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Copper sulfide ore, copper sulfur symbiosis is a common type of ore. The key to copper-sulfur ore flotation is the separation of copper minerals and iron-iron sulfide minerals. Xanthate is a commonly used collector for flotation separation, but the selectivity of xanthate collectors is poor, and a large number of regulators are often used in production practice. Such as lime as an inhibitor of pyrite. When the amount of lime is large, the alkalinity of the slurry is high, which will consume the collector and is not conducive to the comprehensive recovery of resources such as gold , silver and molybdenum . The inhibition of pyrite activation is difficult and requires a large amount of activator. Therefore, for copper sulfide ore, it is especially important to develop collectors with strong capture ability and high selectivity for copper minerals in neutral or low-alkaline pulp. In recent years, domestic and foreign scholars have developed some ideas around this idea. A highly selective collector for copper minerals and a good separation index for copper and sulfur flotation. Based on this concept, this paper studies the selective collection and action mechanism of collector DLZ on chalcopyrite and pyrite by single mineral test, adsorption quantity test and infrared detection, and lays a part for further guiding production practice. basis.
1. Samples, reagents and research methods
(1) Samples and medicaments
The pyrite is taken from the Guangdong Yunfu Pyrite Mine Concentrator, and the chalcopyrite is taken from the Tonglushan Mine of Daye Nonferrous Metals Corporation. The ore sample is crushed, hand-selected and removed, and then subjected to porcelain ball grinding and dry screening, and a -74+32 μm particle grade ore sample is taken. Through chemical analysis, the pyrite ore sample contains 46.2% iron, 49.5% sulfur, and 93% purity. The chalcopyrite ore sample contains 31.3% copper, 29.5% iron, 34.4% sulfur, and an esterity of 90.5%. The vinegar collectors DLZ, calcium oxide, hydrochloric acid and sodium hydroxide are of analytical grade, the foaming agent pine oil is industrial grade, and the test water is once distilled water.
(2) Test equipment and research methods
For the flotation test, the XFG type trough-type flotation machine was used. The volume of the flotation tank was 40 mL. The pure mineral 2.0 g was placed in a l00 mL beaker, and distilled water was added to the ultrasonicator for 5 min. After clarification, the supernatant was decanted. Then add the mineral into the flotation tank with distilled water, stir for 1 min, add the required adjusting agent, stir for 3 min, add the foaming agent for 1 min, float for 3 min. The foam product and the product in the tank were separately weighed and the recovery rate was calculated.
Potentiodynamic test. The ore sample is ground to -5 μm with an agate mortar, 50 mg each time is placed in a 100 mL beaker, 100 ml of distilled water is added, and the pH is adjusted to a suitable value with HCl or NaOH, and then a certain concentration of the adjusting agent is added (or not added). Or collector, stir for 5 min, and conduct the potentiometry using a Coulter Delsa 440sx analyzer.
Infrared spectroscopy. The solid sample was ground in an agate mortar, KBr powder was added, grinding was continued and mixed uniformly, and the ground material was tableted and measured on a Nicolet MR-740 Fourier transform infrared spectrometer.
Second, the test results and discussion
(1) DLZ flotation performance
In the separation of copper and sulfur, lime is used to suppress iron sulfide minerals and flotation of copper minerals. Therefore, the effects of collectors on the floatability of minerals when using NaOH, HCl and CaO to adjust the pH of the slurry were investigated. The amount of fixed DLZ was 2.6×10 -6 mol/L, and the amount of foaming agent pine oil was 22 mg/L. The relationship between the collection performance of collector DIZ and pH is shown in Fig. 1.
Figure 1 Relationship between DLZ capture performance and slurry pH
It can be seen from Fig. 1 that when using NaOH, HC1 to adjust the pH value of the slurry, the floatability of the chalcopyrite is good throughout the pH range (pH 2.7 to 12.05), and the maximum recovery is 95.7%; pyrite is in The floatability of the whole pH range is very poor, the maximum recovery rate is 24.1%, and after the pH is greater than 6.9, the floatability of pyrite decreases rapidly, and the recovery rate is less than 10%. Compared with NaOH, CaO has little effect on the floatability of chalcopyrite at pH 7-11, but the recovery of chalcopyrite is much lower at pH 12, chalcopyrite recovery The rate is 63.3%, CaO has a strong inhibitory effect on the flotation of pyrite, and the recovery rate of pyrite is less than 5%.
The fixed pH was 6.9, and the DIZ dosage test results are shown in Fig. 2. It can be seen from Fig. 2 that the amount of DLZ increased from 2.6×10 -6 mol/L to 15.6×10 -6 mol/L, the recovery rate of chalcopyrite increased from 94.4% to 96.4%, and the recovery rate of pyrite increased from 13.8% to 20.4%. As mentioned above, DLZ is a highly efficient collector for flotation chalcopyrite and is used in small amounts.
Figure 2 Effect of DLZ dosage on mineral floatability
(2) Dynamic potential test of DLZ and mineral surface interaction
The potentiodynamic curves before and after the action of minerals and agents are shown in Figure 3. As the pH increases, the dynamic potential of the mineral surface decreases. The isoelectric point of chalcopyrite and pyrite is about 3. The isoelectric point of unoxidized pyrite is reported to be around pH 3, which indicates that the pyrite surface used in this study may not be oxidized during sample preparation and agitation. It can be seen from Fig. 3 that after the action of minerals and collector DLZ, the surface dynamic potentials of chalcopyrite and pyrite decrease with increasing pH, indicating that DIZ is an anionic collector. Moreover, the surface potential of chalcopyrite is much lower, indicating that the adsorption capacity of DLZ on the surface of chalcopyrite is much larger than that on the surface of pyrite.
Figure 3 Dynamic potential before and after the action of minerals and agents
The effect of DLZ dosage on the dynamic potential of minerals at a fixed pH of 6.9 is shown in Figure 4. It can be seen from Fig. 4 that DLZ can rapidly change the surface potential of chalcopyrite under low dosage conditions, but has little effect on the surface potential of pyrite. When the amount of DLZ is more than 5.2×10 -6 mol/L. Since then, the surface potential of pyrite has rapidly become smaller. Under the range of the amount of test agent, the surface potential of chalcopyrite is much more negative than that of pyrite. It indicates that DLZ adsorbs more on the surface of chalcopyrite, and at low dosage (2.6×10 -6 mol/L), the difference between the surface potential of chalcopyrite and the surface potential of pyrite is the largest, and the flotation test The law is consistent.
Figure 4 Relationship between adsorption on mineral surface and dosage
(III) Infrared spectroscopy test of DLZ and mineral surface interaction
Figure 5 is an infrared spectrum of the chalcopyrite before and after the action of the agent. It can be seen from Fig. 5 that the infrared spectrum of the chalcopyrite before and after the action of the DLZ is obviously different. After the action of the chalcopyrite and the agent DLZ, a C-N stretching vibration absorption peak with a wave number of 1337.7 cm -1 appears; The C=C skeleton vibration absorption peak with a wave number of 1594.7 cm -1 and 1515.8 cm -1 , and the corresponding C-S stretching vibration peak of -(N)-C=S, the chalcopyrite after the action of the agent DLZ The corresponding peaks in the infrared spectrum shift or disappear, indicating that the bond constant of -(N)-C=S in the molecule after the action of DIZ and chalcopyrite has changed. From the above analysis, it is known that DLZ is chemisorbed on the surface of chalcopyrite.
Figure 5: Infrared spectrum before and after the action of chalcopyrite and chemicals
Figure 6 is an infrared spectrum of the pyrite before and after the action of the agent. It can be seen from Fig. 6 that the infrared spectrum curves of the pyrite and the DLZ agent before and after the action are substantially unchanged. The characteristic absorption peak of DLZ agent did not appear on the surface of pyrite. It can be seen from the above analysis that the adsorption of DLZ on the surface of pyrite is only a simple physical adsorption.
Figure 6 Infrared spectrum before and after the action of pyrite and chemicals
Third, the conclusion
(1) The results of flotation tests show that the DLZ captures chalcopyrite in the range of pH 2.7~12.05, which is much stronger than that of pyrite. The maximum recovery of chalcopyrite is 95.7%; and pyrite The floatability is poor throughout the pH range and the recovery is less than 24%. CaO was used to adjust the pH of the slurry. At pH 7-11, CaO had little effect on the floatability of chalcopyrite, but it had a strong inhibitory effect on the flotation of pyrite. The recovery rate of pyrite was less than 5%. . That is, selective separation of chalcopyrite and pyrite can be achieved in a neutral or alkaline medium at low concentrations.
(2) The potentiodynamic test shows that the surface potential of the mineral decreases with the increase of the pulp pH, indicating that DLZ belongs to the anion collector.
(III) Infrared spectroscopy analysis of the action of chemicals and minerals shows that DLZ is chemisorbed on the surface of chalcopyrite, and the adsorption on the surface of pyrite is physical adsorption. The difference in the adsorption form of DLZ on the surface of two minerals is its choice. The main reason for sex.
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