JP3136731B2 - Tellurium recovery equipment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a tellurium recovery apparatus for recovering tellurium from a solution containing tellurium, for example, a solution after leaching copper electrolytic slime.

[0002]

2. Description of the Related Art As a conventional tellurium recovery device, a reaction tank in which a liquid after leaching copper electrolytic slime (hereinafter, simply referred to as a liquid after leaching) is stored together with copper pieces, and a liquid after leaching in the reaction tank is used. Some include a stirrer for stirring. Then, a leached solution (14 cubic meters) containing 2 to 3 g / l of tellurium and a copper piece (50 to 200 kg) are charged into the reaction vessel, and the temperature of the leached solution is set to 80 ° C. and stirred for 36 hours. Then, the tellurium in the liquid after leaching is reacted with copper pieces, the tellurium in the liquid after leaching is collected as a precipitate of copper telluride, and the concentration of tellurium in the liquid after leaching is reduced to 100 ppm. There is something.

[0003]

However, in the conventional tellurium recovery apparatus, the liquid after leaching and copper telluride as a reaction product are mixed in the reaction tank.
The contact efficiency between the copper pieces and the liquid after leaching is poor, and as a result, the reaction time until the concentration of tellurium becomes equal to or lower than a predetermined value is as long as 36 hours. In this way, since the reaction time is long,
The amount of the leached liquid that could not be treated due to the limited amount of treatment was sent to a wastewater treatment plant, where tellurium was discarded as wastewater sludge, and wasted.

The present invention has been made in view of the above circumstances, and can improve the contact efficiency between a solution containing tellurium and a filler that reacts with tellurium in the solution, and can shorten the reaction time. Accordingly, it is an object of the present invention to provide a tellurium recovery device capable of improving the throughput of a solution and recovering tellurium without waste.

[0005]

A tellurium recovery apparatus according to claim 1 of the present invention is a tellurium recovery apparatus for recovering tellurium from a solution containing tellurium, wherein the tellurium is reacted with tellurium in the solution. A reaction tower filled with a filler that produces a reaction product, a tank for storing the solution, a pump for feeding the solution from the tank to a lower portion of the reaction tower, and a pump that overflows from an upper portion of the reaction tower. The solution is reacted
It is characterized by comprising a reflux pipe for refluxing the product together with the product to the tank, and a drain for discharging the reaction product precipitated in the tank.

In the tellurium recovery apparatus according to a second aspect of the present invention, the filler is made of copper pieces containing copper as a main component, and the temperature of the solution supplied to the reaction tower is maintained at 80 ° C. or higher. The flow rate of the solution flowing through the inside is set to 3.7 cm / sec or more.

[0007] The tellurium recovery apparatus according to claim 3 of the present invention is characterized in that the bulk specific gravity of the filler is 1 or less.

[0008]

According to the tellurium recovery apparatus according to the first aspect of the present invention, the tellurium-containing solution is supplied from the tank to the lower part of the reaction tower by the pump, and is supplied from the upper part of the reaction tower to the tank via the reflux pipe. Reflux. The tellurium in the solution reacts with the filler when flowing in the reaction tower to produce a reaction product,
This reaction product is carried to the tank along the flow of the solution,
It settles in the tank and is discharged from the drain.

As described above, since the solution is supplied to the reaction tower by the pump and refluxed to the tank, the contact efficiency between the solution and the filler is improved, and the tellurium concentration in the solution is reduced to a predetermined value or less. The reaction time until becoming shorter. Therefore, the amount of treatment within a predetermined time is improved, and it is not necessary to send the solution to a wastewater treatment plant, so that tellurium can be recovered without waste.

According to the tellurium recovery apparatus of the present invention, tellurium in the solution reacts with copper pieces to produce copper telluride as a reaction product. It is carried to and settles. Here, since the temperature of the solution supplied to the reaction tower is maintained at 80 ° C. or higher, copper telluride generated on the surface of the copper piece is spontaneously exfoliated. The flow rate of the solution flowing in the reaction tower is 3.7 cm / sec.
As described above, since the sedimentation velocity of the generated and spontaneously separated copper telluride particles is increased, the copper telluride is conveyed to the tank without accumulating in the reaction tower.

According to the tellurium recovery apparatus of the third aspect of the present invention, the bulk specific gravity of the packing is set to 1 or more.
A gap larger than the reaction product generated between the packings is formed, and the reaction product is not clogged between the packings,
The reaction products are smoothly carried from the reaction tower to the tank, and settle in the tank.

[0012]

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a perspective view of a tellurium collecting apparatus according to an embodiment of the present invention;

As shown in FIG. 1, a cylindrical reaction tower main body 1 is provided.
A reaction tower 3 filled with copper pieces (filler) 2 for reacting with tellurium in the liquid after leaching to produce copper telluride (reaction product), and a tank 4 for storing a liquid 5 after leaching. A supply pipe 6 for communicating the tank 4 with the lower part of the reaction tower 3, a pump 7 provided at an inlet of the supply pipe 6, for feeding a liquid leached from the tank 4 to the reaction tower 3, and an upper part of the reaction tower 3. ether and communicates the tank 4, the leaching solution after 5 overflowing from the reactor 3
There is provided a reflux pipe 8 for refluxing to the tank together with copper halide, and a drain 9 for discharging copper telluride precipitated in the tank 4.

The inner diameter of the reaction tower body 1 is 600 mm. Inside the reaction tower body 1, a copper piece 2 having a length of 405 mm, a width of 21 mm and a plate thickness of 1.1 mm is bent to a height of 4 mm.
m and a bulk specific gravity of 0.6 TON / cubic meter. If laminated so that the bulk specific gravity becomes 1 or less, the shape and dimensions of the copper pieces 2 can be appropriately selected. This is because it is necessary to ensure a sufficient porosity so that copper telluride generated by reacting with the copper pieces 2 does not clog the gaps between the copper pieces 2.

The discharge flow rate of the liquid 5 after leaching by the pump 7 is
Post-leaching liquid 5 flowing between copper pieces 2 in the reaction tower body 1
Is set to be 3.7 cm / sec or more, and preferably set to be 6 cm / sec or more. This is because the leaching solution 5 and the copper pieces 2
The particle size of copper telluride produced by the reaction with was measured using a laser diffraction type particle size distribution analyzer.
100% of the particles have a size of 0 micrometer or less.
When the sedimentation velocity of the particles of 0 micrometer is determined by Allen's equation, the sedimentation velocity is about 3.7 cm / sec, and the generated copper telluride is flushed into the tank 4 before sedimentation in the reaction tower 3. It is necessary.

The temperature of the leached liquid 5 in the tank 4 is set by a temperature adjusting means (not shown) so that the liquid temperature is 80 ° C. or higher (90 ° C. in the embodiment). This is 8
At 0 ° C. or lower, copper telluride generated by the reaction between the tellurium in the liquid 5 after leaching and the copper pieces 2 strongly adheres to the surface of the copper pieces 2, and the leaching liquid is simply fed into the reaction tower 3. Alone cannot carry copper telluride to tank 4,
If the temperature is 80 ° C. or higher, the copper telluride generated on the surface of the copper piece 2 will be spontaneously peeled off, and the copper telluride can be transported to the tank 4.

Next, as shown in FIG. 2, a procedure for recovering tellurium using the tellurium recovery apparatus of this embodiment will be described.

Copper electrolytic slime (raw slime) containing Cu-20% and Te-2% is decoppered in a decoppering leaching tank at 80 ° C. at room temperature while blowing air. At this time, 30 to 80% of tellurium in the copper electrolytic slime elutes. Then, the decoppered raw slime is leached with a filter, and separated into a leached liquid and gold-silver slime. Gold and silver slime is transported to a precious metal factory.

The leached liquid 5 is guided and stored in the tank 4. Here, the leached liquid 5 heated to 90 ° C. by driving the pump 7 is supplied to the lower part of the reaction tower 3 via the supply pipe 6. The supply flow rate of the liquid 5 after leaching is 2400
1 / min.

The supplied liquid 5 after leaching rises upward while contacting the copper pieces 2 in the reaction tower 3 and tellurium in the liquid 5 after leaching reacts with the copper pieces 2 to produce copper telluride. Since the temperature of the liquid 5 after leaching is 90 ° C., the copper telluride spontaneously peels off from the surface of the copper piece 2.

Although the copper telluride tends to settle, the flow rate of the liquid 5 after leaching supplied by the pump 7 is higher than the sedimentation speed, as described above, so that the liquid 5 after leaching is not settled. Following the flow, it is carried from the upper part of the reaction tower 3 to the tank 4 via the reflux pipe 8. At this time, copper piece 2
Since the bulk density is set to 1 or less, a gap considerably larger than the copper telluride particles is formed between the copper pieces 2, and the generated copper telluride Without the particles clogging between the copper pieces 2,
After the leaching solution 5 containing the precipitate of copper telluride is passed through the reaction tower 3, it can be smoothly refluxed to the tank 4.

The leached liquid 5 containing the precipitate of copper telluride refluxed in the tank 4 is repeatedly supplied to the reaction tower 3 by the pump 7, and the reaction between the leached liquid 5 and the copper pieces 2 proceeds, and the leaching is performed. The tellurium concentration in the post-liquid 5 gradually decreases, and the amount of the copper telluride precipitate in the tank 4 increases accordingly.

Then, the precipitate is discharged from the drain 9 and separated into a filtrate and copper telluride through a filter.
This filtrate is repeatedly sent to a copper electrolysis step, and is subjected to copper electrolysis. The filtered copper telluride is sent to the next step and recovered as tellurium metal.

FIG. 3 shows the time change of the concentration of tellurium in the leached liquid 5 when the leached liquid 5 is circulated between the reaction tower 3 and the tank 4. This tellurium concentration was measured by sampling the liquid 5 after leaching in the tank 4. In the figure, Co indicates the initial concentration of tellurium in the liquid after leaching, and C indicates the measured tellurium concentration. As shown in FIG. 3, the tellurium concentration was changed from 5 g / l to 100-fold 0.05 g in 16 hours.
/ L.

Table 1 shows the time of the concentration of tellurium in the leached liquid 5 when the leached liquid 5 is circulated between the reaction tower 3 and the tank 4 using the tellurium recovery apparatus of the present embodiment. The change and the time change of the concentration of tellurium in the liquid after leaching when the copper piece and the liquid after leaching are mixed and stirred as in the prior art are compared.

[0026]

[Table 1]

As shown in Table 1, in the present example, the tellurium concentration after 16 hours was 16 minutes less than that of the comparative example, even though the initial concentration was twice that of the comparative example. The concentration is reduced to 0.05 g / l, which is the concentration level at which the filtrate can be reused in 16 hours. In the comparative example, even when the concentration of tellurium was measured after 36 hours, the concentration did not reach the reusable concentration level.

[0028]

As described above, according to the first aspect of the present invention,
The tellurium recovery apparatus according to claim 1, wherein the tellurium recovery apparatus recovers the tellurium from a tellurium-containing solution, the reaction being filled with a filler that reacts with tellurium in the solution to generate a reaction product. A tower, a tank for storing the solution, a pump for feeding the solution from the tank to the lower part of the reaction tower, and a reflux pipe for refluxing the solution overflowing from the upper part of the reaction tower to the tank together with the reaction product. And a drain for discharging the reaction product precipitated in the tank, so that the tellurium-containing solution is supplied from the tank to the lower part of the reaction tower by a pump,
Reflux from the top of the reaction tower to the tank via a reflux pipe, tellurium in the solution reacts with the filler when flowing through the reaction tower to produce a reaction product, and the reaction product flows into the solution flow. To reduce the reaction time by increasing the contact efficiency between the solution containing tellurium and the packing that reacts with tellurium in the solution, and thereby the contact efficiency between the solution containing tellurium and the filler reacting with tellurium in the solution can be increased. Therefore, the throughput of the solution can be improved, and tellurium can be recovered without waste.

According to the tellurium recovery apparatus of the second aspect of the present invention, the filler is made of copper pieces containing copper as a main component, the temperature of the solution supplied to the reaction tower is maintained at 80 ° C. or higher,
Since the flow rate of the solution flowing in the reaction tower is set to 3.7 cm / sec or more, tellurium in the solution reacts with copper pieces to produce copper telluride as a reaction product, and this copper telluride is made of copper. The copper telluride is spontaneously peeled off from the surface of the piece, and the copper telluride can be transported to a tank by a solution flowing in the reaction tower, settled, and recovered.

According to the tellurium recovery apparatus of the third aspect of the present invention, since the bulk specific gravity of the filler is 1 or less,
A gap larger than the reaction product generated between the packings is formed, and the reaction product is not clogged between the packings,
The reaction product can be smoothly carried from the reaction tower to the tank and settled in the tank, and a scrap material having no particular shape can be used as the filler.

[Brief description of the drawings]

FIG. 1 is an overall configuration diagram showing a tellurium recovery apparatus according to one embodiment of the present invention.

FIG. 2 is a process chart showing a tellurium recovery procedure using the tellurium recovery apparatus of FIG.

FIG. 3 is a graph showing a temporal change of tellurium concentration when the tellurium recovery device of FIG. 1 is used.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Reaction tower main body 2 Filler 3 Reaction tower 4 Tank 5 Liquid after leaching 6 Supply piping 7 Pump 8 Reflux piping 9 Drain

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-61-223139 (JP, A) JP-A-57-88010 (JP, A) JP-A-61-227906 (JP, A) 35106 (JP, U) (58) Field surveyed (Int. Cl. ⁷ , DB name) C22B 61/00

Claims (3)

(57) [Claims] 1. A tellurium recovery device for recovering tellurium from a tellurium-containing solution, comprising: a reaction tower filled with a filler that reacts with tellurium in the solution to generate a reaction product; A tank for storing the solution, a pump for feeding the solution from the tank to the lower part of the reaction tower, and a solution that overflows from the upper part of the reaction tower to the reaction product.
And a drain for discharging the reaction products settled in the tank. 2. The filler is made of copper pieces containing copper as a main component, the temperature of the solution supplied to the reaction tower is maintained at 80 ° C. or higher, and the flow rate of the solution flowing in the reaction tower is 3.7 cm / sec.
2. The tellurium recovery device according to claim 1, wherein the number is c or more. 3. The tellurium recovery device according to claim 1, wherein the bulk specific gravity of the filler is 1 or less.