CN108823435A - A kind of two step circulating leaching methods of wet process refining indium - Google Patents
A kind of two step circulating leaching methods of wet process refining indium Download PDFInfo
- Publication number
- CN108823435A CN108823435A CN201810745516.7A CN201810745516A CN108823435A CN 108823435 A CN108823435 A CN 108823435A CN 201810745516 A CN201810745516 A CN 201810745516A CN 108823435 A CN108823435 A CN 108823435A
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- CN
- China
- Prior art keywords
- sulfuric acid
- leaching
- indium
- concentrated sulfuric
- wet process
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Classifications
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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
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of two step circulating leaching methods of wet process refining indium, high acidic oils first are carried out to secondary raw materials with 98% concentrated sulfuric acid, solid-liquor separation is carried out using frame filter press after reaction, solution (referred to as high immersion liquid) is used to dilute leaching, solid slag (for sulfate) becomes available sulfate after being rinsed with extract liquor, generally lead sulfate gives lead bullion factory as the raw material of refining lead bullion.High immersion liquid, which is transported to dilute leaching reaction kettle and raw material, to be done dilute leaching and react, consumes sulfuric acid as far as possible, after solution passes through solid-liquor separation, solid becomes secondary raw materials, and into concentrated sulfuric acid height leaching reaction kettle, liquid enters purification process, such circulate operation.The present invention is by carrying out dilute sulfuric acid and the leaching of two step of the concentrated sulfuric acid to mineral containing indium, not only increase the leaching efficiency of the mineral containing indium, and slag and two step diluting concentrated sulfuric acid of heavy indium waste water are leached by being separately added into, the service efficiency of sulfuric acid is not only increased, risk when diluting concentrated sulfuric acid is also reduced.
Description
Technical field
The invention belongs to metal smelt field more particularly to a kind of two step circulating leaching methods of wet process refining indium.
Background technique
Indium metal is a kind of rare metal, is widely used in aerospace, radio and electronics industry, medical treatment, national defence, high-new
The fields such as technology, the energy.Abundance of the indium in the earth's crust is smaller, and disperses very much.Its rich ore had not found, and only existed
Exist in zinc and some other metallic ore as impurity, therefore it is put into rare metal, the content of indium is in mineral
Between 0.0001%~0.1%, the whole world estimates only 50,000 tons of indium reserves.Indium generallys use wet process refining indium at present, that is, passes through dilute sulphur
Acid leaches indium, and then plus water increases pH to 1 or so, so that the precipitated metals such as tin therein, bismuth, antimony get off, then solution is passed through
It crosses extraction and subsequent heavy indium and obtains indium metal.But such method, it is required to be diluted with water when leaching indium every time
The concentrated sulfuric acid, it is not only big with acid amount, and indium is difficult to leach completely, and finally the waste water after heavy indium the more can accumulate the more more, and waste water
Discharge pollutes the environment, and China forbids waste discharge at present.
Summary of the invention
To solve the above problems, the present invention provides a kind of two step circulating leaching methods of wet process refining indium, the present invention passes through
Dilute sulfuric acid is carried out to mineral containing indium and two step of the concentrated sulfuric acid leaches, not only increases the leaching efficiency of the mineral containing indium, and by dividing
Two step diluting concentrated sulfuric acid of slag and heavy indium waste water Jia Ru not be leached, the service efficiency of sulfuric acid is not only increased, also reduces dilution
The risk when concentrated sulfuric acid.
To reach above-mentioned technical effect, the technical scheme is that：
A kind of two step circulating leaching methods of wet process refining indium, include the following steps：
Step 1: mineral containing indium are immersed in the dilution heat of sulfuric acid of setting concentration leached to obtain dilute sulfuric acid leachate and
Slag is leached, dilute sulfuric acid leachate is for the subsequent process for refining indium；
Step 2: filters pressing is by dilute sulfuric acid leachate and leaches slag separation, it will leach in the slag addition concentrated sulfuric acid and leach indium
It obtains concentrated sulfuric acid leachate and leaches waste residue, filters pressing separates concentrated sulfuric acid leachate with waste residue is leached, and then leaches in the concentrated sulfuric acid
Waste water after heavy indium is added in liquid adjusts sulfuric acid concentration in concentrated sulfuric acid leachate to the dilution heat of sulfuric acid of the setting concentration
Concentration obtains pre- leaching dilution heat of sulfuric acid；
It is leached Step 3: indium mineral will be contained and immerse the resulting pre- leaching dilution heat of sulfuric acid of step 2, obtains dilute sulfuric acid
Leachate and leaching slag；
Step 4: circulation carries out step 2 and step 3.
Further to improve, the sulfuric acid concentration of the dilution heat of sulfuric acid for setting concentration is 10%-49%.
Further to improve, the concentration of the concentrated sulfuric acid is 98%.
Further to improve, mineral containing indium, which immerse, set extraction time in the dilution heat of sulfuric acid of concentration as 1-3 hours,
The pre- extraction time leached in dilution heat of sulfuric acid is 1-3 hours；The time for leaching leaching indium in the slag addition concentrated sulfuric acid is that 3-5 is small
When.
Further to improve, when leaching indium obtains concentrated sulfuric acid leachate in the leaching slag addition concentrated sulfuric acid, the concentrated sulfuric acid is leached
The temperature of liquid is 200-300 DEG C.
It is further to improve, in the step 2, obtained after leaching waste water rinsing of the waste residue after raffinate or heavy indium
Sulfate.
Further to improve, the sulfate is lead sulfate.
Further to improve, the dilute sulfuric acid leachate is raffinate through extract liquor waste liquid extracted；Extract liquor packet
Include P2O4And aviation kerosine；P2O4Mass ratio with aviation kerosine is 1:3.
Specific embodiment
Technical solution of the present invention is illustrated below by way of specific embodiment.
Embodiment 1
The present invention is as follows for the improved procedure of wet process refining indium：
One, two circulating leachings：
High acidic oils first are carried out to secondary raw materials (slag charge that this raw material is filters pressing after diluted acid leaching) with 98% concentrated sulfuric acid,
General measured with acid is 200~300 kilograms of siccative per ton, and the reaction time is or so 4 hours, and frame filter press is utilized after reaction
Solid-liquor separation is carried out, solution (referred to as high immersion liquid) is used to dilute leaching, and solid slag (for sulfate) becomes after being rinsed with raffinate can
The sulfate utilized, generally lead sulfate give lead bullion factory as the raw material of refining lead bullion.High immersion liquid be transported to dilute leaching reaction kettle with
Raw material does dilute leaching reaction, using reacting for raw material and sulfuric acid, consumes sulfuric acid as far as possible, and realize the object for being soluble in sulfuric acid and water
Matter enters solution, the solution pass through solid-liquor separation after, solid become secondary raw materials, into concentrated sulfuric acid height soak reaction kettle, liquid into
Enter purification process, such circulate operation.
Two, application of the magnesia in wet process refining indium cleansing phase：
Dilute immersion liquid enters purification section, and general technique is by being diluted with water acidity, when PH reaches 1 or so, in solution
Impurity component (including：Tin, bismuth, antimony) tin can precipitate (referred to as hydrolysis in industry), then scruff is separated by filters pressing
Out, but once adding water to increase the volume in system, so that last water must outlet.Our technique and national environmental protection
It is required that being that water is unable to outlet.Main function using magnesia is neutralizing acid, turns down the pH value of solution to 1, tin is same
It can precipitate, it is same that solid-liquor separation is carried out by filter press, purify impurity.In fact can also be with using the alkaline matters such as piece alkali, but
Using the bad filters pressing of piece alkali, of the invention one above are only at book also high (one 5000 yuan of piece alkali, magnesia one times 600 yuan)
A specific guiding embodiment, but the design concept of the present invention is not limited to this, it is all non-to present invention progress using this design
Substantive change should belong to the behavior for invading protection scope of the present invention.
Claims (8)
1. a kind of two step circulating leaching methods of wet process refining indium, which is characterized in that include the following steps：
It is leached to obtain dilute sulfuric acid leachate and leaching Step 1: mineral containing indium are immersed in the dilution heat of sulfuric acid for setting concentration
Slag, dilute sulfuric acid leachate is for the subsequent process for refining indium；
Step 2: filters pressing is by dilute sulfuric acid leachate and leaches slag separation, leaching indium in the slag addition concentrated sulfuric acid will be leached and obtained
Concentrated sulfuric acid leachate and leaching waste residue, filters pressing separates concentrated sulfuric acid leachate with waste residue is leached, then in concentrated sulfuric acid leachate
Sulfuric acid concentration in concentrated sulfuric acid leachate is adjusted the concentration of the dilution heat of sulfuric acid to the setting concentration by the waste water after heavy indium is added
Obtain pre- leaching dilution heat of sulfuric acid；
It is leached Step 3: indium mineral will be contained and immerse the resulting pre- leaching dilution heat of sulfuric acid of step 2, obtains dilute sulfuric acid leaching
Liquid and leaching slag；
Step 4: circulation carries out step 2 and step 3.
2. two step circulating leaching methods of wet process refining indium as described in claim 1, which is characterized in that described to set the dilute of concentration
The sulfuric acid concentration of sulfuric acid solution is 10%-49%.
3. two step circulating leaching methods of wet process refining indium as described in claim 1, which is characterized in that the concentration of the concentrated sulfuric acid
It is 98%.
4. two step circulating leaching methods of wet process refining indium as described in claim 1, which is characterized in that mineral containing indium immerse setting
Extraction time in the dilution heat of sulfuric acid of concentration is 1-3 hours, is that 1-3 is small leaching the extraction time in dilution heat of sulfuric acid in advance
When；The time for leaching leaching indium in the slag addition concentrated sulfuric acid is 3-5 hours.
5. two step circulating leaching methods of wet process refining indium as described in claim 1, which is characterized in that leach slag and dense sulphur is added
When leaching indium obtains concentrated sulfuric acid leachate in acid, the temperature of concentrated sulfuric acid leachate is 200-300 DEG C.
6. two step circulating leaching methods of wet process refining indium as described in claim 1, which is characterized in that in the step 2, leaching
Sulfate is obtained after waste water rinsing of the waste residue after raffinate or heavy indium out.
7. two step circulating leaching methods of wet process refining indium as claimed in claim 6, which is characterized in that the sulfate is sulfuric acid
Lead.
8. two step circulating leaching methods of wet process refining indium as described in claim 1, which is characterized in that the dilute sulfuric acid leachate
It is raffinate through extract liquor waste liquid extracted；Extract liquor includes P2O4And aviation kerosine；P2O4With the mass ratio of aviation kerosine
It is 1:3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410578A (en) * | 2020-10-23 | 2021-02-26 | 刘罗平 | Comprehensive recovery method for tin precipitation of tin-containing material by oxygen pressure alkaline leaching of calcium salt |
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| CN101525696A (en) * | 2009-04-21 | 2009-09-09 | 中南大学 | Method for leaching indium from leaching residue containing indium |
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2018
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| CN104379778A (en) * | 2011-05-02 | 2015-02-25 | 三金属矿业有限公司 | A method for recovering indium, silver, gold and other rare, precious and base metals from complex oxide and sulfide ores |
| CN103173625A (en) * | 2013-04-19 | 2013-06-26 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410578A (en) * | 2020-10-23 | 2021-02-26 | 刘罗平 | Comprehensive recovery method for tin precipitation of tin-containing material by oxygen pressure alkaline leaching of calcium salt |
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Application publication date: 20181116 |