Basic tungsten ores and their enrichment. Methods for processing tungsten concentrates. the need to create waste-free technology and thereby prevent environmental pollution from production waste
Magnetic methods are widely used in the beneficiation of ferrous, non-ferrous and rare metal ores and in other areas of industry, including food. They are used for the enrichment of iron, manganese, copper-nickel tungsten ores, as well as for finishing concentrates of rare metal ores, regeneration of ferromagnetic weighting agents in installations for separation in heavy suspensions, for removing iron impurities from quartz sands, pyrite from coal, etc.
All minerals have different specific magnetic susceptibility, and to extract weakly magnetic minerals, fields with high magnetic characteristics are required in the working area of the separator.
In ores of rare metals, in particular tungsten and niobium and tantalum, the main minerals in the form of wolframite and columbite-tantalite have magnetic properties and it is possible to use high-gradient magnetic separation with the extraction of ore minerals into the magnetic fraction.
Tests of tungsten and niobium-tantalum ore from the Spoikoininskoye and Orlovskoye deposits were carried out in the laboratory of magnetic enrichment methods at NPO ERGA. For dry magnetic separation, a roller separator SMVI manufactured by NPO ERGA was used.
The separation of tungsten and niobium-tantalum ore took place according to scheme No. 1. The results are presented in the table.
Based on the results of the work, the following conclusions can be drawn:
The content of useful components in the separation tailings is: WO3 according to the first separation scheme - 0.031±0.011%, according to the second - 0.048±0.013%; Ta 2 O 5 and Nb 2 O 5 -0.005±0.003%. This suggests that the induction in the working area of the separator is sufficient to extract weakly magnetic minerals into the magnetic fraction and a magnetic separator of the SMVI type is suitable for obtaining waste tailings.
Tests of the magnetic separator SMVI were also carried out on baddeleyite ore in order to extract weakly magnetic iron minerals (hematite) into the tailings and purify the zirconium concentrate.
The result of separation was a decrease in the iron content in the non-magnetic product from 5.39% to 0.63% with a recovery of 93%. The zirconium content in the concentrate increased by 12%.
The separator operation diagram is shown in Fig. 1
The use of the SMVI magnetic separator has found wide application in the beneficiation of various ores. SMVI can serve both as the main enrichment equipment and as a finishing device for concentrates. This is confirmed by successful pilot tests of this equipment.
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
dissertation for the degree of 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 of the Dzhida VMC will solve current problem raw material base, increase the production of in-demand tungsten concentrate and improve the environmental situation in the Trans-Baikal 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-huebnerite) type of deposits, which play a critical 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 share of large waste has increased
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 reservoir is alluvial technogenic sediments (ATS), which include redeposited flotation tailings molybdenum ores in the river valley section 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 different size classes. 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 large class should: 1) separate the free grains into a rough concentrate, 2) tailings containing intergrowths should be subjected to additional grinding, desliming, combining with the desliming class -0.1+0 mm of the initial mineral raw material and gravity enrichment to extract fine grains of scheelite and pobnerite into the middling product.
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 of different size classes 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 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 the mineral resources of the Dzhidinsky VMC and reduce the negative impact of the enterprise’s production activities 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. Application of a centrifugal separator with continuous discharge of concentrate for the extraction of tungsten and gold from the tailings of the Dzhidinsky VMC, Environmental problems and new technologies complex processing mineral raw materials: Materials 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. Possibility of regulating the selectivity of the action of the collector during flotation of tungsten-containing ores from stale tailings, Directional change physical and chemical properties minerals in mineral processing processes (Plaksinsky 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 of processing 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-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 mining industry in the Russian Federation and 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 reduction in resource consumption in recent years, the 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 the total mass of raw materials supplied for enrichment.
Human impact on the natural environment in the process economic activity is now becoming global. 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 and accumulation on the Earth's surface, in the atmosphere and hydrosphere large number waste, 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 a wide range of minerals contained in them (from main and associated components to the simplest building materials) make it difficult to calculate the total economic effect from their processing and determine individual approach to the assessment of each tailings dump.
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 huge contribution contributed by V.A. 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 of the 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 the scientific direction of the Department of Mineral Processing and Environmental Engineering 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 on the enrichment 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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Navoi Mining and Metallurgical Plant
Navoi State Mining Institute
"Chemical and Metallurgical" Faculty"
Department of Metallurgy
Explanatory note
for final qualifying work
on the topic of: “Selection, justification and calculation of tungsten-molybdenum ore processing technology”
Graduate: K. Sayfiddinov
Navoi-2014
- Introduction
- 1. General information on methods of beneficiation of tungsten ores
- 2. Enrichment of molybdenum-tungsten ores
- 2. Technological section
- 2.1 Calculation of crushing scheme with equipment selection
- 2.2 Calculation of the grinding scheme
- 2.3 Selection and calculation of semi-autogenous grinding mills
- List of used literature
Introduction
Minerals are the basis of the national economy, and there is not a single industry where minerals or their processed products are not used.
Significant mineral reserves in many deposits of Uzbekistan make it possible to build large, highly mechanized mining, processing and metallurgical enterprises that extract and process many hundreds of millions of tons of minerals with high technical and economic indicators.
The mining industry deals with solid minerals from which, with modern technology, it is advisable to extract metals or other minerals. The main conditions for the development of mineral deposits are increasing their extraction from the subsoil and complex use. This is due to:
- significant material and labor costs during exploration and industrial development of new deposits;
- the growing need of various sectors of the national economy for almost all mineral components that make up the ore;
- the need to create waste-free technology and thereby prevent environmental pollution from production waste.
For these reasons, the possibility of industrial use of a deposit is determined not only by the value and content of the mineral, its reserves, geographical location, mining and transportation conditions, and other economic and political factors, but also by the availability of effective technology for processing the mined ores.
1. General information about methods of beneficiation of tungsten ores
Tungsten ores are enriched, as a rule, in two stages - primary gravity enrichment and finishing of rough concentrates using various methods, which is explained by the low tungsten content in the processed ores (0.2 - 0.8% WO3) and high requirements for the quality of standard concentrates (55 - 65% WO3), The total enrichment degree is approximately 300 - 600.
Wolframite (huebnerite and ferberite) bedrock ores and placers usually contain a number of other heavy minerals, therefore, during the primary gravity enrichment of ores, they strive to isolate collective concentrates, which can contain from 5 to 20% WO3, as well as cassiterite, tantalite-columbite, magnetite, sulfides, etc. When finishing collective concentrates, it is necessary to obtain conditioned monomineral concentrates, for which flotation or flotogravity of sulfides, magnetic separation of magnetite in a weak magnetic field, and wolframite in a stronger one can be used. It is possible to use electric separation, gravitational enrichment on tables, flotation of gangue minerals and other processes to separate minerals so that the finished concentrates meet the requirements of GOSTs and technical specifications not only for the content of the base metal, but also for the content of harmful impurities.
Considering the high density tungsten minerals(6 - 7.5 g/cm 3), during enrichment, gravitational enrichment methods can be successfully used on jigs, concentration tables, sluices, jet and screw separators, etc. When valuable minerals are finely disseminated, flotation or a combination of gravitational processes with flotation is used. Considering the possibility of wolframite sludge during gravitational enrichment, flotation is used as an auxiliary process even when enriching coarsely disseminated wolframite ores for more complete extraction of tungsten from sludge.
If there are large tungsten-rich ore pieces or large pieces of waste rock in the ore, sorting of ore with a particle size of 150 + 50 mm on belt conveyors can be used to separate the rich large-lump concentrate or pieces of rock that dilute the ore supplied for enrichment.
When beneficiating scheelite ores, gravity is also used, but most often a combination of gravity methods with flotation and flotation gravity, or flotation alone.
When sorting scheelite ores, luminescent installations are used. Scheelite, when irradiated with ultraviolet rays, glows with a bright blue light, which makes it possible to separate pieces of scheelite or pieces of waste rock.
Scheelite is an easily floated mineral characterized by high sludge properties. The extraction of scheelite increases significantly with flotation enrichment compared to gravity, therefore, in the enrichment of scheelite ores in the CIS countries, flotation has now begun to be used in all factories.
During the flotation of tungsten ores, a number of difficult technological problems arise that require the correct solution depending on the material composition and association of individual minerals. In the process of flotation of wolframite, hübnerite and ferberite, it is difficult to separate from them iron oxides and hydroxides, tourmaline and other minerals containing neutralize their flotation properties with tungsten minerals.
Flotation of scheelite from ores with calcium-containing minerals (calcite, fluorite, apatite, etc.) is carried out by anionic fatty acid collectors, ensuring their good flotation with calcium cations of scheelite and other calcium-containing minerals. Separation of scheelite from calcium-containing minerals is possible only with the use of such regulators as liquid glass, sodium fluorosilicone, soda, etc.
2. Enrichment of molybdenum-tungsten ores
On Tyrnyauzskaya The factory enriches the molybdenum-tungsten ores of the Tyrnyauz deposit, which are complex in the material composition of not only valuable minerals with very fine dissemination, but also associated gangue minerals. Ore minerals - scheelite (tenths of a percent), molybdenite (hundredths of a percent), powellite, partially ferrimolybdite, chalcopyrite, bismuthite, pyrrhotite, pyrite, arsenopyrite. Nonmetallic minerals - skarns (50-70%), hornfels (21-48%), granite (1 - 12%), marble (0.4-2%), quartz, fluorite, calcite, apatite (3-10%) and etc.
In the upper part of the deposit, 50-60% of molybdenum is represented by powellite and ferrimolybdite, in the lower part their content decreases to 10-20%. Molybdenum is present in scheelite as an isomorphic impurity. Part of the molybdenite, oxidized from the surface, is covered with a film of powellite. Part of the molybdenum grows very finely with molybdoscheelite.
More than 50% of oxidized molybdenum is associated with scheelite in the form of powellite inclusions - a decomposition product of the Ca(W, Mo)O 4 solid solution. Such forms of tungsten and molybdenum can only be isolated into a collective concentrate with subsequent separation by hydrometallurgical methods.
Since 1978, the ore preparation scheme at the factory has been completely reconstructed. Previously, ore, after large crushing at the mine, was transported to the factory in trolleys via an overhead cableway. In the crushing department of the factory, the ore was crushed to - 12 mm, unloaded into bunkers and then crushed in one stage in ball mills operating in a closed cycle with double-spiral classifiers, up to 60% of the class - 0.074 mm.
A new ore preparation technology was developed jointly by the Mekhanobr Institute and the plant and put into operation in August 1978.
The ore preparation scheme provides for coarse crushing of the original ore up to -350 mm, screening according to the 74 mm class, separate storage of each class in bunkers in order to more accurately regulate the supply of large and small classes of ore to the autogenous grinding mill.
Self-grinding of coarse ore (-350 mm) is carried out in Cascade type mills with a diameter of 7 m (MMC-70X X23) with additional grinding of the coarse-grained fraction to 62% class -0.074 mm in MSHR-3600X5000 mills operating in a closed cycle with single-spiral classifiers 1KSN-3 and located in a new building on the mountainside at an elevation of about 2000 m above sea level between the mine and the operating factory.
The finished product is supplied from the autogenous vessel to flotation by hydraulic transport. The hydraulic transport route is a unique engineering structure, ensuring the transportation of pulp with a height difference of more than 600 m. It consists of two pipelines with a diameter of 630 mm, a length of 1750 m, equipped with stilling wells with a diameter of 1620 mm and a height of 5 m (126 wells for each pipeline).
The use of a hydraulic transport system made it possible to eliminate the cargo ropeway workshop, the medium and fine crushing building, and the MShR-3200X2100 mills at the processing plant. In the main building of the factory, two main flotation sections, new scheelite and molybdenum finishing departments, a liquid glass melting shop, and recycling water supply systems were built and put into operation. The thickening front for rough flotation concentrates and middlings has been significantly expanded due to the installation of thickeners with a diameter of 30 m, which reduces losses from thickening discharges.
The newly commissioned facilities are equipped with modern automated process control systems and local automation systems. Thus, in the autogenous building the automatic control system operates in direct control mode based on M-6000 computers. In the main building, a system for centralized control of the material composition of the pulp was introduced using X-ray spectral analyzers KRF-17 and KRF-18 in combination with an M-6000 computer. An automated system for sampling and delivery of samples (by pneumatic mail) to the express laboratory, controlled by the KM-2101 computer complex and issuing analyzes by teletype, has been mastered.
One of the most complex processing processes - finishing rough scheelite concentrates according to the method of N. S. Petrov - is equipped with an automatic monitoring and control system, which can work either in the “advisor” mode to the flotation operator, or in the mode of direct control of the process, regulating the flow rate of the suppressor (liquid glass), pulp level in cleaning operations and other process parameters.
The sulfide minerals flotation cycle is equipped with automatic control and dosing systems for collector (butyl xanthate) and suppressor (sodium sulfide) in the copper-molybdenum flotation cycle. The systems operate using ion-selective electrodes as sensors.
Due to the increase in production volume, the factory switched to processing new varieties of ores, characterized by a lower content of certain metals and a higher degree of oxidation. This required improvement of the reagent regime for flotation of sulfide-oxidized ores. In particular, a progressive technological solution was used in the sulfide cycle - a combination of two foaming agents of active and selective types. Reagents containing terpene alcohols are used as an active foaming agent, and a new reagent LV, developed for the enrichment of multicomponent ores, primarily Tyrnyauz ores, is used as a selective agent.
In the flotation cycle of oxidized minerals by fatty acid collectors, intensifying additives of a modifier reagent based on low molecular weight carboxylic acids are used. To improve the flotation properties of circulating industrial products pulp, regulation of their ionic composition has been introduced. Methods of chemical finishing of concentrates have found wider application.
From the autogenous grinding mill, the ore is sent to screening. Class +4 mm is further ground in a ball mill. Mill overflow and under-screen product (--4 mm) are subject to I and II classifications.
690 g/t soda and 5 g/t transformer oil are fed into the ball mill. The classifier discharge goes to the main molybdenum flotation, where 0.5 g/t xanthate and 46 g/t terpineol are fed. After I and II cleaning flotations, the molybdenum concentrate (1.2-1.5% Mo) is subjected to steaming with liquid glass (12 g/t) at 50-70°C, III cleaning flotation and further grinding to 95-98% class --0.074 mm with a supply of 3 g/t sodium cyanide and 6 g/t liquid glass.
The finished molybdenum concentrate contains about 48% Mo, 0.1% Cu and 0.5% WO 3 with a Mo extraction of 50%. The control flotation tailings of the III and IV cleaning operations are thickened and sent to copper-molybdenum flotation with a supply of 0.2 g/t xanthate and 2 g/t kerosene. The twice purified copper-molybdenum concentrate, after steaming with sodium sulfide, is sent to selective flotation, where a copper concentrate containing 8-10% Cu (with an extraction of about 45%), 0.2% Mo, 0.8% Bi is isolated.
The tailings of the control molybdenum flotation, containing up to 0 2% WO 3, are sent to scheelite flotation, which is carried out according to a very branched and complex scheme. After mixing with liquid glass (350 g/t), basic scheelite flotation is carried out with sodium oleate (40 g/t). After the first cleaning flotation and thickening to 60% solid, the scheelite concentrate is steamed with liquid glass (1600 g/t) at 80--90 °C. Next, the concentrate is cleaned twice more and again goes to steaming at 90--95 ° C with liquid glass (280 g/t) and is cleaned again three times.
2. Technological section
2.1 Calculation of crushing scheme with equipment selection
The designed concentration plant is intended for processing molybdenum-containing tungsten ores.
Medium-sized ore (f = 12 ± 14 units on Professor Protodyakonov’s scale) is characterized by a density c = 2.7 t/m 3 and is supplied to the factory with a moisture content of 1.5%. Maximum piece d=1000 mm.
In terms of productivity, the enrichment plant belongs to the category of medium productivity (Table 4/2/), according to the international classification - to group C.
To the factory ore D max. =1000 mm is supplied from open-pit mining.
1. Let's determine the productivity of the coarse crushing shop. We calculate productivity according to Razumov K.A. 1, pp. 39-40. The project adopted the delivery of ore 259 days a year, in 2 shifts of 7 hours, 5 days a week.
Ore strength factor /2/
where: Q c. etc. - daily productivity of the crushing shop, t/day
Coefficient taking into account the uneven properties of raw materials /2/
where: Q h..t. dr - hourly productivity of the crushing shop, t/h
k n - coefficient taking into account the uneven properties of raw materials,
n days - estimated number of working days per year,
n cm - number of shifts per day,
t cm - shift duration,
k" - coefficient for accounting for ore strength,
Calculation of annual working hours:
C = (n day n cm t cm) = 259 2 5 = 2590 (3)
Time utilization rate:
k in = 2590/8760 = 0.29 units = 29%
2. Calculation of crushing scheme. We carry out the calculation according to pp. 68-78 2.
According to the instructions, the moisture content of the initial ore is 1.5%, i.e. e.
Calculation procedure:
1. Determine the degree of fragmentation
2. Let us accept the degree of fragmentation.
3. Let’s determine the maximum size of products after crushing:
4. Let's determine the width of the crusher's discharge slots, taking the typical characteristics Z - coarsening of the crushed product relative to the size of the discharge slot.
5. Let’s check the compliance of the selected crushing scheme with the manufactured equipment.
The requirements that crushers must satisfy are listed in Table 1.
Table 1
In terms of the width of the receiving opening and the range of adjustment of the discharge slot, crushers of the ShchDP 12X15 brand are suitable.
Let's calculate the productivity of the crusher using the formula (109/2/):
Q cat. = m 3 / h
Q fraction. = Q cat. · with n · k f · k cr. · k ow. · k c, m 3 / h (7)
where c n is the bulk density of ore = 1.6 t/m 3,
Q cat. - passport capacity of the crusher, m 3 / h
k f . , k ow. , kcr, kc - correction factors for strength (crushingability), bulk density, ore size and moisture content.
The value of the coefficients is found from the table k f =1.6; k cr =1.05; k ow. =1%;
Q cat. = S pr. / S n · Q n = 125 / 155 · 310 ? 250 m 3 /h
Let's find the actual productivity of the crusher for the conditions defined by the project:
Q fraction. = 250 · 1.6 · 1.00 · 1.05 · 1 · 1 = 420 t/h
Based on the calculation results, we determine the number of crushers:
We accept 12 x 15 boards for installation - 1 pc.
2.2 Calculation of the grinding scheme
The grinding scheme chosen in the project is a type of VA Razumov K.A. page 86.
Calculation procedure:
1. Determining the hourly productivity of the grinding shop , which is actually the hourly productivity of the entire factory, since the grinding shop is the main ore preparation building:
where 343 is the number of working days in a year
24 - continuous work week 3 shifts of 8 hours (3x8=24 hours)
Kv - equipment utilization factor
Kn - coefficient taking into account the uneven properties of raw materials
We accept: K in =0.9 K n =1.0
The coarse ore warehouse provides a two-day supply of ore:
V= 48,127.89 / 2.7 = 2398.22
We accept the initial data
Let's ask ourselves about liquefaction in plums and sands classification:
R 10 =3 R 11 =0.28
(R 13 is based on row 2 p. 262 depending on the size of the drain)
in 1 -0.074 =10% - class content - 0.074 mm in crushed ore
in 10 -0.074 =80% - class content - 0.074 mm in the classification plum.
We accept the optimal circulation load With opt = 200%.
Calculation procedure:
Grinding stages I and II are represented by a type VA scheme, page 86 fig. 23.
Calculation of scheme B comes down to determining the weights of products 2 and 5 (product yields are found according to general formula g n = Q n: Q 1)
Q 7 = Q 1 C opt = 134.9 · 2 = 269.8 t/h;
Q 4 = Q 5 = Q 3 + Q 7 = 404.7 t/h;
g 4 = g 5 = 300%;
g 3 = g 6 = 100%
The calculation is carried out according to Razumov K.A. 1 pp. 107-108.
1. Calculation of scheme A
Q 8 = Q 10 ; Q 11 = Q 12 ;
Q 9 = Q 8 + Q 12 = 134.88 + 89.26 = 224.14 t/h
g 1 = 100%; g 8 = g 10 = 99.987%;
g 11 = g 12 =Q 12: Q 1 = 89.26: 134.88 = 66.2%;
g 9 = Q 9: Q 1 = 224.14: 134.88 = 166.17%
Process flow diagramschleniyamolybdenum-tungsten ores.
CalculationByqualitative-quantitative scheme.
Initial data for calculating qualitative-quantitative schemess.
Extraction of tungsten into the final concentrate - e tungsten 17 = 68%
Extraction of tungsten into collective concentrate - e tungsten 15 =86%
Extraction of tungsten into molybdenum concentrate - e tungsten 21 = 4%
Extraction of molybdenum into the final concentrate - e Mo 21 = 77%
Extraction of molybdenum into tungsten flotation tailings - e Mo 18 =98%
Extraction of molybdenum into control flotation concentrate - eMo 19 =18%
Extraction of molybdenum into collective concentrate - e Mo 15 = 104%
Yield of collective concentrate - g 15 = 36%
Yield of tungsten concentrate - g 17 = 14%
Yield of molybdenum concentrate - g 21 = 15%
Yield of control flotation concentrate - g 19 =28%
Determining the yield of enrichment products
G 18 = g 15 - G 17 =36-14=22%
G 22 = g 18 - G 21 =22-15=7%
G 14 = g 13 + g 19 + g 22 =100+28+7=135%
G 16 = g 14 - G 15 =135-36=99%
G 20 = g 16 - G 19 =99-28=71%
Determining the masses of enrichment products
Q 13 = 127.89t/h.
Q 1 4 = Q 13 XG 14 = 127.89x1.35=172.6 t/h
Q 1 5 = Q 13 XG 15 = 127.89x0.36=46.0 t/h
Q 1 6 = Q 13 XG 16 = 127.89x0.99=126.6t/h
Q 1 7 = Q 13 XG 17 = 127.89x0.14=17.9 t/h
Q 1 8 = Q 13 XG 18 = 127.89x0.22=28.1 t/h
Q 1 9 = Q 13 XG 19 = 127.89x0.28=35.8 t/h
Q 20 = Q 13 XG 20 = 127.89x0.71=90.8 t/h
Q 21 = Q 13 XG 21 = 127.89x0.15=19.1 t/h
Q 22 = Q 13 XG 22 = 127.89x0.07=8.9 t/h
Determining the recovery of enrichment products
For tungsten
e tungsten 13 =100 %
e tungsten 18 = e tungsten 15 - e tungsten 17 =86-68=28 %
e tungsten 22 = e tungsten 18 - e tungsten 21 =28-14=14 %
e tungsten 14 = e tungsten 13 + e tungsten 22 + e tungsten 19 =100+14+10=124 %
e tungsten 16 = e tungsten 14 - e tungsten 15 =124-86=38%
e tungsten 20 = e tungsten 13 - e tungsten 17 + e tungsten 21 =100 - 68+4=28%
e tungsten 19 = e tungsten 16 - e tungsten 20 =38-28=10 %
for molybdenum
e Mo 13 =100%
e Mo 22 = e Mo 18 - e Mo 21 =98-77=11 %
e Mo 14 = e Mo 13 + e Mo 22 + e Mo 19 =100+11+18=129 %
e Mo 16 = e Mo 14 - e Mo 15 =129-94=35 %
e Mo 17 = e Mo 15 - e Mo 18 =104-98=6%
e Mo 20 = e Mo 13 - e Mo 17 + e Mo 21 =100 - 6+77=17%
e Mo 19 = e Mo 16 - e Mo 20 =35-17=18%
Determining the amount of metals in the product Oh enrichment
For tungsten
14 =124 x0.5 / 135=0.46%
15 =86x0.5 / 36=1.19%
16 =38 x0.5 / 99=0.19%
17 =68 x0.5 / 14=2.43%
18 =28 x0.5 / 22=0.64%
19 =10 x0.5 / 28=0.18%
20 =28 x0.5 / 71=0.2%
21 =14 x0.5 / 15=0.46%
22 =14 x0.5 / 7=1%
For molybdenum
14 =129 x0.04/ 135=0.04%
15 =94x0.04/ 36=0.1%
16 =35 x0.04 / 99=0.01%
17 =6 x0.04 / 14=0.017%
18 =98 x0.04 / 22=0.18%
19 =18 x0.04 / 28=0.025%
20 =17 x0.04 / 71=0.009%
21 =77 x0.04 / 15=0.2%
22 =11 x0.04 / 7=0.06%
Table 3. Table of qualitative-quantitative enrichment scheme
|
Operation no. cont. |
|
Q, t/h |
, % |
copper , % |
copper , % |
zinc , % |
zinc , % |
|
|
I |
Grinding stage I |
|||||||
|
arrives |
||||||||
|
crushed ore |
||||||||
|
comes out |
||||||||
|
crushed ore |
||||||||
|
II |
Classification |
|||||||
|
arrives |
||||||||
|
CrushedbChennsth product IArt. grinding |
||||||||
|
CrushedbChennsth product II st .grinding |
||||||||
|
comes out |
||||||||
|
drain |
||||||||
|
sands |
||||||||
|
III |
Grinding I I stage |
|||||||
|
arrives |
||||||||
|
Sands classification |
||||||||
|
comes out |
||||||||
|
Shreddedsth product |
||||||||
|
IV |
Collective Wo 3 -Mo flotation |
|||||||
|
arrives |
||||||||
|
Drain classification |
||||||||
|
|
||||||||
|
TailsMo flotationAnd |
||||||||
|
comes out |
||||||||
|
concentrate |
||||||||
|
tails |
||||||||
|
V |
Control flotation |
|||||||
|
arrives |
||||||||
|
Tailcollective flotation |
||||||||
|
comes out |
||||||||
|
concentrate |
||||||||
|
tails |
||||||||
|
VI |
Tungsten flotation |
|||||||
|
arrives |
||||||||
|
Concentratecollective flotation |
||||||||
|
comes out |
||||||||
|
concentrate |
||||||||
|
tails |
||||||||
|
Mo flotation |
||||||||
|
arrives |
||||||||
|
Tails Wo 3 flotation |
||||||||
|
comes out |
||||||||
|
concentrate |
||||||||
|
tails |
Calculation of water-sludge scheme .
The purpose of calculating the water-sludge scheme is to: ensure optimal liquid: solid ratios in the operations of the scheme; determining the amount of water added to operations or, conversely, released from products during dehydration operations; determination of L:T ratios in the products of the scheme; determination of the total water requirement and specific water consumption per ton of processed ore.
To get high technological indicators ore processing, each operation of the technological scheme must be carried out at optimal values of the L:T ratio. These values are established based on data from ore dressing tests and the operating practices of existing processing plants.
The relatively low specific water consumption per ton of processed ore is explained by the presence of intra-factory water circulation at the designed plant, since the thickener drains are fed into the grinding - classification cycle. Water consumption for flushing floors, washing equipment and for other purposes is 10-15% of the total consumption.
Table 3. Table of qualitative-quantitative enrichment scheme.
|
Opera no.walkie-talkies cont. |
Name of operations and products |
Q, t/h |
, % |
R |
W |
|
|
I |
Grinding stage I |
|||||
|
arrives |
||||||
|
crushed ore |
0 , 0 25 |
|||||
|
comes out |
||||||
|
crushed ore |
||||||
|
II |
Classification |
|||||
|
arrives |
||||||
|
CrushedbChennsth product IArt. grinding |
||||||
|
CrushedbChennsth product II st .grinding |
||||||
|
comes out |
||||||
|
drain |
||||||
|
sands |
||||||
|
III |
Grinding I I stage |
|||||
|
arrives |
||||||
|
Sands classification |
||||||
|
comes out |
||||||
|
Shreddedsth product |
||||||
|
IV |
Collective Wo 3 -Mo flotation |
|||||
|
arrives |
||||||
|
Drain classification |
||||||
|
Control flotation concentrate |
||||||
|
Tails Mo flotationAnd |
||||||
|
comes out |
||||||
|
concentrate |
||||||
|
Tails |
||||||
|
V |
Control flotation |
|||||
|
arrives |
||||||
|
Tailcollective flotation |
||||||
|
comes out |
||||||
|
concentrate |
||||||
|
Tails |
||||||
|
VI |
Tungsten flotation |
|||||
|
Incoming |
||||||
|
Concentratecollective flotation |
||||||
|
It turns out |
||||||
|
Concentrate |
||||||
|
Tails |
||||||
|
Mo flotation |
||||||
|
Incoming |
||||||
|
Tails tungstenflotation |
||||||
|
It turns out |
||||||
|
concentrate |
||||||
|
tails |
Crusher selection and calculation.
The choice of crusher type and size depends on the physical properties of the ore, the required crusher capacity, the size of the crushed product and the hardness of the ore.
Tungsten-molybdenum ore by strength category is an ore of medium strength.
The maximum size of a piece of ore entering the crushing operation is 1000 mm.
To crush the ore coming from the mine, I install a jaw crusher with a simple swing jaw ShchDP 12x15. *
Crusher productivity, Q is equal to:
Q =q*L*i, t/h,
where q - specific productivity of the jaw crusher per 1 cm 2 of the discharge slot area, t/(cm 2 * h);
L is the length of the discharge slot of the neck crusher, cm;
i - width of the unloading slot, see /4/
According to the practice of operating the crushing department of the processing plant, the specific productivity of the jaw crusher is 0.13 t/cm 2 * hour.
The productivity of a jaw crusher will be determined by:
Q= 0.13*150*15.5 = 302.25 t/h.
The crusher accepted for installation provides the specified ore productivity.
The maximum size of a piece in the crusher feed will be:
120*0.8 = 96 cm.
Selection and calculation of grate screen
A grate screen with a hole size of 95 cm (950 mm) is installed in front of the crusher.
The required screening area is determined by the formula:
where Q* - productivity, t/h;
a is a coefficient equal to the width of the gap between the grates, mm. /5/ According to the layout conditions, the width of the grate screen is taken to be 2.7 m, length 4.5 m.
The practice of the crushing department of the factory shows that the ore delivered from the quarry contains about 4.5% of pieces with a particle size of more than 950 mm. Pieces of this size are delivered by a front-end loader to the ore yard, where they are crushed and again fed by the loader to the grate screen.
2.3 Selection and calculation of semi-autogenous grinding mills
Recently, when processing gold ores in world and domestic practice, semi-autogenous grinding mills followed by cyanidation are becoming more common in the first stage of grinding. In this case, the loss of gold from iron scrap and crumbs is eliminated, the consumption of cyanide during cyanidation is reduced, and the sanitary conditions of working on quartz silicate ores are improved. Therefore, I accept a semi-autogenous grinding (SAG) mill for installation in the first stage of grinding.
1. Find the specific productivity for the newly formed class of the operating SSI mill, t/(m 3 * h):
where Q is the productivity of the operating mill, t/h;
- class content -0.074 mm in the mill discharge, %;
- class content -0.074 mm in the original product,%;
D is the diameter of the operating mill, m;
L is the length of the operating mill, m.
2. We determine the specific productivity of the designed mill according to the newly formed class:
where q 1 is the specific productivity of a working mill in the same class;
K and is a coefficient that takes into account differences in the grindability of the ore designed for processing and the ore being processed (Ki = 1);
K k - coefficient taking into account the difference in the size of the initial and final grinding products at the existing and designed factories (K k = 1);
K D is a coefficient that takes into account the difference in the diameters of the drums of the designed and operating mills:
K D = ,
where D and D 1 respectively, the nominal diameters of the drums of the mills being designed for installation and those in operation. (K D =1.1);
Kt is a coefficient that takes into account differences in the type of designed and operating mills (Kt=1).
q = 0.77*1*1*1.1*1 =0.85 t/(m 3 * h).
I accept for installation an autogenous grinding mill "Cascade" with a diameter of 7 m and a length of 2.3 m with a working volume of 81.05 m3
3. We determine the productivity of the mills for ore using the formula:
where V is the working volume of the mill. /4/
4. Determine the estimated number of mills:
n- 101/125.72 = 0.8;
then the accepted one will be equal to 1. The Cascade mill provides the specified productivity.
Screen selection and calculation II screening stage .
Draining of semi-autogenous mills using pumps...
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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.
In search of an alternative method of 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. The best results 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
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Indicators |
Initial food |
Concentrate |
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Recovery, % |
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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 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 with 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 with cold water and dried.
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%