Huili zinc ore mine is a multi-metal containing lead, zinc, silver, cadmium and other metals, selected from plant processing capacity of 1000t / d. The first selection plant uses preferential flotation, lead and zinc re-separation, and produces lead concentrate, zinc concentrate, lead-zinc mixed concentrate. Due to the complex nature of the ore, the selected process is not suitable for the nature of the ore. Therefore, the selection of the standard is extremely poor, which seriously affects the economic benefits of the enterprise. The outstanding performance is that the lead and zinc in lead and zinc concentrates are serious, which not only makes the mineral products difficult to sell, but also affects the comprehensive utilization of mineral resources and the economic benefits of enterprises. The pharmaceutical system is not environmentally friendly, and the wastewater is not directly recycled. It not only threatens the health of the pharmaceutical workers, but also seriously pollutes the downstream waters of the Anning River. In order to solve the above problems carried out research on mineral concentration plant cleaner production technologies. The main technical research contents are as follows:

I. Development of a new process for clean and high-efficiency lead-zinc sulfide ore beneficiation

According to the analysis of ore properties, the zinc ore is a low-lead and high-zinc complex leached zinc-lead ore. According to the general floatability of lead and zinc and the general principle of lead-zinc separation, the priority of zinc-suppressing and floating lead can be used. The selection process or the mixed flotation process of lead-zinc mixing and then lead-zinc separation or floatable processes such as lead and zinc. The specific measures are as follows:

(1) Fine grinding.

(2) Using lime to adjust the pH value of the slurry, and adjusting the pH value of the slurry to suppress lead and zinc in alkaline conditions.

(3) A combination of (ZnSO ₄ + YN) high-efficiency sphalerite inhibitors.

(4) An effective conventional chemical sulfur-nitrogen collector or combination collector using galena.

(5) Properly adjust the dosage of collectors and increase the recovery rate of lead and zinc.

(6) Floating zinc under alkaline conditions.

Laboratory beneficiation test

The test mainly adopts two schemes, namely: (lime + ZnSO ₄ + YN) zinc-suppressing and floating lead scheme and the regulation of slurry potential zinc-suppressing and floating lead by lime. The experiment first explored the types of lead collectors and found that SN-9 ^# has good selectivity to lead and the agent is environmentally friendly, meeting the requirements of cleaner production. At the same time, the test carried out the closed-circuit process of the two kinds of schemes for the pharmaceutical system and process parameters of the two schemes. See Table 1.

Table 1 Small closed-circuit test indicators of two kinds of Fangning /%

It can be seen from Table 1 that the two schemes used have obtained high quality lead-zinc concentrate. Explain that the selected clean and efficient collector SN-9 ^# has good selectivity for lead minerals, whether it is the combination of the first solution (ZnSO ₄ +YN) or the lime control potential of the second scheme. The lead and zinc separation environment is better, and the selection process is simpler, not afraid of the influence of slime, no need to remove mud. Among them, the scheme only adds one kind of agent to the on-site process, and the YN dosage is not large. The collector is selected. The dosage is small and the second method uses lime. The other inhibitors are not used, and the pharmaceutical system is simpler. Therefore, the cost of mineral processing is not high, which will be very beneficial to the mine to improve economic efficiency. From the test results and considering the parameters of the process operation, the industrial test on the first scheme is recommended first.

Table 2 Complex refractory lead-zinc ore clean high-efficiency beneficiation new process industrial test and industrial production application index /%

Although it is subject to objective conditions, after the new process, in the case of lead containing 1.31% lead and 8.68% zinc, 66.34% of lead is contained, 7.60% of zinc is contained, and the recovery rate of lead is 57.14%. The lead concentrate has a lead concentrate of 1.57% and a zinc content of 56.13%, corresponding to a zinc recovery of 76.64%. Compared with the original process, the lead concentrate grade and recovery rate increased by 11.89% and 0.89%, respectively, and the zinc concentrate grade and recovery rate increased by 0.23% and 2.60%, respectively. At the same time, the zinc content in lead concentrate decreased from 11.71% of the original process to 7.60%. At the same time, it can be seen that the application of the new process does not reduce the zinc content in the tailings. The zinc content in the tailings is as high as 2.23%. From the chemical analysis of the tailings, it can be seen that the oxidation rate of zinc in the tailings is as high as 90%, so it is difficult to comprehensively recover this part of zinc in the new process system, so it is necessary to reprocess the tailings.

2. Recovery of zinc oxide in tailings

According to the analysis of the properties of the Huiling zinc ore tailings, the zinc oxide minerals in the tailings are mainly zinc ore, followed by the zinc-zinc ore and heteropolar ore. Gangue minerals are dolomite, calcite, quartz, sericite, chlorite, serpentine like. The primary condition for recovering oxidized minerals from the tailings is to reduce the amount of harmful minerals that interfere with and affect the recovery of zinc oxide and increase the grade of zinc oxide. According to the overall thinking, the specific technical solutions of this study are as follows:

Mineral processing integration new process

(1) Focus on the following aspects in the re-election cycle:

1. Spiral chute-shaker test;

2. Determination of the economic yield of re-elected products.

(2) Focus on the following aspects in the flotation cycle:

1. Test of combination modifier;

2. Comparison test between new zinc oxide collector and conventional collector:

3. Flotation process condition test;

4. Closed circuit test of flotation process.

(3) Focusing on the following aspects in the development of new pharmaceuticals:

1. Screen raw materials, optimize processes, and synthesize new zinc oxide collectors;

2. Comparison test of high efficiency, low cost and low toxicity zinc oxide collector;

A total of 3,731.09 tons of zinc oxide concentrate with a zinc content of 34.22% and a corresponding zinc recovery rate of 85.27% was used for industrial application in the "re-selection + flotation integrated beneficiation process" for one year. The amount of zinc metal was calculated to be 1276.78. Tons, the economic benefits are significant.

It can be seen that after treating the zinc oxide in the tailings with the “reselection + flotation integrated beneficiation new process flow”, the technical and economic indicators of the mineral processing are stable, and good economic benefits and significant social benefits have been achieved. At the same time, the production is clean and meets the requirements of “clean production, environmental protection first” that Huili zinc mine has historically required.

Third, mineral processing wastewater recycling

Although the new process eliminates the influence of aniline black medicine in the beneficiation wastewater, the problem of excessive lead ion in the ore dressing wastewater still exists. In the production process of the concentrator, a large amount of water is needed to maintain production. According to the statistics of Huili zinc mine, the annual production of zinc ore is about 2 million tons. In the process of mineral processing, the content of suspended solids in the water discharged by sorting, concentration filtration, washing, etc. is high, and the perception of water is poor, especially containing heavy metal ions and beneficiation agents, such as xanthate and black, to varying degrees. Medicine, pine oil, sulfide, oxide, acid, alkali, Cu ^{2 +} , Pb ^{2 +} , Zn ^{2 +} and other metal ions, which have some hidden dangers to the environment, so it is necessary to treat the ore dressing wastewater. Recycling and recycling. The “Research on the Process of Wastewater Recycling in the Production of Huili Zinc Ore Dressing Plant” was carried out to solve the problem of reuse of wastewater from zinc ore beneficiation production.

For the Huizhi zinc mine, the beneficiation production wastewater is naturally degraded after being self-flowing to the tailings pond, but it still contains a certain amount of xanthate, SN-9 ^# and foaming agent components, and also contains Cu ² Heavy metal ions such as ⁺ , Pb ^{2 +} and Zn ^{2 +} , these components have different effects on the flotation process, especially in the preferred floating lead cycle, it is necessary to comprehensively consider the remaining xanthate and Cu ^{2 +} , Pb ^{2 in the} ore dressing backwater. The effect of ⁺ ions, because the xanthate has a strong ability to capture the zinc minerals of the zinc ore, and the Cu ^{2 +} and Pb ^{2 +} ions can activate the zinc minerals, such as the beneficiation wastewater, and the residual Xanthate and Cu ^{2 +} , Pb ^{2 +} ions will deteriorate the preferred flotation separation of lead-zinc minerals, which was confirmed in previous studies and in the exploratory experiments of this study, so the recycling of beneficiation wastewater should be considered. It is necessary to treat the remaining xanthate and Cu ^{2 +} and Pb ^{2 +} ions in the wastewater.

According to the experimental research results, the wastewater from the beneficiation plant was treated by coagulation sedimentation-activated carbon adsorption treatment, and the purification treatment and wastewater reuse system of 10,000 tons of wastewater were designed. At the end of April 2007, the rotation and equipment installation were completed. On May 12, 2007, the on-site commissioning of the wastewater purification and reuse engineering system was started. The system has been in normal operation until now, and all the reuse of wastewater discharged from the plant has been realized. After the wastewater is reused, it has basically no influence on the production index, and at the same time, some of the medicament remains in the wastewater, so that the cost of the partial medicament can be saved after the wastewater is reused. Field practice shows that 100% reuse of wastewater can be achieved, and the reuse effect is good and basically stable, which not only saves wastewater treatment costs, but also protects the environment and improves the clean production level of the flotation process.

4. Recovery of copper metal in ore

As the depth of mining continues to deepen, the nature of the copper ore of Huili has undergone major changes, mainly due to the sharp rise in copper grade, forming copper, lead, zinc and polymetallic complex sulfide ore. In order to maintain and improve the existing lead and zinc beneficiation indicators, copper metal is recovered to form an independent copper concentrate product, and the high-efficiency development and utilization of mineral resources can be realized to improve the high copper and sulfur in the deep ore body of the Huizhi zinc mine. Experimental study on comprehensive beneficiation index of lead-zinc ore. To this end, the laboratory small-scale experiments mainly studied the copper-lead mixed-copper-lead separation-re-floating zinc scheme and the copper-lead-zinc sequential preferential flotation scheme.

(1) Copper-lead mixed float-copper-lead separation-zinc solution

According to the results of the exploration test, the test was first carried out on the copper-lead mixed float-lead-lead separation-zinc scheme, and the closed-circuit process test was carried out on the basis of the conditional test. The test results are shown in Table 3.

Table 3 Copper-lead mixed flotation-copper-lead separation-zinc direct flotation scheme small closed-circuit test index/%

(2) Copper-lead-zinc priority flotation scheme

According to the exploratory test results of copper collectors, it was found that both BK-301 and LP-01 can be used as collectors for copper during copper-lead-zinc preferential flotation. Therefore, the test first performed on BK-301 and LP-01. Contrast. The results of the comparative test are shown in Table 4.

Table 4 BK-301 and LP-01 comparison test results /%

It can be seen from Table 4 that LP-O1 is superior to BK-301 in terms of copper grade and copper recovery. Therefore, in the copper-lead-zinc preferential flotation scheme, the collector of copper is LP-01. . After determining the type of collector for copper, the test also explored the pharmaceutical system and process parameters during lead and zinc flotation, and conducted a closed-circuit process test based on the conditional test. The test results are shown in Table 5.

Table 5 Results of the closed copper test of the copper-lead-zinc preferential flotation

Comparing the "copper-lead mixed-copper-lead separation-re-floating zinc" scheme with the "copper-lead-zinc sequential preferential flotation" scheme, although both copper concentrates can be obtained, "copper-lead mixed-copper-lead separation" The separation of copper-lead from the copper-lead mixed concentrate obtained by flotation in the re-floating zinc scheme is difficult, and the environmentally unfriendly K ₂ CrO _{7 is used to} inhibit lead minerals, and the copper-lead separation effect is also poor. The high content of lead and zinc in the copper concentrate obtained also affects the recovery rate of lead and zinc. The use of "copper-lead-zinc in order to optimize flotation" not only obtains relatively good quality copper, lead and zinc concentrates, but also has simple chemicals, easy operation, and easy on-site process modification. It is recommended to consider this scheme for copper lead. Zinc polymetallic sulfide ore is subjected to comprehensive beneficiation recovery.

According to the test results, the copper-lead-zinc in the Huili zinc mine was preferentially floated, and the process was modified to add a copper series. Industrial applications in which copper-lead-zinc is followed by a preferred flotation process are initiated. Industrial application results are shown in Table 6.

Table 6 Copper-lead-zinc sequential preferential flotation process industrial application results /%

It can be seen from Table 6 that the copper-lead-zinc sequential preferential flotation process can obtain copper concentrate with lead content of 21.47% and corresponding copper recovery rate of 56.88% without affecting the lead and zinc index.

V. Results

(1) The new process of clean and efficient beneficiation of complex refractory lead-zinc mines has shown that the new process is completely suitable for the ore properties of the zinc ore, effectively solving the poor quality of lead and zinc concentrates, lead and zinc concentrates. Lead and zinc contain serious problems.

(II) “Re-selection + flotation integration new process” Through small experiments and industrial tests, the new process is completely suitable for the ore properties of the zinc ore flotation tailings, and the zinc oxide in the tailings is effectively recovered. Further benefit and increase the utilization rate of mineral resources and improve the clean production level of enterprises.

(3) After the returning process of the ore dressing wastewater after coagulation sedimentation-activated carbon adsorption treatment, the lead in the original ore is 1.86% and the zinc content is 6.54%, and the lead content is 66.00% and the zinc content is 5.95%. The lead recovery rate is 69.56%, and a zinc concentrate containing 1.65% lead containing 56.80% zinc and corresponding zinc recovery rate of 84.04% can be obtained. The lead and zinc concentrate grades and recovery rates are essentially the same as before the wastewater is reused.

(4) Using LP-01 as the collector, the “copper-lead-zinc” preferential flotation process is adopted, and the copper metal in the ore is effectively recovered while ensuring the quality of the lead and zinc concentrate products.

Conclusion

The application of a series of clean production technologies in Huili zinc mine not only solves the actual problems of the enterprise, but also brings obvious economic and environmental benefits to the enterprise. The total benefit that can be obtained for the enterprise is 90,678,900 yuan per year. It eliminates the influence of toxic chemicals in the original process, realizes the recycling of wastewater, and has a good reference role in similar metal mines.

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