CN108411128B - Method for efficiently enriching indium from low-grade indium-containing smelting slag - Google Patents
Method for efficiently enriching indium from low-grade indium-containing smelting slag Download PDFInfo
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- CN108411128B CN108411128B CN201810309267.7A CN201810309267A CN108411128B CN 108411128 B CN108411128 B CN 108411128B CN 201810309267 A CN201810309267 A CN 201810309267A CN 108411128 B CN108411128 B CN 108411128B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C22B7/007—Wet processes by acid leaching
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Abstract
The invention discloses a method for efficiently enriching indium from low-grade indium-containing smelting slag, which comprises the following steps of 1) carrying out concentrated leaching on underflow slag by adopting high-temperature high-acid to dissolve indium ions into a solution, and enriching lead into the concentrated leaching slag; 2) adding iron powder into the supernatant obtained by the concentrated leaching to reduce ferric iron; 3) adding alkali liquor for neutralizing and precipitating indium, and simultaneously adding neutralizing agent high-purity zinc oxide; 4) and (5) filtering. According to the invention, the reducing agent zinc powder adopted by reducing ferric iron from the leachate is improved into iron powder, so that the comprehensive recycling cost is greatly reduced, the neutralizing agent zinc calcine adopted in the indium neutralizing and precipitating process is improved into high-purity zinc oxide, the consumption of the neutralizing agent is greatly reduced due to the improvement of the leaching rate of the neutralizing agent after the improvement, and the slag amount is reduced, so that the purpose of improving the indium quality is achieved, the grade of the original indium slag is improved to more than 10 kg/ton indium slag from 2 kg/ton indium slag, and the quality leap is realized.
Description
Technical Field
The invention relates to the technical field of chemical smelting, in particular to a method for enriching indium from low-grade indium-containing smelting slag.
Background
Many zinc smelting enterprises do not comprehensively utilize and recycle indium after being put into operation, but sell the zinc-containing material slag in a mode of pricing zinc and non-pricing indium to other enterprises, so that valuable metals and value are lost, and meanwhile, hazardous waste residues can cause adverse effects on the environment in the transferring and transporting processes, so that the zinc smelting enterprises are not in accordance with the requirements of environment-friendly and economical green enterprises advocated in the state at present. For example, in a certain western mining plant, 40000t/a zinc oxide is treated to produce 12000 t/a of zinc oxide bottom leaching slag (the indium content is between 0.070 and 0.85 percent). During a small-scale test process of valuable metal wet separation according to the conventional process of indium recovery in the industry, the grade of indium can not meet the requirement of expecting 6 kilograms per ton indium slag all the time, the grade of indium is below 2 kilograms per ton indium slag, the indium enrichment effect is poor, the selling price is low, the value of indium cannot be reflected, the raw material consumption is high, the comprehensive recycling cost is high, and a company can not make a powerful decision on indium recovery.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for efficiently enriching indium from low-grade indium-containing smelting slag, which is simple in process operation, lower in cost and higher in grade of obtained indium slag.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for efficiently enriching indium from low-grade indium-containing smelting slag, which is underflow slag generated by neutral leaching of secondary zinc oxide in a conventional zinc smelting process through a section of low acid, is characterized by comprising the following steps of: the method comprises the following steps of (1),
1) the underflow slag is subjected to concentrated leaching by adopting high-temperature high acid, so that indium ions are dissolved into the solution, and lead is enriched into the concentrated leaching slag; the concentrated leaching operation conditions are as follows: the temperature is 90-100 ℃, the acid addition multiple is 0.5-0.6, the reaction time is 240min, and the liquid-solid ratio is 3: 1;
2) adding iron powder into the supernatant obtained by the concentrated leaching to reduce ferric iron;
3) adding alkali liquor for neutralizing and precipitating indium, and simultaneously adding neutralizing agent high-purity zinc oxide;
4) and (3) filtering, repeatedly washing the indium slag after liquid-solid separation, and then performing filter pressing to obtain the indium-rich slag with the quality of more than 10 kilograms per ton of indium slag.
Further, in step 2), during the operation of reducing the ferric iron, the iron powder is slowly added, the pH value is controlled to ensure that the ferric iron can be reduced to be below 0.5g/l under 2.0, and the pH value of the hydrolysis precipitation is not higher than 4.5.
Further, in the step 3), adjusting acidity by alkali liquor, adjusting pH value by high-purity zinc oxide to neutralize and precipitate indium, controlling the acidity to be reduced to 40g/L, reducing iron powder to control the pH value to be 1.5, and respectively controlling the pH values to be more than 4.0 by adding alkali liquor and high-purity zinc oxide to carry out hydrolysis precipitation.
Preferably, the supernatant after indium precipitation is added with hydrogen peroxide after the acidity is adjusted, and ferrous iron is oxidized into ferric iron and then returned to the leaching process.
Or the supernatant after indium precipitation is returned to the main system after iron precipitation by an jarosite method.
Preferably, the high-purity zinc oxide contains 70-80% of zinc and has the granularity of more than or equal to 120 meshes.
Further, the leaching process of the underflow slag comprises the steps of firstly adding 1240mL of water into a 2L beaker, then adding 142mL of calculated concentrated sulfuric acid, starting stirring and heating, simultaneously sampling and analyzing the initial acid content, and adding 500g of the underflow slag into the zinc hypoxide when the temperature is raised to be higher than 80 ℃; then stirring for 240min, starting suction filtration, keeping the temperature above 90 ℃ in the reaction process, and analyzing the liquid subjected to suction filtration for Zn and FeAll-purpose、Fe2+、In、H+The contents, the filter residue are weighed and analyzed for Zn, Pb, Fe, In and H2And (4) the content of O.
Further, the specific process of reduction neutralization is that 1000mL of leachate is measured and added into a 2L beaker, stirring and heating are started, the temperature is kept to 60 ℃, and meanwhile, sampling is carried out for H analysis+、FeAll-purpose、Fe2+In content according to H+Adding 120mL of 100-one alkali liquor to adjust the acidity to 40-50g/L, and then adjusting the acidity to Fe according to the content of Fe3+Slowly adding 10-18g of iron powder to make Fe3+Reducing to below 1g/L, adding 20mL of alkali liquor and 10-18g of high-purity zinc oxide to control the acidity to be PH 4.5; stopping the reaction, carrying out suction filtration, analyzing the Zn, Fe and In content of the liquid, weighing the filter residue and analyzing the Zn, Fe, In and H2And (4) the content of O.
According to the invention, the reducing agent zinc powder adopted by reducing ferric iron from the leachate is improved into iron powder, so that the comprehensive recycling cost is greatly reduced, the neutralizing agent zinc calcine adopted in the indium neutralizing and precipitating process is improved into high-purity zinc oxide, the consumption of the neutralizing agent is greatly reduced due to the improvement of the leaching rate of the neutralizing agent after the improvement, and the slag amount is reduced, so that the purpose of improving the indium quality is achieved, the grade of the original indium slag is improved to more than 10 kg/ton indium slag from 2 kg/ton indium slag, and the quality leap is realized.
Drawings
FIG. 1 is a flow chart of the indium enrichment process using a non-deferrization method according to the present invention;
FIG. 2 is a flow chart of the indium enrichment process using the iron removal method of the present invention.
Detailed Description
The invention will be further illustrated with reference to specific embodiments:
1. leaching test
1.1.1 Leaching test procedure
(1) The test conditions are as follows:
the temperature is 90-100 ℃, the initial acidity is 180g/L, the time is 240min, and the liquid-solid ratio is 3:1
(2) The method comprises the following operation steps:
1240mL of water is added into a 2L beaker, then 142mL of calculated concentrated sulfuric acid is added, stirring and temperature rising are started, sampling is carried out at the same time, the initial acid content is analyzed, and 500g of bottom flow slag is added into the zinc hypoxide when the temperature rises to be higher than 80 ℃. Stirring for 240min, suction filtering (maintaining the temperature above 90 deg.C during reaction), and analyzing Zn and Fe in the liquidAll-purpose、Fe2+、In、H+The contents, the filter residue are weighed and analyzed for Zn, Pb, Fe, In and H2And (4) the content of O.
1.1.2 Leaching test results
(1) Leach filtrate volume (mL): 1150 to 1240.
(2) Solution analysis result (g/L):
Zn 105～144、Feall-purpose11～44、In 0.22～0.34、H+32.7～103.2。
(2) Amount of leached slag (g): 239 to 304 (dry basis).
(4) Leaching residue analysis result (%):
Zn 6.27～9.39、Pb 24.7～28.7、H2O 30～36、In 0.023～0.039。
(5) slag rate: 47.78-60.79%
(6) Leaching rate: 80.88% by weight of slag phase and 93.41% by weight of liquid phase
2 reduction neutralization test
2.1 reduction neutralization test procedure
(1) The test conditions are as follows:
the temperature is 60 ℃, the time is 180min, and the end point pH value is 4.5
(2) The method comprises the following operation steps:
weighing 1000mL of leachate, adding the leachate into a 2L beaker, stirring, heating and keeping the temperature to 60 ℃, and simultaneously sampling and analyzing H+、FeAll-purpose、Fe2+In content according to H+Adding 100-120mL of alkali liquor to adjust the acidity to 40-50g/L, and then adjusting the acidity to Fe3 +Slowly adding 10-18g of iron powder to ensure that Fe3+Reducing to below 1g/L (qualitative by potassium thiocyanate), adding about 20mL of alkali liquor and 10-18g of high-purity zinc oxide, controlling the acidity to be 4.5, stopping reaction, carrying out suction filtration, analyzing the contents of Zn, Fe and In the liquid, weighing filter residues, and analyzing the contents of Zn, Fe, In and H2And (4) the content of O.
2.2 reduction neutralization test results
(1) Filtrate volume (mL): 820-940, etc.
(2) Solution analysis result (g/L): zn 120-160, FeAll-purpose16～43、Fe2+16～42、In0.0073～0.062。
(3) Amount of indium-rich slag (g): and 6 groups of data (dry basis) such as 16.8 to 62.50.
(4) Indium-rich slag analysis results (%): zn 16.93-23.87, Fe 6.07-8.13, In 0.30-1.62.
(5) Precipitation rate: 72-98%.
3 metal equilibrium analysis
3.1 Table 1-Leaching test Metal balance sheet
Description of the analysis:
1) the test had three batches, 1#、2#Is a batch, 3#、4#、5#In one batch, 6#Is a batch.
2) The leaching solution yield is basically almost the same, the high phase and the low phase are different by 90mL, and the rest is close.
3) From the comparison of the leaching quality components, the leaching amount and the underflow slag content basically accord with each other, namely the slag content is high, and vice versa; but 6#The samples were low In Fe and In leaching out, and there was a possibility that the analysis of the raw materials was deviated.
4) From the comparison of the amount and the rate of the leached slag, the output is related to the quality components of the underflow slag, namely, the amount and the rate of the leached slag are high and high when the Fe and Pb contents in the middle leached underflow slag are high.
5) From the comparison of the leaching rates, the In leaching rate was 93.41% on average In the liquid phase and 80.88% on average In the slag phase, and 1 In the liquid phase was analyzed#、2#The leaching rate of the samples is higher than 100%, the average value of the two samples after being removed is 82.41% and is basically close to the slag phase, which indicates that the leaching rate is equivalent.
6) In view of the above, the leaching rates of Zn and In from such low-grade indium-containing smelting slag at normal temperature and normal pressure are also preferable.
3.2 Table 2-balance of metals for reduction and neutralization tests
Description of the analysis:
1) the test had three batches, 1#、2#Is a batch, 3#、4#In one batch, 5#、6#Is a batch.
2) From the liquid phase comparison, after the reduction, neutralization and indium precipitation, the highest content of In is 0.062g/L, and the average content of In the liquid phase is 0.014g/L, which is not ideal; the amount of the removed 2# distortion data is 0.0074g/L, and the indium deposition effect is ideal.
3) From the comparison of slag phases, the In content of the liquid phase after reduction and neutralization is 0.77 percent on average (7.7 kilograms per ton of indium slag), the minimum content is 0.30 percent, and the maximum content is 1.62 percent; low indium grade 4#In the data, the fact that the zinc and iron are relatively high is obviously seen, which indicates that the iron powder reduction reaction is not thorough, the ferric iron enters a slag phase, and the high-purity zinc oxide has an excessive medicament in the neutralization process, so that the operation is enhanced.
4) The average indium precipitation rate is 87 percent, the lowest 72 percent and the highest 98 percent in comparison of the indium precipitation rate; therein 6#The experimental precipitation rate is over hundred, the average indium precipitation rate after 6# value removal is 80.7%, and the overall effect is good.
4. TABLE 3 comparison of the indium dross compositions from conventional indium enrichment
| Name (R) | Zinc (%) | Iron (%) | Indium (kilogram/ton. indium slag) | Remarks for note |
| Indium slag produced by conventional process | 32 | 12 | 2.1 | Get the report data of industrial production |
| Indium slag produced by new process | 16.93 | 6.77 | 16.2 | Taking data of small test representatives |
As can be seen from Table 3, the grade of the indium slag produced by the new process is obviously higher than that of the indium slag produced by the conventional process, and the key for effectively improving the quality of the indium slag is to control the impurity elements to be separated from the indium slag as far as possible by analysis.
Therefore, the process for enriching indium by adopting concentrated acid leaching, ferric iron reduction by iron powder, alkali liquor and high-purity zinc oxide neutralization precipitation is feasible, and has the advantages of short process flow, simple operation and better technical and economic indexes.
The present invention has been described in detail, and it should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Claims (8)
1. A method for efficiently enriching indium from low-grade indium-containing smelting slag, which is underflow slag generated by neutral leaching of secondary zinc oxide in a conventional zinc smelting process through a section of low acid, is characterized by comprising the following steps of: the method comprises the following steps of (1),
1) the underflow slag is subjected to concentrated leaching by adopting high-temperature high acid, so that indium ions are dissolved into the solution, and lead is enriched into the concentrated leaching slag; the concentrated leaching operation conditions are as follows: the temperature is 90-100 ℃, the acid addition multiple is 0.5-0.6, the reaction time is 240min, and the liquid-solid ratio is 3: 1;
2) adding iron powder into the supernatant obtained by the concentrated leaching to reduce ferric iron;
3) adding alkali liquor for neutralizing and precipitating indium, and simultaneously adding neutralizing agent high-purity zinc oxide;
4) and (3) filtering, repeatedly washing the indium slag after liquid-solid separation, and then performing filter pressing to obtain the indium-rich slag with the quality of more than 10 kilograms per ton of indium slag.
2. The method for efficiently enriching indium in low-grade indium-containing smelting slag according to claim 1, characterized by comprising the following steps: in the step 2), during the operation of reducing the ferric iron, the iron powder is slowly added, the pH value is controlled to ensure that the ferric iron can be reduced to be below 0.5g/l under 2.0, and the pH value of the hydrolysis precipitation is not higher than 4.5.
3. The method for efficiently enriching indium in low-grade indium-containing smelting slag according to claim 1, characterized by comprising the following steps: in the step 3), adjusting the acidity by alkali liquor, adjusting the pH value by high-purity zinc oxide to neutralize and precipitate the enriched indium, controlling the acidity to be reduced to 40g/L, reducing iron powder to control the pH value to be 1.5, and then adding alkali liquor and high-purity zinc oxide to respectively control the pH value to be more than 4.0 for hydrolysis and precipitation.
4. The method for efficiently enriching indium in low-grade indium-containing smelting slag according to claim 1, characterized by comprising the following steps: and adjusting the acidity of the supernatant after indium precipitation, adding hydrogen peroxide, oxidizing ferrous iron into ferric iron, and returning to the leaching process.
5. The method for efficiently enriching indium in low-grade indium-containing smelting slag according to claim 1, characterized by comprising the following steps: and precipitating iron in the supernatant after indium precipitation by adopting a jarosite method, and returning the supernatant to the main system.
6. The method for efficiently enriching indium in low-grade indium-containing smelting slag according to claim 1, characterized by comprising the following steps: the high-purity zinc oxide contains 70-80% of zinc and has the granularity larger than or equal to 120 meshes.
7. The method for efficiently enriching indium in low-grade indium-containing smelting slag according to claim 1, characterized by comprising the following steps: the leaching process of the underflow slag comprises the steps of firstly adding 1240mL of water into a 2L beaker, then adding 142mL of calculated concentrated sulfuric acid, starting stirring and heating, simultaneously sampling and analyzing the initial acid content, and adding 500g of underflow slag into the zinc hypoxide when the temperature is raised to be higher than 80 ℃; then stirring for 240min, starting suction filtration, and keeping the temperature at 90 ℃ in the reaction processThen the liquid after suction filtration is analyzed for Zn and FeAll-purpose、Fe2+、In、H+The contents, the filter residue are weighed and analyzed for Zn, Pb, Fe, In and H2And (4) the content of O.
8. The method for efficiently enriching indium in low-grade indium-containing smelting slag according to claim 1, characterized by comprising the following steps: the specific process of reduction and neutralization is that 1000mL of leaching solution is measured and added into a 2L beaker, stirring and heating are started, the temperature is kept to 60 ℃, and meanwhile, sampling is carried out to analyze H+、FeAll-purpose、Fe2+In content according to H+Adding 120mL of 100-one alkali liquor to adjust the acidity to 40-50g/L, and then adjusting the acidity to Fe according to the content of Fe3+Slowly adding 10-18g of iron powder to make Fe3+Reducing to below 1g/L, adding 20mL of alkali liquor and 10-18g of high-purity zinc oxide to control the acidity to be PH 4.5; stopping the reaction, carrying out suction filtration, analyzing the Zn, Fe and In content of the liquid, weighing the filter residue and analyzing the Zn, Fe, In and H2And (4) the content of O.
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| CN103667720B (en) * | 2013-12-26 | 2015-07-22 | 河南豫光锌业有限公司 | Method for recovering zinc, indium, iron, and lead from high-iron zinc oxide mixture smelted with zinc |
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