CN101812603A - Method for improving indium grade of enriched indium slag - Google Patents
Method for improving indium grade of enriched indium slag Download PDFInfo
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- CN101812603A CN101812603A CN200910265329A CN200910265329A CN101812603A CN 101812603 A CN101812603 A CN 101812603A CN 200910265329 A CN200910265329 A CN 200910265329A CN 200910265329 A CN200910265329 A CN 200910265329A CN 101812603 A CN101812603 A CN 101812603A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for the indium grade of an enriched indium slag in the process of lead and zinc smelting by-product zinc oxide. The method comprises the following steps: continuously adding acidic liquid into ore pulp after indium-containing acidic solution is replaced by zinc powder and stirring; stirring the ore pulp to perform a reaction for a certain time to form the mixed ore pulp; transporting the mixed ore pulp to a solid-liquid separator to perform solid-liquid separation; and conveying the separated filter residue to a rare indium system for processing, and then recycling the indium and zinc of the separated filter liquid. The main metal such as zinc and the like is reduced and recycled through a new process of increasing and reducing the slag quantity of the enriched indium slag, so that the quantity of the enriched indium slag is reduced and the indium grade of the enriched indium slag is improved.
Description
Technical field
The present invention relates to the Metal smelting technical field, specifically, relate to a kind of method that enriched indium slag contains indium grade that in the operation of producing enriched indium slag, improves.
Background technology
Indium metal becomes one of most important propping material in the hyundai electronics industry owing to have very unique and good physics and chemical property.But it is as one of rare metal, does not find independent mineral deposit so far.90% indium reclaims from the lead-zinc smelting byproduct in the world at present.In zinc ore concentrate fluidized bed roasting process, indium 95% oxidized generation Indium sesquioxide in the zinc ore concentrate, enter in calcining and the flue dust, usually adopt three sections leaching (promptly neutrally leach, low acidleach goes out, peracid leaching) to add the indium in the zinc dust precipitation technology recovery zinc oxide, obtain enriched indium slag, as the main raw material of rare expensive smart indium production.After three sections leachings, zinc, cadmium enter solution in the zinc-oxide calcine more than 95%, the indium of 60%-70% is leached enters solution, some zinc and indium enter in the leached mud with plumbous and silver, the leached mud that produces is the zinc oxide lead skim, send into lead system, and the solution that is leached is low acid and contains solution of indium.Utilize zinc dust precipitation low acid to contain solution of indium, the ore pulp after reaction is finished is delivered directly to the liquid-solid separation equipment chamber-type press filter and carries out press filtration, has just obtained the enriched indium slag of water content 20-60%.Enriched indium slag contains zinc 20-40%, indium 0.1-1 0%, and it on average contains zinc 28%, contains indium about 2%.
The problem that prior art exists is, total amount and throughput that rare your recovery indium operation is handled enriched indium slag every day are limited, if handle the high enriched indium slags of other metal such as containing zinc in a large number again, then the production influence to rare your indium is bigger, can cause the extracted organic phase cycle short, the production cost height increases labour intensity, problems such as restriction throughput make the production technique of rare your indium can not bring into play higher production capacity.
On the one hand, increase year by year along with zinc oxide input amount and indium scheduled production, the enriched indium slag amount also increases a lot, but rare your indium system does not carry out bigger transformation in recent years, the enrichment quantity of slag that increases is difficult to handle, many can only storing up, this can turn round to business capital undoubtedly, profit causes detrimentally affect.
On the other hand, the technology that reduces the enriched indium slag quantity of slag is not set in traditional zinc oxide producing and manufacturing technique, therefore, there is not treated enriched indium slag can cause a large amount of metals such as zinc to be sent to rare your indium system with enriched indium slag, after in the flow process of indium system, handling, the extraction liquid that contains metals such as zinc, arsenic, antimony, germanium, iron is sent back to again enters Zn system, the recovery process and the cost of metals such as zinc had both been increased, increase the production cost and the labour intensity of zinc, indium operation again, reduce the rate of recovery.
In the existing producing and manufacturing technique, also not have to find to effectively reduce the technology of the enriched indium slag quantity of slag, and the processing method that reduces other slag quantity of slag generally all adopts and produces water and carry out methods such as washery slag and minimizing moisture content.As adopt this method to wash enriched indium slag, main drawback is to have enlarged system bulk, has increased system consumption and labour intensity, and the solvable composition in the enriched indium slag is few, it is too little to reduce quantity of slag ability, so can't effectively reach the effect that reduces the quantity of slag with producing the washing enriched indium slag.
In sum, how neither to influence Zn system metal input, reduce the enrichment quantity of slag again,, become the problem that this field presses for solution for the production of rare your recovery indium operation provides good condition.
Summary of the invention
In view of this, the invention provides a kind of method that enriched indium slag contains indium grade that improves, by in the process of preparation enriched indium slag, increasing the novel process process that a kind of acidic substance carry out stir process, improve the purpose that enriched indium slag contains indium grade, reduces the enriched indium slag quantity of slag to reach, and recovery other metals such as zinc wherein, reduce flow process.
The method that raising enriched indium slag provided by the invention contains indium grade comprises: in contain the ore pulp of indium acid solution step after finishing with zinc dust precipitation, continue to add acidic liquid material (being acid solution) and stir; Behind the stirring reaction certain hour, become mixed ore pulp; Carry this mixed ore pulp to carry out solid-liquid separation to solid-liquid separating equipment; Filter residue after separating is delivered to rare your indium system handles, and the filtrate after the separation moves towards constant, carries out the recovery of metals such as indium, zinc.
Preferably, described acid solution is a dilute sulphuric acid, and perhaps in the lead-zinc smelting production technique, described acid solution is the zinc electrolysis waste solution.More preferably, the concentration of dilute sulphuric acid can contain sour 140-220 grams per liter in the zinc electrolysis waste solution in the scope of 100-500g/L.
According to method provided by the present invention, the time that described ore pulp and acid solution are stirred is 10-120 minute.Preferably, the Best Times of stirring is 20-40 minute.
According to method provided by the present invention, preferably, after stirring, the endpoint pH of mixed ore pulp is 3.5-5.5.More preferably, the best endpoint pH of mixed ore pulp is 4.0-5.0.
From the lead-zinc smelting byproduct, reclaim in the enriched indium slag that obtains and contain zinc about 28% usually, according to technical scheme provided by the invention, after the gained enriched indium slag was stirred with acid solution, the zinc content in the enriched indium slag reduced, thereby reduced the quantity of slag, improved the grade of indium in the enriched indium slag.Utilize dilute sulphuric acid or zinc electrolysis waste solution to carry out pickling, just increased short stirring reaction process, do not increase other consumption, and reduced the production cost that next operation is handled enriched indium slag, the stable processing power that has improved enriched indium slag, in addition, do not increase the discharging of waste residue, waste gas, waste water, non-environmental-pollution, the material that is consumed is zinc electrolysis waste solution or the dilute sulphuric acid that produces in the wet type zinc metallurgy process, therefore, method provided by the invention has the economic benefit of highly significant.
Description of drawings
Constitute this specification sheets a part, be used for further understanding accompanying drawing of the present invention and show the preferred embodiments of the present invention, and be used for illustrating principle of the present invention with specification sheets.Fig. 1 a kind ofly improves the schema that enriched indium slag contains the method for indium grade for what the embodiment of the invention provided.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that is obtained under the creative work prerequisite.
The invention provides a kind of method that enriched indium slag contains indium grade that improves, its flow process may further comprise the steps as described in the accompanying drawing 1:
＜100〉in pulp is irritated, contain the indium acid solution, stir with zinc dust precipitation;
＜101〉in step＜100〉in the ore pulp that forms after finishing, continue to add acid solution and stirs, this acid solution can be the zinc electrolysis waste solution that produces in the zinc hydrometallurgy process, also can utilize dilute sulphuric acid to replace the above-mentioned ore pulp of the direct pickling of zinc electrolysis waste solution.In technical scheme provided by the invention; the pH value of used dilute sulphuric acid or zinc electrolysis waste solution is not subjected to certain restriction; so long as according to principle of the present invention, can realize that the present invention improves all dilute sulphuric acids of indium content purpose in the enriched indium slag or zinc electrolysis waste solution in the scope of protection of the invention.In production practice, preferably, the concentration of used dilute sulphuric acid can contain sour 140-220 grams per liter in the used zinc electrolysis waste solution in the scope of 100-500g/L.Utilizing the zinc electrolysis waste solution in the lead-zinc smelting production technique, not only saved the further handling problem of waste liquid, but also realized that the present invention reduces the purpose that contains the indium slag quantity of slag, is a kind of very economical, convenient, effective means;
＜102〉above-mentioned ore pulp and acid solution are stirred, obtain mixed serum.The time of stirring reaction can be at 10-120 minute, and churning time is too short, and then reaction is abundant inadequately; Overlong time is then owing to working continuously in the production process, and retort needs turnover, so be not allowed to; In addition, overlong time can produce hydrolyzate, subsalt.Preferably, the Best Times of stirring is 20-40 minute;
＜103〉be transported to solid-liquid separating equipment with the pump delivery mixed serum and carry out filtering separation;
＜104〉filtrate filtered is recovered to zinc and smelts production leaching operation;
＜105〉filter residue after will filtering is sent to rare your indium system.
The physical and chemical principle of enriched indium slag pickling is as follows:
The enriched indium slag that the zinc oxide production system is produced, wherein solution content is 20-60%, and enriched indium slag contains zinc 20-40%, contains indium 0.1-10%, and it on average contains zinc 28%, contains indium 2%, contains solution amount is about 50%.The present invention considers the technology that reduces the enriched indium slag quantity of slag is set, and purpose just is to search out a kind of effective lotion that can mainly reduce the zinc that content is the highest in the indium slag.The mode of general washery slag process using water slurryization or washing here can not be used, the one, produce volume and do not allow, and employing method for washing, the content of moisture content is little before and after the slag, and washing slag method has only physical change not have chemical transformation, be water not can with enriched indium slag wherein zinc-containing substance react, thereby can not significantly reduce the quantity of slag, neither calculate the purpose can't reach washing again.And the inventor is constantly finding in the production practice, acid solutions such as zinc electrolysis waste solution and dilute sulphuric acid, can with enriched indium slag wherein zinc-containing substance and other hydrolyzates, subsalt reacts, thereby significantly reduce the quantity of slag, therefore adopt acid solution pulp washery slags such as zinc electrolysis waste solution or dilute sulphuric acid, weight metal such as zinc is reduced, in fact the process that is equivalent to " concentrating ", and then improved the grade of indium in the enriched indium slag, can solve the problem that prior art adopts the washing slag to exist, for the production cost of indium operation with reduce labour intensity and create good conditions.In view of the above; according to the physical and chemical principle of the pickling that is provided as can be known; acid solution provided by the present invention can not only be confined to dilute sulphuric acid or zinc electrolysis waste solution; so long as defer to principle of the present invention, can realize that the present invention improves the acidic substance of indium grade all should be in the scope of protection of the invention.
According to method provided by the present invention, preferably, after stirring, the endpoint pH of mixed ore pulp is 3.5-5.5.PH is too high, and pickling effect is insufficient, and hydrolyzate, subsalt, sour molten zinc are residual many; Perhaps pH is low excessively, and acid adds excessive, has accidents such as fire-fighting, safety, environmental protection easily, and the possibility that can make the indium that has been displaced wash again simultaneously to get back in the solution increases, and is not that the present invention wants the result that obtains.More preferably, the described best endpoint pH that mixed ore pulp is stirred is 4.0-5.0.
Embodiment 1:
In pulp is irritated, contain the indium acid solution with zinc dust precipitation, after stirring, its dry weight is 1t, to wherein adding the zinc electrolysis waste solution, the acid content of this electrolytic solution is for containing sour 140 grams per liters, stirring and pickling 10 minutes, and the pH value is 4.5 when adopting pH tester or pH test paper to measure the pickling terminal point, send pressure filter to carry out liquid-solid separation at last, filtrate filtered is recovered to zinc smelts production leaching operation, the filter residue after the filtration is sent to rare your indium system, and finally obtaining the quantity of slag is 0.914t.Adopt atomic absorption instrument analytical method that the indium in the enriched indium slag is analyzed, adopt chemical analysis that the content of zinc is analyzed, pickling the results are shown in Table 1.
Table 1
Annotate: before rate of increase=(after the pickling-pickling before)/pickling
Minimizing quantity of slag %=(the initial quantity of slag-final the quantity of slag)/initial quantity of slag=(1.0-0.914)/1=8.6%
Embodiment 2:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is the zinc electrolysis waste solution, and concentration is 160 grams per liters, and the stirring and pickling time is 20 minutes, and the pickling endpoint pH is 4.5, and pickling the results are shown in Table 2.
Table 2
Embodiment 3:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is the zinc electrolysis waste solution, and concentration is 175 grams per liters, and the stirring and pickling time is 40 minutes, and the pickling endpoint pH is 4.5, and pickling the results are shown in Table 3.
Table 3
Embodiment 4:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is the zinc electrolysis waste solution, and concentration is 200 grams per liters, and the stirring and pickling time is 120 minutes, and the pickling endpoint pH is 4.5, and pickling the results are shown in Table 4.
Table 4
Embodiment 5:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is the zinc electrolysis waste solution, and concentration is 220 grams per liters, and the stirring and pickling time is 30 minutes, and the pickling endpoint pH is 3.5, and pickling the results are shown in Table 5.
Table 5
Embodiment 6:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is the zinc electrolysis waste solution, but the stirring and pickling time be 30 minutes, the pickling endpoint pH is 4.5, pickling the results are shown in Table 6.
Table 6
Embodiment 7:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is the zinc electrolysis waste solution, and concentration is 150 grams per liters, but the stirring and pickling time be 30 minutes, the pickling endpoint pH is 5.5, pickling the results are shown in Table 7.
Table 7
Embodiment 8:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is dilute sulfuric acid solution 200g/L, and the stirring and pickling time is 30 minutes, and the pickling endpoint pH is 4.5, and pickling the results are shown in Table 8.
Table 8
Embodiment 9:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is dilute sulfuric acid solution 100g/L, but the stirring and pickling time be 60 minutes, the pickling endpoint pH is 5.0, pickling the results are shown in Table 9.
Table 9
Embodiment 10:
The experimental implementation process is identical with embodiment 1, and the acid solution of employing is dilute sulfuric acid solution 500g/L, but the stirring and pickling time be 30 minutes, the pickling endpoint pH is 3.5, pickling the results are shown in Table 10.
Table 10
Among the embodiment 1-10 in the rich indium residue content rate of descent of zinc be 11.0%-28.5%, and the content rate of increase of indium is 2.5%-97.1%, the quantity of slag decrement of indium slag is 6%-19.2%.As seen, the acid cleaning process that the present invention increases in the indium slag processing treatment can reduce the quantity of slag, improves the grade of indium in the enriched indium slag, and then has stablized rare your indium production capacity and improved the rate of recovery of indium.And the present invention utilizes the zinc electrolysis waste solution or the dilute sulphuric acid that produce in the zinc hydrometallurgy process directly to carry out pulp and pickling enriched indium slag, significantly reduces the enriched indium slag amount and wherein content, this rate of recovery rare your production capacity is stabilized and increased indium of zinc is greatly favourable.In the operation of this pickling, do not increase the discharging of waste residue, waste gas, waste water, non-environmental-pollution, the acid solution that is consumed also is the raw material of industrial easy acquisition, does not increase other consumption.This method has not only reduced the production cost that next operation is handled enriched indium slag, has also improved the processing power of indium.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined herein General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (9)
1. one kind is improved the method that contains indium grade in the enriched indium slag, it is characterized in that, comprising:
Contain the indium acid solution with zinc dust precipitation, obtain ore pulp after evenly stirring;
In described ore pulp, add acid solution and stir, obtain mixed ore pulp after fully stirring;
Carry described mixed ore pulp to carry out solid-liquid separation to solid-liquid separating equipment;
Filter residue after separating is delivered to rare your indium system handle, reclaim the metal in the filtrate after separating.
2. method according to claim 1 is characterized in that, described acid solution is the zinc electrolysis waste solution.
3. method according to claim 2 is characterized in that, contains sour 140-220 grams per liter in the described zinc electrolysis waste solution.
4. method according to claim 1 is characterized in that described acid solution is a dilute sulphuric acid.
5. method according to claim 4 is characterized in that, the concentration of described dilute sulphuric acid is 100-500g/L.
6. according to each described method among the claim 1-5, it is characterized in that the reaction times that described ore pulp and acid solution are stirred is 10-120 minute.
7. according to the described method of claim 6, it is characterized in that the described stirring reaction time is 20-40 minute.
8. according to each described method among the claim 1-5, it is characterized in that the endpoint pH of described mixed ore pulp is in the scope of 3.5-5.5.
9. described according to Claim 8 method is characterized in that described endpoint pH is in the scope of 4.0-5.0.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699693A (en) * | 2017-09-29 | 2018-02-16 | 南丹县南方有色金属有限责任公司 | A kind of improved method of secondary cobalt nickel treatment technology of leached residue |
| CN108893608A (en) * | 2018-05-30 | 2018-11-27 | 苏州精美科光电材料有限公司 | A kind of refinement method improving indium recovery |
| CN114703368A (en) * | 2022-02-21 | 2022-07-05 | 云锡文山锌铟冶炼有限公司 | Method for treating zinc-indium-containing gypsum slag |
-
2009
- 2009-12-29 CN CN200910265329A patent/CN101812603A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699693A (en) * | 2017-09-29 | 2018-02-16 | 南丹县南方有色金属有限责任公司 | A kind of improved method of secondary cobalt nickel treatment technology of leached residue |
| CN108893608A (en) * | 2018-05-30 | 2018-11-27 | 苏州精美科光电材料有限公司 | A kind of refinement method improving indium recovery |
| CN114703368A (en) * | 2022-02-21 | 2022-07-05 | 云锡文山锌铟冶炼有限公司 | Method for treating zinc-indium-containing gypsum slag |
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Application publication date: 20100825 |