The ore dressing process will produce a large amount of tailings. The tailings not only occupy a large amount of land, but also bring serious pollution and harm to human production and life. It has been widely concerned by the whole society. At the same time, the beneficiation tailings have been called secondary resources. With the decreasing of various primary resources, the comprehensive utilization of tailings has been paid more and more attention. The development and utilization of tailings is the most comprehensive utilization of minerals. One of the areas with the broadest potential, the greatest potential, and the best economic and social benefits. A copper mine tailings reserves 3,000,000 t, for the presence of the recovered copper, sulfur and tungsten minerals. The mine has a mining history of several decades. Due to the low content of tungsten and the low price at the beginning of the mine construction, the recycling was not considered. In addition, due to the backwardness of the ore dressing technology , the copper recovery rate was less than 80%, resulting in some copper and tungsten. metal loss to tailings. Therefore, it is of good practical significance to comprehensively recover copper and tungsten for the tailings. First, the nature of the sample (1) Analysis of main components and chemical composition of samples The sample is mainly composed of copper and tungsten, and contains a small amount of lead , zinc and trace amounts of gold and silver . The main metallic minerals pyrite ores are wolframite and chalcopyrite, relatively few other metals mineral ores, ore gangue of quartz, calcite, dolomite, followed by a andradite, chlorite, white mica and gold mica, a small amount of epidote, feldspar, sphene and zircon. The chemical composition analysis results of the samples are shown in Table 1. Table 1 Results of chemical analysis of main components of the sample element Cu W0 3 S Fe Pb Zn MO P As Quality score 0.24 0.28 4.35 14.53 0.09 0.092 0.004 0.054 0.0028 element CaO MgO A1 2 0 3 SiO 2 K 2 0 Na 2 O Au Ag Quality score 10.29 1.14 2.17 44.47 0.36 0.068 0.07g/t 14.33g/t (2) Analysis of chemical phase of copper and tungsten in samples The chemical phase analysis results of copper and tungsten in the samples are shown in Table 2 and Table 3, respectively. Table 2 Results of phase analysis of copper in samples Copper phase Copper sulfide Copper in copper oxide Total copper content 0.226 0.015 0.241 Occupancy rate 93.78 6.22 100.0 Table 3 Results of chemical phase analysis of tungsten in the sample Tungsten phase Tungsten in black tungsten Tungsten in scheelite Other tungsten Total tungsten content content 0.242 0.021 0.010 0.273 Occupancy rate 88.64 7.70 3.66 100.0 It can be seen from the chemical phase analysis results of copper and tungsten that copper is mainly present in the form of sulfides, and tungsten is mainly present in the form of wolframite. (3) Particle size composition, mineral structure and embedding characteristics of the sample The particle size analysis results of the samples are shown in Table 4. Table 4 Sample particle size analysis results Size/μm Yield grade Distribution rate individual Grand total copper Tungsten copper Tungsten +147 5.54 5.54 0.08 0.20 1.85 4.07 -147+104 16.43 21.97 0.16 0.24 11.01 14.51 -104+74 17.82 39.79 0.24 0.22 17.91 14.43 -74+43 14.54 54.32 0.28 0.34 17.05 18.19 -43+20 15.71 70.04 0.29 0.27 19.09 15.62 -20+15 10.86 80.89 0.27 0.32 12.28 12.79 -15 19.10 100.0 0.26 0.29 20.81 20.39 Feed mine 100.0 0.24 0.27 100.0 100.0 The structure and embedding characteristics of the main metal minerals chalcopyrite and wolframite in the ore are as follows: 1. Chalcopyrite: Chalcopyrite is the main copper mineral in the ore. It is mainly produced in irregular shape. It is rarely embedded in the gangue alone. The chalcopyrite is mostly filled along the pyrite fracture or interlayer. Sometimes it is impregnated with coarse or medium coarse particles between the pyrite crystals. The relationship with pyrite is relatively close. Sometimes the chalcopyrite is filled with veins and veins along the pyrite fissures. Chalcopyrite inclusions, chalcopyrite and pyrite are often seen in coarse pyrite. Or the particle size of the continuous body with gangue is generally 0.005 to 1.00 mm, and the embedding relationship is relatively complicated. 2. Black tungsten ore: Hematite is mainly embedded in gangue minerals such as quartz, mica, fluorite , feldspar and chlorite by plate or columnar single crystal or aggregates in a single or group. Sometimes it is seen that pyrites such as pyrite and chalcopyrite are intercalated or wrapped in hematite. The black tungsten ore inlay has a particle size of 0.01 to 1.5 mm. Second, the experimental study on the conditions of mineral processing (1) Flotation test study According to the study of process mineralogy, the main target minerals to be recovered from the tailings are copper, sulfur and tungsten. Copper is mainly in the form of sulfides. The tungsten is mainly in the form of wolframite. Therefore, the determined test scheme is flotation recovery. Copper and sulfur, copper-sulfur flotation tailings are reprocessed to recover tungsten minerals. (2) Test samples and equipment The ore samples used in the test were collected from the tailings pond of the existing concentrator, and the samples were mixed and packed into 1000 g per pack as test samples for flotation. The laboratory equipment is a cone ball mill , XFD3.OL, XFD1.OL, XFD0.5L, 0.35L flotation machine , LL600×30O spiral chute and XYZ-1600×700 type groove shaker . 1. Comparison test of flotation process Since the content of copper in the sample is low and the sample contains a large amount of pyrite, the presence of pyrite in the subsequent tungsten selection process will affect the recovery of tungsten, and therefore, in the process of flotation of sulfide ore. It is necessary to consider the recovery of copper, but also to remove pyrite before tungsten is selected, to eliminate the impact of pyrite on subsequent tests, and also to recover sulfur comprehensively. In order to explore the optimal conditions of the flotation process, a comparative test of copper preferential flotation and sulfide ore mixed flotation was carried out on the sample. The principle process flow is shown in Figures 1 and 2. The test results are shown in Table 5. Table 5 Process comparison test results Process plan product name Yield grade Recovery rate Cu S WO 3 Cu S WO 3 Copper priority Flotation process Copper concentrate 6.44 2.63 26.88 0.14 67.93 41.28 3.31 Sulfur concentrate 9.44 0.17 19.31 0.12 6.44 43.47 4.15 Sulfide mine tailings 84.12 0.076 0.76 0.30 25.64 15.24 92.54 Raw ore 100.0 0.25 4.19 0.27 100.0 100.0 100.0 Sulfide ore Mixed flotation Process Copper concentrate 4.24 4.02 25.62 0.13 70.44 25.91 2.05 Sulfur concentrate 12.83 0.15 20.77 0.11 7.96 63.60 5.26 Sulfide mine tailings 82.93 0.063 0.53 0.30 21.60 10.49 92.69 Raw ore 100.0 0.24 4.19 0.27 100.0 100.0 100.0 It can be seen from the test results that the index of priority flotation process copper is slightly lower than that of the sulfide ore mixed flotation process. At the same time, the sulfur content of the sulfide ore tailings in the preferential flotation process is higher than that of the sulfide ore mixed flotation process. It is because the lime is used in a large amount, the pH is higher, the copper is inhibited, and a large amount of acid is added to reduce the pH when the sulfur is selected. Since the content of copper in the sample is low and the sample contains a large amount of pyrite, the presence of pyrite in the subsequent tungsten selection process will affect the recovery of tungsten. Therefore, the sulfide ore flotation test uses sulfide ore. The mixed flotation process recovers copper and eliminates the effects of pyrite on subsequent tests. 2, collector type test The sample was ground to -74 μm to account for 80%. The sorting performance of various collectors for copper was examined. The test procedure is shown in Figure 3. The test results are shown in Table 6. Table 6 Collector type test results Collector type and dosage / (g·t -1 ) product name Yield grade Recovery rate Cu S Cu S Z-200 40 Copper concentrate 12.71 1.40 26.12 72.85 75.57 Tailings 87.29 0.076 1.23 27.15 24.43 Raw ore 100.0 0.24 4.39 100.0 100.0 Ethyl xanthate 40 Copper concentrate 13.90 1.25 24.76 74.79 80.31 Tailings 86.10 0.068 0.98 25.21 19.69 Raw ore 100.0 0.23 4.29 100.0 100.0 KD 40 Copper concentrate 17.29 1.15 22.13 78.97 86.37 Tailings 82.71 0.064 0.73 21.03 13.63 Raw ore 100.0 0.25 4.43 100.0 100.0 Butyl xanthate 40 Copper concentrate 21.19 0.91 18.13 80.57 87.44 Tailings 78.81 0.059 0.70 19.43 12.56 Raw ore 100.0 0.24 4.39 100.0 100.0 The test results show that the new collector KD (thiourethane) has strong collection ability and good selectivity for copper. Therefore, KD is used as a collector for recovering copper. 3. Grinding fineness test Due to the coarse particle size of the sample, the grinding fineness test was carried out. The activator was copper sulfate, the dosage was 200g/t, the collector was KD, the dosage was 40 g/t, and the foaming agent was pine oil. 20g / t, the test results are shown in Figure 4. 1—copper recovery rate; 2—copper grade; 3—tungsten recovery rate; 4—tungsten grade It can be seen from the results of the grinding fineness test of Fig. 4 that the direct flotation of the sample is not good, and the copper concentrate is not concentrated. As the fineness of the grinding increases, the copper in the copper concentrate The recovery rate is gradually increased, the copper grade is gradually reduced, and the loss of tungsten in the copper concentrate is gradually reduced. Considering the indicators of copper and tungsten, it is determined that the fineness of grinding is -74μm and accounts for 80%. 4, copper sulfate dosage test The sample was ground to -74 μm, 80%, KD was 40 g/t, the amount of pine oil was 20 g/t, and the test results for copper sulfate were shown in Fig. 5. 1—copper recovery rate; 2—copper grade; 3—sulfur recovery rate; 4—sulfur grade It can be seen from the test results in Fig. 5 that the amount of copper sulfate is increased, the recovery rate of copper and sulfur in the concentrate is gradually increased, and the copper grade is gradually reduced. When the dosage is 200 g/t, the test index is good, therefore, the copper sulfate is determined. The amount used is 200 g/t. 5, collector KD dosage test The sample was ground to -74 μm to 80%, the amount of copper sulfate was 200 g/t, the amount of pine oil was 20 g/t, and the test results of the collector KD were shown in Fig. 6. 1—copper recovery rate; 2—copper grade; 3—sulfur recovery rate; 4—sulfur grade The test results in Figure 6 show that as the amount of KD increases, the recovery of copper and sulfur in the concentrate gradually increases, and the copper grade gradually decreases. Therefore, the amount of KD is determined to be 40 g/t. 6, copper and sulfur separation lime dosage test Lime is an effective inhibitor of pyrite in the separation of copper and sulfur. After a large selection of copper-sulfur crude concentrate, a high-grade copper and sulfur mixed concentrate is obtained, and the separation of copper and sulfur is achieved by using lime. The amount of lime was tested and the test results are shown in Figure 7. 1—copper recovery rate; 2—copper grade; 3—sulfur recovery rate; 4—sulfur grade The test results in Fig. 7 show that the lime can achieve the separation of copper and sulfur. As the amount of lime increases, the grade of copper in the concentrate gradually increases, and the recovery rate of copper gradually decreases. Therefore, the amount of lime is determined to be 1500 g/t. 7, open circuit test On the basis of the conditional test, a laboratory open circuit test was conducted on the sulfide ore. The test procedure is shown in Figure 8, and the test results are shown in Table 7. Table 7 Open circuit test results product name Yield grade Recovery rate Cu S WO 3 Cu S WO 3 Copper concentrate 0.39 23.43 34.23 0.09 36.31 3.09 0.13 Middle mine 1 0.34 8.34 33.45 0.10 11.24 2.63 0.13 Middle mine 2 1.35 1.43 32.56 0.10 7.71 10.22 0.51 Middle mine 3 1.69 0.81 34.13 0.11 5.46 13.39 0.70 Middle mine 4 1.85 0.43 34.24 0.10 3.19 14.78 0.70 Sulfur concentrate 4.33 0.10 35.24 0.14 1.73 35.54 2.29 Middle mine 5 7.25 0.20 6.23 0.17 5.79 10.51 4.65 Middle mine 6 3.54 0.54 7.12 0.14 7.64 5.87 1.87 Middle mine 7 1.69 0.21 1.83 0.19 1.41 0.72 1.21 Tailings 77.57 0.063 0.18 0.30 19.52 3.24 87.81 Raw ore 100.0 0.25 4.30 0.27 100.0 100.0 100.0 (3) Re-election test 1. Spiral chute tailing test Since the density difference between tungsten minerals and gangue minerals is large, the re-election method is an effective means for recovering tungsten minerals. Since the sample contains W0 3 of only 0.27%, it is necessary to carry out the tailing in advance and use a spiral chute to throw the tail. The test adopts LL600×300 spiral chute, and the ore is tailings of sulfide ore flotation. The test results are shown in Table 8. Table 8 Spiral chute test results product name Yield WO 3 grade W0 3 job recovery rate Crude concentrate Tailings Sulfide mine tailings 48.08 51.92 100.0 0.45 0.10 0.27 80.65 19.35 100.0 It can be seen from Table 8 that the use of a spiral chute can remove most of the tailings and achieve the effect of pre-enrichment. 2, shaker test The coarse concentrate produced after the tailing of the spiral chute was selected by a shaker, and an XYZ-1600×700 type grooved shaker was used. The test results are shown in Table 9. Table 9 Shake test results product name Yield W0 3 grade W0 3 job recovery rate Concentrate 0.44 66.01 63.69 Middle mine 5.60 1.48 18.18 Tailings 93.96 0.088 18.13 Crude concentrate 100.0 0.46 100.0 (4) Full process test The flotation-re-election combined process was carried out, and the whole process test was carried out according to Fig. 9. The test results are shown in Table 10. Table 10 Closed circuit test results product name Yield grade Recovery rate Cu S WO 3 Cu S WO 3 Copper concentrate 0.84 22.02 34.34 0.09 74.39 6.57 0.28 Sulfur concentrate 10.82 0.11 35.24 0.14 4.81 87.26 5.70 Tungsten concentrate 0.21 0.100 0.83 65.73 0.08 0.04 50.86 Tungsten mine 2.67 0.094 4.56 1.32 1.02 2.79 13.29 Tailings 1 40.31 0.056 0.16 0.09 9.12 1.48 12.89 Tailings 2 45.15 0.058 0.18 0.10 10.58 1.86 16.99 Raw ore 100.0 0.25 4.37 0.27 100.0 100.0 100.0 Third, the conclusion (1) Through the experimental study on the tailings of the concentrator, it is indicated that the tailings containing 0.24% copper, 4.36% sulfur and 0.27% tungsten can be treated by flotation-re-election combined process, and the copper grade of copper concentrate can be obtained 22.02%, recycling The rate is 74.39%, the sulfur grade of sulfur concentrate is 35.24%, the recovery rate is 87.26%, the tungsten grade of tungsten concentrate is 65.73%, and the recovery rate is 50.86%. (2) From the test results, it is technically and economically feasible to recover valuable elements from the tailings. This study provides a technically feasible and economically reasonable process and process conditions for the comprehensive recovery of copper, sulfur and tungsten in tailings. It also has certain guiding significance for the secondary comprehensive development and utilization of tailings of the same type of concentrator. The comprehensive utilization of tailings resources is an effective way to extend the service life of mines and improve the economic benefits of mines.
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Test for recovering valuable elements from beneficiation tailings
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