CN112680601B - Method for recovering silver and gold from silver and gold-containing anode slime - Google Patents
Method for recovering silver and gold from silver and gold-containing anode slime Download PDFInfo
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Abstract
The invention discloses a method for recovering silver and gold from silver-gold-containing anode mud, which comprises the following steps: adding absolute ethyl alcohol into the anode mud, grinding, drying, adding the obtained powder into aqua regia, and stirring for dissolving; filtering to obtain filtrate and solid residue; adding the filtrate into an adsorption column loaded with the functionalized Zr-MOF material, and performing multi-stage cyclic adsorption treatment; eluting the functional Zr-MOF material by using an eluent, washing the eluted functional Zr-MOF material by using deionized water, drying, recycling, adding the eluent into a reactor, adding sodium sulfite, stirring, reducing, filtering, and drying the filtered solid to prepare gold powder; and adding hydrazine hydrate into the solid slag, carrying out thermal stirring reduction reaction, then cooling to room temperature, filtering, washing the solid obtained by filtering, and drying to obtain the silver powder. The method is simple to operate, mild in condition and low in cost; the adsorbing material adopted by the invention has good adsorption performance and high repeated utilization rate.
Description
The technical field is as follows:
the invention relates to the field of metal recovery, in particular to a method for recovering silver and gold from silver-gold-containing anode slime
Background art:
in the electrolytic refining or electrowinning of soluble anodes, the anodes contain small or trace amounts of other metals or elements in addition to the bulk metal, which are present in the anode in the form of simple substances, alloys or compounds. When the anode is polarized, these metals or elements become anode sludge because (1) their equilibrium potential is positive to the anode potential and thus cannot be ionized into the electrolyte; (2) although ionized into the electrolyte, the electrolyte immediately forms insoluble salt with the electrolyte and is separated out of the electrolyte; (3) partial oxidation forms insoluble compounds or elemental elements. The anode sludge produced is present as a finely divided powder, which is either adhered to the surface of the anode or deposited by gravity on the bottom of the cell or suspended in the electrolyte. Thus, for the electrolysis process to proceed properly, it is generally necessary to periodically brush the adhering sludge from the anodes, to scoop out the precipitated sludge from the tank bottoms and to filter the electrolyte to separate the suspended sludge.
The anode mud is rich in most or most of precious metals and certain scattered elements in ores, concentrates or fluxes, so that the anode mud has high comprehensive recovery value. For example, the values of gold and silver in anode mud produced by copper and lead electrolytic refining can sufficiently offset the processing cost of the whole process of electrolytic refining.
At present, the method for recovering metals such as gold, silver and the like from anode mud mainly comprises a pyrogenic process flow and a wet process flow; the fire process has the characteristics of mature process, easy operation and control of the process, strong adaptability to materials and suitability for large-scale centralized production. Compared with the pyrometallurgical process, the wet-process has the advantages of high direct yield of gold and silver, short process, low energy consumption, short production period, good comprehensive utilization economic benefit, environmental protection and the like. Chinese patent 201210475657.4 discloses a method for selectively recovering gold and silver from copper anode slime, which comprises the steps of selectively leaching gold and silver from a copper anode slime raw material in a weak acid environment by taking ammonium thiocyanate or sodium thiocyanate as a selective agent under the conditions of high temperature and high pressure, adding sodium bicarbonate to adjust pH for first impurity removal and adding sulfuric acid to adjust pH for second impurity removal to obtain impurity-removed and purified enriched gold and silver liquid, and treating by the process to ensure that the direct recovery rates of precious metals gold and silver in the copper anode slime are respectively up to 90% and 94%, thereby being more beneficial to improving the recovery rate of precious metals gold and silver. The method is suitable for selectively extracting gold and silver from various copper and lead anode slime and materials containing gold and silver, has high direct recovery rate and thorough separation, and is more favorable for improving the recovery rate of noble metals of gold and silver. Chinese patent 201210161371.9 discloses a treatment process of gold electrolysis anode mud, which comprises the following steps: (1) separating gold from aqua regia; (2) reducing gold by ethanol to remove nitrate and hydrazine hydrate; (3) dissolving the precipitate with ammonia water to reduce the silver with hydrazine hydrate. The invention adopts wet method to treat the gold electrolysis anode mud, the method can basically and thoroughly separate gold and silver, the loss of silver is reduced to the minimum, the purity of gold is obviously improved to 99.8 percent, and the gold can be directly cast into an anode plate for electrolysis, thereby completely meeting the requirement of gold electrolysis. The efficiency is improved, and the backlog of gold in the process is reduced; the silver in the anode mud is almost completely recovered, and the grade is also improved to more than 99 percent; the method has the advantages of simple operation, high recovery rate, high purity and stable quality. According to the prior art, the anode mud is treated by a wet process to recover gold and silver, so that the recovery rate and the purity are high; but the recovery conditions are harsh and the energy consumption is large.
The invention content is as follows:
the invention aims to solve the technical problem of providing a method for recovering silver and gold from silver-gold-containing anode mud aiming at the defects of the prior art, and the method comprises the steps of firstly dissolving the anode mud by aqua regia to obtain acid liquor and solid residues; performing multi-stage adsorption treatment on the acid liquor by using a functional Zr-MOF material, and eluting the functional Zr-MOF material after adsorption saturation; reducing the eluent by sodium sulfite to recover gold; and reducing the solid residue by hydrazine hydrate to recover silver. The steps of aqua regia dissolution, multistage adsorption, desorption and reduction realize the recovery of gold and silver, and the method has the advantages of simple operation, mild conditions and low cost; the adsorbing material adopted by the invention has good adsorption performance and high repeated utilization rate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for recovering silver and gold from silver-gold-containing anode slime comprises the following steps:
(1) adding absolute ethyl alcohol into the anode mud, grinding, drying, slowly adding the obtained powder into aqua regia, and stirring for dissolving; finally, filtering to obtain filtrate and solid slag;
(2) after the prepared filtrate is subjected to enrichment treatment, sodium sulfite is slowly added, after the addition is finished, the solution is stirred at normal temperature and reduced until no gold ions exist in the solution, the reaction is finished, then the solution is filtered, and the filtered solid is washed to be neutral and then dried to prepare gold powder;
(3) and slowly adding hydrazine hydrate into the prepared solid slag, heating, stirring and reducing after the dripping is finished until no silver ions exist in the liquid, cooling to room temperature, filtering, washing the solid obtained by filtering to be neutral, and drying to obtain the silver powder.
Preferably, in the step (1), the mass ratio of the aqua regia to the anode slime is 1: (2-4).
Preferably, in the step (1), the temperature of the stirring and dissolving treatment is 35-55 ℃, and the time of the stirring and dissolving treatment is 1-3 h; the rotation speed of the stirring and dissolving treatment is 1000-1500 rpm.
Preferably, in the step (2), the enrichment treatment is: adding the prepared filtrate into an adsorption column loaded with a functionalized Zr-MOF material, and performing multi-stage cyclic adsorption treatment; and (2) eluting the functional Zr-MOF material by using a mixed aqueous solution containing 1mol/L hydrochloric acid and 8-10 wt% of thiourea under the ultrasonic action, washing the eluted functional Zr-MOF material by using deionized water, drying and then reusing, wherein the obtained eluent is a solution enriched with gold ions.
Preferably, the functionalized Zr-MOF material is an amino-modified Zr-MOF material; the preparation process comprises the following steps: adding 0.5-1g of zirconium chloride and 0.5-0.8g of 2-amino terephthalic acid into 100ml of DMF, stirring until the solid is dissolved, then adding 2-5ml of acetic acid, carrying out ultrasonic treatment, finally heating and stirring in an oil bath at 100 ℃ and 1500rpm for reaction for 3-7h, cooling to room temperature after the reaction is finished, filtering the reaction solution, washing the obtained solid and drying to obtain the product.
Preferably, the elution is carried out in stages during the elution treatment under the action of ultrasound, and specifically, the elution is carried out in stages as follows: the first stage is ultrasonic treatment at 500W power for 10min, the second stage is not ultrasonic treatment, the immersion treatment is 30min, and the third stage is ultrasonic treatment at 500W power for 30 min.
Preferably, in the step (2), the addition amount of the sodium sulfite is 0.1-1 times of the weight of the gold in the anode slime.
Preferably, in the step (3), the amount of the hydrazine hydrate added is 0.1 to 0.5 times the weight of the silver in the anode slime.
Preferably, in the steps (2) and (3), the drying temperature is 110-150 ℃, and the drying time is 3-5 h.
In the above-mentioned means, in the step (3), the temperature of the heating, stirring and reducing reaction is preferably 55 to 65 ℃.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the functionalized Zr-MOF material has an ordered pore structure, rich functional groups, large specific surface area, good adsorption performance and high selectivity on gold ions, and can preliminarily reduce the gold ions adsorbed in pores of the material; the recovery rate of gold is improved; the functionalized Zr-MOF material is an amino-modified Zr-MOF material, when gold ions are adsorbed, the affinity of the Zr-MOF material to the gold ions is effectively improved through the electrostatic attraction between protonated amino groups and chloroauric acid radical ions, the amino groups have strong electron donating property, electrons can be transferred to the gold ions, Au-Cl bonds are destroyed, and therefore the gold ions are reduced into gold, and the recovery rate of the gold is improved.
The anode mud contains 93% of silver, 4% of gold, 2% of copper, 0.5% of nickel and 0.5% of bismuth, the anode mud is leached by aqua regia, silver ions are separated in the form of silver chloride precipitates, other ions are in filtrate, then the filtrate is subjected to multistage adsorption by adopting an amino-modified Zr-MOF material, the positively charged amino-modified Zr-MOF material effectively adsorbs gold anions in the filtrate through electrostatic attraction, and adsorption of copper cations, nickel cations and bismuth cations can be prevented through electrostatic repulsion, so that the purity of recovered gold powder is improved. Eluting the adsorbed amino modified Zr-MOF material by using an acidic thiourea solution; the eluted amino modified Zr-MOF material can be recycled; reducing the eluent by sodium sulfite to prepare gold powder; and reducing the silver chloride precipitate by adopting hydrazine hydrate to obtain the silver powder. The method disclosed by the invention is simple to operate, mild in recovery condition, low in cost, high in gold and silver recovery rate and high in purity.
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to be limiting.
The anode slime used in the following examples contained 93% silver, 4% gold, 2% copper, 0.5% nickel, and 0.5% bismuth.
Example 1
(1) Adding absolute ethyl alcohol into anode mud, grinding, drying, slowly adding the obtained powder into aqua regia, wherein the mass ratio of the aqua regia to the anode mud is 1: 2, stirring and dissolving at 35 ℃ and 1000rpm for 1 h; finally, filtering to obtain filtrate and solid slag;
(2) 0.5g of zirconium chloride and 0.5g of 2-aminoterephthalic acid were added to 100ml DMF until the solid is dissolved, then 2ml acetic acid is added, ultrasonic treatment is carried out, finally heating and stirring reaction are carried out for 3h in oil bath at 100 ℃ and 1000rpm, the reaction is cooled to room temperature after the reaction is finished, the reaction liquid is filtered, the obtained solid is dried after being washed, and the amino modified Zr-MOF material is obtained, wherein the average particle size is 50 +/-5 nm, the specific surface area is 1045.5m2/g；
(3) Adding the prepared filtrate into an adsorption column loaded with an amino modified Zr-MOF material, and performing multi-stage cyclic adsorption treatment until gold ions are not detected in tail liquid by an ICP method to finish adsorption;
(4) carrying out elution treatment on the amino modified Zr-MOF material under the ultrasonic action by adopting a mixed aqueous solution containing 1mol/L hydrochloric acid and 8 wt% of thiourea, wherein the elution treatment is carried out by stages, and specifically comprises the following steps: carrying out ultrasonic treatment at 500W for 10min in the first stage, carrying out ultrasonic treatment without ultrasonic treatment in the second stage for 30min, and carrying out ultrasonic treatment at 500W for 30min in the third stage; washing the eluted amino modified Zr-MOF material by using deionized water, drying and then reusing, adding eluent into a reactor, slowly adding sodium sulfite, wherein the addition amount of the sodium sulfite is 0.1 time of the weight of gold in the anode mud, stirring and reducing at normal temperature until no gold ions exist in the liquid after the addition is finished, then filtering, washing the filtered solid to be neutral, and drying at 110 ℃ for 3 hours to obtain gold powder;
(4) and slowly adding hydrazine hydrate into the prepared solid slag, wherein the addition amount of the hydrazine hydrate is 0.1 time of the weight of the silver in the anode mud, heating, stirring and reducing at 55 ℃ after dropwise addition is finished until no silver ions exist in the liquid, cooling to room temperature, filtering, washing the filtered solid to be neutral, and drying at 110 ℃ for 3 hours to obtain the silver powder.
Example 2
(1) Adding absolute ethyl alcohol into anode mud, grinding, drying, slowly adding the obtained powder into aqua regia, wherein the mass ratio of the aqua regia to the anode mud is 1: 4, stirring and dissolving at 55 ℃ and 1500rpm for 3 hours; finally, filtering to obtain filtrate and solid slag;
(2) 1g of zirconium chloride and 0.8g of 2-amino pairAdding phthalic acid into 100ml of DMF, stirring until the solid is dissolved, adding 5ml of acetic acid, carrying out ultrasonic treatment, finally heating and stirring in an oil bath at 100 ℃ and 1500rpm for reaction for 3-7h, cooling to room temperature after the reaction is finished, filtering the reaction solution, washing the obtained solid, and drying to obtain an amino modified Zr-MOF material; the average particle size is 50 +/-5 nm, and the specific surface area is 1046.3m2/g；
(3) Adding the prepared filtrate into an adsorption column loaded with an amino modified Zr-MOF material, and performing multi-stage cyclic adsorption treatment until gold ions are not detected in tail liquid by an ICP method to finish adsorption;
(4) carrying out elution treatment on the amino modified Zr-MOF material under the ultrasonic action by adopting a mixed aqueous solution containing 1mol/L hydrochloric acid and 10 wt% of thiourea, wherein the elution treatment is carried out by stages, and specifically comprises the following steps: carrying out ultrasonic treatment at 500W for 10min in the first stage, carrying out ultrasonic treatment without ultrasonic treatment in the second stage for 30min, and carrying out ultrasonic treatment at 500W for 30min in the third stage; washing the eluted amino-modified Zr-MOF material by using deionized water, drying and then reusing, adding an eluent into a reactor, slowly adding sodium sulfite, wherein the addition amount of the sodium sulfite is 1 time of the weight of gold in the anode mud, stirring and reducing at normal temperature after the addition is finished until no gold ions exist in the liquid, finishing the reaction, filtering, washing the filtered solid to be neutral, and drying at 150 ℃ for 5 hours to obtain gold powder;
(4) and slowly adding hydrazine hydrate into the prepared solid slag, wherein the addition amount of the hydrazine hydrate is 0.5 time of the weight of the silver in the anode mud, after the dropwise addition is finished, heating, stirring and reducing at 65 ℃ until no silver ions exist in the liquid, cooling to room temperature, filtering, washing the filtered solid to be neutral, and drying at 150 ℃ for 5 hours to obtain the silver powder.
Example 3
(1) Adding absolute ethyl alcohol into anode mud, grinding, drying, slowly adding the obtained powder into aqua regia, wherein the mass ratio of the aqua regia to the anode mud is 1: stirring and dissolving for 2h at the temperature of 3, 40 ℃ and the pressure of 1200 pm; finally, filtering to obtain filtrate and solid slag;
(2) will be 0.8Adding zirconium chloride and 0.6g of 2-amino terephthalic acid into 100ml of DMF (dimethyl formamide) and stirring until the solid is dissolved, then adding 3ml of acetic acid, carrying out ultrasonic treatment, finally heating and stirring for reaction for 5 hours at 100 ℃ and 1500pm in an oil bath, cooling to room temperature after the reaction is finished, filtering the reaction liquid, washing the obtained solid and drying to obtain an amino modified Zr-MOF material; the average particle size is 50 +/-5 nm, and the specific surface area is 1045.8m2/g；
(3) Adding the prepared filtrate into an adsorption column loaded with an amino modified Zr-MOF material, and performing multi-stage cyclic adsorption treatment until gold ions are not detected in tail liquid by an ICP method to finish adsorption;
(4) carrying out elution treatment on the amino modified Zr-MOF material under the ultrasonic action by adopting a mixed aqueous solution containing 1mol/L hydrochloric acid and 8 wt% of thiourea, wherein the elution treatment is carried out by stages, and specifically comprises the following steps: carrying out ultrasonic treatment at 500W for 10min in the first stage, carrying out ultrasonic treatment without ultrasonic treatment in the second stage for 30min, and carrying out ultrasonic treatment at 500W for 30min in the third stage; washing the eluted amino modified Zr-MOF material by using deionized water, drying and then reusing, adding eluent into a reactor, slowly adding sodium sulfite, wherein the addition amount of the sodium sulfite is 0.5 times of the weight of gold in the anode mud, stirring and reducing at normal temperature until no gold ions exist in the liquid after the addition is finished, finishing the reaction, filtering, washing the filtered solid to be neutral, and drying at 120 ℃ for 4 hours to obtain gold powder;
(4) and slowly adding hydrazine hydrate into the prepared solid slag, wherein the addition amount of the hydrazine hydrate is 0.25 time of the weight of the silver in the anode mud, heating, stirring and reducing at 60 ℃ after dropwise addition is finished until no silver ions exist in the liquid, cooling to room temperature, filtering, washing the filtered solid to be neutral, and drying at 120 ℃ for 4 hours to obtain the silver powder.
Example 4
(1) Adding absolute ethyl alcohol into anode mud, grinding, drying, slowly adding the obtained powder into aqua regia, wherein the mass ratio of the aqua regia to the anode mud is 1: 3, stirring and dissolving at 50 ℃ and 1200rpm for 1 h; finally, filtering to obtain filtrate and solid slag;
(2) adding 0.6g of zirconium chloride and 0.6g of 2-amino terephthalic acid into 100ml of DMF, stirring until the solid is dissolved, then adding 3ml of acetic acid, carrying out ultrasonic treatment, finally heating and stirring at 100 ℃ and 1500rpm in an oil bath for reaction for 5 hours, cooling to room temperature after the reaction is finished, filtering the reaction solution, washing the obtained solid, and drying to obtain an amino modified Zr-MOF material; the average particle size is 50 +/-5 nm, and the specific surface area is 1045.5m2/g；
(3) Adding the prepared filtrate into an adsorption column loaded with an amino modified Zr-MOF material, and performing multi-stage cyclic adsorption treatment until gold ions are not detected in tail liquid by an ICP method to finish adsorption;
(4) carrying out elution treatment on the amino modified Zr-MOF material under the ultrasonic action by adopting a mixed aqueous solution containing 1mol/L hydrochloric acid and 9 wt% of thiourea, wherein the elution treatment is carried out by stages, and specifically comprises the following steps: carrying out ultrasonic treatment at 500W for 10min in the first stage, carrying out ultrasonic treatment without ultrasonic treatment in the second stage for 30min, and carrying out ultrasonic treatment at 500W for 30min in the third stage; washing the eluted amino modified Zr-MOF material by using deionized water, drying and then reusing, adding eluent into a reactor, slowly adding sodium sulfite, wherein the addition amount of the sodium sulfite is 0.5 times of the weight of gold in the anode mud, stirring and reducing at normal temperature until no gold ions exist in the liquid after the addition is finished, finishing the reaction, filtering, washing the filtered solid to be neutral, and drying at 120 ℃ for 4 hours to obtain gold powder;
(4) and slowly adding hydrazine hydrate into the prepared solid slag, wherein the addition amount of the hydrazine hydrate is 0.25 time of the weight of the silver in the anode mud, heating, stirring and reducing at 60 ℃ after dropwise addition is finished until no silver ions exist in the liquid, cooling to room temperature, filtering, washing the filtered solid to be neutral, and drying at 120 ℃ for 3 hours to obtain the silver powder.
Example 5
(1) Adding absolute ethyl alcohol into anode mud, grinding, drying, slowly adding the obtained powder into aqua regia, wherein the mass ratio of the aqua regia to the anode mud is 1: stirring and dissolving at 45 ℃ for 3h at 1000 rpm; finally, filtering to obtain filtrate and solid slag;
(2) adding 0.65g of zirconium chloride and 0.75g of 2-amino terephthalic acid into 100ml of DMF, stirring until the solid is dissolved, then adding 5ml of acetic acid, carrying out ultrasonic treatment, finally heating and stirring in an oil bath at 100 ℃ and 1500rpm for reaction for 6 hours, cooling to room temperature after the reaction is finished, filtering the reaction solution, washing the obtained solid, and drying to obtain an amino modified Zr-MOF material; the average particle size is 50 +/-5 nm, and the specific surface area is 1046.0m2/g；
(3) Adding the prepared filtrate into an adsorption column loaded with an amino modified Zr-MOF material, and performing multi-stage cyclic adsorption treatment until gold ions are not detected in tail liquid by an ICP method to finish adsorption;
(4) carrying out elution treatment on the amino modified Zr-MOF material under the ultrasonic action by adopting a mixed aqueous solution containing 1mol/L hydrochloric acid and 8 wt% of thiourea, wherein the elution treatment is carried out by stages, and specifically comprises the following steps: carrying out ultrasonic treatment at 500W for 10min in the first stage, carrying out ultrasonic treatment without ultrasonic treatment in the second stage for 30min, and carrying out ultrasonic treatment at 500W for 30min in the third stage; washing the eluted amino modified Zr-MOF material by using deionized water, drying and then reusing, adding eluent into a reactor, slowly adding sodium sulfite, wherein the addition amount of the sodium sulfite is 0.5 times of the weight of gold in the anode mud, stirring and reducing at normal temperature until no gold ions exist in the liquid after the addition is finished, finishing the reaction, filtering, washing the filtered solid to be neutral, and drying at 120 ℃ for 4 hours to obtain gold powder;
(4) and slowly adding hydrazine hydrate into the prepared solid slag, wherein the addition amount of the hydrazine hydrate is 0.25 time of the weight of the silver in the anode mud, heating, stirring and reducing at 55 ℃ after dropwise addition is finished until no silver ions exist in the liquid, cooling to room temperature, filtering, washing the filtered solid to be neutral, and drying at 120 ℃ for 4 hours to obtain the silver powder.
Comparative example
The filtrate obtained after the aqua regia is dissolved is directly reduced without adopting the functional Zr-MOF material for adsorption, and other process conditions are the same as those in the example 5.
The recovery and purity of gold and silver were tested in examples 1-5 and comparative examples and the results are shown in table 1:
TABLE 1
From the test results, the gold and silver recovery rate and the purity of the gold and silver prepared by the gold and silver recovery method are high.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (8)
1. A method for recovering silver and gold from silver-gold-containing anode slime is characterized by comprising the following steps:
(1) adding absolute ethyl alcohol into the anode mud, grinding, drying, slowly adding the obtained powder into aqua regia, and stirring for dissolving; finally, filtering to obtain filtrate and solid slag;
(2) after the prepared filtrate is subjected to enrichment treatment, sodium sulfite is slowly added, after the addition is finished, the solution is stirred at normal temperature and reduced until no gold ions exist in the solution, the reaction is finished, then the solution is filtered, and the filtered solid is washed to be neutral and then dried to prepare gold powder;
(3) slowly adding hydrazine hydrate into the prepared solid slag, heating, stirring and reducing after the dropwise addition is finished until no silver ions exist in the liquid, cooling to room temperature, filtering, washing the filtered solid to be neutral, and drying to obtain silver powder;
the enrichment treatment comprises the following steps: adding the prepared filtrate into an adsorption column loaded with a functionalized Zr-MOF material, and performing multi-stage cyclic adsorption treatment; eluting the functional Zr-MOF material by using a mixed aqueous solution containing 1mol/L hydrochloric acid and 8-10 wt% of thiourea under the action of ultrasound, washing the eluted functional Zr-MOF material by using deionized water, drying and then reusing the washed functional Zr-MOF material, wherein the obtained eluent is a solution enriched with gold ions;
the functionalized Zr-MOF material is an amino-modified Zr-MOF material; the preparation process comprises the following steps: adding 0.5-1g of zirconium chloride and 0.5-0.8g of 2-amino terephthalic acid into 100ml of DMF, stirring until the solid is dissolved, then adding 2-5ml of acetic acid, carrying out ultrasonic treatment, finally heating and stirring in an oil bath at 100 ℃ and 1500rpm for reaction for 3-7h, cooling to room temperature after the reaction is finished, filtering the reaction solution, washing the obtained solid and drying to obtain the product.
2. The method for recovering silver and gold from silver-gold-containing anode slime according to claim 1, wherein in the step (1), the mass ratio of the aqua regia to the anode slime is 1: (2-4).
3. The method for recovering silver and gold from silver-gold containing anode slime according to claim 1, wherein in the step (1), the temperature of the stirring and dissolving treatment is 35-55 ℃, and the time of the stirring and dissolving treatment is 1-3 h; the rotation speed of the stirring and dissolving treatment is 1000-1500 rpm.
4. The method for recovering silver and gold from silver-and gold-containing anode slime according to claim 1, characterized in that elution is carried out in stages during elution treatment under the action of ultrasound, specifically: the first stage is ultrasonic treatment at 500W power for 10min, the second stage is not ultrasonic treatment, the immersion treatment is 30min, and the third stage is ultrasonic treatment at 500W power for 30 min.
5. The method of claim 1, wherein in step (2), the amount of sodium sulfite added is 0.1-1 times the weight of gold in the anode slime.
6. The method for recovering silver and gold from anode mud containing silver and gold according to claim 1, wherein in the step (3), the hydrazine hydrate is added in an amount which is (0.1-0.5) times of the weight of the silver in the anode mud.
7. The method as claimed in claim 1, wherein the drying temperature in steps (2) and (3) is 110-150 ℃, and the drying time is 3-5 h.
8. The method for recovering silver and gold from silver-gold containing anode slime as claimed in claim 1, wherein in the step (3), the temperature of the heating, stirring and reducing reaction is 55-65 ℃.
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| CN110841598A (en) * | 2019-11-15 | 2020-02-28 | 昆明理工大学 | Preparation method and application of synthetic metal organic framework adsorbent |
| CN111545171A (en) * | 2020-04-16 | 2020-08-18 | 南昌航空大学 | Preparation method of acid-resistant Zr-MOF material for selectively adsorbing hexavalent chromium |
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