CN102719668B - Technology for extracting zinc, lead and silver step by step by processing zinc-leached residues by full wet process - Google Patents
Technology for extracting zinc, lead and silver step by step by processing zinc-leached residues by full wet process Download PDFInfo
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Abstract
The invention relates to a technology for extracting zinc, lead and silver step by step by processing zinc-leached residues by a full wet process, and belongs to the technical field of zinc-leached residue recycle. The technology comprises the following steps of: preparing sulfuric acid into an appropriate concentration, and performing two-stage acid leaching in an appropriate liquid-solid ratio and at a high temperature to obtain slurry; filtering and separating the slurry to obtain lead-silver residues and a zinc-containing solution; oxidizing, neutralizing and deironing the zinc-containing solution, and depositing zinc by using sodium sulphide; and eluting the lead-silver residues, blending with caustic lye at an appropriate concentration to obtain slurry at a certain concentration, reacting at a certain temperature and in a certain solid-liquid ratio, and filtering and separating to obtain a filter cake and a filtrate, wherein the filtrate is directly added with sodium sulphide for lead deposition and the filter cake returns to a silver cyaniding leaching process. The technology is short in process, simple in operation, low in cost and mild and loose in reaction conditions; an acid solution and an alkali solution at high concentrations are not required; requirements on equipment are low; the extraction rate of metal is higher than that in the conventional method; no additional waste solid, waste liquid and waste gas are discharged; the recycle of the eluate and the filtrate is realized; and environment pollution is avoided from the source.
Description
Technical field
The present invention relates to the technique of a kind of Whote-wet method process zinc leaching residue step by step arithmetic zinc, lead, silver, belong to zinc leaching residue recovery technology field.
Background technology
The great majority employing of current zinc hydrometallurgy factory leaches flow process continuously again, is generally two sections of leachings, and through above-mentioned two-stage leaching process, still high containing zinc in the leached mud of gained, in addition also containing silver and lead etc., utility value is higher.Its principal feature is that mineral granularity is thin, argillization phenomenon is serious, mineral composition is more complicated, heavy metal ion containing some amount.Owing to lacking suitable treatment technology means, storing up of a large amount of slag not only occupies cultivated land, containing plurality of heavy metal element in slag, and serious environment pollution.Current nonferrous metal price goes up, and Mineral resources are fewer and feweri.The wet method zinc smelting dreg quantity being rich in non-ferrous metal is large, containing in a large number can the valuable metal of synthetical recovery in slag, use value is higher, if will wherein separate by valuable metal, it can be used as the secondary recycling resource of non-ferrous metal but not waste is banked up, there is obvious Social benefit and economic benefit.Zinc smelting dreg is as a kind of composite multi-component metallic ore metallurgical slag, and in slag, the grade of zinc is at 5-20%, and plumbous grade is about 10%, and the grade of silver is at 200-600g/t.
In order to the valuable metal element in efficient recovery zinc leaching residue, experts and scholars both domestic and external conduct extensive research, and develop kinds of processes method, mainly concentrate on the following aspects: rotary kiln fuming volatilization method, and hot acid leaches heavy iron processes.Rotary kiln evaporation method is that China processes wet method zinc leaching residue typical process flow used.This technique is allocate coke or coal dust in zinc leaching residue after, and at revolution roasting in kilns, the cadmium in leached mud, indium, germanium are easy to volatilization, enter in oxide powder and zinc with gas cleaning, in flue dust, obtain enrichment, reclaim the valuable metals such as Pb, Cd, Zn, the metallic elements such as Ag, Fe, Ga enter kiln slag.By rotary kiln fuming volatilization can reclaim 92 ~ 94% zinc and 82 ~ 84% plumbous and about 10% silver, major part is silver-colored to be discarded, and causes Mineral resources to waste.This processing technological flow is longer, maintenance of equipment amount is large and requirement continues high temperature resistant, and investment is large, and Working environment is relatively poor, and equipment is huge, consume energy high, need to allocate into fire Coal and coke in a large number, refractory consumption rate is large, and oxide powder and zinc enter flow process before to first deviate from fluorine chlorine, containing sulfurous gas in rotary kiln flue gas, directly do not enter air yet, need purifying treatment.
It is make zinc leaching residue under the condition of high temperature, peracid that hot acid leaches heavy iron processes essence, obtains solution of zinc sulfate, after heavy alum iron purification, return original leaching system.The leaching yield of the method zinc is more than 95%, and the processing technological flow of slag is short, and invest less, energy consumption is low.But Slag treatment section liquor capacity large and in solution iron and dioxide-containing silica high, be unfavorable for the recovery of other metal, sulfur acid and heavy metal ion in waste, need to set up jumbo slag anti-leaking storehouse and store up, easily cause secondary pollution.
Patent at present for the method application of zinc leaching residue process has following several, as shown in table 1:
Table 1 is at present for the several method list of zinc leaching residue process
Summary of the invention
The invention provides the technique of a kind of Whote-wet method process zinc leaching residue step by step arithmetic zinc, lead, silver, this technological operation is simple, cost is low, reaction conditions is gentle loose, without the need to high concentrated acid alkali lye, the extraction yield of metal is high, and whole technique achieves the recycle of washing lotion, filtrate, avoids environmental pollution from source.
The technique of process zinc leaching residue step by step arithmetic zinc of the present invention, lead, silver, comprises the steps:
(1) carry out first paragraph leaching after mixing in normal-pressure reaction kettle with zinc leaching residue with low-concentration sulfuric acid solution, obtain slip;
(2) step (1) gained slurry filtration is obtained filter cake and filtrate, filter cake is without the need to washing, and filtrate oxidation neutralized ex iron after vulcanization sodium sinks zinc;
(3) carry out second segment leaching after filter cake step (2) obtained and the sulphuric acid soln of higher concentration mix in a kettle., obtain slip;
(4) by step (3) gained slurry filtration, the filter cake obtained washs, and returns step (1) first paragraph and leach operation by filtering the filtrate that obtains and recycle;
(5) filter cake after step (4) being washed and certain density caustic solution carry out alkali leaching after normal-pressure reaction kettle mixing, filter and obtain filter cake and filtrate;
(6) step (5) gained filter cake is not washed, without the need to adjust ph, directly return silver-colored industrial Cyanide Leaching operation; Namely the cyaniding leaching silver-zinc directly entering industry replaces silver-colored operation;
(7) step (5) gained filtrate being added appropriate sodium sulphite carries out heavy plumbous, obtains concentrate of lead sulfide ore after filtration, and filtrate returns step (5) alkali leaching operation and recycles after regulating with caustic alkali.
The mass percent concentration of the low-concentration sulfuric acid described in step (1) is 10 ~ 20wt.%, liquid-solid ratio 2 ~ 5:1, extraction time 2 ~ 4 hours, and extraction temperature is 80 ~ 90 DEG C.
The sulfuric acid concentration configured in step (1) is 10 ~ 20wt.%, and concentration can not be high, and excessive concentration can cause the high density of iron to leach.
The mass percent concentration of the sulphuric acid soln of the higher concentration described in step (3) is 20 ~ 40wt.%, liquid-solid ratio 2 ~ 5:1, extraction time 2 ~ 4 hours, and extraction temperature is 80 ~ 90 DEG C.
Sulfuric acid concentration preferably 25 ~ 30wt.% in step (3), because concentration is too low, the leaching yield of zinc is low, excessive concentration, has a lot of impurity and forms silica gel as silicon leaches, cause filtration difficulty.
Bath water described in step (4) is deionized water at normal temperature, and washing adopts the mode of static counter flow washing, and washing times is 2 ~ 4 times, and washing plant is mobile band filter.
The washing lotion that step (4) produces, for acid, directly return one section of Ore Leaching operation, realizes the recycle of washing lotion and filtrate after quantitative sulfuric acid.
Caustic sodium concentration described in step (5) is 15 ~ 40wt.%, liquid-solid ratio 2 ~ 4:1, and alkali extraction temperature is 80 ~ 90 DEG C, alkali extraction time 2 ~ 5 hours.
The add-on of the sodium sulphite described in step (7) and the mass ratio of lead ion are 1 ~ 2:1, and carry out at normal temperatures.
The alkali that the filtrate that step (7) obtains returns step (5) leaches splicer's sequence, realizes the recycle of mixed base, gets rid of without additional waste liquid.
Reaction principle is as follows:
Following reaction is there is in the normal-pressure reaction kettle that sulphuric leaching goes out:
ZnO·Fe
2O
3+4H
2SO
4＝ZnSO
4+Fe
2(SO
4)
3+4H
2O （1）
ZnO+H
2SO
4＝ZnSO
4+H
2O （2）
ZnO·SiO
2+H
2SO
4=ZnSO
4+H
2SiO
3 （3）
First paragraph leaches main based on equation (2) and (3), in lower acid concentration range, can not form silica gel, slip easily filters, in second segment acidleach process, acid concentration increases, franklinite decomposes, a large amount of stripping of zinc, and leach liquor returns one section of leaching again, by hydrolysis remove portion iron, the leaching yield of zinc reaches 80 ~ 90%.
In second segment leaching process, except above three reactions of generation, also may there is following reaction:
ZnO+ZnSO
4=ZnO·ZnSO
4 （4）
Raised with temperature by its thermodynamic property this reaction tendency known and raise, when temperature is greater than 100 DEG C, this reaction tendency is very large, the zinc in zinc lixiviating solution can be made to come back in slag, cause the loss of zinc, therefore in this invention, temperature, between 80 ~ 90 DEG C, is no more than 100 DEG C, both ensure that the leaching yield of higher zinc, in turn ensure that comparatively fast carrying out of reaction.
Lead sulfate and the Sulfuric acid disilver salt of plumbous and silver-colored generation are all water insoluble, and sulphuric leaching goes out process makes lead and silver obtain enrichment, and grade improves, and is conducive to next step extraction.Following reaction is there is in filter cake (lead smelting gas) and caustic solution in closed reactor:
This process silver and compound thereof do not participate in reaction, and in filter cake, silver obtains enrichment, and filter cake itself is in alkalescence, without the need to washing and adding alkali adjust ph, directly can return the cyaniding operation that silver is produced.
Beneficial effect of the present invention is as follows:
Present invention process flow process is short, simple to operate, cost is low, reaction conditions is gentle loose, without the need to high concentrated acid alkali lye, not high to equipment requirements, the extraction yield of metal is higher than traditional method, the leaching yield of zinc reaches 80 ~ 90wt.%, plumbous leaching yield can reach 88 ~ 98wt.%, and the leaching yield of silver reaches 85 ~ 95wt.%, and the three wastes that the whole technique of the present invention is not added are discharged, achieve the recycle of washing lotion, filtrate, avoid environmental pollution from source.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Zinc leaching residue 750g is added, wherein Zn content 9.36wt.%, lead content 4.75wt.%, silver content 239g/t in normal-pressure reaction kettle.The sulphuric acid soln 2800g of 15wt.%, is heated to 90 DEG C, reacts 4 hours, stir speed (S.S.) is 400rpm, and the slip obtained is easy to be separated, and the filter cake that separation obtains is without the need to washing and drying, be weighed as 465g, wherein moisture content 20wt.%, puts into normal-pressure reaction kettle, add the sulfuric acid 1488g of 30wt.%, be warming up to 80 DEG C, react 3 hours, stir speed (S.S.) is 400rpm, the slip obtained is easy to filtering separation, is separated the filter cake (lead smelting gas) obtained and washs 2 times; Be weighed as 297.6g.One section is leached filtrate 3095ml, adds 30% H wherein
2o
269ml is oxidized 0.5h, and add unslaked lime 178.34g deironing reaction 2.5h, filter and obtain scum 615g, filtrate 2727ml, filtrate adds sodium sulphite 130.46g and obtains zinc sulfide concentrates 42.99g.Lead smelting gas is placed in normal-pressure reaction kettle, add the sodium hydroxide solution 1116g of 30wt.%, be heated to 90 DEG C, react after 3 hours and filter, claim to obtain filter cake (silver-colored slag) 174.64g, gained filtrate adds 63.93g sodium sulphite solid and reclaims lead ore concentrate 28.14g, silver-colored slag without the need to washing and drying, with 14.16ml/L sodium cyanide solution 565ml Leaching of Silver.Washing lotion regulating vitriol oil concentration after second segment acid leaching, washing is the leach liquor as first paragraph after 15wt.%, and the filtrate after caustic alkali leaches regulates naoh concentration to be return alkali leaching operation as alkali leaching liquor after 30wt.%, realizes the recycle of washing lotion.The leaching yield of zinc reaches 88.71wt.%, and plumbous leaching yield reaches 92.15wt.%, the cyanide leaching 93.24wt.% of silver.The three wastes that whole flow process is not added are discharged, and avoid pollution from source.
Embodiment 2
Zinc leaching residue 500g is added, wherein Zn content 5.94wt.%, lead content 5.91wt.%, silver content 196g/t in normal-pressure reaction kettle.The sulphuric acid soln 2000g of 15wt.%, is heated to 90 DEG C, reacts 4 hours, stir speed (S.S.) is 400rpm, and the slip obtained is easy to be separated, and the filter cake that separation obtains is without the need to washing and drying, be weighed as 367g, wherein moisture content 18wt.%, puts into normal-pressure reaction kettle, add the sulfuric acid 1200g of 20wt.%, be warming up to 80 DEG C, react 3 hours, stir speed (S.S.) is 400rpm, the slip obtained is easy to filtering separation, is separated the filter cake (lead smelting gas) obtained and washs 2 times; Be weighed as 241g.30% H is added in filtrate
2o
238.17ml is oxidized 0.5h, adds unslaked lime 98.57g deironing reaction 2.5h, filters and obtain scum 135.84g.Filtrate 2002.1ml after deironing, filtrate adds sodium sulphite 130.46g and obtains zinc sulfide concentrates 42.99g.Lead smelting gas is placed in normal-pressure reaction kettle, add the sodium hydroxide solution 956g of 40wt.%, be heated to 90 DEG C, react after 3 hours and filter, claim to obtain filter cake (silver-colored slag) 133.41g, gained filtrate adds 48.3g sodium sulphite solid and reclaims lead ore concentrate 21.03g, silver-colored slag without the need to washing and drying, with 12.14ml/L sodium cyanide solution 482ml Leaching of Silver.Washing lotion regulating vitriol oil concentration after second segment acid leaching, washing is the leach liquor as first paragraph after 15wt.%, and the filtrate after caustic alkali leaches regulates naoh concentration to be return alkali leaching operation as alkali leaching liquor after 30wt.%, realizes the recycle of washing lotion.The leaching yield of zinc reaches 86.00wt.%, and plumbous leaching yield reaches 94.15wt.%, the cyanide leaching 92.34wt.% of silver.The three wastes that whole flow process is not added are discharged, and avoid pollution from source.
Embodiment 3
Zinc leaching residue 500g is added, wherein Zn content 5.94wt.%, lead content 5.91wt.%, silver content 196g/t in normal-pressure reaction kettle.The sulphuric acid soln 1500g of 15wt.%, is heated to 90 DEG C, reacts 3 hours, stir speed (S.S.) is 400rpm, and the slip obtained is easy to be separated, and the filter cake that separation obtains is without the need to washing and drying, be weighed as 352g, wherein moisture content 19wt.%, puts into normal-pressure reaction kettle, add the sulfuric acid 1200g of 15wt.%, be warming up to 80 DEG C, react 3 hours, stir speed (S.S.) is 400rpm, the slip obtained is easy to filtering separation, is separated the filter cake (lead smelting gas) obtained and washs 2 times; Be weighed as 232g.30% H is added in filtrate
2o
238.17ml is oxidized 0.5h, adds unslaked lime 98.57g deironing reaction 2.5h, filters and obtain scum 133g.Filtrate 2010.13ml after deironing, filtrate adds sodium sulphite 130.46g and obtains zinc sulfide concentrates 44g.Lead smelting gas is placed in normal-pressure reaction kettle, add the sodium hydroxide solution 696g of 35wt.%, be heated to 90 DEG C, react after 4 hours and filter, claim to obtain filter cake (silver-colored slag) 131g, gained filtrate adds 50g sodium sulphite solid and reclaims lead ore concentrate 22g, silver-colored slag without the need to washing and drying, with 12.14ml/L sodium cyanide solution 482ml Leaching of Silver.Washing lotion regulating vitriol oil concentration after second segment acid leaching, washing is the leach liquor as first paragraph after 15wt.%, and the filtrate after caustic alkali leaches regulates naoh concentration to be return alkali leaching operation as alkali leaching liquor after 35wt.%, realizes the recycle of washing lotion.The leaching yield of zinc reaches 87.89wt.%, and plumbous leaching yield reaches 95.25wt.%, the cyanide leaching 91.61wt.% of silver.The three wastes that whole flow process is not added are discharged, and avoid pollution from source.
Embodiment 4
Zinc leaching residue 500g is added, wherein Zn content 5.94wt.%, lead content 5.91wt.%, silver content 196g/t in normal-pressure reaction kettle.The sulphuric acid soln 1500g of 10wt.%, is heated to 90 DEG C, reacts 4 hours, stir speed (S.S.) is 400rpm, and the slip obtained is easy to be separated, and the filter cake that separation obtains is without the need to washing and drying, be weighed as 389g, wherein moisture content 19wt.%, puts into normal-pressure reaction kettle, add the sulfuric acid 1500g of 15wt.%, be warming up to 80 DEG C, react 3 hours, stir speed (S.S.) is 400rpm, the slip obtained is easy to filtering separation, is separated the filter cake (lead smelting gas) obtained and washs 2 times; Be weighed as 229g.30% H is added in filtrate
2o
238.17ml is oxidized 0.5h, adds unslaked lime 98.57g deironing reaction 2.5h, filters and obtain scum 129g.Filtrate 1659ml after deironing, filtrate adds sodium sulphite 130.46g and obtains zinc sulfide concentrates 39g.Lead smelting gas is placed in normal-pressure reaction kettle, add the sodium hydroxide solution 1145g of 40wt.%, be heated to 90 DEG C, react after 3 hours and filter, claim to obtain filter cake (silver-colored slag) 150g, gained filtrate adds 50g sodium sulphite solid and reclaims lead ore concentrate 24g, silver-colored slag without the need to washing and drying, with 12.14ml/L sodium cyanide solution 500ml Leaching of Silver.Washing lotion regulating vitriol oil concentration after second segment acid leaching, washing is the leach liquor as first paragraph after 10wt.%, and the filtrate after caustic alkali leaches regulates naoh concentration to be return alkali leaching operation as alkali leaching liquor after 40wt.%, realizes the recycle of washing lotion.The leaching yield of zinc reaches 85.89wt.%, and plumbous leaching yield reaches 96.31wt.%, the cyanide leaching 92.32wt.% of silver.The three wastes that whole flow process is not added are discharged, and avoid pollution from source.
Claims (4)
1. a technique for Whote-wet method process zinc leaching residue step by step arithmetic zinc, lead, silver, is characterized in that comprising the steps:
(1) carry out first paragraph leaching after mixing in normal-pressure reaction kettle with zinc leaching residue with low-concentration sulfuric acid solution, obtain slip;
(2) step (1) gained slurry filtration is obtained filter cake and filtrate, filter cake is without the need to washing, and filtrate is through H
2o
2oxidation, neutralized ex iron after vulcanization sodium sinks zinc;
(3) carry out second segment leaching after filter cake step (2) obtained and the sulphuric acid soln of higher concentration mix in a kettle., obtain slip;
(4) by step (3) gained slurry filtration, the filter cake obtained washs, and returns step (1) first paragraph and leach operation by filtering the filtrate that obtains and recycle;
(5) filter cake after step (4) being washed and caustic solution carry out alkali leaching after normal-pressure reaction kettle mixing, filter and obtain filter cake and filtrate;
(6) step (5) gained filter cake is not washed, without the need to adjust ph, directly return silver-colored industrial Cyanide Leaching operation;
(7) step (5) gained filtrate being added appropriate sodium sulphite carries out heavy plumbous, obtains concentrate of lead sulfide ore after filtration, and filtrate returns step (5) alkali leaching operation and recycles after regulating with caustic alkali;
The mass percent concentration of the low-concentration sulfuric acid described in step (1) is 10 ~ 20wt.%, liquid-solid ratio 2 ~ 5:1, extraction time 2 ~ 4 hours, and extraction temperature is 80 ~ 90 DEG C;
The mass percent concentration of the sulphuric acid soln of the higher concentration described in step (3) is 20 ~ 40wt.%, liquid-solid ratio 2 ~ 5:1, extraction time 2 ~ 4 hours, and extraction temperature is 80 ~ 90 DEG C.
2. the technique of step by step arithmetic zinc according to claim 1, lead, silver, is characterized in that the bath water described in step (4) is deionized water at normal temperature, and washing adopts the mode of static counter flow washing, and washing times is 2 ~ 4 times.
3. the technique of step by step arithmetic zinc according to claim 1, lead, silver, it is characterized in that the caustic sodium concentration described in step (5) is 15 ~ 40wt.%, liquid-solid ratio 2 ~ 4:1, alkali extraction temperature is 80 ~ 90 DEG C, alkali extraction time 2 ~ 5 hours.
4. the technique of step by step arithmetic zinc according to claim 1, lead, silver, is characterized in that the add-on of the sodium sulphite described in step (7) and the mass ratio of lead ion are 1 ~ 2:1, and carries out at normal temperatures.
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| CN102978418A (en) * | 2012-12-07 | 2013-03-20 | 来宾华锡冶炼有限公司 | Processing method of casting zinc dross |
| CN103409622B (en) * | 2013-07-22 | 2016-01-20 | 昆明理工大学科技产业经营管理有限公司 | A kind of method of individual curing high-iron zinc sulfide concentrate |
| MX2016003805A (en) | 2013-09-27 | 2017-01-05 | Técnicas Reunidas S A | Process for the selective recovery of lead and silver. |
| CN103695662B (en) * | 2013-12-13 | 2014-12-10 | 中南大学 | Comprehensive utilization method of slag iron concentrates of wet-type zinc smelting furnace |
| CN104195338B (en) * | 2014-08-20 | 2016-05-25 | 山东国大黄金股份有限公司 | A kind of from degold containing the method that reclaims copper zinc cyanogen lean solution |
| CN104862489A (en) * | 2015-04-23 | 2015-08-26 | 张伟晓 | Method of recycling gold, silver, zinc and lead from zinc leaching residues |
| CN106399707A (en) * | 2016-11-07 | 2017-02-15 | 南昌专腾科技有限公司 | Comprehensive recovery method and system for zinc and silver in zinc smelting waste slag |
| CN106381400A (en) * | 2016-11-07 | 2017-02-08 | 南昌专腾科技有限公司 | Efficient enrichment recovery method and system for lead and silver in lead smelting waste |
| CN108239699B (en) * | 2016-12-26 | 2019-10-01 | 有研工程技术研究院有限公司 | A kind of method of valuable metal in the leaded zinc-silver material of synthetical recovery |
| CN113787085A (en) * | 2021-10-14 | 2021-12-14 | 中钢集团马鞍山矿山研究总院股份有限公司 | Method for extracting Fe, Zn and Pb from electric furnace dust removal ash and realizing high-value utilization |
| CN114671411B (en) * | 2022-04-18 | 2023-07-28 | 中南大学 | Method for separating heavy metal and sulfur in sulfur-oxygen-containing pressure leaching slag |
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