CN109852808A - A kind of technique for extracting tin from silver separating residues - Google Patents
A kind of technique for extracting tin from silver separating residues Download PDFInfo
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- CN109852808A CN109852808A CN201910259273.0A CN201910259273A CN109852808A CN 109852808 A CN109852808 A CN 109852808A CN 201910259273 A CN201910259273 A CN 201910259273A CN 109852808 A CN109852808 A CN 109852808A
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- silver
- colored slag
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- tin
- separating residues
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- 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
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- Manufacture And Refinement Of Metals (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of from silver separating residues extracts the technique of tin, takes suitable silver-colored slag to carry out break process, smashed silver-colored slag is carried out mixing defibrination with flocculant according to the mass ratio of 1:10, and be uniformly mixed, obtain the mixed solution of silver-colored slag and water；The mixed solution of silver-colored slag and water is injected in holding furnace, and is warming up to 560-850 DEG C, and is stirred 20 minutes, stirring stands 3-6h after completing；Four filtration treatments are carried out to the mixed liquor for stirring completion in step 2 using high pressure filter group, filtering is filtered for the first time with the speed of 40m/h, a kind of technique for extracting tin from silver separating residues of the present invention, by being filtered for multiple times, it can guarantee that the contaminant filter in silver-colored slag is abundant, improve the purity that product is made, the impurity in silver-colored slag can be precipitated under the atmosphere of carbon dioxide simultaneously, further improve the purity that product is made, in addition it is carried out under the atmosphere of nitrogen, it is carried out conducive to stablizing for chemical reaction, the preparation process is simple, it is at low cost, with better prospect of the application.
Description
Technical field
The invention belongs to field of new materials, in particular to a kind of technique that tin is extracted from silver separating residues.
Background technique
Tin, metallic element, a kind of metallic element for the low melting point having silvery white gloss, is divalent or four in compound
Valence, will not oxidation by air, mainly with the form of dioxide (cassiterite) and various sulfide (such as sulphur cassiterite) presence；
And the existing technique that tin is extracted from silver separating residues, the glass putty in mining site can not be made to extract completely, be easy to make production obtained
Product degree of purity is inadequate, while wastage of material is be easy to cause in production process, and technics comparing is complicated, for this purpose, it is proposed that it is a kind of from
The technique of tin is extracted in silver separating residues.
Summary of the invention
The main purpose of the present invention is to provide a kind of from silver separating residues extracts the technique of tin, can effectively solve background skill
The problems in art.
To achieve the above object, the technical scheme adopted by the invention is as follows:
It is a kind of from silver separating residues extract tin technique, should from silver separating residues extract tin technique the following steps are included:
Step 1: suitable silver-colored slag is taken to carry out break process, by smashed silver-colored slag and flocculant according to 1:10 mass ratio into
Row mixing defibrination, and be uniformly mixed, obtain the mixed solution of silver-colored slag and water；
Step 2: the mixed solution of silver-colored slag and water is injected in holding furnace, and it is warming up to 560-850 DEG C, and stirred 20 minutes, stirred
It mixes completion and stands 3-6h later；
Step 3: carrying out four filtration treatments to the mixed liquor for stirring completion in step 2 using high pressure filter group, for the first time
Filtering is filtered with the speed of 40m/h, and second of the speed with 45m/h filters, and is filtered for the third time with the speed of 50m/h, the 4th time
It is filtered with the speed of 55m/h；
Step 4: carrying out low-temperature oxidation roasting processing to the silver-colored slag by filtering, add by the silver-colored slag that low-temperature oxidation roasting is handled
Enter after adding flocculant in reactor, stand 5-8h, then appropriate phosphoric acid is added into reactor, it is anti-to be warming up to 260 DEG C of leachings
After answering 6-8h, then calcium dihydrogen phosphate is added into reactor, is warming up to 100 DEG C, reacts 2-4h, obtain mixture A；
Step 5: mixture A is added in smelting furnace, and when being warming up to 800 DEG C, under the protection of nitrogen, stir 30 minutes,
Carbon dioxide gas is passed through with the rate of 20L per minute again, the other compositions in silver-colored slag are precipitated, finally filter to get metal
Tin.
Preferably, within 50 DEG C, the rate for being passed through oxygen-enriched air is 6-8L/min for temperature control in low-temperature oxidation roasting.
Preferably, one of aluminum sulfate, aluminium chloride, ferric sulfate, iron chloride can be selected in flocculant.
Preferably, partial size is less than 0.3cm after crushing.
Preferably, the phosphoric acid filter liquor density in step 2 is 0.25g/cm3.
Preferably, the charge velocity of nitrogen is 20-38L/min.
Preferably, the purity of carbon dioxide gas is passed through between 97-99%.
Compared with prior art, the invention has the following beneficial effects: this extracts the technique of tin from silver separating residues, through excessive
Secondary filtering can guarantee that the contaminant filter in silver-colored slag is abundant, improve the purity that product is made, while under the atmosphere of carbon dioxide
The impurity in silver-colored slag can be precipitated, further improve the purity that product is made, in addition carry out, be conducive under the atmosphere of nitrogen
Stablizing for chemical reaction carries out, and the preparation process is simple, at low cost, has better prospect of the application.
Specific embodiment
To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, below with reference to
Specific embodiment, the present invention is further explained.
A kind of technique that tin is extracted from silver separating residues of the invention when preparation, takes suitable silver-colored slag to carry out break process, will
Smashed silver slag and flocculant mix defibrination according to the mass ratio of 1:10, flocculation be all small colloidal solid and
Suspended particle neutralizes Particle surface charge, reduces or eliminates between particle under the action of colloidal substance or electrolyte
Repulsive force is combined together particle, and volume constantly becomes larger, and when particle aggregation reaches a certain level volume, (grain strength is about
When for 0.01cm), it just is separated from the water out, and be uniformly mixed, obtains the mixed solution of silver-colored slag and water；By the mixed of silver-colored slag and water
It closes in solution injection holding furnace, and is warming up to 560-850 DEG C, and stir 20 minutes, stirring stands 3-6h after completing；Utilize height
It presses through filter group and four filtration treatments is carried out to the mixed liquor for stirring completion in step 2, filtering is for the first time with the speed of 40m/h
Filtering, second of the speed with 45m/h are filtered, are filtered for the third time with the speed of 50m/h, and the 4th speed with 55m/h filters；
Low-temperature oxidation roasting processing is carried out to the silver-colored slag by filtering, temperature control is passed through richness within 50 DEG C in low-temperature oxidation roasting
The rate of oxygen air is 6-8L/min, after the silver-colored slag of low-temperature oxidation roasting processing is added in reactor and adds flocculant,
One of aluminum sulfate, aluminium chloride, ferric sulfate, iron chloride can be selected in flocculant, stands 5-8h, then is added in right amount into reactor
Phosphoric acid, phosphoric acid filter liquor density are 0.25g/cm3, after being warming up to 260 DEG C of leaching reaction 6-8h, then di(2-ethylhexyl)phosphate are added into reactor
Hydrogen calcium is warming up to 100 DEG C, reacts 2-4h, obtains mixture A；Mixture A is added in smelting furnace, and is warming up to 800 DEG C
When, under the protection of nitrogen, the charge velocity of nitrogen is 20-38L/min, it stirs 30 minutes, and nitrogen is a kind of under normal condition
The gas of colorless and odorless, duty gas fraction about 78%, fusing point are 63 K, and boiling point is 77 K, and critical-temperature is 126 K, it is difficult to
Liquefaction, solubility very little can be used as protective gas, avoid the intervention of other impurities in chemical reaction, improve reactant purity,
Controlling temperature and pressure simultaneously makes nitrogen reach supercriticality, then is passed through carbon dioxide gas with the rate of 20L per minute, leads to
Enter the purity of carbon dioxide gas between 97-99%, to improve its solubility in supercritical carbon dioxide, then to its into
Row selective extraction；The carbon dioxide dissolved with impurity is filtered out, carbon dioxide is higher than 31 DEG C of critical-temperature (Tc), pressure in temperature
Power is higher than in the state of critical pressure (Pc) 3MPa, and property can change, and density is bordering on liquid, and viscosity is bordering on gas, expands
100 times that coefficient is liquid are dissipated, thus there is very strong solvability, many kinds of substance is can dissolve with it, then extracts therein
Effective component is precipitated the other compositions in silver-colored slag, finally filters to get metallic tin.
Embodiment 1
It takes suitable silver-colored slag to carry out break process, smashed silver-colored slag and flocculant is subjected to mixer mill according to the mass ratio of 1:10
Slurry, and be uniformly mixed, obtain the mixed solution of silver-colored slag and water；The mixed solution of silver-colored slag and water is injected in holding furnace, and is heated up
It to 560 DEG C, and stirs 20 minutes, stirring stands 3h after completing；Stirring in step 2 is completed using high pressure filter group
Mixed liquor carries out four filtration treatments, and filtering is filtered for the first time with the speed of 40m/h, and second of the speed with 45m/h filters, the
It is filtered three times with the speed of 50m/h, the 4th speed with 55m/h filters；Low-temperature oxidation roasting is carried out to the silver-colored slag by filtering
Burning is handled, and temperature control is within 50 DEG C in low-temperature oxidation roasting, and the rate for being passed through oxygen-enriched air is 6L/min, by cryogenic oxygen
Change calcination process silver-colored slag be added reactor in add flocculant after, flocculant can be selected aluminum sulfate, aluminium chloride, ferric sulfate,
One of iron chloride stands 5h, then appropriate phosphoric acid is added into reactor, and phosphoric acid filter liquor density is 0.25g/cm3, is warming up to
After 260 DEG C of leaching reaction 6h, then calcium dihydrogen phosphate is added into reactor, is warming up to 100 DEG C, reacts 2h, obtain mixture A；
When mixture A being added in smelting furnace, and being warming up to 800 DEG C, under the protection of nitrogen, the charge velocity of nitrogen is 20L/
Min is stirred 30 minutes, while controlling temperature and pressure makes nitrogen reach supercriticality, then is passed through with the rate of 20L per minute
Carbon dioxide gas is passed through the purity of carbon dioxide gas between 97%, to improve its dissolution in supercritical carbon dioxide
Degree, then selective extraction is carried out to it；The other compositions in silver-colored slag are precipitated, finally filter to get metallic tin, through detection tin
Purity is 95%, and the utilization rate of silver-colored slag reaches 78%.
Embodiment 2
It takes suitable silver-colored slag to carry out break process, smashed silver-colored slag and flocculant is subjected to mixer mill according to the mass ratio of 1:10
Slurry, and be uniformly mixed, obtain the mixed solution of silver-colored slag and water；The mixed solution of silver-colored slag and water is injected in holding furnace, and is heated up
It to 850 DEG C, and stirs 20 minutes, stirring stands 6h after completing；Stirring in step 2 is completed using high pressure filter group
Mixed liquor carries out four filtration treatments, and filtering is filtered for the first time with the speed of 40m/h, and second of the speed with 45m/h filters, the
It is filtered three times with the speed of 50m/h, the 4th speed with 55m/h filters；Low-temperature oxidation roasting is carried out to the silver-colored slag by filtering
Burning is handled, and temperature control is within 50 DEG C in low-temperature oxidation roasting, and the rate for being passed through oxygen-enriched air is 8L/min, by cryogenic oxygen
Change calcination process silver-colored slag be added reactor in add flocculant after, flocculant can be selected aluminum sulfate, aluminium chloride, ferric sulfate,
One of iron chloride stands 8h, then appropriate phosphoric acid is added into reactor, and phosphoric acid filter liquor density is 0.25g/cm3, is warming up to
After 260 DEG C of leaching reaction 6-8h, then calcium dihydrogen phosphate is added into reactor, is warming up to 100 DEG C, reacts 4h, obtain mixture
A；When mixture A being added in smelting furnace, and being warming up to 800 DEG C, under the protection of nitrogen, the charge velocity of nitrogen is 38L/
Min is stirred 30 minutes, while controlling temperature and pressure makes nitrogen reach supercriticality, then is passed through with the rate of 20L per minute
Carbon dioxide gas is passed through the purity of carbon dioxide gas between 99%, to improve its dissolution in supercritical carbon dioxide
Degree, then selective extraction is carried out to it；The other compositions in silver-colored slag are precipitated, finally filter to get metallic tin, through detection tin
Purity is 97%, and the utilization rate of silver-colored slag reaches 82%.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (7)
1. a kind of technique for extracting tin from silver separating residues, which is characterized in that it includes following for should extracting the technique of tin from silver separating residues
Step:
Step 1: suitable silver-colored slag is taken to carry out break process, by smashed silver-colored slag and flocculant according to 1:10 mass ratio into
Row mixing defibrination, and be uniformly mixed, obtain the mixed solution of silver-colored slag and water；
Step 2: the mixed solution of silver-colored slag and water is injected in holding furnace, and it is warming up to 560-850 DEG C, and stirred 20 minutes, stirred
It mixes completion and stands 3-6h later；
Step 3: carrying out four filtration treatments to the mixed liquor for stirring completion in step 2 using high pressure filter group, for the first time
Filtering is filtered with the speed of 40m/h, and second of the speed with 45m/h filters, and is filtered for the third time with the speed of 50m/h, the 4th time
It is filtered with the speed of 55m/h；
Step 4: carrying out low-temperature oxidation roasting processing to the silver-colored slag by filtering, add by the silver-colored slag that low-temperature oxidation roasting is handled
Enter after adding flocculant in reactor, stand 5-8h, then appropriate phosphoric acid is added into reactor, it is anti-to be warming up to 260 DEG C of leachings
After answering 6-8h, then calcium dihydrogen phosphate is added into reactor, is warming up to 100 DEG C, reacts 2-4h, obtain mixture A；
Step 5: mixture A is added in smelting furnace, and when being warming up to 800 DEG C, under the protection of nitrogen, stir 30 minutes,
Carbon dioxide gas is passed through with the rate of 20L per minute again, the other compositions in silver-colored slag are precipitated, finally filter to get metal
Tin.
2. a kind of technique for extracting tin from silver separating residues according to claim 1, it is characterised in that: in low-temperature oxidation roasting
Temperature controls within 50 DEG C, and the rate for being passed through oxygen-enriched air is 6-8L/min.
3. a kind of technique for extracting tin from silver separating residues according to claim 1, it is characterised in that: sulphur can be selected in flocculant
One of sour aluminium, aluminium chloride, ferric sulfate, iron chloride.
4. a kind of technique for extracting tin from silver separating residues according to claim 1, it is characterised in that: partial size is less than after crushing
0.3cm。
5. a kind of preparation process of technique for extracting tin from silver separating residues according to claim 1, it is characterised in that: step
Phosphoric acid filter liquor density in two is 0.25g/cm3.
6. a kind of technique for extracting tin from silver separating residues according to claim 1, it is characterised in that: the charge velocity of nitrogen
For 20-38L/min.
7. a kind of technique for extracting tin from silver separating residues according to claim 1, it is characterised in that: be passed through carbon dioxide gas
The purity of body is between 97-99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910259273.0A CN109852808A (en) | 2019-04-02 | 2019-04-02 | A kind of technique for extracting tin from silver separating residues |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910259273.0A CN109852808A (en) | 2019-04-02 | 2019-04-02 | A kind of technique for extracting tin from silver separating residues |
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| CN109852808A true CN109852808A (en) | 2019-06-07 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05239568A (en) * | 1992-02-28 | 1993-09-17 | Mitsubishi Alum Co Ltd | Method for refining of pure al sheet material by heating |
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
| CN105296757A (en) * | 2014-11-29 | 2016-02-03 | 董亚伦 | Treating method for tin stripping waste solution |
| CN109881001A (en) * | 2019-04-02 | 2019-06-14 | 柳州光华科技有限公司 | The method of tin material is extracted in a kind of tin ore |
-
2019
- 2019-04-02 CN CN201910259273.0A patent/CN109852808A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05239568A (en) * | 1992-02-28 | 1993-09-17 | Mitsubishi Alum Co Ltd | Method for refining of pure al sheet material by heating |
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
| CN105296757A (en) * | 2014-11-29 | 2016-02-03 | 董亚伦 | Treating method for tin stripping waste solution |
| CN109881001A (en) * | 2019-04-02 | 2019-06-14 | 柳州光华科技有限公司 | The method of tin material is extracted in a kind of tin ore |
Non-Patent Citations (3)
| Title |
|---|
| 张深根等: "《重金属固废处理及资源化技术》", 31 December 2016, 冶金工业出版社 * |
| 郑丙辉: "《水体污染事件应急处置技术手册》", 30 November 2018, 中国环境出版集团 * |
| 韩长日等: "《精细无机化学品制造技术》", 31 August 2008, 科技文献出版社 * |
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Application publication date: 20190607 |
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