I. Leaching method and technical conditions
Antimony sulfide ore, lead ore concentrates Jamesonite chloride - split-cycle leach leaching process leaching and acyclic forms. A # is the leaching cycle - as a chlorinating agent is necessary leaching embodiment leaching agent: A # as chlorinating agent must be prepared by the leaching agent is regenerated and returned. Chlorine leaching is a non-circulating leaching, the leaching conditions are: (1) to ensure the free acidity of 2.5 ~ 3.0mol ∕ L, can also use NaCl to replace part of the free acid; (2) reaction temperature of 80 ~ 85 ° C; (3) reaction time 2.0 ~ 4.0 h; (4) the amount of chlorine gas, the leaching end of the leaching solution containing Sb 5 + 10g ∕ L; (5) must be washed with 2.0 ~ 2.5mol · dm -3 acid leaching slag 3 to 5 times, then washed 3 ~ 5 times. The circulating leaching conditions are: (1) the excess coefficient of the chlorinating agent is 0.1 to 0.15; (2) the number of fractions of the leaching solution, calculated according to the relevant formula, for a single strontium sulfide ore, generally about 60%, and for the brittle sulphur bismuth ore concentrate Mines are as high as 72% to 75%: (3) leaching agent acidity: HCl 1.5 ~ 2.0mol ∕ L; H 2 SO 4 0.75 ~ 1.0mol ∕ L, H 2 SO 4 is mainly used to inhibit lead into the leachate; 4) The temperature and time are the same as the general leaching; (5) The leaching end point is judged: the leaching solution is reddish brown, and Sb 5 + 5 to 10 g/L is taken as the standard. (6) using mixed acid washing slag, acid acidity is the same as leaching agent, the amount is equal to the amount of leaching liquid in the open circuit; (7) after pickling, the leaching slag is washed 3 to 5 times, and the washing water is 50% of the concentrate. The acid washing is prepared from the returned hydrolyzate or leaching water washing solution and concentrated hydrochloric acid and concentrated sulfuric acid (used in the treatment of high lead bismuth concentrate). According to their acidity and the volume of acid to be mixed, a binary or ternary triplet is established. The group, the solution can be used to find their respective usage. In this way, acid is used, and complex antimony ore can save more than 40% of acid, and a single antimony ore can save more than 30% of acid, and reduce wastewater discharge.
Second, the leaching process practice and equipment
Leaching Leaching cyclic operation as an example: the leaching process, including configuration and A # regeneration of the chlorinating agent, plus mineral, heat, stirring, filtering and washing step forty. A # chlorinating agent prepared by the regeneration liquid before the leachate and returned all the acid wash, to check its main component, the acidity and volume to meet the requirements, i.e., chlorine gas, and the regeneration rate ([Sb 5 +] / [ Sb] T) When ≥95%, regeneration is completed. The leaching and regeneration are carried out in the same reactor. After the regeneration is completed, the ore leaching can be carried out, and a large amount of heat is released by leaching and regeneration, so that the speed of chlorine and ore is accelerated. Cooling measures must be taken to remove excess heat. Generally, an enamel reaction kettle (with a jacket) is used as the leaching and regeneration tank, and a reaction tank made of other corrosion-resistant materials can also be used, but a cooling and heat-discharging device must be attached. The leaching tank cover is provided with four uniformly distributed chlorine pipes made of steel pipes with polytetraethylene inside, and the exhaust pipes are exhausted by the exhaust fan. During the leaching process, maintain a temperature of about 80-85 ° C, check whether it reaches the end point, if the leaching solution is grayish white, the oxidant is not enough, need to supplement the oxygen, make the leaching solution turn brown red, and Sb 5 + is 5 ~ 10g ∕L It can be filtered, and the filtration can be carried out on a vacuum suction tank or a belt filter; since it is pickled and washed, it is not filtered by a filter press. If it is a filter belt, it is necessary to set a filter section, a pickling section and a water washing section, and the filter residue is automatically removed after washing, and the labor intensity is small. When the filter is filtered by the suction filter, the leaching solution is just filtered, but the filter residue is pickled before it is cracked, so that it is washed 3 to 5 times; after the acid wash is completed, it is washed with water. Of course, filtration with a suction filter tank is much more labor intensive.
Third, the leaching process technical data and indicators
The actual production data of the cyclic chlorination-leaching of the brittle bismuth lead ore is taken as an example. The composition of concentrate, leaching residue, immersion liquid, pickling liquid and water washing liquid is as follows.
Table leaching process raw materials and product chemical composition
name | Sb | Pb | Zn | Fe | Cu | Ag | Mn | As |
Concentrate ∕% | 29.41 | 34.94 | 3.92 | 8.69 | 0.12 | 0.07 | 0.16 | 0.58 |
Leaching solution (g·L -1 ) | 323.33 | 1.96 | 29.83 | 71.31 | 0.57 | 0.56 | 2.42 | 0.355 |
Leaching residue % | 0.80 | 49.29 | 0.652 | 3.69 | 0.058 | 0.0219 | 0.015 | 0.817 |
Pickling solution g (g·L -1 ) | 138.91 | 1.66 | - | 37.36 | - | 0.196 | - | - |
Washing liquid ∕ (g·L -1 ) | 18.69 | 1.14 | - | 8.66 | - | 0.024 | - | - |
Continued on the table
name | Ca | Sn | Mg | Bi | In | S(SO 4 2- ) | Cl - | H + |
Concentrate ∕% | 1.03 | 0.46 | 0.048 | 0.017 | 0.0026 | 31.33 | - | - |
Leaching solution (g·L -1 ) | 0.23 | 0.16 | 0.83 | - | 0.006 | (32.98) | 488.39 | 2.504 |
Leaching residue % | 0.82 | 0.317 | 0.002 | 34.92 | 11.69 | |||
Pickling solution g (g·L -1 ) | - | - | - | - | - | (70.23) | 252.36 | - |
Washing liquid ∕ (g·L -1 ) | - | - | - | - | - | (21.95) | 67.69 | - |
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