CN109868489A - A kind of refinement of tin and recovery method - Google Patents
A kind of refinement of tin and recovery method Download PDFInfo
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- CN109868489A CN109868489A CN201910260028.1A CN201910260028A CN109868489A CN 109868489 A CN109868489 A CN 109868489A CN 201910260028 A CN201910260028 A CN 201910260028A CN 109868489 A CN109868489 A CN 109868489A
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a kind of refinement of tin and recovery methods, choose suitable tin ore soil, tin ore soil to be refined are worn into miberal powder, smashed partial size is in 0.5-0.8cm；Smashed tin ore soil is injected in reactor, while tin ore soil and dispersing agent are passed through nitrogen, control temperature and pressure makes nitrogen reach supercriticality according in the mass ratio injection reactor of 1:16 thereto；Electrolyte is added simultaneously, applies voltage in yin-yang interpolar and is electrolysed, the voltage applied makes cathode solid metal oxide electrochemical reduction occur but without decomposition molten salt electrolyte；Carbon dioxide is injected into solution, a kind of refinement of tin of the present invention and recovery method, purifying technique is simple, refining effect is good, can be widely used for the purification recycling of various metals, realizes the separation of the metal ion of different-grain diameter, simplify subsequent purification purifying technique, product purity obtained is higher simultaneously, can avoid wastage of material by raw material using sufficiently.
Description
Technical field
The invention belongs to field of new materials, in particular to the refinement of a kind of tin and recovery method.
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 refinement and the recovery method of existing tin, production technology are easy to bring pollution, are easy to keep product degree of purity obtained inadequate,
It is be easy to cause wastage of material in production process simultaneously, for this purpose, it is proposed that refinement and the recovery method of a kind of tin.
Summary of the invention
The main purpose of the present invention is to provide a kind of refinement of tin and recovery methods, can effectively solve in background technique
The problem of.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of refinement of tin and recovery method, refinement and the recovery method of the tin the following steps are included:
Step 1: choosing suitable tin ore soil, tin ore soil to be refined is worn into miberal powder, smashed partial size is in 0.5-0.8cm；
Step 2: smashed tin ore soil is injected in reactor, while tin ore soil and dispersing agent are infused according to the mass ratio of 1:16
Enter in reactor, be passed through nitrogen thereto, control temperature and pressure makes nitrogen reach supercriticality；
Step 3: electrolyte is added simultaneously, applies voltage in yin-yang interpolar and be electrolysed, the voltage applied keeps cathode solid-state golden
Belong to oxide and electrochemical reduction occurs but without decomposition molten salt electrolyte；
Step 4: injecting carbon dioxide into solution, to improve its solubility in supercritical carbon dioxide, then it is carried out
Selective extraction；
Step 5: filtering out the carbon dioxide dissolved with impurity, after carbon dioxide gas evacuator body, required metallic tin is obtained.
Preferably, electrolyte Na2CO3-K2CO。
Preferably, the volume of reactor is 5*6*5.5m3.
Preferably, the rate for injecting nitrogen is 3-5L/min.
Preferably, it is filled with temperature in nitrogen post-reactor and maintains 120-150 DEG C, pressure limit 0.9-2kpa.
Preferably, hydrochloric acid solution and sulfuric acid solution can be selected in electrolyte, and concentration is 0.1-0.03 μm of ol/L.
Preferably, it is 2-8V that yin-yang interpolar, which applies voltage range,.
Compared with prior art, the invention has the following beneficial effects: the refinement of the tin and recovery method, purifying technique letters
Single, refining effect is good, can be widely used for the purification recycling of various metals, realizes the separation of the metal ion of different-grain diameter, letter
Change subsequent purification purifying technique, while product purity obtained is higher, raw material can have been used sufficiently, avoids raw material unrestrained
Take.
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 refinement of tin of the invention and recovery method when preparation, choose suitable tin ore soil, by tin ore to be refined
Soil wears into miberal powder, and smashed partial size is in 0.5-0.8cm；Smashed tin ore soil is injected in reactor, the volume of reactor
For 5*6*5.5m3, while tin ore soil and dispersing agent are passed through nitrogen thereto, fill according in the mass ratio injection reactor of 1:16
Enter temperature in nitrogen post-reactor and maintain 120-150 DEG C, pressure limit 0.9-2kpa, the rate for injecting nitrogen is 3-5L/
Min, and nitrogen is a kind of gas of colorless and odorless under normal condition, duty gas fraction about 78%, fusing point is 63 K, and boiling point is
77 K, critical-temperature are 126 K, it is difficult to be liquefied, solubility very little can be used as protective gas, avoid other in chemical reaction
The intervention of impurity improves reactant purity, while controlling temperature and pressure makes nitrogen reach supercriticality；Electrolysis is added simultaneously
Matter, electrolyte Na2CO3-K2CO applies voltage in yin-yang interpolar and is electrolysed, and it is 2-8V that yin-yang interpolar, which applies voltage range,
The voltage applied makes cathode solid metal oxide electrochemical reduction occur but without decomposition molten salt electrolyte；Into solution
Carbon dioxide is injected, to improve its solubility in supercritical carbon dioxide, then selective extraction is carried out to it；It filters out molten
Solution has the carbon dioxide of impurity, and carbon dioxide is higher than 31 DEG C of critical-temperature (Tc), pressure higher than critical pressure (Pc) in temperature
In the state of 3MPa, property can change, and density is bordering on liquid, and viscosity is bordering on gas, and diffusion coefficient is the 100 of liquid
Times, thus there is very strong solvability, it can dissolve many kinds of substance with it, then extract effective component therein, therefore be passed through
Carbon dioxide can extract metallic tin.
Embodiment 1
Suitable tin ore soil is chosen, tin ore soil to be refined is worn into miberal powder, smashed partial size is in 0.5cm；It will be smashed
Tin ore soil injects in reactor, and the volume of reactor is 5*6*5.5m3, while tin ore soil and dispersing agent are according to the mass ratio of 1:16
It injects in reactor, is passed through nitrogen thereto, is filled with temperature in nitrogen post-reactor and maintains 120 DEG C, pressure limit 0.9kpa,
The rate for injecting nitrogen is 3L/min；Electrolyte, electrolyte Na are added simultaneously2CO3-K2CO, yin-yang interpolar apply voltage into
Row electrolysis, it is 2V that yin-yang interpolar, which applies voltage range, and the voltage applied makes cathode solid metal oxide that electrochemistry occur also
It is former but without decomposing molten salt electrolyte；Carbon dioxide is injected into solution, therefore be passed through carbon dioxide to extract metal
Tin, through detecting, tin purity obtained is 98.6%, cell parameter: a=0.5832nm, c=0.3181nm, contains 4 Sn originals in structure cell
Son, density 7.28g/cm3, hardness 2.
Embodiment 2
Suitable tin ore soil is chosen, tin ore soil to be refined is worn into miberal powder, smashed partial size is in 0.8cm；It will be smashed
Tin ore soil injects in reactor, and the volume of reactor is 5*6*5.5m3, while tin ore soil and dispersing agent are according to the mass ratio of 1:16
It injects in reactor, is passed through nitrogen thereto, be filled with temperature in nitrogen post-reactor and maintain 150 DEG C, pressure limit 2kpa, note
The rate for entering nitrogen is 3-5L/min；Electrolyte, electrolyte Na are added simultaneously2CO3-K2CO, yin-yang interpolar apply voltage into
Row electrolysis, it is 8V that yin-yang interpolar, which applies voltage range, and the voltage applied makes cathode solid metal oxide that electrochemistry occur also
It is former but without decomposing molten salt electrolyte；Carbon dioxide is injected into solution, therefore be passed through carbon dioxide to extract metal
Tin, through detecting, tin purity obtained is 98.8%, cell parameter: a=0.5832nm, c=0.3181nm, contains 4 Sn originals in structure cell
Son, density 7.59g/cm3, hardness 2.1.
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. refinement and the recovery method of a kind of tin, which is characterized in that the refinement of the tin and recovery method the following steps are included:
Step 1: choosing suitable tin ore soil, tin ore soil to be refined is worn into miberal powder, smashed partial size is in 0.5-0.8cm；
Step 2: smashed tin ore soil is injected in reactor, while tin ore soil and dispersing agent are infused according to the mass ratio of 1:16
Enter in reactor, be passed through nitrogen thereto, control temperature and pressure makes nitrogen reach supercriticality；
Step 3: electrolyte is added simultaneously, applies voltage in yin-yang interpolar and be electrolysed, the voltage applied keeps cathode solid-state golden
Belong to oxide and electrochemical reduction occurs but without decomposition molten salt electrolyte；
Step 4: injecting carbon dioxide into solution, to improve its solubility in supercritical carbon dioxide, then it is carried out
Selective extraction；
Step 5: filtering out the carbon dioxide dissolved with impurity, after carbon dioxide gas evacuator body, required metallic tin is obtained.
2. refinement and the recovery method of a kind of tin according to claim 1, it is characterised in that: electrolyte Na2CO3-
K2CO。
3. refinement and the recovery method of a kind of tin according to claim 1, it is characterised in that: the volume of reactor is 5*6*
5.5m³。
4. refinement and the recovery method of a kind of tin according to claim 1, it is characterised in that: the rate for injecting nitrogen is 3-
5L/min。
5. a kind of refinement of tin according to claim 1 and the preparation process of recovery method, it is characterised in that: be filled with nitrogen
Temperature maintains 120-150 DEG C in post-reactor, pressure limit 0.9-2kpa.
6. refinement and the recovery method of a kind of tin according to claim 1, it is characterised in that: it is molten that hydrochloric acid can be selected in electrolyte
Liquid and sulfuric acid solution, concentration are 0.1-0.03 μm of ol/L.
7. refinement and the recovery method of a kind of tin according to claim 1, it is characterised in that: yin-yang interpolar applies voltage model
It encloses for 2-8V.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268555A (en) * | 2011-09-05 | 2011-12-07 | 大连富井合金厂 | Method for refining platinum |
| CN102899689A (en) * | 2011-07-26 | 2013-01-30 | 武汉大学 | Environment protection type metal refining method |
| CN103906861A (en) * | 2011-11-04 | 2014-07-02 | 住友电气工业株式会社 | Molten salt electrolysis metal fabrication method and apparatus for use in same |
| US20170183759A1 (en) * | 2014-05-09 | 2017-06-29 | Stephen L. Cunningham | Arc furnace smeltering system & method |
| CN107513619A (en) * | 2017-08-14 | 2017-12-26 | 中南大学 | A kind of method of recovery indium and tin in waste material from ito glass |
-
2019
- 2019-04-02 CN CN201910260028.1A patent/CN109868489A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899689A (en) * | 2011-07-26 | 2013-01-30 | 武汉大学 | Environment protection type metal refining method |
| CN102268555A (en) * | 2011-09-05 | 2011-12-07 | 大连富井合金厂 | Method for refining platinum |
| CN103906861A (en) * | 2011-11-04 | 2014-07-02 | 住友电气工业株式会社 | Molten salt electrolysis metal fabrication method and apparatus for use in same |
| US20170183759A1 (en) * | 2014-05-09 | 2017-06-29 | Stephen L. Cunningham | Arc furnace smeltering system & method |
| CN107513619A (en) * | 2017-08-14 | 2017-12-26 | 中南大学 | A kind of method of recovery indium and tin in waste material from ito glass |
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Application publication date: 20190611 |