# Tailings Utilization and Zinc Extraction Based on Mechanochemical Activation

^{1}

^{2}

^{3}

^{4}

^{5}

^{*}

## Abstract

**:**

_{2}SO

_{4}concentration stabilization within 0.5 to 0.6% led to a 3-time increase in the zinc yield from the pulp, according to the polynomial law (from 28 to 91%). The obtained results expand the idea of the mechanism of the strength gain by the filling mass under mechanical activation on the components of the filling mixture, as well as changes in the efficiency of zinc leaching at different ratios of two types of lixiviants (sulphuric acid and sodium chloride) in the leaching solution.

## 1. Introduction

^{2}) halos of chemical pollution of soils, watercourses and their sediments have been formed.

_{2}SO

_{4}and HCl in [33]). Chalcopyrite grinding into a pin type vertical stirred mill leads to the fact that the Cu leaching kinetics (in terms of crystallinity) is 30% greater when treated with sulfuric acid than that treated with HCL (increase in the dissolution rate = 35 vs 25%). This confirms that the ratio of the concentrations of the two-component solutions on the final yield of polymetallic raw materials is an important factor, the influence of which is not fully understood.

## 2. Materials and Methods

_{2}—0.03%, Al

_{2}O

_{3}—0.8%, K

_{2}O—3.5%, Mn—0.015%, Cu—0.18%, Ag—0.015%, S—1.88%, CaO—1.96%, Fe

_{2}O

_{3}—4.4%, SiO

_{2}—31.4%. The Box-Behnken design scheme was implemented in the work in a similar manner [34].

^{−1}and 200 min

^{−1}(maximum shock rate—up to 240 m/s) for 60 min. The disintegrator consists of two rotors (corfs) rotating in opposite directions, mounted on separate coaxial shafts and enclosed in a casing (whose parts are locked with clamp 3), equipped with electric motors for two spaced-apart sections (2) of the device. Either two or four rows of round cylindrical pins are arranged along concentric circles on the rotor disks so that each row of one rotor freely enters between two rows of the other. The material is fed through a hopper (1) into the central part of the rotor and, moving to the periphery, it is subjected to multiple blows of pins rotating in opposite directions. The processed geomaterials were collected in container 5. The disintegration exposure time was selected based on the available experience, as well as experiments [35,36] on the enrichment of nickel, iron and cobalt. The work [37] found that during ore treatment with 20% sulfuric acid solution, from minute 60 to minute 120 min of enrichment, the Ni yield changed from 88% to 98%, Co—from 96% to 98%, and Fe—from 82% to 90%, which indicates the significance of the first hour of treatment to obtain Zn from the tailings.

_{2}SO

_{4}content as follows: h(H

_{2}SO

_{4}) = (2, 6 and 10 g/L); h(NaCl) = (20, 90 and 160 g/L). Therefore, 1 L of the standard solution was formed separately for each variant. The volume of water in the solution for each variant was determined as follows:

_{2}O) in a 1000 mL solution (based on the water density = 998.2 g/L at 20 °C). The total weight of the 1 L solution was then determined by simple addition:

_{S}) = 50 g, the weight of the liquid fractions (leaching solution—M

_{L}) was 200, 350 and 500 g, respectively. Next, the weights of the reagents in the total weight of the liquid fraction were determined as follows (using sulfuric acid as an example):

_{P}) in each case was determined by the simple addition of different M

_{L}and constant values of M

_{S}. An example of the results of the calculations and the plan of the experiments is shown in Table 1.

_{2}SO

_{4}); h (NaCl); g/L; solid fraction mass (ML); presence/absence of the disintegrator, activation time). To reduce this seven-dimensional problem to three three-dimensional problems, we proceeded from the following logic. The last most significant factor for us (disintegrator influence) was introduced into three separate response functions, while the activation and agitation leaching time was assumed to be constant (60 min), thereby removing it from the brackets: (I) without activation; (II) with a rotor speed of 50 min

^{−1}; (III) with a rotor speed of 200 min

^{−1}. One of the most difficult issues was reducing the dimension to two inside the brackets. For this purpose, all of the operations in Table 1 were carried out to transfer from volume concentrations in the leached mixture to the mass concentration in the treated pulp (see Table 2). At the same time, the experiment planning (the ratio of volume concentrations of lixivants) was carried out so that the experimental points were dispersed as widely as possible along the H

_{2}SO

_{4}plane, from 0.3 to 0.9%, and along the NaCl plane, from 1 to 13%.

^{−1}; (III) with rotor speed = 200 min

^{−1}.

## 3. Results

_{2}SO

_{4}concentration, from 0.2 to 0.9% (Figure 3), activates zinc leaching only at the optimal ratio with NaCl ≤ 1/10. If the NaCl fraction exceeds 6%, then an increase in the H

_{2}SO

_{4}from 0.2 to 0.9% does not lead to the expected effect. The local maximum Zn yield is in the range of 0.5–0.6% for H

_{2}SO

_{4}and 4–1% for NaCl. The excess of the H

_{2}SO

_{4}fraction above 0.7% reduces the Zn concentration from 82 to 55%. The reasons for such phenomenon need further clarification and specification.

_{2}SO

_{4}= 0.9%, the increase in the NaCl fraction, from 1 to 13%, leads to a monotonous decline in the zinc yield, from 55% to slightly less than 28%, which is slightly higher than H

_{2}SO

_{4}= 0.2% (slightly less than 19%). The area of the local maximum (Zn = 82%) is limited to 0.35 to 0.72% for H

_{2}SO

_{4}and from 1 to 2% for NaCl. As a result of the analysis of the data in Table 2, a polynomial dependence (Taylor series) of the zinc extraction rate on the parameters of the leaching solution (R

^{2}= 0.96) was established:

_{2}SO

_{4—}mass concentration of sulfuric acid according to pulp weight,%; NaCl—mass concentration of sodium chloride according to pulp weight,%.

^{2}= 0.98) to the test results. The linear trend equation has the form:

_{2}SO

_{4}concentration (0.2–0.4%), while the NaCl concentration should be ≤8%. The H

_{2}SO

_{4}change from 0.2 to 0.8% (NaCl—2–6%) leads to alternating changes in the Zn yield (from 91 to 55%). The increase in the H

_{2}SO

_{4}concentration from 0.2 to 0.9% affects the yield of Zn only at the ratio of NaCl ≤ 1/15. If the NaCl fraction exceeds 8%, the increase in H

_{2}SO

_{4}from 0.2 to 0.9% does not lead to significant changes. The first local maximum of the Zn fraction is in the range of 0.28% for H

_{2}SO

_{4}and 2–4% for NaCl, and the second, from 0.3 to 0.68% for H

_{2}SO

_{4}and 1–1.8% for NaCl.

_{2}SO

_{4}= 0.9%, the NaCl fraction increases from 1% to 13% and leads to a monotonous decline in the zinc yield, from 65% to slightly less than 19% and less, which is higher than during agitation leaching. The area of the local maximum (Zn of about 100%) is limited by the region, from 0.27 to 0.73% for H

_{2}SO

_{4}and from 1 to 43% for NaCl (when H

_{2}SO

_{4}≤ 0.4%), as well as from 1 to 2.4% for NaCl (when H

_{2}SO

_{4}is from 0.6 to 0.7%).

_{2}SO

_{4}(0.8–0.9%) and NaCl from 10 to 13%. The H

_{2}SO

_{4}change from 0.2 to 0.8% (NaCl = 10–13%) leads to an increase in the Zn yield (from 10 to 64%). The increase in the H

_{2}SO

_{4}concentration from 0.2 to 0.9% affects the yield of Zn only at NaCl ≤ 8%. The first local maximum of the Zn fraction is in the range between 0.5 and 0.6% for H

_{2}SO

_{4}and 1–2.5% for NaCl; the second is between 0.85 and 0.9% for H

_{2}SO

_{4}and 10–13% for NaCl.

^{−1}is sufficient for effective activation. In this regard, the dry mixture TsKhSh was subjected to disintegration with a rotor speed of 50 min

^{−1}before concrete mixing for at least an hour.

^{3}of the filling mass is shown in Table 3.

- -
- for the mass fraction of tailings (t) = 43% (800 kg), the logarithmic dependence of the filling strength on the hardening duration (R
^{2}= 0.98) is established:$${\mathrm{R}}_{\mathrm{c}}=1.78\mathrm{ln}\left(\mathrm{t}\right)-0.06,$$ - -
- for the mass fraction of tailings (t) = 44% (835 kg), the logarithmic dependence of the filling strength on the hardening duration (R
^{2}= 0.97) is established:$${\mathrm{R}}_{\mathrm{c}}=1.71\mathrm{ln}\left(\mathrm{t}\right)-0.19,$$ - -
- for the mass fraction of tailings (t) = 45% (860 kg), the logarithmic dependence of the bookmark strength on the hardening duration (R
^{2}= 0.97) is established:$${\mathrm{R}}_{\mathrm{c}}=1.52\mathrm{ln}\left(\mathrm{t}\right)-0.09,$$_{c}—compressive strength, MPa; t—strength gain duration, days.

## 4. Discussion

_{2}SO

_{4}(versus 0.5–0.6% for agitation leaching) when NaCl = from 2 to 4%, which significantly saves acid consumption. The analysis of the results of the first problem shows the general regularity of sodium chloride operation similar to studies [42,43]. In addition, study [37] revealed the effects of the mechanical processing (from 60 to 480 min

^{−1}) of nickel ore in the ball mill during the leaching of Ni, Fe and Co. The concentration of H

_{2}SO

_{4}varied between 200 and 400 g/L (at S/L—1/3), while approximately 80% of the total increase in the yield of the polymetallic raw materials was leached in the first 60 min. The difference for the minimum and maximum rotor frequency, in terms of the leaching efficiency, did not exceed 35%, which is confirmed by the use of low-speed mechanical exposure in our studies. In another similar study [44,45], the mechanical activation of the ore in the stirred ball milling was conducted with the rotor RPM from 110 to 428 min

^{−1}with subsequent exposure to H

_{2}SO

_{4}to obtain Cu. It was found that in the first 10% of the enrichment time, up to 80% of the productivity of leaching the metal from the pulp was achieved, while the difference in the productivity of Cu separation at low and high rotations did not exceed 42%. The results of the enrichment of bauxitic clay to obtain Li, Al, Fe and Mg during the calcination of the samples (600 °C)m with subsequent exposure to sulfuric acid at the ratio S/L = 1/5, are indirectly confirmed [46]. In general, the parameters of Zn leaching efficiency are confirmed by the results of studies conducted by foreign authors [47,48]. The considered problem was reflected in the works of mining experts [26,27].

## 5. Conclusions

- -
- for the first time, during agitation leaching, a decrease in the NaCl mass concentration, from 13 to 1% at the H
_{2}SO_{4}concentration from 0.5 to 0.6%, has been found to lead to the 3-time Zn yield increase (accompanied by the local maximum area formation (Zn = 91%) from the pulp, according to the polynomial dependence. - -
- at a low rotation speed of the disintegrator rotors, for the first time, the H
_{2}SO_{4}concentration decreased from 0.8 to 0.26% at a NaCl concentration from 3 to 4%, and has been established to lead to a Zn yield increase in the pulp, from 64 to 91%. At that, the local maximum area has been shifted towards a lower consumption of sulfuric acid and its area by an order of magnitude is higher than that in the case of agitation leaching. - -
- the amount of zinc concentration in the mechanically activated pulp is increased from three to four times, with a decrease in the concentration of sodium chloride and an increase in the fraction of sulfuric acid in the leaching solution.
- -
- the peculiarities of the strength gain mechanism by the filling mass caused by the effect of mechanical activation on the components of the mixture composition include the increase in the mass uniaxial compression strength according to the logarithmic law to the required values, and the main increase in the strength characteristics is achieved during the first 28 days of hardening.

^{−1}and 200 min

^{−1}; the sulfuric acid content in the leaching solution ranging between 2 and 10 g/L; the leaching solution content of sodium chloride ranging from 20 to 160 g/L; the ratio of solid and liquid fractions (S/L) ranging between 1/4 and 1/10. The obtained results determine the need for further research on using disintegrators to increase the metal leaching productivity when using various types of lixiviants (for example, HCl, HNO

_{3}or other acids).

## Author Contributions

## Funding

## Institutional Review Board Statement

## Informed Consent Statement

## Data Availability Statement

## Conflicts of Interest

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**Figure 1.**Laboratory device for mechanical activation of geomaterials: 1—hopper for the initial material; 2—disintegrator section with the electric motor; 3—clamping device; 4—control block; 5—storage capacity.

**Figure 2.**Laboratory bench for sample testing on the IP-1250press: 1—disintegrator; 2—cubic sample; 3—press control unit.

N | h (H _{2}SO_{4}) | h (NaCl) | V (H _{2}SO_{4}) | V (NaCl) | V (H _{2}O) | h (H _{2}O) | M_{L} | S/L | M_{L} | m_{L}(H _{2}SO_{4}) | m_{L}(NaCl) | M_{P} |
---|---|---|---|---|---|---|---|---|---|---|---|---|

g/L | g/L | mL | mL | mL | g/L | g | g | g | g | g | ||

1 | 2 | 20 | 1.1 | 9.2 | 989.7 | 987.9 | 1009.9 | 1/4 | 200 | 0.40 | 3.96 | 250 |

2 | 10 | 20 | 5.5 | 9.2 | 985.3 | 983.5 | 1013.5 | 1/4 | 200 | 1.97 | 3.95 | 250 |

3 | 2 | 160 | 1.1 | 73.9 | 925.0 | 923.3 | 1085.3 | 1/4 | 200 | 0.37 | 29.48 | 250 |

4 | 10 | 160 | 5.5 | 73.9 | 920.6 | 918.9 | 1088.9 | 1/4 | 200 | 1.84 | 29.39 | 250 |

5 | 2 | 20 | 1.1 | 9.2 | 989.7 | 987.9 | 1009.9 | 1/10 | 500 | 0.99 | 9.90 | 550 |

6 | 10 | 20 | 5.5 | 9.2 | 985.3 | 983.5 | 1013.5 | 1/10 | 500 | 4.93 | 9.87 | 550 |

7 | 2 | 160 | 1.1 | 73.9 | 925.0 | 923.3 | 1085.3 | 1/10 | 500 | 0.92 | 73.71 | 550 |

8 | 10 | 160 | 5.5 | 73.9 | 920.6 | 918.9 | 1088.9 | 1/10 | 500 | 4.59 | 73.47 | 550 |

9 | 6 | 90 | 3.3 | 41.6 | 955.1 | 953.4 | 1049.4 | 1/7 | 350 | 2.00 | 30.02 | 400 |

10 | 6 | 20 | 3.3 | 9.2 | 987.5 | 985.7 | 1011.7 | 1/4 | 200 | 1.19 | 3.95 | 250 |

11 | 6 | 160 | 3.3 | 73.9 | 922.8 | 921.1 | 1087.1 | 1/4 | 200 | 1.10 | 29.44 | 250 |

12 | 6 | 20 | 3.3 | 9.2 | 987.5 | 985.7 | 1011.7 | 1/10 | 500 | 2.97 | 9.88 | 550 |

13 | 6 | 160 | 3.3 | 73.9 | 922.8 | 921.1 | 1087.1 | 1/10 | 500 | 2.76 | 73.59 | 550 |

14 | 2 | 90 | 1.1 | 41.6 | 957.3 | 955.6 | 1047.6 | 1/7 | 350 | 0.67 | 30.07 | 400 |

15 | 10 | 90 | 5.5 | 41.6 | 952.9 | 951.2 | 1051.2 | 1/7 | 350 | 3.33 | 29.97 | 400 |

N | m_{P} (H_{2}SO_{4}) | m_{P} (NaCl) | Experiment | ||
---|---|---|---|---|---|

% | % | (I) | (II) | (III) | |

1 | 0.16 | 1.58 | 45 | 27 | 32 |

2 | 0.79 | 1.58 | 70 | 79 | 61 |

3 | 0.15 | 11.79 | 11 | 11 | 13 |

4 | 0.73 | 11.75 | 28 | 28 | 27 |

5 | 0.18 | 1.80 | 49 | 47 | 42 |

6 | 0.90 | 1.79 | 50 | 55 | 53 |

7 | 0.17 | 13.40 | 16 | 6 | 12 |

8 | 0.83 | 13.36 | 19 | 16 | 65 |

9 | 0.50 | 7.50 | 43 | 32 | 27 |

10 | 0.47 | 1.58 | 87 | 97 | 81 |

11 | 0.44 | 11.77 | 28 | 21 | 7 |

12 | 0.54 | 1.80 | 88 | 99 | 82 |

13 | 0.50 | 13.38 | 27 | 21 | 15 |

14 | 0.17 | 7.52 | 20 | 40 | 31 |

15 | 0.83 | 7.49 | 38 | 38 | 23 |

N | Concrete | Tailings | Slag | Water | Strength Gain Duration, Days | |||||
---|---|---|---|---|---|---|---|---|---|---|

kg | kg | kg | kg | 3 | 7 | 28 | 60 | 90 | 180 | |

1 | 130 | 800 | 450 | 400–450 | 1.8 | 3.9 | 5.5 | 6.8 | 8 | 9.6 |

2 | 115 | 835 | 430 | 400–450 | 1.6 | 3.7 | 5 | 6.4 | 7.5 | 9.2 |

3 | 100 | 860 | 420 | 400–450 | 1.5 | 3.3 | 4.6 | 5.7 | 6.9 | 8.1 |

Pb | Zn | TiO_{2} | Al_{2}O_{3} | K_{2}O | Mn | Cu | Ag | S | CaO | Fe_{2}O_{3} | SiO_{2} | |
---|---|---|---|---|---|---|---|---|---|---|---|---|

I | 0.84 | 0.95 | 0.03 | 0.80 | 3.50 | 0.02 | 0.18 | 0.02 | 1.88 | 1.96 | 4.40 | 31.40 |

II | 0.35 | 0.51 | 0.02 | 0.56 | 2.63 | 0.01 | 0.14 | 0.01 | 1.32 | 1.31 | 3.96 | 21.98 |

T, % | Formula | R^{2} |
---|---|---|

43 | ${\mathrm{R}}_{\mathrm{c}}=1.78\mathrm{ln}\left(\mathrm{t}\right)-0.06$ | 0.98 |

44 | ${\mathrm{R}}_{\mathrm{c}}=1.71\mathrm{ln}\left(\mathrm{t}\right)-0.19$ | 0.97 |

45 | ${\mathrm{R}}_{\mathrm{c}}=1.52\mathrm{ln}\left(\mathrm{t}\right)-0.09$ | 0.97 |

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## Share and Cite

**MDPI and ACS Style**

Golik, V.I.; Klyuev, R.V.; Martyushev, N.V.; Brigida, V.; Efremenkov, E.A.; Sorokova, S.N.; Mengxu, Q.
Tailings Utilization and Zinc Extraction Based on Mechanochemical Activation. *Materials* **2023**, *16*, 726.
https://doi.org/10.3390/ma16020726

**AMA Style**

Golik VI, Klyuev RV, Martyushev NV, Brigida V, Efremenkov EA, Sorokova SN, Mengxu Q.
Tailings Utilization and Zinc Extraction Based on Mechanochemical Activation. *Materials*. 2023; 16(2):726.
https://doi.org/10.3390/ma16020726

**Chicago/Turabian Style**

Golik, Vladimir I., Roman V. Klyuev, Nikita V. Martyushev, Vladimir Brigida, Egor A. Efremenkov, Svetlana N. Sorokova, and Qi Mengxu.
2023. "Tailings Utilization and Zinc Extraction Based on Mechanochemical Activation" *Materials* 16, no. 2: 726.
https://doi.org/10.3390/ma16020726