CN115747476A - Method for wet processing of copper antimony tin material containing medium-low gold and silver - Google Patents
Method for wet processing of copper antimony tin material containing medium-low gold and silver Download PDFInfo
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Abstract
The invention discloses a method for wet processing a copper antimony tin material containing medium and low gold and silver, which comprises the following steps: roasting (1), leaching (2), reducing (4), hydrolyzing (5), recovering copper (6), leaching silver (7), reducing silver powder (8), leaching gold (9) and reducing gold powder. The method of the invention is more practical for the production flow of the anode mud containing low-degree gold and silver crude tin, especially for the anode mud which is partially oxidized, the recovery rate of tin is higher, the recovery rate of gold and silver is more ideal, the method is especially suitable for enterprises with a more complete industrial chain, a small part of un-leached gold and silver enter a pyrogenic process working section along with tin materials, and the recycling is realized, so that the economic benefit is obvious.
Description
Technical Field
The invention belongs to the technical field of separation and enrichment of nonferrous metals, and particularly relates to a wet method for treating a copper-antimony-tin material containing low-content gold and silver.
Background
In the technical field of separation and enrichment of nonferrous technologies, precious metals are expensive, so that the separation and purification of the precious metals are always important. For separating and enriching copper, antimony and tin materials with low gold and silver contents, the existing treatment method mainly comprises a wet method and a fire methodThe method theory and the wet-fire method combination method aim at different materials and methods which are different from each other and have great difficulty. As the existing wet processing thinking is that the base metals such as Sb, sn, cu and the like in the material are completely dissolved through high acidity and then are separated step by step, the direct yield of Sn is low because Sn is lost in the solution more or less in the process of separating elements such as Sb, cu and the like because Sn enters into the aqueous solution. Last Sn 2+ 、Sn 4+ Precipitation to Sn (OH) by neutralization 2 ，Sn(OH) 4 The recovery consumes a large amount of alkali, and the cost is high. And through CaO, ca (OH) with relatively low cost 2 The precipitated tin mud cannot completely remove Cu due to the process 2+ 、Cl - Cleaning the mixture to obtain CaCl 2 When the Sn is brought into a pyrogenic process working section, the Sn is brought into smoke dust, so that the recovery of tin is directly influenced, and the Sn is also the reason that the cost coefficient of the raw material market to the tin mud produced by a hydrochloric acid system is low. The last reason is that if the materials are stored carelessly, the materials are easy to be partially oxidized when being stacked, and Sn is SnO 2 The hydrochloric acid cannot be dissolved after the form is finished, and the subsequent pyrometallurgical refining is influenced.
Disclosure of Invention
The invention aims to provide a novel method for separating materials with Sn content of 40-58%, ag content of 4-8% and Au content of less than 100g/t, the process flow is shown in figure 1, and the method comprises the following steps:
(1) Roasting: the materials are naturally oxidized or added into a rotary kiln, a roasting furnace, an open hearth furnace or roasted, the high temperature section is controlled to be 550-650 ℃, the reaction time of the high temperature zone is more than or equal to 120min, and the main reaction of the oxidation process is as follows:
Cu+O 2 ＝2CuO
4Sb+3O 2 ＝2Sb 2 O 3
2Sb+5O 2 ＝2Sb 2 O 5
Sb 2 O 3 +O 2 ＝Sb 2 O 5
Sn+O 2 ＝SnO 2
2SnO+O 2 ＝2SnO 2
(2) Leaching: leaching the roasted material in the step 1 by using 2-4 mol/L hydrochloric acid, wherein the liquid-solid ratio is = 3: 1, the reaction time is 180min, the reaction temperature is 60-80 ℃, and then filtering and washing are carried out;
(3) Reduction: adding crude antimony powder into the filtrate obtained in the step 2 to obtain SbCl 5 Reduction to SbCl 3 ，2Sb+3SbCl 5 ＝5SbCl 3 . Due to the oxidizing roasting, part of the antimony may be oxidized to 5-valent, sbCl 5 Is not hydrolysable and requires reduction;
(4) Hydrolysis: adding water with 5 times volume of the reduced solution obtained in the step (4) into the reduced solution for hydrolysis, wherein the temperature is 30-40 ℃, the stirring speed is 85-120 r/min, the stirring time is 30min, then filtering,
SbCl 3 +H 2 O＝SbOCl+2HCl
the hydrolysate SbOCl can be smelted into crude antimony by using an intermediate frequency furnace or an electric furnace, or neutralized by using ammonia water to prepare finished antimony white for sale.
2SbOCI+2NH 3 H 2 O＝Sb 2 O 3 +2NH 4 Cl+H 2 O
(5) And (3) copper recovery: adding Fe powder into the filtrate obtained in the step 4 for replacing and recovering copper, fe + Cu2 + ＝Fe 2+ The Cu and copper powder is washed and then enters a copper refining workshop or sold outside, the Fe-containing solution is blown by an exhaust-heat boiler for concentration and evaporation to prepare FeCl 3 Spare, 4FeCl 2 +O 2 +4HCl＝4FeCl 3 +2H 2 O；
(6) Leaching silver: adding Na into the filter residue obtained in the step 2 2 SO 3 Separating silver and leaching, and controlling the conditions: na (Na) 2 SO 3 The concentration is 200g/L, the liquid-solid ratio is =5:1, the pH is 8.5-9.0, the T is 30 ℃, the t is =4h, the leaching material is filtered and washed, the filtrate is reduced by formaldehyde or hydrazine hydrate, the filter residue is leached by thiourea to Au and the rest Ag, agCl +2Na 2 SO 3 ＝Ag(SO 3 ) 2 3- +NaCl+3Na + ；
(7) Reducing silver powder: reducing the filtrate generated in the step 6 by using formaldehyde or hydrazine hydrate, and filtering after reduction;
(8) Leaching gold: will be provided withSelecting thiourea solution and FeCl as the filter residue produced in the step 6 3 Au is leached, and part of the rest silver can be leached by thiourea, so that the recovery rate of the silver is improved;
(9) Reducing gold powder: and reducing the filtrate obtained after gold leaching by thiourea by using Zn or Fe powder, returning the reduced solution to leach gold and silver, realizing the maximization of economic benefit, and removing impurities from the reduced gold powder to obtain gold and silver alloy powder, and also performing electrolytic separation or acid dissolution separation.
Further, air, pure oxygen or H-mixed gas may be added in step (1) 2 O 2 Feeding materials, and fully oxidizing Cu, sb and Sn in the materials. .
Further, in the step (8), the concentration of the thiourea is 35g/l, the pH is =1.0, the liquid-solid ratio is =5:1, the temperature is 30 ℃, the leaching time is 6-8h, and FeCl is added 3 The addition amount is 5-9 kg/t, the Au leaching efficiency of the raw material can reach 91-95%, and the leaching rate of silver can reach 40-50%.
Further, in the step (7), the mass ratio of the reducing agent to the mass ratio of Ag is =1: 2.5-3, the reduction temperature is 40-50 ℃, the reaction pH is controlled to be =10, and the duration is 3h; the actual addition amount of the reducing agent is 92-98% of the theoretical amount, and the situation that the direct yield is low due to the fact that the reducing agent remaining in the replacement solution reduces silver in the subsequent leaching solution into metal silver retention slag is prevented.
The method is more practical for the production flow of the anode mud containing the coarse tin with moderate gold and silver, particularly for the anode mud which is partially oxidized, the recovery rate of tin is higher, the recovery rate of gold and silver is more ideal, the method is particularly suitable for enterprises with a more complete industrial chain, a small part of un-leached gold and silver enter a pyrometallurgical section along with tin materials, and the economic benefit is remarkable.
Detailed Description
The present invention is further described with reference to the following examples, which are not intended to limit the invention, and it should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Example 1: 100g of leaching residue after antimony and copper removal is taken, and the leaching residue mainly comprises the following components: sn:52.45% Cu:0.32%, sb:0.13%, au:72.5g/t, ag:5.17 percent.
500ml of deionized water is taken and 100g of Na is added 2 SO 3 Stirring to dissolve, slowly adding 100g of leaching residue, adding a little NaOH solution to adjust the pH =8.5, controlling the reaction temperature of 38 ℃ (in winter) to be normal temperature in summer, carrying out leaching reaction for 5-6 h, clarifying, filtering, washing a filter cake, drying and weighing 92.5g. Leaching residue components: sn:56.72%, au:78.35g/t, ag:0.308 percent. 625ml of a filtrate (containing a washing solution), 7.81g/l of Ag, 94.41% of leaching rate, reduction of the filtrate with formaldehyde, control of the temperature at 50 ℃ and pH =10, addition of 2.5g of a reducing agent, stirring and reaction for 3 hours, filtration, washing, drying and weighing of the obtained silver powder for 4.84g, and a yield of 93.62%.
Leaching gold with thiourea in the amount of 92.5g of leached residue, adding 13.0g of thiourea into 370ml of deionized water, slowly adding 92.5g of filter residue, and leaching with H 2 SO 4 Adjusting pH =1.0, adding FeCl 3 1.0g, stirring and leaching for 6 hours, controlling the reaction temperature to be about 30 ℃, clarifying, filtering and washing after the reaction is ended, drying and weighing 91.8g of filter cake, and comprising the following components: au:6.87g/t, ag:0.125%, sn:56.84 percent.
And (3) reducing the filtrate by iron powder, removing impurities, dissolving and separating Au and Ag to obtain pure Au powder of 6.62mg, wherein the direct yield is 91.3%, the silver powder is 0.13g, the recovery rate of the silver in the process is 46.43%, and the total yield is 96.13%.
Example 2: taking 500g of leaching residue after removing Cu and Sb, wherein the main components are as follows: sn:46.22%, cu:0.28%, sb:0.17%, au:95.32g/t, ag:7.25 percent.
2500ml of the obtained product was taken, water was removed, and 500g of Na was added 2 SO 3 Stirring to dissolve, adding a little NaOH to adjust pH =9.0, slowly adding 500g of leaching residue, controlling the temperature at 30 ℃, reacting for 5h, clarifying, filtering, washing with water, and drying a filter cake to obtain 454.2g. The components are as follows: sn:50.78%, au:104.98g/t, ag:0.392%. 2840ml of filtrate (containing washing liquor), ag:12.14g/l, the leaching rate of silver is as follows: 95.08 percent, reducing the filtrate by hydrazine hydrate, controlling the pH value to 10 and the temperature to 50 ℃, reacting for 3 hours, filtering, washing, drying and weighing 33.98g of the obtained silver powder, and obtaining the yield of 93.74 percent.
454.2g of Ag-leaching residue is slowly added into the prepared thiourea leaching solution, the pH value is adjusted to 1.0, and FeCl is added 3 3.8g, stirring and leaching for 5 hours, controlling the reaction temperature to be about 30 ℃, after the reaction is finished, clarifying, filtering, washing, drying and weighing 448.2g of filter residue, and detecting the components: sn:51.32%, au:7.68g/t, ag:0.197 percent, filtrate is adsorbed, dissolved and separated by active carbon to obtain pure Au powder of 44.08mg, and the direct yield of gold is as follows: 92.49%, ag powder 0.86g, the recovery rate of the silver in the process 48.31%, and the total recovery rate of the Ag leached twice 96.11%.
Example 3
A method for wet processing a copper antimony tin material containing middle-low gold and silver comprises the following steps:
(1) Roasting: the materials are naturally oxidized or added into a rotary kiln, a roasting furnace, an open hearth furnace or roasted, the high temperature section is controlled to be 550-650 ℃, the reaction time in the high temperature zone is more than or equal to 120min, and oxygen is introduced in the roasting process;
(2) Leaching: leaching the roasted material in the step 1 by using 2-4 mol/L hydrochloric acid, wherein the liquid-solid ratio is = 3: 1, the reaction time is 180min, the reaction temperature is 60-80 ℃, and then filtering and washing are carried out;
(3) Reduction: adding crude antimony powder into the filtrate obtained in the step 2 to obtain SbCl 5 Reduced to SbCl 3 ；
(4) Hydrolysis: adding water with the volume 5 times that of the reduced solution obtained in the step 4 into the reduced solution for hydrolysis, wherein the temperature is 30-40 ℃, the stirring speed is 85-120 r/min, the stirring time is 30min, then filtering is carried out, and a hydrolysate SbOCl can be smelted into crude antimony by using an intermediate frequency furnace or an electric furnace, or neutralized by using ammonia water to prepare a finished product of antimony white for sale;
(5) And (3) copper recovery: adding Fe powder into the filtrate obtained in the step 4 for replacement and recovery of copper;
(6) Leaching silver: adding Na into the filter residue obtained in the step 2 2 SO 3 Leaching with silver, in which Na is 2 SO 3 The concentration is 200g/L, the liquid-solid ratio is =5:1, the pH is 8.5-9.0, the T is 30 ℃, and t =4h;
(7) Reducing silver powder: reducing the filtrate generated in the step 6 by formaldehyde, wherein the mass ratio of the formaldehyde to the Ag is =1: 3, the reduction temperature is 40-50 ℃, the reaction pH is controlled to =10, and the duration is 3h; the actual addition amount of the reducing agent is 93 percent of the theoretical amount;
(8) Leaching gold: selecting thiourea solution and FeCl from the filter residue produced in the step 6 3 Leaching Au, and leaching partial residual silver by thiourea with the concentration of 35g/l, the pH =1.0, the liquid-solid ratio =5:1, the temperature is 30 ℃, the leaching time is 6-8h, feCl 3 The addition amount is 5kg/t, the leaching rate of the silver can reach 41.5 percent, and the total recovery rate of the silver is 95.3 percent.
(9) Reducing gold powder: the filtrate after thiourea gold leaching is reduced by Zn or Fe powder, the direct yield of Au can reach 92.5%, the reduced solution can be returned to leach gold and silver, the economic benefit maximization is realized, and the gold and silver alloy powder is obtained after the gold powder after reduction is subjected to impurity removal, and electrolytic separation or acid dissolution separation can also be carried out.
Example 4
A wet method for treating a copper-antimony-tin material containing low-grade gold and silver comprises the following steps:
(1) Roasting: the materials are naturally oxidized or added into a rotary kiln, a roasting furnace, an open hearth furnace or roasted, the high temperature section is controlled to be 550-650 ℃, the reaction time of the high temperature zone is more than or equal to 120min, and H is added in the roasting process 2 O 2 ；
(2) Leaching: leaching the roasted material in the step 1 by using 2-4 mol/L hydrochloric acid, wherein the liquid-solid ratio is = 3: 1, the reaction time is 180min, the reaction temperature is 60-80 ℃, and then filtering and washing are carried out;
(3) Reduction: adding crude antimony powder into the filtrate obtained in the step 2 to obtain SbCl 5 Reduction to SbCl 3 ；
(4) Hydrolysis: adding water with the volume 5 times that of the reduced solution obtained in the step 4 into the reduced solution for hydrolysis, wherein the temperature is 30-40 ℃, the stirring speed is 85-120 r/min, the stirring time is 30min, then filtering is carried out, and a hydrolysate SbOCl can be smelted into crude antimony by using an intermediate frequency furnace or an electric furnace, or neutralized by using ammonia water to prepare a finished product of antimony white for sale;
(5) And (3) copper recovery: adding Fe powder into the filtrate obtained in the step 4 for replacement and recovery of copper;
(6) Leaching silver: adding Na into the filter residue obtained in the step 2 2 SO 3 Leaching with silver, in which Na is 2 SO 3 The concentration is 200g/L, the liquid-solid ratio is =5:1, the pH is 8.5-9.0, the T is 30 ℃, and t =4h;
(7) Reducing silver powder: reducing the filtrate generated in the step 6 by hydrazine hydrate, wherein the mass ratio of hydrazine hydrate to Ag is =1:2.5, the reduction temperature is 40-50 ℃, the reaction pH is controlled to =10, and the reaction time is 3h; the actual addition amount of the reducing agent is 97 percent of the theoretical amount;
(8) Leaching gold: selecting thiourea solution and FeCl from the filter residue produced in the step 6 3 Leaching Au, and leaching partial residual silver by thiourea with the concentration of 35g/l, the pH =1.0, the liquid-solid ratio =5:1, the temperature is 30 ℃, the leaching time is 6-8h, feCl 3 The addition amount is 9kg/t, the leaching rate of the silver can reach 43.5 percent, and the total recovery rate of the silver is 96.3 percent.
(9) Reducing gold powder: the filtrate after thiourea gold leaching is reduced by Zn or Fe powder, the direct yield of Au can reach 94.5%, the reduced solution can be returned to leach gold and silver, the economic benefit maximization is realized, and the gold and silver alloy powder is obtained after the gold powder after reduction is subjected to impurity removal, and electrolytic separation or acid dissolution separation can also be carried out.
Example 5
A wet method for treating a copper-antimony-tin material containing low-grade gold and silver comprises the following steps:
(1) Roasting: the materials are naturally oxidized or added into a rotary kiln, a roasting furnace, an open hearth furnace or roasted, the high temperature section is controlled to be 550-650 ℃, the reaction time of the high temperature zone is more than or equal to 120min, and H is added in the roasting process 2 O 2 ；
(2) Leaching: leaching the roasted material in the step 1 by using 2-4 mol/L hydrochloric acid, wherein the liquid-solid ratio is = 3: 1, the reaction time is 180min, the reaction temperature is 60-80 ℃, and then filtering and washing are carried out;
(3) Reduction: adding crude antimony powder into the filtrate obtained in the step 2 to obtain SbCl 5 Reduction to SbCl 3 ；
(4) Hydrolysis: adding water with the volume 5 times that of the reduced solution obtained in the step 4 into the reduced solution for hydrolysis, wherein the temperature is 30-40 ℃, the stirring speed is 85-120 r/min, the stirring time is 30min, then filtering is carried out, and a hydrolysate SbOCl can be smelted into crude antimony by using an intermediate frequency furnace or an electric furnace, or neutralized by using ammonia water to prepare a finished product of antimony white for sale;
(5) And (3) copper recovery: adding Fe powder into the filtrate obtained in the step 4 for replacement and recovery of copper;
(6) Leaching silver: adding Na into the filter residue obtained in the step 2 2 SO 3 Leaching with silver, in which Na is 2 SO 3 The concentration is 200g/L, the liquid-solid ratio is =5:1, the pH is 8.5-9.0, the T is 30 ℃, and t =4h;
(7) Reducing silver powder: reducing the filtrate generated in the step 6 by hydrazine hydrate, wherein the mass ratio of hydrazine hydrate to Ag is =1: 3, the reduction temperature is 40-50 ℃, the reaction pH is controlled to =10, and the reaction time is 3h; the actual addition amount of the reducing agent is 95 percent of the theoretical amount;
(8) Leaching gold: selecting thiourea solution and FeCl from the filter residue produced in the step 6 3 Leaching Au, and leaching partial residual silver by thiourea with the concentration of 35g/l, the pH =1.0, the liquid-solid ratio =5:1, the temperature is 30 ℃, the leaching time is 6-8h, feCl 3 The addition amount is 7kg/t, the leaching rate of the silver can reach 44.5 percent, and the total recovery rate of the silver is 97.1 percent;
(9) Reducing gold powder: the filtrate after thiourea gold leaching is reduced by Zn or Fe powder, the direct yield of Au can reach 94.8%, the reduced solution can be returned to leach gold and silver, the economic benefit maximization is realized, and the gold and silver alloy powder is obtained after the gold powder after reduction is subjected to impurity removal, and electrolytic separation or acid dissolution separation can also be carried out.
Claims (6)
1. A wet method for treating a copper-antimony-tin material containing low-grade gold and silver comprises the following steps:
(1) Roasting: the materials are naturally oxidized or added into a rotary kiln, a roasting furnace, an open hearth furnace or roasted, the high temperature section is controlled to be 550-650 ℃, and the reaction time in the high temperature zone is more than or equal to 120min;
(2) Leaching: leaching the roasted material in the step 1 by using 2-4 mol/L hydrochloric acid, wherein the liquid-solid ratio is = 3: 1, the reaction time is 180min, the reaction temperature is 60-80 ℃, and then filtering and washing are carried out;
(3) Reduction: adding crude antimony powder into the filtrate obtained in the step 2 to obtain SbCl 5 Reduction to SbCl 3 ；
(4) Hydrolysis: adding water with the volume 5 times that of the reduced solution obtained in the step 4 into the reduced solution for hydrolysis, wherein the temperature is 30-40 ℃, the stirring speed is 85-120 r/min, the stirring time is 30min, then filtering is carried out, and a hydrolysate SbOCl can be smelted into crude antimony by using an intermediate frequency furnace or an electric furnace, or neutralized by using ammonia water to prepare a finished product of antimony white for sale;
(5) And (3) copper recovery: adding Fe powder into the filtrate obtained in the step 4 for replacement and recovery of copper;
(6) Leaching silver: adding Na into the filter residue obtained in the step 2 2 SO 3 Silver separation and leaching;
(7) Reducing silver powder: reducing the filtrate generated in the step 6 by using formaldehyde or hydrazine hydrate, and filtering after reduction;
(8) Leaching gold: selecting thiourea solution and FeCl from the filter residue produced in the step 6 3 Au is leached, and part of the rest silver can be leached by thiourea, so that the recovery rate of the silver is improved;
(9) Reducing gold powder: and reducing the filtrate obtained after gold leaching by thiourea by using Zn or Fe powder, returning the reduced solution to leach gold and silver, realizing the maximization of economic benefit, and removing impurities from the reduced gold powder to obtain gold and silver alloy powder, and also performing electrolytic separation or acid dissolution separation.
2. The method as claimed in claim 1, wherein air, pure oxygen or H-mixed gas is added in step (1) 2 O 2 Feeding materials, and fully oxidizing Cu, sb and Sn in the materials.
3. The method of claim 1, wherein in step (8), the thiourea concentration is 35g/l, the pH is =1.0, the liquid-solid ratio is =5:1, the temperature is 30 ℃, the leaching time is 6-8h, and the FeCl is added into the solution 3 The addition amount is 5-9 kg/t, the Au leaching efficiency of the raw material can reach 91-95%, and the leaching rate of silver can reach 40-50%.
4. The method according to claim 1, wherein in the step (7), the mass ratio of the reducing agent to the mass ratio of Ag is (1) from 2.5 to 3, the reduction temperature is from 40 to 50 ℃, the reaction pH is controlled to be =10, the time is 3 hours, the actual adding amount of the reducing agent is 92 to 98 percent of the theoretical amount, and the reducing agent remained in the replacement solution is prevented from reducing the silver in the subsequent leachate into the metal silver retention slag, so that the direct yield is low.
5. The method according to claim 1, wherein in step (6), na 2 SO 3 The concentration is 200g/L, the liquid-solid ratio is =5, 1, the pH is 8.5-9.0, T is 30 ℃, t is =4h, the leaching material is filtered and washed, the filtrate is reduced by formaldehyde or hydrazine hydrate, and the filter residue is leached by thiourea into Au and the rest Ag, agCl +2Na 2 SO 3 ＝Ag(SO 3 ) 2 3- +NaCl+3Na + 。
6. The process according to claim 1, wherein the direct yield of gold is > 91% and the direct yield of silver is > 95%.
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