CN102094126B - Process for smelting zinc with wet method of high temperature and high acid-jarosite iron removing-iron vitriol slag pickling by two stages - Google Patents
Process for smelting zinc with wet method of high temperature and high acid-jarosite iron removing-iron vitriol slag pickling by two stages Download PDFInfo
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Abstract
The invention provides a process for smelting zinc with a wet method of high temperature and high acid-jarosite iron removing-iron vitriol slag pickling at two stages, belonging to the technical field of non-ferrous metal smelting. The process comprises the following steps of neutral leaching, acid leaching at the first stage, acid leaching at the second stage, pre-neutralizing, settling vitriol and pickling to obtain zinc metal with a high recovery rate. The total recovery rate of zinc metal is 94.45%. The loss of valuable metal in iron vitriol slag is less, the recovery rate of metal is high, and the pollution of vitriol slag to the environment is improved.
Description
Technical field
The invention belongs to the non-ferrous metal metallurgy technical field, relate to a kind of Zinc hydrometallurgy process, relate in particular to a kind of two sections high temperature peracid-low pollution jarosite deironing
-Iron vitriol slag pickling Zinc hydrometallurgy process.
Background technology
The production technology of zinc is divided into pyrogenic process and zinc hydrometallurgy.Current have 80% zinc to originate from wet method.The zinc hydrometallurgy main method has methods such as conventional lixiviation process, hot acid lixiviation process and zinc ore concentrate pressure leaching process, zinc ore concentrate normal pressure lixiviation process, the direct leaching of zinc oxide ore.In the past, one of main drawback of zinc hydrometallurgy is that zinc recovery is low.Now, Zinc Hydrometallurgy Technology has large development, mainly is to improve the recovery and raw material comprehensive utilization aspect, production process mechanize and robotization control, and some difficult point technology are resolved in succession.
At present, the most employing of zinc hydrometallurgy factory in the world leached flow process continuously again, and promptly one section is neutral the leaching, and second section is that acidity leaches or hot acid leaches.Acid leached mud is generally handled by the fire reduction volatilization and is reclaimed zinc.The conventional flow process zinc roasted ore that leaches adopts one section neutral leaching, second section acid leaching, and acid slag is used pyrogenic attack.Recovery rate of valuable metals in the leached mud (%) is as follows: Zn90～92; In80～85; Pb82～84; Ca90～92:Cd90～92.This shows that slag contains the zinc height, the recovery is low; The pyrogenic process environment of system is seriously polluted; Fuel cost is high.
Chinese patent 200610101223.2 discloses a kind of low pollution vanadium settling iron-removing wet zinc smelting method; This method comprises that mainly neutral leaching, low temperature pre-neutralization, high temperature peracid leach and four process steps of low pollution vanadium settling iron-removing; Before low pollution vanadium settling iron-removing, leach through the high temperature peracid earlier, iron is leached out to greatest extent; Adjust the composition of solution then through the low temperature pre-neutralization, so that in heavy alum process, need not add just deironing satisfactorily of neutralizing agent.This technology is suitable for handling the zinc ore concentrate of complicated component, improves metal recovery rate, strengthens the ability that removes impurity, improves end product quality, reduces raw and auxiliary material and energy consumption, reduces and pollutes, and is beneficial to environment protection, is convenient to the comprehensive recovery of valuable metal etc.But the recovery of this technology zinc is lower, and the insoluble zinc of iron vitriol slag is higher.
Summary of the invention
It is lower to the objective of the invention is to be directed against existing zinc hydrometallurgical processes leaching yield, and two slags contain the zinc height, and the problem that metal recovery rate is low provides a kind of two sections high temperature peracid-low jarosite deironing-iron vitriol slag pickling Zinc hydrometallurgy process that pollutes.
Two sections high temperature peracid of the present invention-low jarosite deironing-iron vitriol slag pickling Zinc hydrometallurgy process that pollutes may further comprise the steps:
(1) neutral leaching: zinc baking sand is leached with the electrowinning zinc waste liquid is neutral: solid-to-liquid ratio is 1:8 ~ 10, beginning acid 60～80 g/L, whole sour pH=5.2～5.4,60～70 ℃ of temperature, 1.5 ~ 2 hours time;
The neutral supernatant that leaches contains zinc 155～165 g/L, Fe ﹤ 0.03 g/L.Supernatant extracts zinc through purification, electrodeposition; Leach underflow liquid and get into the acidleach operation;
(2) one sections acidleach: in neutrality leaching underflow liquid, add sulfuric acid and carry out one section acidleach: beginning acid 40～90 g/L, eventually sour 20～35 g/L, 85 ~ 90 ℃ of temperature, 2 ~ 3 hours time;
The content of Fe is 5 ~ 15 g/L in the supernatant of one section acidleach.The one section dense back of acidleach supernatant gets into pre-neutralization technology, and underflow liquid gets into the two-stage acid leaching operation;
(3) two-stage acid leaching: in one section acidleach underflow liquid, add sulfuric acid, the electrowinning zinc waste liquid carries out two-stage acid leaching: solid-to-liquid ratio is 1:12 ~ 15, beginning acid 80～130 g/L, acid 50～100 g/L eventually, 90 ~ 95 ℃ of temperature, 4 ~ 6 hours time;
The content of Fe is 13 ~ 25 g/L in the supernatant of two-stage acid leaching.The dense back of two-stage acid leaching supernatant gets into one section acidleach operation, and underflow liquid obtains plumbous silver-colored slag after washing through second adverse current, and filtrating continuation gets into the two-stage acid leaching operation;
(4) pre-neutralization: in the supernatant of one section acidleach, add zinc baking sand and carry out pre-neutralization: solid-to-liquid ratio is 1:10 ~ 12, beginning acid 20～35g/L, eventually sour 8～13 g/L, 60 ~ 70 ℃ of temperature, 2 ~ 3 hours time;
Fe content is 5 ~ 15 g/L in the supernatant of pre-neutralization.The dense back of pre-neutralization underflow liquid gets into one section acidleach operation; Supernatant gets into heavy alum operation;
(5) precipitating alum and removing iron: in the pre-neutralization supernatant, add bicarbonate of ammonia and carry out deironing: solid-to-liquid ratio is 1:8 ~ 10 beginnings acid, 8～13 g/L, eventually sour 8～20 g/L, 90 ~ 100 ℃ of temperature, 5 ~ 6 hours time;
Fe ﹤ 2 g/L in the supernatant of precipitating alum and removing iron.After heavy alum was dense, supernatant got into the neutral operation that leaches; Underflow liquid gets into pickling process;
(6) pickling: adding electrowinning zinc waste liquid, the vitriol oil carry out pickling in heavy alum underflow liquid, and solid-to-liquid ratio is 1:6 ~ 8, beginning acid 60～100 g/L, eventually sour 30～70 g/L, 85 ~ 90 ℃ of temperature, 4 ~ 5 hours time;
Content 3 ~ 8 g/L of Fe in the supernatant of pickling.The dense back of pickling supernatant gets into one section acidleach operation, and underflow liquid obtains iron vitriol slag after washing through second adverse current, and it is dense that filtrating gets into pickling.
The present invention is relative, and prior art has the following advantages:
1, zinc leaching rate is high, metal recovery rate high (total yield reaches 94.45%);
2, the application of iron vitriol slag acid cleaning process has further reduced the insoluble zinc of iron vitriol slag (less than 3%);
3, need not add neutralizing agent in the heavy alum process, precipitablely go out purer iron vitriol slag, the slag iron content is higher, and it is less to contain the valency metal;
4, the loss of valuable metal is less in the iron vitriol slag, can improve the pollution of alum slag to environment, and metal recovery rate is high;
5, the application of this technology, the anti-silicon ability that makes system bring up to 4.0% from 3.0%, have increased substantially the flexibility of system to raw material;
6, iron vitriol slag filters and adopts second adverse current washing pulp, makes slag contain acid and reduces significantly, has reduced the pollution of iron vitriol slag to environment.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Embodiment
Two sections high temperature peracid-low jarosite deironing-iron vitriol slag pickling Zinc hydrometallurgy process that pollute may further comprise the steps:
(1) the neutral leaching
The neutral operation that leaches is provided with a title groove i.e. (oxidation trough), five series connection, with the leaching vat of an overflow groove connection, the thickener of two ￠ 21m.
Waste electrolyte, low overflow, Manganse Dioxide ore pulp, lean cadmium solution, the anode sludge that pollutes jarosite separation thickener of modified form are processed even oxidation liquid in a groove.Oxidation liquid is with being pumped to first leaching vat, and adds quantitative calcining.In the first leaching vat overflow place pH appearance is housed, regulates the oxidation flow quantity automatically.The first leaching vat ore pulp overflow gets into second leaching vat, and the zinc oxide in the calcining dissolves fully, and oxidation of divalent becomes ferric iron.The whole acid of second leaching vat is not less than 13 g/L.In soak operation pH control be to accomplish at the 3rd leaching vat, the calcining amount that adds this groove is through a pH meter control.Through the 5th leaching vat to guarantee the required reaction times.In soak the back ore pulp and get into thickener and carry out solid-liquid separation, the overflow supernatant purifies the back electrodeposition and extracts zinc by being pumped to cleaning section, underflow pumps into one section hot acid and soaks operation.
Neutral leaching-out technique condition: solid-to-liquid ratio is 1:8 ~ 10, beginning acid 60～80 g/L, whole sour pH=5.2～5.4,60～70 ℃ of temperature, 1.5～2 hours time.The neutral supernatant composition that leaches is: Zn:155～165g/L; Fe: ﹤ 0.03 g/L; Cu:0.17 g/L; Cd:0.38 g/L.
(2) one sections hot acid acidleach
The equipment of one section hot acid leaching operation is with interconnected four the placed in-line leaching vat of overflow groove and a ￠ 15m thickener.In soak thickener underflow and pre-neutralization thickener underflow by being pumped to first groove, required acid-containing solution is from the overflow of two-stage acid leaching thickener.In first groove overflow place an automatic acidity analyser is housed, adds the solution amount of first groove with control.After four platform troughs leached, ore pulp got into thickener, its supernatant liquid pump to pre-neutralization operation, first groove of underflow pump to two-stage acid leaching.
The processing condition of one section acidleach technology: solid-to-liquid ratio is 1:10 ~ 12, beginning acid 40～90 g/L, and acid 20～35 g/L eventually, temperature is more than 85 ~ 90 ℃, 2 ~ 3 hours time.
In the supernatant of one section acidleach, Fe content is 5 ~ 15 g/L.
(3) two sections high acidleach of high temperature
Two-stage acid leaching equipment is four series connection leaching vat and a ￠ 15m thickener.One section acidleach thickener underflow pumps into first groove, leaches with the waste electrolyte and the vitriol oil; After four platform troughs leached, ore pulp flowed into thickener through chute, thickener underflow after filtering plumbous silver-colored slag, section acidleach of overflow supernatant pump to.
The two-stage acid leaching technical qualification: solid-to-liquid ratio is 1:12 ~ 15, beginning acid 80～130 g/L, eventually sour 50～100 g/L, 90 ~ 95 ℃ of temperature, 4 ~ 6 hours time.
Fe in the supernatant behind the two-stage acid leaching: 13 ~ 25 g/L.
(4) pre-neutralization
The purpose of pre-neutralization is the acidity that reduces from one section acidleach thickener overflowing liquid, and low to pollute the jarosite deironing be 1.5 ~ 2.0 processing condition at pH to meet next step modified form.This operation is provided with the reactive tank of couplet in three and the thickener of a ￠ 15m.One section acidleach thickener overflow supernatant liquid pump to the first groove; And add quantitative calcining at this; The calcining amount that an automatic acidity analyser adds with adjustment is equipped with in first groove overflow outlet, and through after second groove, the three-flute reaction, ore pulp gets into thickener again; Thickener overflow supernatant pump is to low jarosite operation, underflow pump to section acidleach first groove of polluting.
The solid-to-liquid ratio technical qualification: solid-to-liquid ratio is 1:10 ~ 12, beginning acid 20～35g/L, eventually sour 8～13 g/L, 60 ~ 70 ℃ of temperature, 2 ~ 3 hours time.Contain Fe: 5 ~ 12g/L in the supernatant of solid-to-liquid ratio.
(5) the low heavy iron of jarosite that pollutes
This operation is provided with seven cascade reaction grooves, interconnects a ￠ 21m with an overflow chute and separates thickener.The dense overflow supernatant of pre-neutralization, bicarbonate of ammonia pulp liquid add first groove simultaneously; After the reaction through seven leaching vat; Ore pulp gets into thickener; Thickener overflow supernatant liquid pump in soak the operation oxidation trough, low first groove that pollutes the jarosite reactive tank of underflow 1/3rd pumps to modified form is as crystal seed, all the other pump into iron vitriol slag pickling first groove.
The low jarosite control condition of polluting: solid-to-liquid ratio is 1:8 ~ 10, beginning acid 8～13 g/L, whole acid 8～20 g/L, 90 ~ 100 ℃ of temperature, time 5-6 hour.
The supernatant of the heavy iron of siderotil contains Fe ﹤ 2 g/L.
(6) iron vitriol slag pickling
The iron vitriol slag pickling installation is three series connection leaching vat and a ￠ 15m thickener.The low pollution of modified form jarosite thickener underflow pumps into first groove and leaches with the waste electrolyte and the vitriol oil, and after three platform troughs leached, ore pulp flowed into thickener through chute, and thickener underflow gets iron vitriol slag, section acidleach of overflow supernatant pump to after filtering.
Iron vitriol slag pickling technical qualification: solid-to-liquid ratio is 1:6 ~ 8, beginning acid 60～100 g/L, eventually sour 30～70 g/L, 85 ~ 90 ℃ of temperature, 4 ~ 5 hours time.
Contain Fe:3 ~ 8 g/L in the iron vitriol slag acid supernatant.
Through above-mentioned process step, the total yield of zinc metal is 94.45%; The insoluble zinc of iron vitriol slag is 4.5%, and the insoluble zinc of plumbous silver-colored slag is less than 3%.
Claims (1)
1. two sections high temperature peracid-jarosite deironing-pickling Zinc hydrometallurgy process may further comprise the steps:
(1) neutral leaching: zinc baking sand is leached with the electrowinning zinc waste liquid is neutral: solid-to-liquid ratio is 1:8 ~ 10, beginning acid 60～80 g/L, whole sour pH=5.2～5.4,60～70 ℃ of temperature, 1.5 ~ 2 hours time; Supernatant extracts zinc through purification, electrodeposition; Leach underflow liquid and get into the acidleach operation;
(2) one sections acidleach: in neutrality leaching underflow liquid, add sulfuric acid and carry out one section acidleach: beginning acid 40～90 g/L, eventually sour 20～35 g/L, 85 ~ 90 ℃ of temperature, 2 ~ 3 hours time; The one section dense back of acidleach supernatant gets into pre-neutralization technology, and underflow liquid gets into the two-stage acid leaching operation;
(3) two-stage acid leaching: in one section acidleach underflow liquid, add sulfuric acid, the electrowinning zinc waste liquid carries out two-stage acid leaching: solid-to-liquid ratio is 1:12 ~ 15, beginning acid 80～130 g/L, acid 50～100 g/L eventually, 90 ~ 95 ℃ of temperature, 4 ~ 6 hours time; The dense back of two-stage acid leaching supernatant gets into one section acidleach operation, and underflow liquid obtains plumbous silver-colored slag after washing through second adverse current, and filtrating continuation gets into the two-stage acid leaching operation;
(4) pre-neutralization: in the supernatant of one section acidleach, add zinc baking sand and carry out pre-neutralization: solid-to-liquid ratio is 1:10 ~ 12, beginning acid 20～35g/L, eventually sour 8～13 g/L, 60 ~ 70 ℃ of temperature, 2 ~ 3 hours time; The dense back of pre-neutralization underflow liquid gets into one section acidleach operation; Supernatant gets into heavy alum operation;
(5) precipitating alum and removing iron: in the pre-neutralization supernatant, add bicarbonate of ammonia and carry out deironing: solid-to-liquid ratio is 1:8 ~ 10, beginning acid 8～13 g/L, eventually sour 8～20 g/L, temperature 90-100 ℃, 5 ~ 6 hours time; After heavy alum was dense, supernatant got into the neutral operation that leaches; Underflow liquid gets into pickling process;
(6) pickling: adding electrowinning zinc waste liquid, the vitriol oil carry out pickling in heavy alum underflow liquid, and solid-to-liquid ratio is 1:6 ~ 8, beginning acid 60～100 g/L, eventually sour 30～70 g/L, 85 ~ 90 ℃ of temperature, 4 ~ 5 hours time; The dense back of pickling supernatant gets into one section acidleach operation, and underflow liquid obtains iron vitriol slag after washing through second adverse current, and it is dense that filtrating gets into pickling.
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| CN102676805B (en) * | 2012-05-30 | 2013-05-01 | 巴彦淖尔紫金有色金属有限公司 | Low grade zinc concentrate associated lead and silver recovery process |
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| CN103952572B (en) * | 2014-05-22 | 2015-11-25 | 北京矿冶研究总院 | Method for optimizing zinc hydrometallurgy hot acid leaching process by pressure leaching |
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| CN107604180A (en) * | 2017-09-07 | 2018-01-19 | 湖南三立集团股份有限公司 | A kind of zinc hydrometallurgy purifying and impurity-removing method |
| CN111069232A (en) * | 2019-12-10 | 2020-04-28 | 赤峰中色锌业有限公司 | Method for washing and recovering zinc from zinc hydrometallurgy jarosite slag and innocent treatment of recovered slag |
| CN114517258A (en) * | 2022-01-11 | 2022-05-20 | 云南云铜锌业股份有限公司 | Two-stage zinc hydrometallurgy leaching method for improving copper recovery rate |
| CN114737064A (en) * | 2022-03-17 | 2022-07-12 | 云南云铜锌业股份有限公司 | Zinc jarosite hydrometallurgy method |
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| CN1080265A (en) * | 1993-04-09 | 1994-01-05 | 洛阳蓝天化工厂 | The full wet method of improved bicarbonate of ammonia is produced high-active zinc oxide |
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| CN101838745A (en) * | 2010-04-15 | 2010-09-22 | 赤峰中色库博红烨锌业有限公司 | Zinc hydrometallurgy process with high yield by precipitating alum and removing iron |
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| CN1080265A (en) * | 1993-04-09 | 1994-01-05 | 洛阳蓝天化工厂 | The full wet method of improved bicarbonate of ammonia is produced high-active zinc oxide |
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