stale ore dressing tailings of the Dzhidinsky VMC in terms of WO3 and sulfide sulfur content have been established. It has been proven that the initial mineral raw materials belong to the category of non-contrasting ores. A reliable and reliable correlation between the contents of WO3 and S (II) was revealed.

Quantitative patterns of gravitational enrichment of stale tailings from the Dzhida VMC have been established. It has been proven that for source material of any size, an effective method for extracting W is gravitational enrichment. Forecast technological indicators of gravitational enrichment of initial mineral raw materials in various sizes have been determined.

Quantitative patterns of distribution of stale ore dressing tailings of the Dzhida VMC into fractions of different specific magnetic susceptibility have been established. The effectiveness of the sequential use of magnetic and centrifugal separation has been proven to improve the quality of rough W-containing products. The technological modes of magnetic separation have been optimized.

Conclusion Dissertation on the topic "Beneficiation of mineral resources", Artemova, Olesya Stanislavovna

The main results of the research, development and their practical implementation are as follows:

1. An analysis of the current situation in the Russian Federation with mineral resources of the ore industry, in particular tungsten, was carried out. Using the example of the Dzhidinsky VMC, it is shown that the problem of involving stale ore dressing tailings in the processing is relevant, having technological, economic and environmental significance.

2. The material composition and technological properties of the main W-containing technogenic formation of the Dzhida VMC have been established.

The main useful component is tungsten, the content of which stale tailings are a non-contrasting ore, represented mainly by hübnerite, which determines the technological properties of technogenic raw materials. Tungsten is unevenly distributed across size classes and its main amount is concentrated in sizes -0.5+0.1 and -0.1+0.02 mm.

It has been proven that the only effective method for enriching W-containing stale tailings of the Dzhida VMC is gravity. Based on the analysis of generalized gravity enrichment curves of stale W-containing tailings, it was established that dump tailings with minimal tungsten losses are a distinctive feature of the enrichment of technogenic raw materials in a size of -0.1+0 mm. New patterns of separation processes have been established that determine the technological indicators of gravitational enrichment of stale tailings from the Dzhida VMC in a size of +0.1 mm.

It has been proven that among the gravitational devices used in the mining industry for the enrichment of W-containing ores, a screw separator and a KNELSON centrifugal concentrator are suitable for maximum extraction of tungsten from the technogenic raw materials of the Dzhida VMC into rough W-concentrates. The effectiveness of using the KNELSON concentrator has also been confirmed for the additional extraction of tungsten from the tailings of the primary enrichment of technogenic W-containing raw materials in a particle size of 0.1 mm.

3. An optimized technological scheme for extracting tungsten from the stale ore dressing tailings of the Dzhidinsky VMC made it possible to obtain a standard W-concentrate, solve the problem of depletion of mineral resources of the Dzhidinsky VMC and reduce the negative impact of the enterprise’s production activities on the environment.

The essential features of the developed technology for extracting tungsten from the stale tailings of the Dzhida VMC are:

Narrow classification by feed size of primary enrichment operations;

Preferred use of gravity equipment.

During semi-industrial testing of the developed technology for extracting tungsten from the stale tailings of the Dzhida VMC, a standard W-concentrate was obtained with a WO3 content of 62.7% with an extraction of 49.9%. The payback period for the processing plant for processing stale tailings from the Dzhida VMC in order to extract tungsten was 0.55 years.

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Tungsten ores in our country were processed at large mining and processing plants (Orlovsky, Lermontovsky, Tyrnauzsky, Primorsky, Dzhidinsky VMK) according to classic technological schemes with multi-stage grinding and enrichment of the material, divided into narrow size classes, usually in two cycles: primary gravity enrichment and finishing of rough concentrates using various methods. This is explained by the low tungsten content in the processed ores (0.1-0.8% WO3) and high requirements for the quality of concentrates. Primary enrichment for coarsely disseminated ores (minus 12+6 mm) was carried out by jigging, and for medium-, finely and finely disseminated ores (minus 2+0.04 mm) screw devices of various modifications and sizes were used.

In 2001, the Dzhidinsky tungsten-molybdenum plant (Buryatia, Zakamensk) ceased its activities, having accumulated a multimillion-dollar volume of sand in the Barun-Narynskoye technogenic tungsten deposit. Since 2011, this deposit has been processed by ZAO Zakamensk at a modular processing plant.

The technological scheme was based on enrichment in two stages on Knelson centrifugal concentrators (CVD-42 for the main operation and CVD-20 for cleaning), additional grinding of middlings and flotation of the collective gravity concentrate to produce KVGF grade concentrate. During operation, a number of factors were noted in the operation of Knelson concentrators that negatively affected the economic performance of sand processing, namely:

High operating costs, incl. energy costs and the cost of spare parts, which, given the remoteness of production from generating facilities and the increased cost of electricity, this factor becomes especially important;

Low degree of extraction of tungsten minerals into gravity concentrate (about 60% from the operation);

The complexity of this equipment in operation: when the material composition of the enriched raw material fluctuates, centrifugal concentrators require intervention in the process and prompt adjustment (changes in the pressure of the burning water, the rotation speed of the enrichment bowl), which leads to fluctuations in the quality characteristics of the resulting gravity concentrates;

Considerable distance from the manufacturer and, as a result, long waiting times for spare parts.

Looking for alternative method gravitational concentration, the Spirit company conducted laboratory tests of the technology screw separation using industrial screw separators SVM-750 and SVSh-750 produced by PC Spirit LLC. Enrichment took place in two operations: main and control, producing three enrichment products - concentrate, middlings and tailings. All enrichment products obtained as a result of the experiment were analyzed in the laboratory of JSC Zakamensk. top scores are presented in table. 1.

Table 1. Results of screw separation in laboratory conditions

The data obtained showed the possibility of using screw separators instead of Knelson concentrators in the primary enrichment operation.

The next stage was to conduct pilot tests on the existing enrichment circuit. An experimental semi-industrial installation was installed with screw devices SVSh-2-750, which were installed in parallel with Knelson CVD-42 concentrators. Enrichment was carried out in one operation, the resulting products were sent further according to the scheme of the existing enrichment plant, and sampling was carried out directly from the enrichment process without stopping the operation of the equipment. The indicators of pilot tests are presented in table. 2.

Table 2. Results of comparative pilot tests of screw devices and centrifugal concentratorsKnelson

The results show that sand enrichment occurs more efficiently using screw devices than centrifugal concentrators. This translates into lower concentrate yield (16.87% vs. 32.26%) with increased recovery (83.13% vs. 67.74%) in the tungsten mineral concentrate. This results in a higher quality WO3 concentrate (0.9% versus 0.42%),

Tungsten is the most refractory metal, melting point 3380°C. And this determines its scope. It is also impossible to build electronics without tungsten; even the filament in a light bulb is tungsten.

And, naturally, the properties of the metal also determine the difficulties in obtaining it...

First, you need to find ore. These are just two minerals - scheelite (calcium tungstate CaWO 4) and wolframite (iron and manganese tungstate - FeWO 4 or MnWO 4). The latter has been known since the 16th century under the name "wolf's foam" - "Spuma lupi" in Latin, or "Wolf Rahm" in German. This mineral accompanies tin ores and interferes with the smelting of tin, turning it into slag. Therefore, it is possible to find it already in antiquity. Rich tungsten ores usually contain 0.2 - 2% tungsten. Tungsten was actually discovered in 1781.

However, this is the easiest thing to find in tungsten mining.
Next, the ore needs to be enriched. There are a bunch of methods and they are all quite complex. First of all, of course. Then - magnetic separation (if we have wolframite with iron tungstate). Next is gravitational separation, because the metal is very heavy and the ore can be washed, much like when mining gold. Nowadays they still use electrostatic separation, but it is unlikely that the method will be useful to the endangered person.

So, we have separated the ore from the gangue. If we have scheelite (CaWO 4), then we can skip the next step, but if we have wolframite, then we need to turn it into scheelite. To do this, tungsten is extracted with a soda solution under pressure and at elevated temperatures (the process takes place in an autoclave), followed by neutralization and precipitation in the form of artificial scheelite, i.e. calcium tungstate.
It is also possible to sinter wolframite with an excess of soda, then we obtain tungstate not of calcium, but of sodium, which for our purposes is not so significant (4FeWO 4 + 4Na 2 CO 3 + O 2 = 4Na 2 WO 4 + 2Fe 2 O 3 + 4CO 2).

The next two stages are leaching with water CaWO 4 -> H 2 WO 4 and decomposition with hot acid.
You can take different acids - hydrochloric (Na 2 WO 4 + 2HCl = H 2 WO 4 + 2NaCl) or nitric.
As a result, tungsten acid is isolated. The latter is calcined or dissolved in an aqueous solution of NH 3, from which paratungstate is crystallized by evaporation.
As a result, it is possible to obtain the main raw material for the production of tungsten - WO 3 trioxide with good purity.

Of course, there is also a method for producing WO 3 using chlorides, when tungsten concentrate is treated with chlorine at elevated temperatures, but this method will not be simple for the outsider.

Tungsten oxides can be used in metallurgy as an alloying additive.

So, we have tungsten trioxide and there is only one step left - reduction to metal.
There are two methods here - reduction with hydrogen and reduction with carbon. In the second case, the coal and the impurities it always contains react with tungsten, forming carbides and other compounds. Therefore, tungsten comes out “dirty”, brittle, and for electronics it is pure that is very desirable, because having only 0.1% iron, tungsten becomes brittle and it is impossible to draw the thinnest wire for incandescent filaments from it.
The coal process also has one more drawback - high temperature: 1300 – 1400°C.

However, production with hydrogen reduction is also not a gift.
The reduction process takes place in special tube furnaces, heated in such a way that as it moves through the tube, the “boat” of WO3 passes through several temperature zones. A stream of dry hydrogen comes towards it. Recovery occurs in both “cold” (450...600°C) and “hot” (750...1100°C) zones; in “cold” ones – to the lower oxide WO 2, then – to the elemental metal. Depending on the temperature and duration of the reaction in the “hot” zone, the purity and grain size of the powdered tungsten released on the walls of the “boat” change.

So, we have obtained pure tungsten metal in the form of a tiny powder.
But this is not yet an ingot of metal from which something can be made. The metal is produced by powder metallurgy. That is, it is first pressed, sintered in a hydrogen atmosphere at a temperature of 1200-1300 °C, then an electric current is passed through it. The metal is heated to 3000 °C, and sintering occurs into a monolithic material.

However, we rather need not ingots or even rods, but thin tungsten wire.
As you yourself understand, here again everything is not so simple.
Wire drawing is carried out at a temperature of 1000°C at the beginning of the process and 400-600°C at the end. In this case, not only the wire, but also the die is heated. Heating is carried out by a gas burner flame or an electric heater.
In this case, after drawing, the tungsten wire is coated with graphite lubricant. The surface of the wire must be cleaned. Cleaning is carried out using annealing, chemical or electrolytic etching, and electrolytic polishing.

As you can see, the task of producing a simple tungsten filament is not as simple as it seems. And only the basic methods are described here; there are probably a lot of pitfalls there.
And, of course, even now tungsten is not a cheap metal. Now one kilogram of tungsten costs more than $50, the same molybdenum is almost two times cheaper.

Actually, there are several uses for tungsten.
Of course, the main ones are radio and electrical engineering, where tungsten wire goes.

The next one is the production of alloy steels, which are distinguished by their particular hardness, elasticity and strength. Added together with chromium to iron, it produces so-called high-speed steels, which retain their hardness and sharpness even when heated. They are used to make cutters, drills, milling cutters, as well as other cutting and drilling tools (in general, drilling tools contain a lot of tungsten).
Tungsten-rhenium alloys are interesting - they are used to make high-temperature thermocouples that operate at temperatures above 2000°C, although only in an inert environment.

Well, and one more thing interesting application- These are tungsten welding electrodes for electric welding. Such electrodes are non-consumable and it is necessary to supply additional metal wire to the welding site to provide a weld pool. Tungsten electrodes are used in argon arc welding - for welding non-ferrous metals such as molybdenum, titanium, nickel, as well as high-alloy steels.

As you can see, tungsten production is not for ancient times.
And why is tungsten there?
Tungsten can only be obtained with the construction of electrical engineering - with the help of electrical engineering and for electrical engineering.
No electricity means no tungsten, but you don’t need it either.

Tungsten minerals and ores

From tungsten minerals practical significance have minerals of the wolframite and scheelite group.

Wolframite (xFeWO4 yMnWO4) is an isomorphic mixture of iron and manganese tungstates. If a mineral contains more than 80% iron, the mineral is called ferberite. If the mineral contains more than 80% manganese, then the mineral is called hubernite.

Scheelite CaWO4 is almost pure calcium tungstate.

Tungsten ores contain small amounts of tungsten. The minimum WO3 content at which their processing is advisable. is 0.14-0.15% for large deposits and 0.4-0.5% for small deposits. In ores, tungsten is accompanied by tin in the form of cassiterite, as well as the minerals molybdenum, bismuth, arsenic and copper. The main gangue rock is silica.

Tungsten ores undergo beneficiation. Wolframite ores are enriched using the gravity method, and scheelite ores are enriched by flotation.

Tungsten ore enrichment schemes are varied and complex. They combine gravitational enrichment with magnetic separation, flotation gravity and flotation. By combining various enrichment methods, concentrates containing up to 55-72% WO3 are obtained from ores. The extraction of tungsten from ore into concentrate is 82-90%.

The composition of tungsten concentrates varies within the following limits,%: WO3-40-72; MnO-0.008-18; SiO2-5-10; Mo-0.008-0.25; S-0.5-4; Sn-0.03-1.5; As-0.01-0.05; P-0.01-0.11; Cu-0.1-0.22.

Technological schemes for processing tungsten concentrates are divided into two groups: alkaline and acidic.

Methods for processing tungsten concentrates

Regardless of the method of processing wolframite and scheelite concentrates, the first stage of their processing is opening, which is the transformation of tungsten minerals into easily soluble chemical compounds.

Wolframite concentrates are opened by sintering or fusion with soda at a temperature of 800-900°C, which is based on chemical reactions:

4FeWO4 + 4Na2CO3 + O2 = 4Na2WO4 + 2Fe2O3 +4CO2 (1)

6MnWO4 + 6Na2CO3 + O2 = 6Na2WO4 + 2Mn3O4 +6CO2 (2)

When sintering scheelite concentrates at a temperature of 800-900°C, the following reactions occur:

CaWO4 + Na2CO3 = Na2WO4+ CaCO3 (3)

CaWO4 + Na2CO3 = Na2WO4+ CaO + CO2 (4)

In order to reduce soda consumption and prevent the formation of free calcium oxide, silica is added to the charge to bind calcium oxide into a sparingly soluble silicate:

2CaWO4 + 2Na2CO3 + SiO2 = 2Na2WO4+ Ca2SiO4 + CO2 (5)

Sintering of scheelite concentrate with soda and silica is carried out in drum furnaces at a temperature of 850-900°C.

The resulting cake (alloy) is leached with water. During leaching, sodium tungstate Na2WO4 and soluble impurities (Na2SiO3, Na2HPO4, Na2AsO4, Na2MoO4, Na2SO4) and excess soda pass into the solution. Leaching is carried out at a temperature of 80-90°C in steel reactors with mechanical stirring, operating in batch mode, or in continuous drum rotary kilns. The recovery of tungsten into the solution is 98-99%. The solution after leaching contains 150-200 g/l WO3. The solution is filtered, and after separating the solid residue, it is sent for purification from silicon, arsenic, phosphorus and molybdenum.

Purification from silicon is based on the hydrolytic decomposition of Na2SiO3 by boiling a solution neutralized at pH = 8-9. Neutralization of excess soda in the solution is carried out hydrochloric acid. As a result of hydrolysis, slightly soluble silicic acid is formed:

Na2SiO3 + 2H2O = 2NaOH + H2SiO3 (6)

To remove phosphorus and arsenic, the method of precipitation of phosphate and arsenate ions in the form of poorly soluble ammonium-magnesium salts is used:

Na2HPO4 + MgCl2+ NH4OH = Mg(NH4)PO4 + 2NaCl + H2O (7)

Na2HAsO4 + MgCl2+ NH4OH = Mg(NH4)AsO4 + 2NaCl + H2O (8)

Purification from molybdenum is based on the decomposition of molybdenum sulfosalt, which is formed when sodium sulfide is added to a solution of sodium tungstate:

Na2MoO4 + 4NaHS = Na2MoS4 + 4NaOH (9)

Upon subsequent acidification of the solution to pH = 2.5-3.0, the sulfosalt is destroyed with the release of slightly soluble molybdenum trisulfide:

Na2MoS4 + 2HCl = MoS3 + 2NaCl + H2S (10)

Calcium tungstate is first precipitated from a purified solution of sodium tungstate using CaCl2:

Na2WO4 + CaCl2 = CaWO4 + 2NaCl. (eleven)

The reaction is carried out in a boiling solution containing 0.3-0.5% alkali

while stirring with a mechanical stirrer. The washed sediment of calcium tungstate in the form of a pulp or paste is subjected to decomposition with hydrochloric acid:

CaWO4 + 2HCl = H2WO4 + CaCl2 (12)

During decomposition, the high acidity of the pulp is maintained at about 90-120 g/l HCl, which ensures the separation of impurities of phosphorus, arsenic and partly molybdenum, which are soluble in hydrochloric acid, from the tungstic acid sediment.

Tungstic acid can also be obtained from a purified solution of sodium tungstate by direct precipitation with hydrochloric acid. When the solution is acidified with hydrochloric acid, H2WO4 precipitates as a result of hydrolysis of sodium tungstate:

Na2WO4 + 2H2O = 2NaOH + H2WO4 (11)

The alkali formed as a result of the hydrolysis reaction reacts with hydrochloric acid:

2NaOH + 2HCl = 2NaCl + 2H2O (12)

The addition of reactions (8.11) and (8.12) gives the total reaction of precipitation of tungstic acid with hydrochloric acid:

Na2WO4 + 2HCl = 2NaCl + H2WO4 (13)

However, in this case, great difficulties arise in washing the sediment from sodium ions. Therefore, at present, the latter method of tungstic acid deposition is used very rarely.

The technical tungstic acid obtained by precipitation contains impurities and therefore needs to be purified.

The most widely used method is the ammonia method for purifying technical tungsten acid. It is based on the fact that tungstic acid is highly soluble in ammonia solutions, while a significant part of the impurities it contains are insoluble in ammonia solutions:

H2WO4 + 2NH4OH = (NH4)2WO4 + 2H2O (14)

Ammonia solutions of tungstic acid may contain impurities of molybdenum and alkali metal salts.

Deeper cleaning is achieved by isolating large crystals of ammonium paratungstate from the ammonia solution, which are obtained by evaporating the solution:

12(NH4)2WO4 = (NH4)10W12O41 5H2O + 14NH3 + 2H2O (15)

tungsten acid anhydride precipitation

Deeper crystallization is impractical to avoid contamination of the crystals with impurities. From the mother liquor, enriched with impurities, tungsten is precipitated in the form of CaWO4 or H2WO4 and returned to the previous stages.

Paratungstate crystals are squeezed out on filters, then in a centrifuge, washed cold water and dry.

Tungsten oxide WO3 is obtained by calcining tungstic acid or paratungstate in a rotating tubular furnace with a stainless steel pipe and heated by electricity at a temperature of 500-850oC:

H2WO4 = WO3 + H2O (16)

(NH4)10W12O41 5H2O = 12WO3 + 10NH3 +10H2O (17)

In tungsten trioxide intended for the production of tungsten, the WO3 content must be no lower than 99.95%, and for the production of hard alloys - no lower than 99.9%