CN104726720A - Method for reclaiming silver from silver converter slag table tailings - Google Patents
Method for reclaiming silver from silver converter slag table tailings Download PDFInfo
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- CN104726720A CN104726720A CN201510138529.4A CN201510138529A CN104726720A CN 104726720 A CN104726720 A CN 104726720A CN 201510138529 A CN201510138529 A CN 201510138529A CN 104726720 A CN104726720 A CN 104726720A
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Abstract
The invention provides a method for reclaiming silver from silver converter slag table tailings. The method comprises the following steps: S1, adding water into silver converter slag table tailings for mixing, then adding acid to regulate the pH value to be 0.5-1 for pickling, filtering and washing to obtain pickling residues and pickling liquid without calcium, magnesium and other impurities; S2, adding water into the pickling residues obtained in the step S1, adding acid to regulate the pH value to be 1-2, then adding oxidant soluble trivalent ferric salt and thiourea to react, filtering and washing to obtain thiourea leaching liquid and leaching residues; S3, adding zinc powder into the thiourea leaching liquid obtained in the step S2 to carry out replacement reaction, and filtering to obtain silver. The method can be used for effectively reclaiming silver from the silver converter slag table tailings and effectively treating slag of calcium, magnesium and other impurities, the leaching rate of silver can be over 95 percent since the metal silver in the silver converter slag table tailings is leached by adopting the acidic thiourea solution, and the replacement rate is over 99 percent since the prepared silver-containing leaching liquid is replaced by zinc powder to obtain silver.
Description
Technical field
The invention belongs to lead-zinc smelting chemical technology field, be specifically related to the recovery method of silver in the silver converter slag shaking table mine tailing produced in a kind of Lead-Zinc Sintering Process.
Background technology
Along with the exhaustion day by day of Mineral resources, develop renewable resource extremely urgent, e.g., tailings or metallurgical slag etc., the comprehensive utilization of renewable resource is also the important channel realizing Sustainable development simultaneously.
In the production technique of zinc hydrometallurgy, usually containing silver in the plumbous zinc anode sludge produced, therefore, in the lead-zinc smelting production equipment of Zinc hydrometallurgy process, usually be provided with silver and smelt retrieving arrangement, silver is smelted retrieving arrangement and is comprised main treatment facility silver converter and separation shaking table, the silver adopted is smelted the technical process of reclaiming and is generally: sent into by the anode sludge produced in lead-zinc smelting in the silver converter of liner magnesite chrome brick and carry out the precious metals containing lead that melting obtains containing gold and silver, namely gold and silver is enriched in precious metals containing lead further, precious metals containing lead carries out oxidation blowing again in this converter, obtain alloy sheets, this alloy sheets is obtained gold and silver through electrorefining.Because the proportion of precious metals containing lead and alloy is larger, in precious metals containing lead fusion process, the metal liquid having a small amount of melting infiltrates in converter lining magnesite chrome brick and gap thereof, and this chromium magnesium lining brick need irregularly carry out repairing and changing, therefore, the converter slag disassembled during maintenance and lining brick contain certain gold and silver, have very high recovery value.Equally, after separation by shaking table, mine tailing is also containing certain gold and silver, and also have very high recovery value, both converter slag and shaking table mine tailing can synchronously reclaim.But this solid slag intractability through high melt is very large, mainly contain following reason: 1, contain the higher impurity such as calcium, magnesium in lining brick, if and still directly adopt converter carry out pyrogenic attack, the working order therefore pyrogenic attack difficulty that converter is difficult to reach desirable is large.2, traditional wet method silver leaching process is mainly cyanide process, and this method exists the major defect of several aspect: prussiate toxicity is high, easily causes environmental pollution; And reagent is expensive, cost is high.3, non-cyanogen recover silver technology has applications well prospect, and as Leaching In Thiourea Solutions gold and silver is usually used in zinc hydrometallurgy waste residue, compared with cyanide process, its leaching velocity is fast, and environmentally safe is the main direction of studying of silver leaching process.But it is not high to there is concentration of precious metal rate, sulfuric acid dosage is large, the shortcoming that silver leaching rate is low.
Summary of the invention
The present invention is exactly for above-mentioned existing technical problem and deficiency, provides a kind of method of recover silver from silver converter slag shaking table mine tailing.
The invention provides the recovery method of silver in a kind of silver converter slag shaking table mine tailing, said method comprising the steps of:
S1, removal of impurities: the ratio adding 4 ~ 5mL water according to 1g silver converter slag shaking table mine tailing adds water and is mixed to get the first mixture in silver converter slag shaking table mine tailing, then in described first mixture, add acid for adjusting pH=0.5 ~ 1 and carry out pickling, then add additive villaumite to react, then after filtration, washing after, the pickling slag of the impurity such as the calcium that is removed, magnesium, silicon and pickle solution;
S2, Leaching of Silver: add water in the pickling slag that the ratio adding 4 ~ 6mL water according to 1g pickling slag obtains to step S1 and obtain the second mixture, add acid for adjusting pH=1 ~ 2 again, then add oxygenant solubility trivalent iron salt and thiocarbamide reacts, then after filtration, washing obtains Leaching In Thiourea Solutions fluid and leached mud;
S3, displacement silver: in the Leaching In Thiourea Solutions fluid that step S2 obtains, add zinc powder carry out replacement(metathesis)reaction, filter and obtain silver.
According to recovery method provided by the present invention, preferably, in described step S1, the temperature of described pickling is 70 ~ 80 DEG C, and the time of described pickling is 1 ~ 2h.
According to recovery method provided by the present invention, preferably, in described step S2, described temperature of reaction 70 ~ 80 DEG C, reacts 1 ~ 2h under keeping the condition of terminal pH=1 ~ 2.
According to recovery method provided by the present invention, preferably, in described step S3, the solution obtained after described replacement(metathesis)reaction returns step S2 and continues Leaching of Silver.
According to recovery method provided by the present invention, in order to the impurity calcium in silver converter slag shaking table mine tailing, magnesium are removed completely, preferably, in step sl, described acid is the vitriol oil, the weight used of the wherein said vitriol oil is the vitriol oil and calcium, 1.2 ~ 1.4 times of weight needed for the theory of magnesium complete reaction, be 140 ~ 160g/L; Described sodium-chlor consumption and the ratio of the first mixture are 20 ~ 25(g): 1(L).
According to recovery method provided by the present invention, in order to the silver in silver converter slag shaking table mine tailing is leached completely, preferably, in step s 2, described solubility trivalent iron salt is ferric sulfate and/or iron(ic) chloride, wherein the consumption of trivalent iron salt and the ratio 10 ~ 20(g of the second thing): 1(L).
According to recovery method provided by the present invention, preferably, in described step S2, the concentration of described thiocarbamide is 50 ~ 80 g/L.
Silver in energy recover silver converter slag of the present invention, technical process is short, and silver raising recovery rate is up to 95%; Calcium sulfate solubleness in an acidic solution can be increased by adding sodium-chlor, thus improve the accumulation rate of precious metal; By removal of impurities enrichment valuable metal wherein, accumulation rate is high, then adds oxygenant solubility trivalent iron salt and thiocarbamide reacts, and makes silver enter in Leaching In Thiourea Solutions fluid further, carries out displacement and reclaims.The present invention can process the slag type containing the impurity such as high calcium, magnesium, and in pickling, silver-colored accumulation rate is higher, creates favorable conditions for follow-up leaching test simultaneously; The argentiferous leach liquor that the present invention obtains, can obtain silver through zinc dust precipitation, and displaced liquid can recycle simultaneously; And extracting method provided by the invention is Whote-wet method treating processes, nontoxic, technique is simple, easy to operate, production cost is low.
The principal reaction related to has:
After leaching, in system, silver etc. are converted into solution, after filtration, and silver enrichment in filtrate, can displacement operation be carried out, and the solution after displacement, feeding leaching process can also be returned, thiocarbamide in solution after displacement achieves recycle, effectively can reduce total consumption of thiocarbamide, reduce costs.
The present invention is Whote-wet method treating processes, and compared with current technology, extraction time is short, can process the slag that calcium-magnesium-containing foreign matter content is high, pickling concentration effect is good, can reduce energy consumption and the production cost of slag treatment, nontoxic, technique is simple, easy to operate, to equipment without particular requirement, cost is low.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The invention provides the recovery method of silver in a kind of silver converter slag mine tailing, said method comprising the steps of:
S1, removal of impurities: the ratio adding 4 ~ 5mL water according to 1g silver converter slag shaking table mine tailing adds water and is mixed to get the first mixture in silver converter slag shaking table mine tailing, then in described first mixture, add acid for adjusting pH=0.5 ~ 1 and carry out pickling, then add additive villaumite to react, then after filtration, washing after, the pickling slag of the impurity such as calcium, magnesium that is removed and pickle solution;
S2, Leaching of Silver: add water in the pickling slag that the ratio adding 4 ~ 6mL water according to 1g pickling slag obtains to step S1 and obtain the second mixture, add acid for adjusting pH=1 ~ 2 again, then add oxygenant solubility trivalent iron salt and thiocarbamide reacts, then after filtration, washing obtains Leaching In Thiourea Solutions fluid and leached mud;
S3, displacement silver: in the Leaching In Thiourea Solutions fluid that step S2 obtains, add zinc powder carry out replacement(metathesis)reaction, filter and obtain silver.
According to recovery method provided by the present invention, preferably, in step S1, in 1L first mixture, add 140 ~ 160g acid; In step s 2,30 ~ 40g acid is added in 1L second mixture.
According to recovery method provided by the present invention, preferably, in described step S1, the temperature of described pickling is 70 ~ 80 DEG C, and the time of described pickling is 1 ~ 2h.
According to recovery method provided by the present invention, preferably, in described step S2, described temperature of reaction 70 ~ 80 DEG C, reacts 1 ~ 2h under keeping the condition of terminal pH=1 ~ 2.
According to recovery method provided by the present invention, preferably, in described step S3, the solution obtained after described replacement(metathesis)reaction returns step S2 and continues Leaching of Silver.
According to recovery method provided by the present invention, in order to the impurity calcium in silver converter slag shaking table mine tailing, magnesium are removed completely, preferably, in step sl, described acid is the vitriol oil, the weight used of the wherein said vitriol oil is the vitriol oil and calcium, 1.2 ~ 1.4 times of weight needed for the theory of magnesium complete reaction, be 140 ~ 160g/L; Described sodium-chlor consumption and the ratio of the first mixture are 20 ~ 25(g): 1(L).
According to recovery method provided by the present invention, in order to the silver in silver converter slag shaking table mine tailing is leached completely, preferably, in step s 2, described solubility trivalent iron salt is ferric sulfate and/or iron(ic) chloride, wherein the consumption of trivalent iron salt and the ratio 10 ~ 20(g of the second thing): 1(L).
According to recovery method provided by the present invention, preferably, in described step S2, the concentration of described thiocarbamide is 50 ~ 80 g/L.
According to recovery method provided by the present invention, in order to the silver in silver converter slag shaking table mine tailing is displaced completely, in described step S3, the amount used of described zinc powder 1.2 ~ 1.5 times of weight needed for theory that silver in leach liquor is precipitated completely.
Below by specific embodiment, the present invention is further described.
Embodiment 1
In the present embodiment, in silver converter slag shaking table mine tailing S1, the main ingredient of valuable metal is: Au0.0007%, Ag0.3215%, Mg 43.21%, Ca 4.28%, SiO
22.8%.
1, by 200g silver converter slag shaking table mine tailing and the mixing of 1000mL water, then add 80mL sulphuric acid soln and regulate pH=1, add sodium-chlor 20g, control temperature of reaction stirring and pickling 1h at 70 DEG C, then after filtration, after washing, obtain pickling slag and the pickle solution of the impurity such as deliming, magnesium, the slag yield in this step is 58.5%;
2, pickling slag obtained for step 1 being added that 20mL sulphuric acid soln to regulate after pH=2 according to liquid-solid ratio is that 5:1mL/g joins in the thiourea solution of 50g/L, add 10g oxygenant trivalent iron salt again to react, control temperature of reaction 75 DEG C, 2h is leached under keeping the condition of terminal pH=2, then after filtration, washing obtains Leaching In Thiourea Solutions fluid and leached mud, the composition of this step leach liquor is: Au<0.0001%, Ag0.0439%, and silver leaching rate is 95%;
3, in the obtained Leaching In Thiourea Solutions fluid of step 2, add 3g zinc powder to replace, filter and obtain silver, rate of displacement reaches more than 99%, returns step 2 and continue Leaching of Silver after displaced liquid being adjusted thiourea concentration to 50g/L.
Embodiment 2
In the present embodiment, in silver converter slag mine tailing S2, the main ingredient of valuable metal is: Au0.0006%, Ag0.3358%, Mg46.22%, Ca 4.25%, SiO
22.58%.
1, by 200g silver converter slag shaking table mine tailing and the mixing of 800mL water, then add 85mL sulphuric acid soln and adjust pH=0.5, add sodium-chlor 20g, control temperature of reaction stirring and pickling 2h at 80 DEG C, then after filtration, after washing, obtain pickling slag and the pickle solution of the impurity such as deliming, magnesium, silicon, the slag yield in this step is 52.5%;
2, pickling slag obtained for step 1 being added that 15mL sulphuric acid soln to regulate after pH=1 according to liquid-solid ratio is that 4:1mL/g joins in the thiourea solution of 60g/L, add 10g oxygenant trivalent iron salt again and thiocarbamide obtains mixing liquid, control temperature of reaction 70 DEG C, 2h is leached under keeping the condition of terminal pH=1, then after filtration, washing obtains Leaching In Thiourea Solutions fluid and leached mud, the composition of this step leach liquor is: Au<0.0001%, Ag0.0385%, and silver leaching rate is 95.5%;
3, in the obtained Leaching In Thiourea Solutions fluid of step 2, add 3g zinc powder to replace, filter and obtain silver, rate of displacement reaches more than 99%, returns step 2 and continue Leaching of Silver after displaced liquid being adjusted thiourea concentration to 60g/L.
Embodiment 3
In the present embodiment, in silver converter slag mine tailing S3, the main ingredient of valuable metal is: Au0.0007%, Ag0.346%, Mg48.54%, Ca 4.0%, SiO
22.5%.
A, will add in 200g silver converter slag shaking table mine tailing 1000mL water mixing, then add 90mL sulphuric acid soln and adjust pH=0.5, add sodium-chlor 25g, control temperature of reaction stirring and pickling 1.5h at 75 DEG C, then after filtration, after washing, obtain pickling slag and the pickle solution of the impurity such as deliming, magnesium, silicon, the slag yield in this step is 51%;
2, decalcification obtained for step 1, magnesium pickling slag being added that 10mL sulphuric acid soln to regulate after pH=2 according to liquid-solid ratio is that 6:1mL/g joins in the thiourea solution of 80g/L, add 10g oxygenant trivalent iron salt again and thiocarbamide obtains mixing liquid, control temperature of reaction 80 DEG C, 2h is leached under keeping the condition of terminal pH=2, then after filtration, washing obtains Leaching In Thiourea Solutions fluid and leached mud, in this step, the composition of leach liquor is: Au<0.0001%, Ag0.0259%, and silver leaching rate is 97%;
3, in the obtained Leaching In Thiourea Solutions fluid of step 2, add 3g zinc powder to replace, filter and obtain silver, rate of displacement reaches more than 99%, returns step 2 and continue Leaching of Silver after displaced liquid being adjusted thiourea concentration to 80g/L.
The present invention can process the slag type containing impurity such as high calcium, magnesium, silicon; By removal of impurities enrichment valuable metal wherein, for follow-up test creates favorable conditions; The acid thiourea solution that the present invention adopts is to the leaching of removing impurities mine tailing, and obtain the infusion solution containing silver, silver leaching rate is greater than 95%; The argentiferous leach liquor obtained, can obtain silver through zinc dust precipitation, rate of displacement reaches more than 99%, and the solution simultaneously obtained after displacement can recycle.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a recovery method silver-colored in silver converter slag mine tailing, is characterized in that, said method comprising the steps of:
S1, removal of impurities: the ratio adding 4 ~ 5mL water according to 1g silver converter slag shaking table mine tailing adds water and is mixed to get the first mixture in silver converter slag shaking table mine tailing, then in described first mixture, add acid for adjusting pH=0.5 ~ 1 and carry out pickling, then add additive villaumite to react, then after filtration, washing after, the pickling slag of the impurity such as calcium, magnesium that is removed and pickle solution;
S2, Leaching of Silver: add water in the pickling slag that the ratio adding 4 ~ 6mL water according to 1g pickling slag obtains to step S1 and obtain the second mixture, add acid for adjusting pH=1 ~ 2 again, then add oxygenant solubility trivalent iron salt and thiocarbamide reacts, then after filtration, washing obtains Leaching In Thiourea Solutions fluid and leached mud;
S3, displacement silver: in the Leaching In Thiourea Solutions fluid that step S2 obtains, add zinc powder carry out replacement(metathesis)reaction, filter and obtain silver.
2. recovery method according to claim 1, is characterized in that, in described step S1, the temperature of described pickling is 70 ~ 80 DEG C, and the time of described pickling is 1 ~ 2h.
3. recovery method according to claim 1, is characterized in that, in described step S2, described temperature of reaction is 70 ~ 80 DEG C, reacts 1 ~ 2h under keeping the condition of terminal pH=1 ~ 2.
4. recovery method according to claim 1, is characterized in that, in described step S3, the solution obtained after described replacement(metathesis)reaction returns step S2 and continues Leaching of Silver.
5. recovery method according to claim 1, is characterized in that, in step sl, described acid is the vitriol oil, and the weight used of the wherein said vitriol oil is the vitriol oil and calcium, 1.2 ~ 1.4 times of weight needed for the theory of magnesium complete reaction.
6. recovery method according to claim 1, is characterized in that, in step sl, described additive is sodium-chlor, and wherein the consumption of sodium-chlor and the ratio of the first mixture are 20 ~ 25(g): 1(L).
7. recovery method according to claim 1, is characterized in that, in step s 2, described solubility trivalent iron salt is ferric sulfate and/or iron(ic) chloride, and wherein the consumption of trivalent iron salt and the ratio of the second mixture are 10 ~ 20(g): 1(L).
8. recovery method according to claim 1, is characterized in that, in described step S2, the concentration of described thiocarbamide is 50 ~ 80 g/L.
9. recovery method according to claim 1, is characterized in that, in described step S3, and the amount used of described zinc powder 1.2 ~ 1.5 times of weight needed for theory that silver in leach liquor is precipitated completely.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510138529.4A CN104726720A (en) | 2015-03-27 | 2015-03-27 | Method for reclaiming silver from silver converter slag table tailings |
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| CN201510138529.4A CN104726720A (en) | 2015-03-27 | 2015-03-27 | Method for reclaiming silver from silver converter slag table tailings |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632976A (en) * | 2018-12-29 | 2019-04-16 | 紫金矿业集团股份有限公司 | Golden diagnostic method in gold mine pressure pre-oxidation cyanide residue |
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2015
- 2015-03-27 CN CN201510138529.4A patent/CN104726720A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632976A (en) * | 2018-12-29 | 2019-04-16 | 紫金矿业集团股份有限公司 | Golden diagnostic method in gold mine pressure pre-oxidation cyanide residue |
| CN109632976B (en) * | 2018-12-29 | 2021-08-24 | 紫金矿业集团股份有限公司 | Diagnosis method for gold in gold ore pressurized pre-oxidation cyanide slag |
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