CN102978411B - Comprehensive recycling method for crude indium casting slag - Google Patents
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Abstract
The invention provides a comprehensive recycling method for crude indium casting slag. The comprehensive recycling method comprises the following steps: A, leaching crude indium casting slag with sulfuric acid; B, carrying out purification to the leached liquid with sponge indium; C, replacing the purified liquid with a zinc sheet, and obtaining the sponge indium after separation; D, briquetting and casting mould, i.e. briquetting the leached slag obtained in the Step A and the sponge indium obtained in the Step C after cleaning with water, and mixing and casting mould to obtain zinc contained crude indium; and E, eliminating zinc and tin, i.e. adding zinc contained crude indium into molten alkali, adding sodium nitrate after the zinc contained crude indium is molten, and eliminating the zinc and tin in the zinc contained crude indium to obtain crude indium with an indium content grade of more than 99wt percent. According to the comprehensive recycling method provided by the invention, the recycling rate of extracting indium from the crude indium casting slag is more than 98 percent; the grade of the obtained crude indium is more than 99wt percent; zinc and cadmium can be extracted, so that valuable metal such as lead, tin, and the like is concentrated, which is good for the recycling in the subsequent working procedures; and the process is reliable as well as the production cost is low.
Description
Technical field
The present invention relates to a kind of Non-ferrous Metallurgy field, particularly the comprehensive recovering process of thick indium casting mold slag in a kind of zinc hydrometallurgy.
Background technology
The smelting technology of indium has generally comprised the pressure group and casting mold operation of sponge indium, and in casting mold process, except obtaining thick indium, also can produce a kind of alkaline residue is thick indium casting mold slag.In thick indium casting mold slag, the general indium that contains, in 20% left and right, also contains the valuable metals such as a certain amount of zinc, lead, tin simultaneously, and particularly, in the time that sponge indium is second-rate, in thick indium casting mold slag, the content of indium exceedes 50%.Some Enterprises is taked to stack to casting mold slag and is processed, and has both disorderly taken resource, has taken again place simultaneously, also becomes source of pollution; Some enterprise returns casting mold slag to leach operation and again leach, and cause complex manufacturing, production cost high, and indium recovery is low, other valuable metal disperses, and can not get efficient recovery.
Therefore, how valuable metal and the high efficiente callback indium such as comprehensive recovery of indium, zinc, lead from thick indium casting mold slag, and isolate the valuable metals such as zinc, cadmium and enriched lead, tin, improving production environment simultaneously and reducing production costs is to need the difficult problem further explored.
Summary of the invention
The invention solves in currently available technology and process the above-mentioned defect existing in the method for thick indium casting mold slag, a kind of comprehensive recovering process of thick indium casting mold slag is provided.
Particularly, technical scheme of the present invention is:
A comprehensive recovering process for thick indium casting mold slag, comprises the following steps:
A, sulfuric acid leaching: thick indium casting mold slag is adopted to sulfuric acid leaching, after separation, obtain leach liquor and leached mud;
B, sponge indium purify: in the leach liquor of steps A, add sponge indium to purify, the valuable metal ions in leach liquor is reduced into metal and is enriched in slag, be purified liquid after separation;
C, zinc metal sheet displacement: the scavenging solution of step B is replaced with zinc metal sheet, after separation, obtain displacement liquid and sponge indium;
D, the group of pressure and casting mold: the leached mud washing of steps A is obtained to washery slag, by the group of pressure after the sponge indium washing of step C, then with washery slag mixing casting mold, obtain containing the thick indium of zinc;
E, dezincify tin: by adding in the alkali of melting containing the thick indium of zinc of step D, after containing the thick indium fusing of zinc, add SODIUMNITRATE, slough containing the zinc-tin in the thick indium of zinc, obtaining containing indium grade is thick indium more than 99wt%.
As a further improvement on the present invention, in steps A, the concentration of described sulfuric acid is 150～200g/L, and the quality liquid-solid ratio of sulfuric acid and thick indium casting mold slag is 3:1～6:1.
As a further improvement on the present invention, in steps A, the condition of leaching comprises: temperature of reaction is 60～85 DEG C, extraction time 1～3 hour, and in leach liquor, sulfur acid is 20～80g/L.
As a further improvement on the present invention, in step B, the consumption of described sponge indium is 0.95～1.05 times of required theoretical consumption that valuable metal ions Restore All in leach liquor is become to metal.
As a further improvement on the present invention, in step B, the condition of purification comprises: temperature is 50～85 DEG C, and the time is 40～120 minutes.
As a further improvement on the present invention, in step C, the consumption of zinc metal sheet is excessive, and the condition of displacement comprises: temperature is 50～80 DEG C, and the reaction times is 6～12 hours, and endpoint pH is 4～4.5.
As a further improvement on the present invention, in step C, also comprise the step of displacement liquid being returned to wet zinc-making system recovery zinc and cadmium.
As a further improvement on the present invention, in steps A, the condition of leached mud washing comprises: the quality liquid-solid ratio of washing water and leached mud is 3:1～8:1, and wash temperature is 50～70 DEG C, and washing time is 20～60 minutes; In step D, the condition of sponge indium washing comprises: the quality liquid-solid ratio of washing water and sponge indium is 5:1～10:1, and washing time is 15～45 minutes.
As a further improvement on the present invention, in step D, it is 40～80 tons that the sponge indium after washing is pressed the pressure of group, and the temperature of fusion of casting mold is 300～450 DEG C, and the fusion time is 45～90 minutes, is 3 ~ 7wt% containing the zinc content in the thick indium of zinc.
As a further improvement on the present invention, in step e, the consumption of SODIUMNITRATE is containing 5～10% of the thick indium quality of zinc; The condition of dezincify tin comprises: temperature is 420～500 DEG C, and the time is 30～60 minutes.
Beneficial effect of the present invention is:
The comprehensive recovering process of thick indium casting mold slag provided by the invention, the rate of recovery of extracting indium from thick indium casting mold slag is up to more than 98%, and the thick indium grade obtaining is more than 99wt%; And in the displacement liquid obtaining, cl content, lower than 0.05g/L, can directly enter wet zinc-making system and reclaim zinc cadmium; The valuable metals such as while lead, tin obtain enrichment, are conducive to subsequent handling and reclaim.To sum up, comprehensive recovering process provided by the invention, has advantages of process, production cost is low, indium recovery is high and comprehensively reclaims other various valuable metals, suitable from thick indium casting mold slag the valuable metal such as comprehensive recovery of indium, zinc, lead.
Brief description of the drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
The comprehensive recovering process that the invention provides a kind of thick indium casting mold slag, as shown in Figure 1, comprises the following steps:
A, sulfuric acid leaching: thick indium casting mold slag is adopted to sulfuric acid leaching, after separation, obtain leach liquor and leached mud;
B, sponge indium purify: in the leach liquor of steps A, add sponge indium to purify, the valuable metal ions in leach liquor is reduced into metal and is enriched in slag, be purified liquid after separation;
C, zinc metal sheet displacement: the scavenging solution of step B is replaced with zinc metal sheet, after separation, obtain displacement liquid and sponge indium;
D, the group of pressure and casting mold: the leached mud washing of steps A is obtained to washery slag, by the group of pressure after the sponge indium washing of step C, then with washery slag mixing casting mold, obtain containing the thick indium of zinc;
E, dezincify tin: by adding in the alkali of melting containing the thick indium of zinc of step D, after containing the thick indium fusing of zinc, add SODIUMNITRATE, slough containing the zinc-tin in the thick indium of zinc, obtaining containing indium grade is thick indium more than 99wt%.
The method according to this invention, first adopts sulfuric acid to leach processing to thick indium casting mold slag, and the valuable metals such as the indium in thick indium casting mold slag, zinc, cadmium are immersed in solution, then passes through liquid-solid separation, obtains leach liquor and leached mud.Leached mud send to be washed and starched, and the washery slag obtaining send casting mold operation; Leach liquor send subsequent processing---and sponge indium purifies.
In the present invention, the sulfuric acid adopting when leaching is the various sulfuric acid that those skilled in the art commonly use, and the concentration of for example its sulfuric acid is 150～200g/L.Under preferable case, when leaching, sulfuric acid is 3:1～6:1 with the quality liquid-solid ratio of thick indium casting mold slag.In the present invention, the condition of leaching comprises: temperature of reaction is 60～85 DEG C, extraction time 1～3 hour, and in leach liquor, sulfur acid is 20～80g/L.
The condition that leached mud is washed and starched comprises: the quality liquid-solid ratio of washing water and leached mud is 3:1～8:1, and wash temperature is 50～70 DEG C, and washing time is 20～60 minutes;
The step that sponge indium purifies comprises: toward the leach liquor of steps A in, add sponge indium to purify, make in leach liquor the various valuable metal ions such as leaded, tin, bismuth be reduced into metal, and be enriched in slag, after separation, be purified liquid and purification slag.Wherein, purification slag can return lead system and reclaim the valuable metals such as lead, tin, and scavenging solution send subsequent processing---zinc metal sheet displacement.
In this step B, the consumption of described sponge indium is 0.95～1.05 times of required theoretical consumption that valuable metal ions Restore All in leach liquor is become to metal.The condition purifying comprises: temperature is 50～85 DEG C, and the time is 40～120 minutes.
The step of zinc metal sheet displacement is: in scavenging solution, add zinc metal sheet to replace, obtain displacement liquid and sponge indium after separation.In displacement liquid, contain zinc and cadmium, its cl content, lower than 0.05g/L, therefore can directly return wet zinc-making system and reclaim zinc cadmium, and wherein zinc is for the production of electric zinc, and cadmium is for the production of pure cadmium.
In the present invention, for ensureing that the indium in scavenging solution is thoroughly replaced, the consumption of zinc metal sheet is excessive.The condition of displacement comprises: temperature is 50～80 DEG C, and the reaction times is 6～12 hours, and endpoint pH is 4～4.5.
The method according to this invention, then washes the sponge indium obtaining after displacement, sloughs the soluble impurity in sponge indium.Under preferable case, the condition of sponge indium washing comprises: the quality liquid-solid ratio of washing water and sponge indium is 5:1～10:1, and washing time is 15～45 minutes.
In the present invention, wash water in wash water after the washing of sponge indium and steps A after leached mud washing all can return for sulfuric acid leaching, valuable metal indium in recyclable wash water and the acid in wash water on the one hand, also can reduce on the other hand the consumption of water in leaching process, in improving indium recovery, save production cost.
Then the sponge indium after washing is pressed to group, the pressure of the group of pressure is 40～80 tons; Then mix with the washery slag obtaining after leached mud washing in steps A, carry out together casting mold; During due to displacement, zinc metal sheet is excessive, in the thick indium therefore obtaining after casting mold, also contains a small amount of zinc, is containing the thick indium of zinc.Under preferable case, the temperature of fusion of casting mold is 300～450 DEG C, and the fusion time is 45～90 minutes.The zinc content containing in the thick indium of zinc obtaining after casting mold is 3 ~ 7wt%.
Then to carrying out the processing of dezincify tin containing the thick indium of zinc, specifically comprising this is added in the alkali of melting containing the thick indium of zinc, after containing the thick indium fusing of zinc, add SODIUMNITRATE, react and slough the zinc-tin containing containing in the thick indium of zinc, is thick indium more than 99wt% thereby obtain containing indium grade.
In this step, described ammonium nitrate can directly adopt industrial ammonium nitrate.Under preferable case, the consumption of SODIUMNITRATE is containing 5～10% of the thick indium quality of zinc.The condition of dezincify tin comprises: temperature is 420～500 DEG C, and the time is 30～60 minutes.
In the comprehensive recovering process of thick indium casting mold slag provided by the invention, extract indium from thick indium casting mold slag time, make in displacement liquid cl content lower than 0.05g/L, it can directly return wet zinc-making system and reclaim zinc cadmium, successfully solve in the removal process of Liao Xin smeltery byproduct indium the problem that the displaced liquid of generation is directly returned Zn system and produced chlorine in electric zinc; And exceeding 99wt% through the grade that method of the present invention reclaims the thick indium obtaining, the valuable metal such as lead, tin obtains enrichment simultaneously, is more conducive to subsequent handling recovery; And have process, production cost is low, indium recovery is high and comprehensively reclaims the advantage of other various valuable metals, suitable from thick indium casting mold slag the valuable metal such as comprehensive recovery of indium, zinc, lead.
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.In embodiment, the raw material that adopts is all commercially available.
Embodiment 1
Steps A: thick indium casting mold slag is joined by quality liquid-solid ratio in the sulfuric acid of 150g/L at 3: 1, and controlling temperature of reaction is 60 DEG C, extraction time 1 hour, in leach liquor, sulfur acid is 20g/L, and solid-liquid separation obtains leach liquor and leached mud, and leach liquor send subsequent processing; Leached mud is washed and starched, and wash conditions is: the quality liquid-solid ratio of washing water and leached mud is 3:1, and wash temperature is 50 DEG C, and washing time is 20min, obtains washery slag.
At step B:50 DEG C, in leach liquor, add fresh sponge indium to purify, the add-on of sponge indium is 1.0 times of theoretical consumption of valuable metal in leach liquor all being replaced to the required indium of reduction, reaction times is 40 minutes, liquid-solid scavenging solution and the purification slag of separating to obtain, purification slag returns lead system and reclaims Pb and Sn as valuable metal, and scavenging solution send subsequent processing.
Step C: add excessive zinc metal sheet displacement in scavenging solution, it is 50 DEG C that replacement process keeps temperature, and in 6 hours reaction times, endpoint pH is 4, obtains sponge indium and displacement liquid, and sponge indium send subsequent processing, and displacement liquid returns wet zinc-making system recovery zinc cadmium.
Step D: the sponge indium of step C is washed, and wash conditions is: the quality liquid-solid ratio of washing water and sponge indium is 5:1, washing time is 15min; The condition that is 40 tons at pressure by the sponge indium after washing presses down group, and carry out casting mold, the temperature of fusion of casting mold with together with the washery slag of steps A: 300 DEG C, the fusion time: 45min, obtain containing the thick indium of zinc, its composition is by mass percentage: In 92.73%, Zn 6.71%, Sn 0.142%.
Step e: by step D carry out dezincify tin containing the thick indium of zinc, 500 DEG C of the temperature of dezincify tin, will be added in the sheet alkali of melting containing the thick indium of zinc, and the add-on of industrial sodium nitrate is 10% of thick indium weight, the dezincify tin time: 60 minutes.
By above-mentioned steps, obtaining thick indium grade is 99.53%, and its impurity composition is by mass percentage: Sn 0.012%, Bi 0.084%, Pb 0.084%, Cu 0.0032%, the rate of recovery of indium is 98. 37%.
Embodiment 2
Steps A: thick indium casting mold slag is joined by quality liquid-solid ratio in the sulfuric acid of 180g/L at 5: 1, and controlling temperature of reaction is 75 DEG C, extraction time 2 hours, in leach liquor, sulfur acid is 50g/L; Solid-liquid separation obtains leach liquor and leached mud, and leach liquor send subsequent processing; Leached mud is washed and starched, and wash conditions is: liquid-solid ratio is 6:1, and wash temperature is 60 DEG C, and washing time is 40min, obtains washery slag.
At step B:60 DEG C, in leach liquor, add fresh sponge indium to purify, the add-on of sponge indium is 1.1 times of theoretical consumption of valuable metal in leach liquor all being replaced to the required indium of reduction, reaction times is 80 minutes, liquid-solid scavenging solution and the purification slag of separating to obtain, purification slag returns lead system and reclaims Pb and Sn as valuable metal, and scavenging solution send subsequent processing.
Step C: add excessive zinc metal sheet displacement in scavenging solution, replacement process control temperature is at 65 DEG C, and in 9 hours reaction times, endpoint pH is 4.2, obtains sponge indium and displacement liquid, and sponge indium send subsequent processing, and displacement liquid returns wet zinc-making system recovery zinc cadmium.
Step D: the sponge indium of step C is washed, and wash conditions is: the quality liquid-solid ratio of washing water and sponge indium is 8:1, washing time is 30min; The condition that is 60t at pressure by the sponge indium after washing presses down group, and carry out casting mold, the temperature of fusion of casting mold with together with the washery slag of steps A: 380 DEG C, the fusion time: 70min, obtain containing the thick indium of zinc, its composition is by mass percentage: In 94.16%, Zn 5.18%, Sn 0.108%
Step e: by step D carry out dezincify tin containing the thick indium of zinc, 480 DEG C of the temperature of dezincify tin, will be added in the sheet alkali of melting containing the thick indium of zinc, and the add-on of industrial sodium nitrate is 8% of thick indium weight, the dezincify tin time: 45 minutes.
By above-mentioned steps, obtaining thick indium grade is 99.65%, and its impurity composition is by mass percentage: Sn 0.0071%, Bi 0.074%, Pb 0.063%, Cu 0.0024%, the rate of recovery of indium is 98. 95%.
Embodiment 3
Steps A: thick indium casting mold slag is joined by quality liquid-solid ratio in the sulfuric acid of 200g/L at 6: 1, and controlling temperature of reaction is 85 DEG C, extraction time 3 hours, in leach liquor, sulfur acid is 80g/L; Solid-liquid separation obtains leach liquor and leached mud, and leach liquor send subsequent processing; Leached mud is washed and starched, and wash conditions is: liquid-solid ratio is 8:1, and wash temperature is 70 DEG C, and washing time is 60min, obtains washery slag.
At step B:70 DEG C, in leach liquor, add fresh sponge indium to purify, the add-on of sponge indium is 1.2 times of theoretical consumption of valuable metal in leach liquor all being replaced to the required indium of reduction, reaction times is 120 minutes, liquid-solid scavenging solution and the purification slag of separating to obtain, purification slag returns lead system and reclaims Pb and Sn as valuable metal, and scavenging solution send subsequent processing.
Step C: add excessive zinc metal sheet displacement in scavenging solution, replacement process control temperature is at 80 DEG C, and in 12 hours reaction times, endpoint pH is 4.5, obtains sponge indium and displacement liquid, and sponge indium send subsequent processing, and displacement liquid returns wet zinc-making system recovery zinc cadmium.
Step D: the sponge indium of step C is washed, and wash conditions is: the quality liquid-solid ratio of washing water and sponge indium is 10:1, washing time is 45min; The condition that is 80t at pressure by the sponge indium after washing presses down group, and carry out casting mold, the temperature of fusion of casting mold with together with the washery slag of steps A: 450 DEG C, the fusion time: 90min, obtain containing the thick indium of zinc, its composition is by mass percentage: In 95.51%, Zn 4.15%, Sn 0.87%
Step e: by step D carry out dezincify tin containing the thick indium of zinc, 420 DEG C of the temperature of dezincify tin, will be added in the sheet alkali of melting containing the thick indium of zinc, and the add-on of industrial sodium nitrate is 5% of thick indium weight, the dezincify tin time: 30 minutes.
By above-mentioned steps, obtaining thick indium grade is 99.76%, and its impurity composition is by mass percentage: Sn 0.0067%, Bi 0.037%, Pb 0.082%, Cu 0.0033%, the rate of recovery of indium is 99.05%.
Claims (4)
1. a comprehensive recovering process for thick indium casting mold slag, is characterized in that, comprises the following steps:
A, sulfuric acid leaching: thick indium casting mold slag is adopted to sulfuric acid leaching, obtain leach liquor and leached mud after separation, leached mud is washed and starched and obtained washery slag; The concentration of described sulfuric acid is 150～200g/L, and the quality liquid-solid ratio of sulfuric acid and thick indium casting mold slag is 3:1～6:1; The condition leaching comprises: temperature of reaction is 60～85 DEG C, extraction time 1～3 hour, and in leach liquor, sulfur acid is 20～80g/L;
B, sponge indium purify: in the leach liquor of steps A, add sponge indium to purify, the valuable metal ions in leach liquor is reduced into metal and is enriched in slag, be purified liquid after separation; The consumption of described sponge indium is 0.95～1.05 times of required theoretical consumption that valuable metal ions Restore All in leach liquor is become to metal; The condition purifying comprises: temperature is 50～85 DEG C, and the time is 40～120 minutes;
C, zinc metal sheet displacement: the scavenging solution of step B is replaced with zinc metal sheet, after separation, obtain displacement liquid and sponge indium; The consumption of zinc metal sheet is excessive, and the condition of displacement comprises: temperature is 50～80 DEG C, and the reaction times is 6～12 hours, and endpoint pH is 4～4.5; Also comprise the step of displacement liquid being returned to wet zinc-making system recovery zinc and cadmium;
D, the group of pressure and casting mold: by the group of pressure after the sponge indium washing of step C, then mix and carry out casting mold with the washery slag of steps A, obtain containing the thick indium of zinc;
E, dezincify tin: by adding in the alkali of melting containing the thick indium of zinc of step D, after containing the thick indium fusing of zinc, add SODIUMNITRATE, slough containing the zinc-tin in the thick indium of zinc, obtaining containing indium grade is thick indium more than 99wt%; The consumption of SODIUMNITRATE is containing 5～10% of the thick indium quality of zinc;
In wash water after the washing of described step D sponge indium and steps A, the wash water of leached mud after washing and starching all returns for sulfuric acid leaching.
2. comprehensive recovering process according to claim 1, is characterized in that, in steps A, the condition that leached mud is washed and starched comprises: the quality liquid-solid ratio of washing water and leached mud is 3:1～8:1, and wash temperature is 50～70 DEG C, and washing time is 20～60 minutes; In step D, the condition of sponge indium washing comprises: the quality liquid-solid ratio of washing water and sponge indium is 5:1～10:1, and washing time is 15～45 minutes.
3. comprehensive recovering process according to claim 1, is characterized in that, in step D, it is 40～80 tons that sponge indium after washing is pressed the pressure of group, the temperature of fusion of casting mold is 300～450 DEG C, and the fusion time is 45～90 minutes, is 3 ~ 7wt% containing the zinc content in the thick indium of zinc.
4. comprehensive recovering process according to claim 1, is characterized in that, the condition of dezincify tin comprises: temperature is 420～500 DEG C, and the time is 30～60 minutes.
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| CN103695651A (en) * | 2013-12-31 | 2014-04-02 | 济源豫金靶材科技有限公司 | Method for recovering indium and stannum from indium-tin alloy |
| CN104120266A (en) * | 2014-08-02 | 2014-10-29 | 蒙自矿冶有限责任公司 | Method for preparing high-quality anti-position indium feed liquid by using complex indium copper enrichment residues |
| CN105219970B (en) * | 2015-10-29 | 2017-07-07 | 红河锌联科技发展有限公司 | A kind of method that many metals and calcium chloride are reclaimed in roasting dirt |
| CN105349800B (en) * | 2015-11-18 | 2017-11-17 | 来宾华锡冶炼有限公司 | A kind of method and its purification tank of solution of zinc sulfate displacement removal of impurities |
| CN106148735A (en) * | 2016-08-30 | 2016-11-23 | 南丹县南方有色金属有限责任公司 | The process that indium reclaims is improved further during a kind of electrolytic zinc |
| CN111330900A (en) * | 2020-04-08 | 2020-06-26 | 恩施市致纯电子材料有限公司 | Sponge indium washing and spin-drying equipment and using method thereof |
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| CN1487102A (en) * | 2003-07-30 | 2004-04-07 | 株洲冶炼集团有限责任公司 | Method of recovering In from waste In-Sn oxide target |
| CN101289712B (en) * | 2008-05-27 | 2010-08-11 | 株洲冶炼集团股份有限公司 | Process for recovering indium from indium-containing material |
| CN101831550B (en) * | 2010-05-21 | 2012-07-04 | 葫芦岛锌业股份有限公司 | Method for extracting indium from alkali oxidation scum rich in indium |
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