KR101542286B1 - Thallium and potassium nitrate recovery method and recovery apparatus - Google Patents
Thallium and potassium nitrate recovery method and recovery apparatus Download PDFInfo
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- KR101542286B1 KR101542286B1 KR1020117002508A KR20117002508A KR101542286B1 KR 101542286 B1 KR101542286 B1 KR 101542286B1 KR 1020117002508 A KR1020117002508 A KR 1020117002508A KR 20117002508 A KR20117002508 A KR 20117002508A KR 101542286 B1 KR101542286 B1 KR 101542286B1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
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Abstract
The object of the present invention is to provide a method and a device for recovering thallium and potassium nitrate recovering metal thallium contained in molten salt of thallium-containing potassium nitrate and recovering molten salt from which thallium has been removed as potassium nitrate . In the method of recovering thallium and potassium nitrate according to the present invention, potassium thallium-containing potassium nitrate is charged into a magnetic crucible 11 of a melting furnace 2, the molten salt S is heated to a temperature not higher than the melting point of potassium nitrate not higher than the thermal decomposition temperature, A molten metal thallium MT is deposited on the bottom portion 11a of the magnetic crucible 11 by supplying a direct current to the molten salt S through the anode 21 and the electrode terminal 22, (MT) is taken out by the take-out pipe (14), and then potassium nitrate is taken out by the take-out pipe (14).
Description
The present invention relates to a method and a device for recovering thallium and potassium nitrate, and more particularly, to a method and apparatus for recovering metal thallium and potassium nitrate, which are rare metals, from a molten salt in which thallium- Thallium and potassium nitrate, and a recovering apparatus.
The present application claims priority based on Japanese Patent Application No. 2008-222551 filed on August 29, 2008, the contents of which are incorporated herein by reference.
Recently, as the protection of the global environment has increased, environmental measures have become very important for cement manufacturing facilities that effectively utilize industrial wastes, final disposal facilities for industrial wastes, petrochemical plants, and various factories. For example, in a cement manufacturing facility, a chlorine bypass device is installed to remove volatile components such as chlorine contained in industrial wastes.
However, since the chlorine bypass dust discharged from the chlorine bypass device contains useful heavy metals such as thallium, it is necessary to remove these chlorine compounds and recover useful heavy metals such as thallium in order to be reused as a cement raw material.
Various conventional methods for recovering thallium have been proposed as follows.
(1) The thallium-containing raw material is subjected to reduction and leaching using sulfuric acid and a reducing agent to neutralize the leached solution obtained by filtration, to obtain a thallium leaching solution and a neutralized product (neutralized product), dissolving the neutralized product in hydrochloric acid and then adding a reducing agent A method of recovering thallium by precipitating precipitates by solid-liquid separation (Patent Document 1).
(2) The thallium-containing material is oxidized and leached and then subjected to solid-liquid separation to obtain a thallium-containing liquid. A reducing agent and a chlorine source are added to the thallium-containing liquid to precipitate thallium chloride. The thallium chloride is heated and dissolved with concentrated sulfuric acid, And the metal thallium is recovered by reducing the thallium sulfate solution (Patent Document 2).
On the other hand, in industrial wastes discharged from factories or distribution facilities, or general wastes discharged from households, wastewater generated when the waste is washed, or when water such as municipal waste incinerator, fly ash, plastic incinerator is washed, Since metals such as lead, cadmium, chromium, and mercury are contained, it is necessary to purify the water quality by removing these heavy metals as much as possible from the waste water, and to recover useful heavy metals such as thallium.
Therefore, there has been proposed a method for removing metal from drainage that discharges a metal dissolved in the drainage by passing a direct current through the drainage and separating the metal oxide from the drainage (Patent Document 3).
In addition, there is thallium-containing glass debris generated when optical glass such as an optical lens containing thallium is processed into one of industrial wastes. As a method of recovering thallium from the thallium-containing glass debris, a glass debris containing thallium There has been proposed a method of recovering thallium from a glass scrap containing thallium which is obtained by pulverizing the obtained glass scrap with a particle size of 300 mu m or less and extracting the obtained glass scrap with an inorganic acid to add metal which is baser than thallium to precipitate metal thallium (Patent Document 4).
However, when thallium is contained in potassium nitrate such as thallium-containing potassium nitrate, thallium and potassium nitrate must be recovered by completely separate processes in the conventional thallium recovery method and metal removal method, and thallium and potassium nitrate It is difficult to effectively utilize thallium-containing potassium nitrate as a resource because there is a problem that the time and cost for recovery are excessively large.
As described above, there is also proposed a method of recovering thallium from a glass scrap containing thallium. However, this method is a method mainly aimed at recovering thallium, and is a method of grinding, extracting, adding a base metal , It has a problem in that the time and cost for recovering are too much. Therefore, the glass scrap with thallium removed has not been effectively used and has been treated as industrial waste.
As described above, potassium thallium-containing potassium nitrate has not been effectively used as a resource in the past, nor is there been studied a method for effectively utilizing it, and the present situation is that it is treated as waste in view of safety.
The present invention has been made to solve the above problems, and it is an object of the present invention to provide a method for recovering thallium, which is a rare metal contained in a molten salt, by recovering thallium as metal thallium by effectively melting potassium thallium containing nitrate, And a method for recovering and recovering thallium and potassium nitrate, which can be effectively recovered as potassium nitrate.
In order to solve the above-described problems, the present invention provides the following method and apparatus for recovering thallium and potassium nitrate.
That is, the method of recovering thallium and potassium nitrate according to the present invention is a method of recovering thallium and potassium nitrate from thallium-containing potassium nitrate, wherein the thallium-containing potassium nitrate is heated and melted to form a molten salt, Thereby separating thallium dissolved in the molten salt as metal thallium and recovering the molten salt from which the metal thallium and thallium are separated.
In the method for recovering thallium and potassium nitrate, potassium thallium containing potassium nitrate is heated and melted to be a molten salt, and a direct current is passed through the molten salt to separate thallium dissolved in the molten salt as metal thallium. Thereafter, the molten salt from which the metal thallium and thallium are removed is recovered, respectively.
As a result, thallium and potassium nitrate contained in the thallium-containing potassium nitrate can be efficiently recovered, and the recovered thallium and potassium nitrate can be effectively used.
It is preferable that thallium dissolved in the molten salt is precipitated as metal thallium by inserting a positive electrode and a negative electrode into a molten salt heated and melted with the thallium-containing potassium nitrate and conducting a direct current between the positive electrode and the negative electrode.
It is preferable that molten metal thallium separated from the molten salt is used as a negative electrode and a direct current is passed between the negative electrode and the positive electrode to precipitate thallium dissolved in the molten salt as metal thallium.
The temperature of the molten salt is preferably higher than the melting point of potassium nitrate or lower than the pyrolysis temperature.
The apparatus for recovering thallium and potassium nitrate according to the present invention is a device for recovering thallium and potassium nitrate from thallium-containing potassium nitrate, comprising: a melting furnace for heating and melting the thallium-containing potassium nitrate to form a molten salt; And electrolysis means for separating the thallium dissolved in the molten salt as metal thallium by conducting electricity.
In the thallium and potassium nitrate recovery apparatus, potassium thallium containing potassium nitrate is heated and melted to be a molten salt by a melting furnace, and a direct current is supplied to the molten salt by an electrolytic means to dissolve thallium dissolved in the molten salt, .
As a result, it is possible to efficiently recover thallium and potassium nitrate contained in the thallium-containing potassium nitrate with a simple apparatus, and to use the recovered thallium and potassium nitrate effectively.
Wherein the electrolytic means includes an electrode inserted into the molten salt and an electrode terminal made of molten metal thallium as a negative electrode by contacting the molten metal thallium generated from the molten salt and a DC current passing between the positive electrode and the negative electrode It is preferable that it is provided with an energizing means.
It is preferable that the melting furnace is a magnetic crucible having an outlet at the bottom.
According to the thallium and potassium nitrate recovery method of the present invention, thallium potassium nitrate is heated and melted to be a molten salt, and a direct current is passed through the molten salt to separate thallium dissolved in the molten salt as metal thallium, Since the molten salt in which the metal thallium and thallium are separated is recovered separately, thallium and potassium nitrate contained in the thallium-containing potassium nitrate can be efficiently recovered by a simple operation. Therefore, thallium and potassium nitrate can be recovered from potassium thallium-containing potassium nitrate, respectively, and these can be used again effectively.
In addition, since only the thallium-containing potassium nitrate is heated and melted to supply a direct current to the molten salt, the cost and time for recovering metal thallium and potassium nitrate can be suppressed to a low level.
According to the thallium and potassium nitrate recovery apparatus of the present invention, there is provided a melting furnace for heating and melting molten salt of thallium containing potassium nitrate, and a melting furnace for separating thallium dissolved in the molten salt into metal thallium It is possible to efficiently recover thallium and potassium nitrate contained in the thallium-containing potassium nitrate with a simple apparatus. Therefore, thallium and potassium nitrate recovered from potassium thallium-containing potassium nitrate can be effectively used again.
In addition, since it is a simple apparatus having a melting furnace and electrolytic means, the cost for recovering thallium and potassium nitrate can be suppressed to be low.
1 is a schematic diagram showing an apparatus for recovering thallium and potassium nitrate according to an embodiment of the present invention.
2 is a diagram showing a powder X-ray diffraction (XRD) diagram of the metallic material of Example 1 of the present invention.
3 is a diagram showing a powder X-ray diffraction (XRD) diagram of a white substance according to Example 1 of the present invention.
4 is a graph showing the change in thallium concentration in the molten salt in the magnetic crucible.
Best Mode for Carrying out the Thallium and Potassium Nitrate Recovery Method and Recovery Apparatus of the Present Invention will be described with reference to the drawings.
In addition, the present invention will be described in detail in order to better understand the spirit of the invention and is not intended to limit the present invention unless otherwise specified.
1 is a schematic view showing an apparatus for recovering thallium and potassium nitrate according to an embodiment of the present invention, and is an example of an apparatus for recovering metal thallium (Tl) and potassium nitrate (KNO 3 ) from potassium thallium containing potassium nitrate.
The apparatus for recovering thallium and
The
The
The
Instead of the
The
Next, a method for recovering thallium and potassium nitrate of the present invention using the above-described recovery device (1) will be described.
The recovering method of this embodiment separates thallium dissolved in the molten salt as metal thallium by heating and melting the thallium-containing potassium nitrate as a molten salt and conducting a direct current to the molten salt, And recovering the separated molten salt, respectively.
The "thallium-containing potassium nitrate" used in this recovery method was prepared by dissolving potassium thallium in potassium nitrate (melting point: 206 ° C., boiling point: 430 ° C., specific gravity: 5.556 ), And the purity of potassium nitrate is approximately 97 to 99.8% by weight. This potassium nitrate contains Na, Pb, Ca, Fe and the like as impurities.
Next, each step of the recovery method will be described in detail.
<Heating and melting of potassium nitrate containing thallium>
A predetermined amount of thallium potassium nitrate is added to the
Here, the temperature of potassium thallium-containing potassium nitrate is set to be not lower than the melting point (334.3 ° C) of potassium nitrate and not higher than the thermal decomposition temperature (400 ° C) in order to stably maintain the molten salt (S) of potassium thallium-containing potassium nitrate stably.
If the temperature is lower than the melting point (334.3 占 폚) of potassium nitrate, potassium thallium-containing nitrate does not melt, and if it exceeds the thermal decomposition temperature (400 占 폚), potassium nitrate of potassium thallium-containing potassium nitrate is thermally decomposed.
≪ Current conduction to molten salt >
The
As a result, potassium nitrate in the molten salt (S) is electrolyzed to become metallic thallium (MT). The temperature of this metal thallium (specific gravity: 11.85, melting point: 303.5 ° C, boiling point: 1487 ° C) (MT) is within the range of the molten salt (S) (specific gravity: 2.11) (334.3 ° C to 400 ° C) Because the difference in specific gravity between the thallium (MT) and the molten salt (S) is large, it precipitates in the molten state at the bottom 11a of the
Here, if molten metal thallium (MT) is used as a negative electrode by the
<Recovery of metal thallium and potassium nitrate>
The molten metal thallium MT precipitated in the
When the molten metal thallium (MT) is taken out, the temperature of the molten salt (S) is adjusted not lower than the melting point (303.5 ° C) of the metal thallium and not higher than the melting point (334.3 ° C) of the potassium nitrate, It is preferable since only metal thallium (MT) can be efficiently taken out.
The thus recovered metal thallium and potassium nitrate are subjected to a predetermined treatment as required and reused.
As described above, according to the thallium and potassium nitrate recovery method of the present embodiment, potassium thallium-containing potassium nitrate is heated and melted to be a molten salt, and a direct current is passed through the molten salt to dissolve thallium dissolved in the molten salt The molten metal thallium (MT) is separated, and the molten metal thallium and thallium are recovered respectively as the separated molten salt potassium nitrate. Therefore, thallium and potassium nitrate contained in the thallium-containing potassium nitrate can be efficiently recovered individually by a simple operation . Therefore, thallium and potassium nitrate can be recovered from potassium thallium-containing potassium nitrate, respectively, and these can be used again effectively.
Further, since molten metal thallium (MT) can be taken out and subsequently potassium nitrate can be extracted, the cost and time for recovering thallium and potassium nitrate can be suppressed to a low level.
The apparatus for recovering thallium and potassium nitrate according to the present embodiment comprises a
In addition, since the structure of the apparatus is simple, the cost for recovering molten metal thallium and potassium nitrate can be suppressed to a low level.
Example
Hereinafter, the method for recovering thallium and potassium nitrate of the present invention will be described in detail with reference to examples, but the present invention is not limited at all by the following examples unless the gist thereof is exceeded.
< Example 1>
500 g of thallium-containing potassium nitrate having a thallium content of 7500 ppm was charged into the
Then, a pair of platinum electrodes having a width of 10 mm, a length of 100 mm and a thickness of 1 mm were inserted into the molten salt S at a distance of 10 cm from the
By the electrolysis, the metallic material was deposited on the
The molten metallic material precipitated in the
This metal substance was identified by powder X-ray diffraction (XRD) and found to be metallic thallium. Fig. 2 shows a powder X-ray diffraction (XRD) diagram of the metallic material of Example 1. Fig.
Subsequently, the molten transparent phase material was taken out from the take-out
When this white substance was identified by powder X-ray diffraction (XRD), it was confirmed to be potassium nitrate with good crystallinity. Figure 3 shows a powder X-ray diffraction (XRD) figure of the white material of Example 1.
The content of thallium in this white substance was analyzed by IPC-AES, and found to be 745 mg / kg, and the content of thallium was about 1/10 as compared with the initial amount of potassium thallium-containing potassium nitrate.
< Example 2>
500 g of thallium-containing potassium nitrate having a thallium content of 7500 ppm was charged into the
Subsequently, the prepared metal thallium was slowly submerged in the molten salt (S). This metal thallium was melted and settled at the bottom of the
Subsequently, metal thallium melted at the bottom of the
By the electrolysis, the metallic material was deposited on the
The molten metallic material precipitated in the
This metal substance was identified by powder X-ray diffraction (XRD) and found to be metallic thallium.
Subsequently, the molten transparent phase material was taken out from the take-out
When this white substance was identified by powder X-ray diffraction (XRD), it was confirmed to be potassium nitrate with good crystallinity.
Fig. 4 is a diagram showing the change in thallium concentration due to the energization time (seconds) in a sample taken from a molten salt in a magnetic crucible. Fig.
4, the thallium concentration in the molten salt before energization is 7500 mg / kg, the thallium concentration in the molten salt after 1000 sec is 8,400 mg / kg, the thallium concentration in the molten salt before and after 2000 sec is 2300 mg / It can be seen that the thallium concentration in the molten salt decreases with the passage of time.
(Industrial applicability)
According to the thallium and potassium nitrate recovery method of the present invention, thallium potassium nitrate is heated and melted to be a molten salt, and a direct current is passed through the molten salt to separate thallium dissolved in the molten salt as metal thallium , The molten salt in which the metal thallium and thallium are separated is recovered, respectively, so that thallium and potassium nitrate contained in the thallium-containing potassium nitrate can be efficiently recovered by a simple operation. Therefore, thallium and potassium nitrate are recovered from potassium thallium-containing potassium nitrate, respectively, and they can be effectively used again, which is very useful in industry.
1 Thallium and potassium nitrate recovery device
2 melting furnace
3 Electrolysis device
11 magnetic crucible
11a bottom
12 outlet
13 valves
14 Piping for extraction
21 bar type anode
22 Plate-like electrode terminal
23 DC Stabilized Power Supply
S molten salt
MT Molten metal thallium
Claims (10)
The thallium-containing potassium nitrate is heated and melted to form a molten salt, and a direct current is passed through the molten salt to separate thallium dissolved in the molten salt as metal thallium, and the molten salt from which the metal thallium and thallium are separated And recovering potassium thallium and potassium nitrate.
Characterized in that thallium dissolved in the molten salt is precipitated as metal thallium by inserting a positive electrode and a negative electrode into molten salt heated and melted with the thallium containing nitrate and conducting a direct current between the positive electrode and the negative electrode, And recovering potassium nitrate.
Wherein molten metal thallium separated from the molten salt is used as a negative electrode and a direct current is passed between the negative electrode and the positive electrode to precipitate thallium dissolved in the molten salt as metal thallium .
Wherein the temperature of the molten salt is higher than the melting point of potassium nitrate and lower than the thermal decomposition temperature.
Wherein the temperature of the molten salt is higher than the melting point of potassium nitrate and lower than the thermal decomposition temperature.
Wherein the temperature of the molten salt is higher than the melting point of potassium nitrate and lower than the thermal decomposition temperature.
A melting furnace which is a magnetic crucible in which a thallium-containing potassium nitrate is heated and melted to be used as a molten salt,
And electrolytic means for passing a direct current through said molten salt to separate thallium dissolved in said molten salt as metal thallium, said electrolytic means comprising: a positive electrode inserted in said molten salt; a molten metal disposed on the bottom of said molten metal, An electrode terminal made of molten metal thallium as a negative electrode by being brought into contact with thallium, and a direct current energizing means for energizing a direct current between the positive electrode and the negative electrode,
Wherein the thallium and potassium nitrate recovery device comprises:
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008222551A JP5293007B2 (en) | 2008-08-29 | 2008-08-29 | Method and apparatus for recovering thallium and potassium nitrate |
| JPJP-P-2008-222551 | 2008-08-29 |
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| Publication Number | Publication Date |
|---|---|
| KR20110060883A KR20110060883A (en) | 2011-06-08 |
| KR101542286B1 true KR101542286B1 (en) | 2015-08-06 |
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| KR1020117002508A KR101542286B1 (en) | 2008-08-29 | 2009-08-28 | Thallium and potassium nitrate recovery method and recovery apparatus |
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| JP (1) | JP5293007B2 (en) |
| KR (1) | KR101542286B1 (en) |
| CN (1) | CN102137958A (en) |
| WO (1) | WO2010023936A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI411579B (en) * | 2011-08-16 | 2013-10-11 | Univ Nat Formosa | A method for purifying potassium nitrate from waste from the glass hardening process |
| CN103539167B (en) * | 2012-07-09 | 2015-07-15 | 虎尾科技大学 | Method of continuously purifying potassium nitrate in batch in waste generated by glass hardening process |
| KR102241464B1 (en) * | 2014-06-30 | 2021-04-16 | 재단법인 포항산업과학연구원 | Lithium recovering device in electrolysis apparatus, method for recovering lithium and electrolysis apparatus |
| KR101978140B1 (en) * | 2017-11-22 | 2019-05-15 | 재단법인 포항산업과학연구원 | Appratus for producing aluminum-scandium alloy and method using the same |
| KR101978141B1 (en) * | 2017-11-22 | 2019-05-15 | 재단법인 포항산업과학연구원 | Appratus for producing aluminum-scandium alloy and method using the same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000016813A (en) | 1998-07-02 | 2000-01-18 | Mitsubishi Materials Corp | High-purity thallium iodide, its sphered substance and its production |
| JP2004230289A (en) | 2003-01-30 | 2004-08-19 | Takuma Co Ltd | Method and equipment for treating thallium-containing liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5693887A (en) * | 1979-12-27 | 1981-07-29 | Nippon Mining Co Ltd | Pecovery of tallium from lead electrolyte |
| GB0027929D0 (en) * | 2000-11-15 | 2001-01-03 | Univ Cambridge Tech | Metal and alloy powders |
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2008
- 2008-08-29 JP JP2008222551A patent/JP5293007B2/en active Active
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2009
- 2009-08-28 KR KR1020117002508A patent/KR101542286B1/en active IP Right Grant
- 2009-08-28 WO PCT/JP2009/004202 patent/WO2010023936A1/en active Application Filing
- 2009-08-28 CN CN2009801339250A patent/CN102137958A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000016813A (en) | 1998-07-02 | 2000-01-18 | Mitsubishi Materials Corp | High-purity thallium iodide, its sphered substance and its production |
| JP2004230289A (en) | 2003-01-30 | 2004-08-19 | Takuma Co Ltd | Method and equipment for treating thallium-containing liquid |
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| Publication number | Publication date |
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| JP2010053432A (en) | 2010-03-11 |
| CN102137958A (en) | 2011-07-27 |
| WO2010023936A1 (en) | 2010-03-04 |
| JP5293007B2 (en) | 2013-09-18 |
| KR20110060883A (en) | 2011-06-08 |
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