KR101447493B1 - Multiple extraction apparatus and recovery method of indium using the apparatus - Google Patents

Abstract

The present invention includes a plurality of extraction stages, a plurality of cleaning stages, and a plurality of back extraction stages arranged in sequence, wherein each of one extraction stage, one cleaning stage, and one back extraction stage is a mixing tank, Wherein the mixing tank at the first stage in the extraction stage, the cleaning stage and the back extraction stage are positioned adjacent to the second stage discharge tank, and the mixing tank in the second stage is positioned adjacent to the exhaust tank in the first stage And the mixing tank is connected to the discharging tank of the previous stage through the conduit and is connected to the tank tank of the next stage through another conduit, and the tank is provided with a passage through which the organic tank and the water tank are separated, The discharge port is provided at the lower portion and the discharge port is connected to the mixing tank at the previous stage and the discharge tank is connected to the mixing tank at the next stage through the conduit It relates to a multi-stage extraction apparatus and an indium recovering method using the same that. According to the present invention, tin (Sn) other than indium (In) is selectively extracted and removed from an indium-containing material containing indium (In) and tin (Sn) in a short period of time to selectively recover indium (In) Of indium (In) can be easily obtained.

Description

[0001] The present invention relates to a multi-stage extraction apparatus and an indium recovery method using the same,

The present invention relates to an extraction apparatus and an indium recovery method, and more particularly, to a multi-stage extraction apparatus capable of efficiently recovering indium (In) from an indium dissolution solution containing indium (In) and tin (Sn) And a method for recovering indium.

Most of indium is indium tin oxide (ITO) and is used for transparent conductive film. It occupies about 70% of the whole indium market and it reaches 80% when it is regenerated.

On the other hand, in the flat panel display (FPD) industry in which a transparent conductive film is used, there is a great increase in the demand for thin-type large-sized televisions as well as computer liquid-crystal display devices. In addition, as the European Union (EU) strengthens lead regulations, the demand for lead-free solder consisting of low melting point alloys including indium is expected to increase and demand will increase.

In line with this market trend, indium prices are showing a tendency to increase, and at the same time, there is a possibility that a contest will take place in order to secure raw materials.

Due to this background, the atmosphere for regeneration of indium is spreading, and the regeneration of indium is not a simple environmental technology but a material recovery technology having significant economical efficiency.

In addition, in the case of indium, there is no main ore that can be extracted, and it has been produced industrially by recovering by-products of zinc smelting or by-products of lead smelting, especially indium concentrated in soot.

In order to recover high purity indium, the equipment is complicated and the process is complicated. Accordingly, there is a need for an economical and simple means or method for producing high purity indium, preferably a method capable of selectively removing tin except for indium in a short time and selectively recovering indium.

A problem to be solved by the present invention is to selectively extract and remove indium (In) from indium containing material containing indium (In) and tin (Sn) in a short period of time, Which can recover indium (In) of high purity, and an indium recovery method using the same.

The present invention includes a plurality of extraction stages, a plurality of cleaning stages, and a plurality of back extraction stages arranged in sequence, wherein each of one extraction stage, one cleaning stage, and one back extraction stage is a mixing tank, Wherein the mixing tank at the first stage in the extraction stage, the cleaning stage and the back extraction stage are positioned adjacent to the second stage discharge tank, and the mixing tank in the second stage is positioned adjacent to the exhaust tank in the first stage And the mixing tank is connected to the discharging tank of the previous stage through the conduit and is connected to the tank tank of the next stage through another conduit, and the tank is provided with a passage through which the organic tank and the water tank are separated, A discharge port is provided at the lower portion and the discharge port is connected to the mixing tank at the previous stage and the discharge tank is connected to the mixing tank at the next stage through the conduit, The solution mixed in the mixing tank is moved to the settling tank, and the settling tank provides a space separated by the organic phase and the water phase. The mixed solution is separated into the organic phase and the water phase while staying in the settling tank. Wherein the organic phase is small in specific gravity compared with the water phase and is transported to the discharge tank, and the water phase is moved to the mixing tank of the previous stage through the discharge port provided at one side of the bottom of the tank.

The mixing chamber and the settling chamber are separated by a first separating wall having a height higher than a virtual horizontal line separating the water phase separated from the organic phase and the second separating wall, Wherein the second separation wall is formed to have a higher height than a virtual horizontal line separating the water phase separated from the organic phase and the second separation wall is formed at a lower height than the first separation wall .

The mixing tank is provided with an impeller, which is agitated in the mixing tank by the impeller, the impeller rotates at a speed of 100 to 500 rpm, and the impeller rotates the organic phase And the water phase is introduced through the conduit in the next stage of the tank. The organic phase introduced from the discharge tank of the previous stage by the rotation of the impeller is mixed with the water stream introduced from the next stage tank.

The multi-stage extracting apparatus may further include an indium dissolution liquid supply unit, an organic solvent supply unit, a cleaning acid solution supply unit, and a back extract liquid supply unit. The indium dissolution liquid supply unit supplies indium (In) And the tin (Sn), and the organic solvent supply unit supplies the organic solvent to the mixing tank of the first extraction stage through the pump, and the cleaning acid solution supply unit supplies the organic solvent through the pump P3 to the last cleaning And the reverse extract supply unit can supply the reverse extract to the mixing tank of the last reverse extraction stage through the pump.

Wherein the concentration of the acid solution supplied through the cleansing acid solution supply unit is in the range of 0.5 to 5M and the back extract liquid supplied through the back extract liquid supply unit is the acid solution, The organic solvent may be at least one selected from an alkyl monocarboxylic acid, tributyl phosphate, 2-ethylhexyl 2-ethylhexyl phosphate and di- (2-ethylhexyl) phosphate, And the amount of the acid solution supplied from the cleaning acid solution supply part is in the range of 1: 1 to 5: 1.

The organic phase transferred to the discharge tank of the last reverse extraction stage is recycled to be supplied to the organic solvent supply section. First, the reverse extraction solution which is submerged in the lower tank of the reverse extraction stage, The first indium solution, which is located in the lower part of the settling zone of the extraction stage, is configured to be discharged to the outside through a discharge port provided at the lower part of the first stage of the extraction stage desirable.

Further, the present invention is characterized by comprising a plurality of extraction stages, a plurality of cleaning stages, and a plurality of back extraction stages arranged in sequence, wherein each of the one extraction stage, the one cleaning stage, Wherein the mixing stage of the first stage in the extraction stage, the cleaning stage and the back extraction stage is located adjacent to the second stage stage of the discharge vessel and the second stage mixing vessel is positioned adjacent to the first stage stage discharge vessel And the mixing tank is connected to the discharge tank of the previous stage through the conduit and is connected to the next stage tank tank through another conduit and the tank is divided into the organic tank and the water storage tank, And the discharge port is connected to the mixing tank of the previous stage and the discharge tank is connected to the mixing tank of the next stage through the conduit, And an indium dissolution liquid containing indium (In) and tin (Sn) is supplied through a pump to the mixing tank of the last extraction stage, and the organic solvent supply unit supplies the indium dissolution liquid containing the first extraction stage The acid solution supply unit supplies the acid solution to the mixing tank of the last cleaning stage via the pump and the reverse extract supply unit supplies the reverse extract liquid to the mixing tank of the last reverse extraction stage through the pump, The solution in which the solution is mixed in the tank and mixed in the mixing tank is moved to the settling tank and the solution moved to the settling tank is phase separated into the water phase and the organic phase while staying in the settling tank. And the water phase is moved to the mixing tank of the previous stage through the discharge port provided on the lower side of the bottom of the tank, And the organic phase supplied to the discharge tank of the last reverse extraction stage is supplied to the organic solvent supply source. The first reverse extraction stage, which is submerged in the lower tank of the reverse extraction stage, The indium liquid, which is the water-soluble indium liquid which is trapped in the bottom of the first extraction stage, is discharged to the outside through the discharge port provided at the lower side of the first side of the extraction stage And is discharged and collected.

Wherein the concentration of the acid solution supplied through the cleansing acid solution supply unit is in the range of 0.5 to 5M and the back extract liquid supplied through the back extract liquid supply unit is the acid solution, The organic solvent may be at least one selected from an alkyl monocarboxylic acid, tributyl phosphate, 2-ethylhexyl 2-ethylhexyl phosphate and di- (2-ethylhexyl) phosphate, And the acid solution supplied from the cleaning acid solution supply part is in the range of 1: 1 to 5: 1.

The mixing chamber and the settling chamber are separated by a first separating wall having a height higher than a virtual horizontal line separating the water phase separated from the organic phase and the second separating wall, Wherein the second separation wall is formed to have a higher height than a virtual horizontal line separating the water phase separated from the organic phase and the second separation wall is formed at a lower height than the first separation wall .

The mixing tank is provided with an impeller, which is agitated in the mixing tank by the impeller, the impeller rotates at a speed of 100 to 500 rpm, and the impeller rotates the organic phase And the water phase is introduced through the conduit in the next stage of the tank, and the organic phase introduced from the discharge vessel of the previous stage by the rotation of the impeller can be mixed with the water stream introduced from the next stage tank.

The indium dissolution liquid is obtained by a method comprising the steps of pulverizing an indium-tin oxide scrap, dissolving the pulverized product in an acid to obtain an acid solution containing indium and tin, filtering the acid solution, And supplying the solution to the indium solution supply part.

According to the present invention, tin excluding indium can be selectively extracted and removed from an indium-containing material containing indium and tin in a short time, and indium can be selectively recovered to easily obtain indium of high purity.

Since indium (In) contained in indium-tin oxide can be selectively recovered and recycled, environmental pollution can be prevented, resources can be recycled, resources can be saved, and indium can be effectively recovered in a short period of time at a low process cost .

1 is a schematic view of a multi-stage extraction apparatus according to a preferred embodiment of the present invention.
FIG. 2 is a view schematically showing a mixing tank, a settling tank and a draining tank of an extracting stage, a washing stage and a backward extraction stage.
Fig. 3 is a view showing a multi-stage extraction apparatus used in Embodiment 1. Fig.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, it should be understood that the following embodiments are provided so that those skilled in the art will be able to fully understand the present invention, and that various modifications may be made without departing from the scope of the present invention. It is not. Wherein like reference numerals refer to like elements throughout.

In the present invention, tin (Sn) excluding indium (In) is selectively extracted and removed from an indium-containing material containing indium (In) and tin (Sn) in a short period of time to selectively recover indium (In) A multi-stage extraction apparatus capable of easily obtaining indium (In) and an indium recovery method using the same are presented.

The indium-tin oxide is collected as the indium-containing material. The indium-tin oxide may be a scrap of an ITO target (hereinafter referred to as " ITO waste scrap ") which has been used for manufacturing a flat panel display electrode or the like and has reached the end of its life. The ITO waste scrap contains indium (In) and tin (Sn) in a high content. INDUSTRIAL APPLICABILITY The indium recovery method of the present invention can be applied to a case where indium (Sn) is contained in a small amount (for example, 1 to 10 wt%) of indium-tin oxide (ITO scrap) There is an advantage that not only ITO waste scrap but also a substance containing a small amount of indium in the manufacturing process using ITO target material can be used.

The collected indium-tin oxide can be pulverized or classified. The pulverization may use ball milling, and the classification may use a sieve. The pulverizing step and the classifying step can be used together. It goes without saying that the pulverizing step may be followed by the classifying step.

First, the grinding process will be described. It is charged into a ball milling machine to be crushed and mixed with a solvent such as ethanol. The indium-tin oxide is mechanically pulverized by rotating it at a constant speed using a ball milling machine. The ball used for ball milling is preferably a ball of ceramic material such as alumina or zirconia having high hardness, and the balls may be all the same size or may be used together with balls having two or more sizes. The size of the balls, the milling time, and the rotation speed per minute of the ball miller are adjusted so as to be crushed to the target particle size. For example, in consideration of the size of the particles, the size of the balls is set in the range of about 1 mm to 50 mm, and the rotational speed of the ball miller is set in the range of about 10 to 500 rpm. The ball milling is carried out for 1 to 48 hours in consideration of the target particle size and the like. By ball milling, the indium-tin oxide is pulverized into fine-sized particles.

In the classification process, a sieve having a mesh of a desired size is used. Since the indium-tin oxide may be aggregated, the particles larger than a certain size may be sieved to selectively separate indium-tin oxide having a particle size smaller than a predetermined size.

The indium-tin oxide is dissolved in an acid to form an acid solution. When indium-tin oxide is added to the acid, indium and tin, which are the main constituents of indium-tin oxide (ITO), are dissolved in the acid.

The acid is preferably at least one selected from hydrochloric acid (HCl) and sulfuric acid (H ₂ SO ₄ ), more preferably hydrochloric acid (HCl). At this time, it is preferable that the acid concentration of the dissolution liquid is about 1M to 3M, and when the concentration of the acid solution is in the above range, dissolution of the indium-tin oxide can be facilitated and the amount of residue after dissolution can be minimized , The recovery rate of indium is improved in the subsequent process and the separation rate with respect to the impurities is increased.

Hereinafter, a method of selectively recovering indium (In) from an indium dissolution solution containing a large amount of indium (In) through filtration using a filter and passing through a filter will be described.

The acid concentration of the indium dissolution solution can be adjusted by adding an acid or an alkali to the indium purification process using a subsequent organic solvent. At this time, it is preferable to use at least one substance selected from hydrochloric acid (HCl) and sulfuric acid (H ₂ SO ₄ ) to control the acid concentration of the indium dissolution solution, more preferably hydrochloric acid (HCl) do. There may be added an alkali to adjust the high acid concentration, sodium hydroxide (NaOH), ammonium hydroxide (NH ₄ OH), potassium hydroxide (KOH), sodium carbonate (Na ₂ CO ₃₎ and potassium carbonate (K ₂ CO ₃₎ And the like. The acid concentration of the indium dissolution solution is preferably about 1 to 3 M in consideration of the tin extraction process using a subsequent organic solvent.

In order to recover high purity indium from the indium dissolution solution, tin (Sn) is extracted using an organic solvent, and extraction of tin (Sn) with an organic solvent is performed using a multi-stage extraction apparatus as shown in FIG. use. 1 is a schematic view of a multi-stage extraction apparatus according to a preferred embodiment of the present invention. FIG. 2 is a view schematically showing a mixing tank, a settling tank and a draining tank of an extracting stage, a washing stage and a backward extraction stage.

1 and 2, the multi-stage extraction apparatus includes a plurality of extraction stages A1, A2, and A3 sequentially arranged, a plurality of cleaning stages B1, B2, and B3, and a plurality of back extraction stages C1 and C2 , C3). In FIG. 1, three extraction stages A1, A2, and A3, three cleaning stages B1, B2, and B3, and three reverse extraction stages C1, C2, and C3 are shown. For example, six or more extraction stages are possible, and five or more cleaning stages and reverse extraction stages are possible.

In the following description, a multi-stage extraction device including a plurality of extraction stages A1, A2, and A3, a plurality of cleaning stages B1, B2, and B3, and a plurality of back extraction stages C1, Will be described.

The extraction stages A 1, A 2 and A 3 are provided with a mixing tank 110, a settling tank 120 and a discharge tank 130 and are provided with one mixing tank 110, one settling tank 120, The jaw 130 constitutes one extraction end. The mixing tank 110 of the first extraction stage A1 in the extraction stages A1, A2 and A3 is positioned adjacent to the discharge tank 130 of the second extraction stage A2 and the mixing tank 110 of the second extraction stage A2 130 may be disposed adjacent to the mixing chamber 110 of the first extraction stage A1 repeatedly.

The cleaning stages B1, B2 and B3 are provided with a mixing tank 110, a settling tank 120 and a discharging tank 130 and are provided with a mixing tank 110, a settling tank 120, The discharge chamber 130 of the cleaning unit 130 constitutes one cleaning stage. The mixing chamber 110 of the first cleaning stage B1 in the cleaning stages B1, B2 and B3 is located adjacent to the discharge tank 130 of the second cleaning stage B2 and the mixing tank 110 of the second cleaning stage B2 130 may be disposed adjacent to the mixing chamber 110 of the first cleaning stage B1 repeatedly.

The back extraction stages C1, C2, and C3 include a mixing tank 110, a settling tank 120, and a discharge tank 130, and are provided with one mixing tank 110, one settling tank 120, One discharge chamber 130 constitutes one back extraction stage. The mixing tank 110 of the first reverse extraction stage C1 in the reverse extraction stages C1, C2 and C3 is provided adjacent to the discharge tank 130 of the second reverse extraction stage C2, It is preferable that the discharge chamber 130 of the first back extraction stage C1 is positioned adjacent to the mixing chamber 110 of the back extraction stage C1.

The mixing tank 110 is a region where the solution is mixed, and the solution mixed in the mixing tank 110 is provided to be moved to the settling tank 120.

The mixed solution in the mixing tank 110 is moved to the settling tank 120 and the mixed solution is supplied to the settling tank 120. The mixed tank 110 is filled with the solution, And is separated from the organic phase and the water phase while being kept stationary for a predetermined time. The organic phase is transferred to the discharge tank 130 and the water phase is supplied to the mixing tank 130 through the discharge port 122 provided at one side of the lower side of the settling tank 120, 110). The discharge port 122 of the settling tank 120 is connected to the mixing tank 110 of the previous stage.

The discharge vessel 130 of each stage is connected to the mixing vessel 110 of the next stage through a conduit 132. And a discharge port connected to the conduit 132 for discharging the organic phase.

The mixing vessel 110 at each stage is connected to the discharge vessel 130 at the previous stage through the conduit 132 and is connected to the settling vessel 120 at the next stage through the conduit 112. A lower portion of the mixing chamber 110 is provided with an inlet connected to the conduit 132 for introducing the organic phase and has an inlet connected to the conduit 112 for introducing water into the lower portion of the basin 120 . The mixing chamber 110 is provided with an impeller 114 and may be stirred in the mixing chamber 110 by the impeller 114. The stirring may be performed at a speed of 100 to 500 rpm using an impeller 114. The rotation of the impeller 114 causes the organic phase to flow in the discharge vessel 130 of the previous stage through the conduit 132 and the aqua to flow into the settling vessel 120 at the next stage, The organic phase introduced from the discharge vessel 130 in the previous stage is mixed with the water entering from the next settling tank 120 and the mixed solution is transferred to the settling tank 120.

The discharge port 122 is provided in the settling chamber 120 in the extraction tanks A1, A2, A3, the cleaning stages B1, B2, B3 and the back extraction stages C1, C2, . The organic phase and the water phase are separated from each other by the specific gravity difference in the settling tank 120. The water phase having a large specific gravity is located at the lower portion and thus the exhaust port 122 provided at the lower portion of the settling tank 120 can be discharged .

The mixing chamber 110 and the settling chamber 120 are separated by the first separating wall 140 and the first separating wall 140 is formed to have a higher height than the virtual horizontal line 150 separating the water phase from the organic phase do.

In addition, the settling tank 120 and the discharge tank 130 are separated by the second separation wall 145 and the second separation wall 145 has a height higher than the virtual horizontal line 150 separating the water phase and the organic phase Respectively.

Further, it is preferable that the second separating wall 145 has a lower height than the first separating wall 140.

The indium solution supplying part G serves to store the indium dissolution solution and when the indium is to be recovered by using the organic solvent, the indium dissolution solution G is supplied to the mixing bath 110 of the last extraction stage A3 through the pump P1 And supplies the liquid.

In order to extract Sn from the organic solvent, the organic solvent supply part D serves to store the organic solvent. When the tin Sn is extracted using the organic solvent, the organic solvent supply part D may be connected to the mixing tank 110 of the first extraction stage A1 through the pump P2. And serves to supply a solvent.

The cleaning acid solution supply part F serves to store the acid solution and serves to supply the cleaning acid solution to the mixing bath 110 of the final cleaning stage B3 through the pump P3 . At this time, the concentration of the cleaning acid solution supplied through the cleaning acid solution supply part (F) is preferably about 0.5 to 5 M. When the concentration of the cleaning acid solution is less than 0.5 M, the cleaning effect is insufficient, When the concentration of the acid solution exceeds 5M, it is difficult to expect a further cleaning effect, which is not economical.

The reverse extract liquid supply unit E serves to store the reverse extract liquid and serves to supply the reverse extract liquid to the mixing tank 110 of the last reverse extraction stage C3 through the pump P4. At this time, the back extract liquid supplied through the reverse extract liquid supplier (E) is an acid solution, and the concentration of the acid solution of the back extract liquid is preferably about 5 to 12 M. When the concentration of the acid solution of the back extract liquid is less than 5 M, And the concentration of the acid solution of the reverse extract is more than 12M, it is not economical.

The organic phase supplied to the discharge tank 130 of the last reverse extraction stage C3 may be supplied to the organic solvent supply unit D and recycled.

First, the reverse extract which is the water that is submerged in the lower part of the settling tank 120 of the reverse extraction stage C1 is discharged to the outside through the discharge port 122 provided at the lower side of the one side of the settling tank 120 of the reverse extraction stage C1 Out2).

The purified indium solution which is the water which is seated on the bottom of the settling tank 120 of the first extraction stage A1 is discharged to the outside through the discharge port 122 provided at the lower side of the first side of the settling tank 120 of the extraction stage A1 Out1) is discharged and collected.

In order to separate, remove and purify tin (Sn) contained in the indium dissolution solution from indium (In), an organic solvent which extracts tin (Sn) is used in the indium dissolution solution.

The organic solvent used in the step of extracting tin (Sn) is preferably a carboxylic acid type, an organic phosphoric acid type or a mixture thereof. For example, as the organic solvent, alkyl monocarboxylic acid, neodecanoic acid, tributyl phosphate (TBP), 2-ethylhexyl 2-ethylhexyl phosphate phosphoric acid (PC88A) or di- (2-ethylhexyl) phosphoric acid (D2EHPA).

When the organic solvent is mixed with the indium dissolution solution, tin (Sn) is extracted into the organic solvent and separated into an organic phase containing tin (Sn) and an aqueous phase containing indium (In) Separation of tin (Sn) is possible. The organic phase is separated and separated from the acidic aqueous phase, tin (Sn) is extracted and contained in the organic phase, and indium (In) is included in the aqueous phase. This can be used to separate the water phase present in the lower part of the organic phase.

The volume ratio of the organic solvent supplied from the organic solvent supply unit and the acid solution supplied from the supply source for the cleansing acid solution is preferably from 1: 1 to 5: 1 as the volume ratio (organic phase: water phase) of the organic phase to the aqueous phase, 3: 1. When the volume ratio of the organic phase to the water phase (organic phase / water phase) is less than 1, the effect of extracting tin (Sn) by the organic solvent is weak, and when the volume ratio (organic phase / water phase) Can not do it.

The step of extracting tin (Sn) using an organic solvent is preferably carried out at 20 ° C to 80 ° C in consideration of extraction rate and energy consumption.

Hereinafter, a method of extracting tin (Sn) using the multi-stage extraction apparatus shown in FIG. 1 will be described in detail.

The impeller 114 provided in each mixing tank 110 is operated to mix the solution in the mixing tank 110 while the impeller 114 is rotated.

The cleaning acid solution supply portion F supplies the cleaning acid solution to the mixing bath 110 of the cleaning stage B3 through the pump P3. The cleaning acid solution supplied to the mixing tank 110 of the cleaning stage B3 is transferred to the settling tank 120 of the cleaning stage B3 and is sent to the settling tank 120 of the cleaning stage B3 Since the acid solution is acidic, it sinks to the bottom and flows through the conduit 112 connected to the discharge port 122 provided at the bottom of one side of the settling tank 120 of the washing stage B3, And the cleaning acid solution flowing into the mixing tank 110 of the cleaning stage B2 is transferred to the settling tank 120 of the cleaning stage B2, The cleaning acid solution transferred to the settling tank 120 of the washing tank B2 is connected to the discharge port 122 provided at the bottom of one side of the settling tank 120 of the washing tank B2, And flows into the mixing chamber 110 of the cleaning stage B1 through the conduit 112. [

The cleaning acid solution flowing into the mixing tank 110 of the cleaning stage B1 is mixed with the organic phase introduced through the conduit 132 from the discharge tank 130 of the extraction stage A3, The solution mixed in the mixing tank 110 of the cleaning tank B1 is transferred to the settling tank 120 of the cleaning tank B1. When the organic phase and the cleansing acid solution are mixed, indium (In) remaining in the organic solvent, which is an organic phase, is back extracted from the mixing bath 110 of the cleaning stage B1 to be an organic phase with indium (In) In the settling tank 120 of the washing stage (B1), the organic phase is separated from the aqueous phase, and indium (In) is included in the aqueous phase.

The water containing indium (In) in the settling tank 120 of the washing stage B1 sinks downward and is connected to the discharge port 122 provided at the lower side of the one side of the settling tank 120 of the washing stage B1 The organic phase containing tin Sn in the settling tank 120 of the washing stage B1 flows into the mixing tank 110 of the extraction stage A3 through the conduit 112 where the cleaning stage B1 The organic phase transferred to the tank 130 and transferred to the discharge tank 130 of the cleaning stage B1 flows into the mixing tank 110 of the cleaning stage B2 through the conduit 132. [

The organic phase introduced into the mixing tank 110 of the cleaning stage B2 is mixed with the acid solution for cleaning which is the water phase introduced through the conduit 112 from the settling tank 120 of the cleaning stage B3, B2 is fed to the settling tank 120 of the washing stage B2. When the organic phase and the cleansing acid solution are mixed, indium (In) remaining in the organic solvent, which is an organic phase, is back extracted from the mixing bath 110 of the cleansing stage B2 to form an organic phase containing indium (In) In the settling tank 120 of the washing stage (B2), the organic phase is separated from the aqueous phase, and indium (In) is included in the aqueous phase.

In the settling chamber 120 of the washing stage B2, the water containing indium (In) sinks downward and is connected to the discharge port 122 provided at a lower side of one side of the settling tank 120 of the washing stage B2 The organic phase containing tin Sn in the settling tank 120 of the washing stage B2 flows into the mixing tank 110 of the washing stage B1 through the conduit 112 in which the washing stage B2 is discharged And the organic phase transferred to the discharge tank 130 of the cleaning stage B2 flows into the mixing tank 110 of the cleaning stage B3 through the conduit 132. [

The organic phase flowing into the mixing tank 110 of the cleaning stage B3 is mixed with the acid solution for cleaning supplied through the cleaning acid solution supply part F and mixed in the mixing tank 110 of the cleaning stage B3, Is transferred to the settling tank 120 of the cleaning stage B3. When the organic phase and the cleansing acid solution are mixed, indium (In) remaining by the organic solvent is back extracted in the mixing bath 110 of the cleaning stage B3 to be an organic phase containing indium (In) All the indium (In) remaining in the organic phase is back-extracted with aqueous acid solution for cleaning. In the settling tank 120 of the cleaning stage B3, the organic phase is separated from the aqueous phase, (In) will be included in the water.

The water containing indium (In) in the settling tank 120 of the washing stage B3 sinks to the bottom and is connected to the drain port 122 provided at the bottom of one side of the settling tank 120 of the washing stage B3 And the organic phase containing tin (Sn) in the settling tank 120 of the washing stage B3 flows into the mixing tank 110 of the washing stage B2 through the conduit 112 where the washing stage B3 is discharged The organic phase transferred to the tank 130 and transferred to the discharge tank 130 of the cleaning stage B3 flows into the mixing tank 110 of the back extraction stage C1 through the conduit 132. [

The back extract liquid supply unit E supplies the back extract liquid to the mixing tank 110 of the back extraction stage C3 through the pump P4. The back extraction liquid supplied to the mixing tank 110 of the back extraction stage C3 is transferred to the settling tank 120 of the back extraction stage C3 and then transferred to the stationary stage 120 of the back extraction stage C3 The extracted liquid flows into the mixing chamber 110 of the backward extraction stage C2 through the conduit 112 connected to the discharge port 122 provided at the lower side of the fixed tank 120 of the backward extraction stage C3, The back extraction liquid introduced into the mixing tank 110 of the back extraction stage C2 is transferred to the settling tank 120 of the back extraction stage C2 and is then transferred to the stationary stage 120 of the back extraction stage C2 The extracted liquid is introduced into the mixing chamber 110 of the back extraction stage C1 via the conduit 112 connected to the discharge port 122 provided at the lower side of the fixed tank 120 of the backward extraction stage C2.

The organic phase transferred to the discharge tank 130 of the cleaning stage B3 and the back extraction liquid introduced from the settling tank 120 of the back extraction stage C2 are mixed in the mixing tank 110 of the back extraction stage C1 The solution mixed in the mixing tank 110 of the back extraction stage C1 is transferred to the settling tank 120 of the back extraction stage C1. When the organic phase and the acidic reverse extract are mixed, tin (Sn) extracted in the organic solvent in the organic solvent is back extracted in the mixing tank 110 of the back extraction stage (C1) to form an aqueous phase containing tin In the settling tank 120 of the back extraction stage C1, the organic phase is separated from the aqueous phase, and the tin (Sn) is back extracted and included in the water phase.

The water containing tin (Sn) in the settling tank 120 of the back extraction stage C1 sinks downward and is discharged through the discharge port 122 provided at the bottom of one side of the settling tank 120 of the back extraction stage C1 And the organic phase is transferred to the discharge tank 130 of the backward extraction stage C1 at the settling stage 120 of the backward extraction stage C1 and is discharged through the conduit 112 connected to the backward extraction stage C1, The organic phase transferred to the discharge tank 130 of the first condenser C1 flows into the mixing chamber 110 of the back extraction stage C2 through the conduit 132. [

The organic phase introduced into the mixing tank 110 of the reverse extraction stage C2 is mixed with the reverse extraction liquid that has flowed through the conduit 112 from the settling tank 120 of the reverse extraction stage C3, The mixed solution in the mixing tank 110 of the second recovery unit C2 is transferred to the settling tank 120 of the reverse extraction stage C2. When the organic phase and the acid solution are mixed, tin (Sn) remaining in the organic solvent as an organic phase is back-extracted in the mixing tank 110 of the reverse extraction stage (C2) to form an organic phase with the aqueous phase containing tin In the settling tank 120 of the extraction stage C2, the organic phase is separated from the aqueous phase, and the tin (Sn) is back extracted and contained in the water phase.

The water containing tin (Sn) in the settling tank 120 of the back extraction stage C2 is submerged to the bottom and is discharged through the discharge port 122 provided at a lower side of the settling tank 120 of the back extraction stage C2 The organic phase remaining in the settling tank 120 of the backward extraction stage C2 flows into the mixing tank 110 of the backward extraction stage C1 through the connected conduit 112 and is discharged The organic phase transferred to the tank 130 and transferred to the discharge tank 130 of the backward extraction stage C2 flows into the mixing tank 110 of the backward extraction stage C3 through the conduit 132. [

The organic phase introduced into the mixing tank 110 of the reverse extraction stage C3 is mixed with the reverse extraction liquid supplied through the reverse extraction liquid supply unit E and mixed in the mixing tank 110 of the reverse extraction stage C3. The solution is transferred to the settling tank 120 of the back extraction stage C3. When the organic phase and the acid solution are mixed, tin (Sn) remaining in the organic solvent as the organic phase is back-extracted in the mixing tank (110) of the back extraction stage (C3) to remove both tin and water- The organic phase is separated from the aqueous phase, and the tin (Sn) is back extracted and contained in the water phase.

The water containing tin (Sn) in the settling tank (120) of the back extraction stage (C3) sinks to the bottom and is discharged through the discharge port (122) provided at the lower side of one side of the settling tank (120) The organic phase is introduced into the mixing tank 110 of the back extraction stage C2 through the connected conduit 112 and the organic phase in the settling tank 120 of the back extraction stage C3 is discharged into the discharge tank 130 and the organic phase transferred to the discharge tank 130 of the reverse extraction stage C3 is supplied to the organic solvent supply unit D through the conduit 132 and recycled.

The organic solvent supply unit D supplies the organic solvent to the mixing tank 110 of the extraction stage A1 through the pump P2. The organic solvent supplied to the mixing tank 110 of the extraction stage A1 is transferred to the discharge tank 130 through the settling tank 120 of the extraction stage A1 and discharged to the discharge tank 130 of the extraction stage A1, Is introduced into the mixing chamber 110 of the extraction stage A2 through the conduit 132. [ The organic solvent supplied to the mixing tank 110 of the extraction stage A2 is transferred to the discharge tank 130 through the settling tank 120 of the extraction stage A2 and discharged to the discharge tank 130 of the extraction stage A2, Is introduced into the mixing chamber 110 of the extraction end A3 through the conduit 132. [

The indium solution supply part G supplies the indium solution to the mixing bath 110 of the extraction end A3 through the pump P1.

The acid solution in the settling tank 120 of the washing stage B1 is discharged through the conduit 112 connected to the discharge port 122 provided at one side of the lower side of the settling tank 120 of the washing stage B1, (A3).

The solution in which the indolol solution, the organic solvent and the cleansing acid solution are mixed in the mixing tank 110 of the extraction stage A3 and the solution mixed in the mixing tank 110 is mixed with the solution in the settling tank 120 of the extraction stage A3, . When the indium solution, the organic solvent, and the acid solution for cleaning are mixed, tin is extracted by the organic solvent to form an organic phase containing an aqueous phase containing indium (In) and tin, 120) is phase-separated into an aqueous phase containing indium (In) and an organic phase containing tin (Sn), and the organic phase is separated from the aqueous phase, and indium (In) .

The organic phase containing tin (Sn) in the settling tank 120 of the extraction stage A3 is transferred to the discharge tank 130 of the extraction stage A3 and is conveyed to the discharge tank 130 of the extraction stage A3, Is introduced into the mixing tank 110 of the cleaning stage B1 through the conduit 132 and separated from the organic phase in the settling tank 120 of the extraction stage A3, Is introduced into the mixing chamber 110 of the extraction stage A2 through the conduit 112 connected to the discharge port 124 provided at one side of the tank 120. [

The organic phase in the discharge vessel 130 of the extraction stage A1 flows into the mixing vessel 110 of the extraction stage A2 via the conduit 132. [

The organic phase and water phase are mixed in the mixing tank 110 of the extraction stage A2 and the mixed solution in the mixing tank 110 is transferred to the settling tank 120 of the extraction stage A2. When the organic phase and the water phase are mixed, tin (Sn) is extracted by an organic solvent in an organic solvent in the settling tank 120 of the extraction stage A2 to form an organic phase containing indium (In) Phase separation, the organic phase is separated from the aqueous phase, and indium (In) is included in the aqueous phase.

The organic phase containing tin (Sn) in the settling tank 120 of the extraction stage A2 is transferred to the discharge tank 130 of the extraction stage A2 and transferred to the discharge tank 130 of the extraction stage A2, Is introduced into the mixing tank 110 of the extraction end A3 through the conduit 132 and separated from the organic phase in the settling tank 120 of the extraction end A2 so that the water present at the bottom is separated from the Is introduced into the mixing chamber 110 of the extraction stage A1 through the conduit 112 connected to the discharge port 122 provided at one side of the tank 120. [

The organic phase introduced through the organic solvent supply unit D and the water phase introduced from the settling tank 120 of the extraction stage A2 are mixed in the mixing tank 110 of the extraction stage A1, The solution mixed in the mixing tank 110 of the extraction stage A1 is transferred to the settling tank 120 of the extraction stage A1. When the organic phase and the water phase are mixed, tin (Sn) is extracted by an organic solvent, which is an organic phase, to be separated into an organic phase containing indium (In) and tin (Sn) The band is separated from the water phase, and indium (In) is included in the water phase.

The organic phase containing tin (Sn) in the settling tank 120 of the extraction stage A1 is conveyed to the discharge tank 130 of the extraction stage A1 and is conveyed to the discharge tank 130 of the extraction stage A1, Is introduced into the mixing tank 110 of the extraction stage A2 through the conduit 132 and separated from the organic phase in the settling tank 120 of the extraction stage A1, And is discharged to the outside through the conduit 112 connected to the discharge port 122 provided at one side of the tank 120. The solution to be discharged to the outside is an indium liquid containing only indium (In) and containing almost no tin (Sn).

Through the above process, the indium solution obtained from the indium dissolution solution may be dried to remove indium to obtain indium, or the indium may be reduced and cast to form an anode, and the indium solution may be electrolytically refined. The electrolytic refining of the indium can be carried out by a commonly used electrolytic refining method. The drying is preferably carried out at a temperature of 40 ° C to 90 ° C for 1 to 48 hours.

Using this process, high purity indium of 99.995% purity or more can be obtained.

EXAMPLES Hereinafter, examples according to the present invention will be specifically shown, and the present invention is not limited to the following examples.

≪ Example 1 >

The multi-stage extraction apparatus used was one comprising three sequentially arranged extraction ends (A1, A2, A3), two cleaning stages (B1, B2) and three back extraction stages (C1, C2, C3). Fig. 3 is a view showing such a multi-stage extraction apparatus.

Referring to FIG. 3, the impeller 114 provided in each mixing tank 110 is operated to mix the solution in the mixing tank 110 while the impeller 114 is rotated.

The cleaning acid solution supply part F supplied the cleaning acid solution to the mixing bath 110 of the cleaning stage B2 through the pump P3. The cleaning acid solution supplied to the mixing tank 110 of the cleaning stage B2 is conveyed to the settling tank 120 of the cleaning stage B2 and is conveyed to the settling tank 120 of the cleaning stage B2, Since the acid solution is acidic, it sinks to the bottom and flows to the cleaning stage B1 through the conduit 112 connected to the discharge port 122 provided at the bottom of one side of the settling tank 120 of the washing stage B2. ) Into the mixing chamber 110 of the reaction vessel.

The cleaning acid solution flowing into the mixing tank 110 of the cleaning stage B1 is mixed with the organic phase introduced through the conduit 132 from the discharge tank 130 of the extraction stage A3, The solution mixed in the mixing tank 110 of the cleaning tank B1 was transferred to the settling tank 120 of the cleaning tank B1. When the organic phase and the cleansing acid solution are mixed, indium (In) remaining in the organic solvent as the organic phase is back-extracted in the mixing tank 110 of the cleaning stage (B1), and the aqueous solution containing the indium (In) And the organic phase in the settling tank 120 of the washing stage B1 is separated from the aqueous phase having an acidity and the indium In is extracted back to be included in the water phase.

The water containing indium (In) in the settling tank 120 of the washing stage B1 sinks downward and is connected to the discharge port 122 provided at the lower side of the one side of the settling tank 120 of the washing stage B1 The organic phase containing tin Sn in the settling tank 120 of the washing stage B1 flows into the mixing tank 110 of the extraction stage A3 through the conduit 112 where the cleaning stage B1 And the organic phase transferred to the discharge tank 130 of the cleaning stage B1 flows into the mixing tank 110 of the cleaning stage B2 through the conduit 132. [

The organic phase introduced into the mixing tank 110 of the cleaning stage B2 is mixed with the acid solution for cleaning supplied through the cleaning acid solution supply part F and mixed in the mixing tank 110 of the cleaning stage B2, And the resulting solution was transferred to the settling tank 120 of the cleaning stage B2. When the organic phase and the cleaning acid solution are mixed, indium (In) remaining in the organic solvent as the organic phase is back extracted in the mixing tank 110 of the cleaning stage (B2) to form an organic phase with the aqueous phase containing indium (In) In the settling zone 120 of the washing stage (B2), the organic phase is separated from the aqueous phase, and the indium (In) is back extracted and included in the aqueous phase.

In the settling chamber 120 of the washing stage B2, the water containing indium (In) sinks downward and is connected to the discharge port 122 provided at a lower side of one side of the settling tank 120 of the washing stage B2 The organic phase containing tin Sn in the settling tank 120 of the washing stage B2 flows into the mixing tank 110 of the washing stage B1 through the conduit 112 in which the washing stage B2 is discharged And the organic phase transferred to the discharge tank 130 of the cleaning stage B2 is introduced into the mixing tank 110 of the back extraction stage C1 through the conduit 132. [

The back extract liquid supply part E supplies the back extract liquid to the mixing tank 110 of the back extraction stage C3 through the pump P4. The back extraction liquid supplied to the mixing tank 110 of the back extraction stage C3 is transferred to the settling tank 120 of the back extraction stage C3 and then transferred to the stationary stage 120 of the back extraction stage C3 The extracted liquid flows into the mixing chamber 110 of the backward extraction stage C2 through the conduit 112 connected to the discharge port 122 provided at the lower side of the fixed tank 120 of the backward extraction stage C3, The back extraction liquid introduced into the mixing tank 110 of the back extraction stage C2 is transferred to the settling tank 120 of the back extraction stage C2 and is then transferred to the stationary stage 120 of the back extraction stage C2 The extracted liquid is introduced into the mixing tank 110 of the back extraction stage C1 through the conduit 112 connected to the discharge port 122 provided at the lower side of the one side of the settling tank 120 of the back extraction stage C2 .

The organic phase transferred to the discharge tank 130 of the cleaning stage B2 and the back extraction liquid introduced from the settling tank 120 of the back extraction stage C2 are mixed in the mixing tank 110 of the back extraction stage C1 The solution mixed in the mixing tank 110 of the back extraction stage C1 was transferred to the settling tank 120 of the back extraction stage C1. When the organic phase and the acidic reverse extract are mixed, the tin (Sn) remaining in the organic solvent as the organic solvent is back-extracted in the mixing tank 110 of the reverse extraction stage (C1) to form an organic phase with the aqueous phase containing tin , The organic phase in the settling tank 120 of the back extraction stage C1 is separated from the aqueous phase and the tin Sn is back extracted and included in the aqueous phase.

The water containing tin (Sn) in the settling tank 120 of the back extraction stage C1 sinks downward and is discharged through the discharge port 122 provided at the bottom of one side of the settling tank 120 of the back extraction stage C1 And the organic phase is transferred to the discharge tank 130 of the backward extraction stage C1 at the settling stage 120 of the backward extraction stage C1 and is discharged through the conduit 112 connected to the backward extraction stage C1, The organic phase transferred to the discharge tank 130 of the first condenser C1 flows into the mixing chamber 110 of the back extraction stage C2 through the conduit 132. [

The organic phase introduced into the mixing tank 110 of the reverse extraction stage C2 is mixed with the reverse extraction liquid that has flowed through the conduit 112 from the settling tank 120 of the reverse extraction stage C3, The mixed solution in the mixing tank 110 of the second extracting column C2 was transferred to the settling tank 120 of the back extraction stage C2. When the organic phase and the acid solution are mixed, the tin (Sn) remaining in the organic solvent as an organic phase is back-extracted in the mixing tank (110) of the back extraction stage (C2) to form an organic phase with the aqueous phase containing tin In the settling tank 120 of the extraction stage C2, the organic phase is separated from the aqueous phase, and the tin (Sn) is back extracted and contained in the water phase.

The water containing tin (Sn) in the settling tank 120 of the back extraction stage C2 is submerged to the bottom and is discharged through the discharge port 122 provided at a lower side of the settling tank 120 of the back extraction stage C2 The organic phase is introduced into the mixing tank 110 of the back extraction stage C1 through the connected conduit 112 and the organic phase in the settling stage 120 of the back extraction stage C2 is discharged to the discharge tank 130 and the organic phase transferred to the discharge tank 130 of the reverse extraction stage C2 flows into the mixing tank 110 of the reverse extraction stage C3 through the conduit 132. [

The organic phase introduced into the mixing tank 110 of the reverse extraction stage C3 is mixed with the reverse extraction liquid supplied through the reverse extraction liquid supply unit E and mixed in the mixing tank 110 of the reverse extraction stage C3. The solution was transferred to the settling tank 120 of the back extraction stage (C3). When the organic phase and the acid solution are mixed, the tin (Sn) remaining in the organic solvent as the organic phase is back-extracted in the mixing tank 110 of the back extraction stage (C3) to form an organic phase with the aqueous phase containing tin In the settling tank 120 of the extraction stage C3, the organic phase is separated from the aqueous phase, and the tin (Sn) is back extracted and included in the water phase.

The water containing tin (Sn) in the settling tank (120) of the back extraction stage (C3) sinks to the bottom and is discharged through the discharge port (122) provided at the lower side of one side of the settling tank (120) The clean organic phase in which the tin is completely removed from the settling tank 120 of the back extraction stage C3 is introduced into the mixing tank 110 of the back extraction stage C2 through the connected conduit 112, And the organic phase transferred to the discharge tank 130 of the reverse extraction stage C3 is supplied to the organic solvent supply unit D through the conduit 132 to be recycled.

The organic solvent supply unit D supplies the organic solvent to the mixing tank 110 of the extraction stage A1 through the pump P2. The organic solvent supplied to the mixing tank 110 of the extraction stage A1 is transferred to the discharge tank 130 through the settling tank 120 of the extraction stage A1 and discharged to the discharge tank 130 of the extraction stage A1, The organic solvent transferred into the mixing tank 110 of the extraction stage A2 through the conduit 132. [ The organic solvent supplied to the mixing tank 110 of the extraction stage A2 is transferred to the discharge tank 130 through the settling tank 120 of the extraction stage A2 and discharged to the discharge tank 130 of the extraction stage A2, The organic solvent transferred into the mixing tank 110 of the extraction end A3 through the conduit 132. [

The indium solution supply part G supplied the indium solution to the mixing bath 110 of the extraction end A3 through the pump P1.

The cleaning acid solution in the settling tank 120 of the cleaning stage B1 is supplied through the conduit 112 connected to the discharge port 122 provided at one side of the lower side of the settling tank 120 of the cleaning stage B1 And introduced into the mixing tank 110 of the extraction stage A3.

The solution in which the indolol solution, the organic solvent and the cleansing acid solution are mixed in the mixing tank 110 of the extraction stage A3 and the solution mixed in the mixing tank 110 is mixed with the solution in the settling tank 120 of the extraction stage A3, . Tin (Sn) is extracted by the organic solvent in the mixing tank 110 of the extraction end A3 to form an aqueous solution containing indium (In) and tin Sn), the organic phase is separated from the aqueous phase, and indium (In) is included in the aqueous phase.

The organic phase containing tin (Sn) in the settling tank 120 of the extraction stage A3 is transferred to the discharge tank 130 of the extraction stage A3 and is conveyed to the discharge tank 130 of the extraction stage A3, Is introduced into the mixing tank 110 of the cleaning stage B1 through the conduit 132 and separated from the organic phase in the settling tank 120 of the extraction stage A3, And is introduced into the mixing chamber 110 of the extraction end A2 through the conduit 112 connected to the discharge port 124 provided at one side of the tank 120. [

The organic phase in the discharge vessel 130 of the extraction stage A1 is introduced into the mixing vessel 110 of the extraction stage A2 via the conduit 132. [

The organic phase and the aqueous phase are mixed in the mixing tank 110 of the extraction stage A2 and the mixed solution in the mixing tank 110 is conveyed to the settling tank 120 of the extraction stage A2. When the organic phase and the water phase are mixed, tin (Sn) is extracted by an organic solvent, which is an organic phase, in the mixing bath 110 of the extraction stage A2 to form an organic phase containing an aqueous phase containing indium (In) , The organic phase is separated from the aqueous phase, and indium (In) is included in the aqueous phase.

The organic phase containing tin (Sn) in the settling tank 120 of the extraction stage A2 is transferred to the discharge tank 130 of the extraction stage A2 and transferred to the discharge tank 130 of the extraction stage A2, Is introduced into the mixing tank 110 of the extraction end A3 through the conduit 132 and separated from the organic phase in the settling tank 120 of the extraction end A2 so that the water present at the bottom is separated from the And is introduced into the mixing chamber 110 of the extraction stage A1 through the conduit 112 connected to the discharge port 122 provided at one side of the tank 120. [

The organic phase introduced through the organic solvent supply unit D and the water phase introduced from the settling tank 120 of the extraction stage A2 are mixed in the mixing tank 110 of the extraction stage A1, The solution mixed in the mixing tank 110 of the extraction stage A1 was transferred to the settling tank 120 of the extraction stage A1. When the organic phase and the water phase are mixed, tin (Sn) is extracted by an organic solvent in an organic phase in the mixing bath 110 of the extraction stage A1 to form an organic phase containing an aqueous phase containing indium (In) , The organic phase is separated from the aqueous phase, and indium (In) is included in the aqueous phase.

The organic phase containing tin (Sn) in the settling tank 120 of the extraction stage A1 is conveyed to the discharge tank 130 of the extraction stage A1 and is conveyed to the discharge tank 130 of the extraction stage A1, Is introduced into the mixing tank 110 of the extraction stage A2 through the conduit 132 and separated from the organic phase in the settling tank 120 of the extraction stage A1, And is discharged to the outside through the conduit 112 connected to the discharge port 122 provided at one side of the tank 120.

Tables 1 and 2 below show that when extracting tin (Sn) using a multi-stage extraction apparatus according to Example 1, the amounts of indium (In), tin (Sn), and lead (Pb). The contents of indium (In), tin (Sn) and lead (Pb) show the contents measured in the settling tank 120, the cleaning tank and the backward extraction stage. The indium dissolution solution supplied to the mixing bath 110 of the extraction end A3 through the indium solution supply part G contained 228.758 g / L of indium (In), 18720.960 ppm of tin (Sn) and 2.19498 ppm of lead (Pb) .

Singular name In (g / L) Sn (ppm) Pb (ppm) Volume ratio of organic phase / water phase The extraction stage (A1) 214.411 7.841 0
3
Extraction stage (A2) 228.127 2.871 1.98042 The extraction stage (A3) 230.130 39.447 1.56446 Cleaning Stage (B1) 6.307 17.073 0 2
The cleaning stage (B2) 0.048 16.480 0 The back extraction stage (C1) 0.006 10359.560 0
2
The reverse extraction stage (C2) 0.000 10294.220 0 Reverse extraction stage (C3) 0.005 4687.740 0

Singular name In (g / L) Sn (ppm) Pb (ppm) Volume ratio of organic phase / water phase The extraction stage (A1) 199.658 0.000 1.243
3
Extraction stage (A2) 211.517 0.000 2.133 The extraction stage (A3) 213.445 28.074 2.950 Cleaning Stage (B1) 5.764 12.288 0.000 2
The cleaning stage (B2) 0.052 12.808 0.000 The back extraction stage (C1) 0.000 10440.920 0.000
2
The reverse extraction stage (C2) 0.000 9286.540 0.000 Reverse extraction stage (C3) 0.000 4194.580 0.000

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, This is possible.

A1, A2, A3: Extraction stage
B1, B2, B3: Cleaning stage
C1, C2, C3: Reverse extraction stage
G: Indium solution supply part
D: organic solvent supply unit
F: cleaning solution supply part
E: Reverse extraction liquid supplier
110: mixing tank
112: conduit
120: Political group
122: exhaust port
130: Emission tank
132: conduit
140: first separating wall
145: second separating wall
150: virtual horizontal line

Claims (11)

A plurality of extraction stages arranged in sequence, a plurality of cleaning stages and a plurality of back extraction stages,
An indium dissolution liquid supply unit, an organic solvent supply unit, a cleaning acid solution supply unit, and a reverse extract liquid supply unit,
Each of the one extraction stage, the one cleaning stage and the one back extraction stage has a mixing tank, a settling tank and a discharging tank,
Wherein the mixing unit of the first stage in the extraction stage, the cleaning stage and the back extraction stage is located adjacent to the second stage discharge vessel and the mixing vessel of the second stage is positioned adjacent to the discharge vessel of the first stage,
The mixing tank is connected to the discharging tank of the previous stage through the conduit and to the next tank tank through another conduit,
In the settling tank, a discharge port is provided at the lower portion for providing a passage through which the water phase having a specific gravity is separated by the organic phase and the water phase, and the discharge port is connected to the mixing tank at the previous stage,
The discharge vessel is connected to the next stage vessel through the conduit,
The mixing chamber and the control tank are separated from each other by a first separating wall having a height higher than a virtual horizontal line separating the water phase separated from the organic phase and the first separating wall,
The second separation wall is formed to have a height higher than a virtual horizontal line separating the water phase separated from the organic phase and the second separation wall,
The second partition wall is formed at a lower height than the first partition wall,
The indium dissolution solution supply unit supplies an indium dissolution solution containing indium (In) and tin (Sn) to a mixing tank of the last extraction stage through a pump,
The organic solvent supply unit supplies the organic solvent to the mixing tank of the first extraction stage through a pump,
The cleaning acid solution supply unit supplies the cleaning acid solution to the mixing tank of the last cleaning stage via the pump P3,
The reverse extraction liquid supplier supplies the reverse extraction liquid to the mixing tank of the last reverse extraction stage through the pump,
The mixing chamber is a region where the solution is mixed, and the solution mixed in the mixing chamber is moved to a fixed bath,
The settling zone separates the organic phase and the water phase, and the mixed solution is separated into the organic phase and the water phase while staying in the settling tank. The organic phase is smaller in weight than the aqueous phase, Through a discharge port provided on one side of the lower part, to the mixing vessel of the previous stage,
The organic phase transferred to the discharge tank of the last reverse extraction stage is recycled to be supplied to the organic solvent supply unit,
First, the reverse extract, which is located at the lower part of the regrowth of the reverse extraction stage, is configured to be discharged to the outside through the discharge port provided at the lower side of the first reverse extraction stage,
Wherein the indium liquid, which is a water-immiscible indium liquid that is submerged in the bottom of the first extraction stage, is discharged to the outside through a discharge port provided at a lower side of the first side of the extraction stage.
delete The impeller according to claim 1, wherein the mixing tank is provided with an impeller, the impeller is stirred in a mixing tank, the impeller rotates at a speed of 100 to 500 rpm, The organic phase is introduced through the conduit and the water phase is introduced through the conduit through the conduit in the next stage. The organic phase introduced from the discharge vessel of the previous stage by the rotation of the impeller is mixed with the water phase introduced from the next stage Wherein the multi-stage extraction device is a multi-stage extraction device.
delete The cleaning method according to claim 1, wherein the concentration of the cleaning acid solution supplied through the cleaning acid solution supply portion is in the range of 0.5 to 5M,
The back extract liquid supplied through the back extract liquid supply unit is an acid solution, and the concentration of the acid solution of the back extract liquid is in the range of 5 to 12M,
The organic solvent may be at least one selected from an alkyl monocarboxylic acid, tributyl phosphate, 2-ethylhexyl 2-ethylhexyl phosphate and di- (2-ethylhexyl)
Wherein the volume ratio of the organic solvent supplied from the organic solvent supply unit to the acid solution supplied from the cleansing acid solution supply unit is in the range of 1: 1 to 5: 1.
delete A plurality of cleaning stages, and a plurality of back extraction stages, wherein one extraction stage, one cleaning stage, and one back extraction stage each include a mixing tank, a flotation tank, and a flotation tank Wherein the mixing stage in the extraction stage, the mixing stage in the first stage in the cleaning stage and the reverse stage is located adjacent to the second stage discharge vessel, and the mixing vessel in the second stage is positioned adjacent to the discharge vessel in the first stage, The mixing tank is connected to the discharging tank of the previous stage through the conduit and is connected to the tank tank of the next stage through another conduit. In the tank, the discharging port which provides the passage for discharging the heavy water tank separated by the organic tank and the water tank, And the discharge port is connected to the mixing tank of the previous stage, and the discharge tank is connected to the mixing tank of the next stage through the conduit. And,
The mixing chamber and the control tank are separated from each other by a first separating wall having a height higher than a virtual horizontal line separating the water phase separated from the organic phase and the first separating wall,
The second separation wall is formed to have a height higher than a virtual horizontal line separating the water phase separated from the organic phase and the second separation wall,
The second partition wall is formed at a lower height than the first partition wall,
The indium dissolution liquid supply unit supplies the indium dissolution liquid containing indium (In) and tin (Sn) to the mixing tank of the last extraction stage through the pump,
The organic solvent supply unit supplies the organic solvent to the mixing tank of the first extraction stage through the pump,
The cleaning acid solution supply unit supplies the cleaning acid solution through the pump to the mixing tank of the last cleaning stage,
The reverse extract supply unit supplies the reverse extract to the mixing tank of the last reverse extraction stage through the pump,
The solution mixed in the mixing bath and mixed in the mixing bath is moved to the bath,
The organic phase is separated into a water phase and an organic phase while the solution moved to the settling tank stays in the settling tank. The organic phase is smaller in specific gravity than the water phase and is moved upward to the discharge tank. Lt; / RTI >
The organic phase, which has been moved to the discharge tank, is discharged through a conduit into a mixing tank at the next stage,
The organic phase supplied to the discharge tank of the last reverse extraction stage is supplied to the organic solvent supply unit,
First, the reverse extract, which is located at the lower part of the regrowth of the reverse extraction stage, is discharged to the outside through the discharge port provided at the lower side of the first side of the reverse extraction stage,
Wherein the indium solution, which is a water-immiscible indium solution, is collected and discharged to the outside through a discharge port provided at a lower portion of the first side of the extraction column.
The cleaning method according to claim 7, wherein the concentration of the cleaning acid solution supplied through the cleaning acid solution supply unit is in the range of 0.5 to 5M,
The back extract liquid supplied through the back extract liquid supply unit is an acid solution, and the concentration of the acid solution of the back extract liquid is in the range of 5 to 12M,
The organic solvent may be at least one selected from an alkyl monocarboxylic acid, tributyl phosphate, 2-ethylhexyl 2-ethylhexyl phosphate and di- (2-ethylhexyl)
Wherein the volume ratio of the organic solvent supplied from the organic solvent supply unit to the acid solution supplied from the cleaning acid solution supply unit is in the range of 1: 1 to 5: 1.
delete The impeller according to claim 7, wherein the mixing tank is provided with an impeller, stirring is performed in the mixing tank by the impeller, the impeller rotates at a speed of 100 to 500 rpm, The organic phase is introduced through the conduit and the water phase is introduced through the conduit through the conduit in the next stage. The organic phase introduced from the discharge vessel of the previous stage by the rotation of the impeller is mixed with the water phase introduced from the next stage ≪ / RTI >
The method according to claim 7, wherein the indium-
Pulverizing the indium-tin oxide scrap;
Dissolving the pulverized product in an acid to obtain an acid solution containing indium and tin; And
And filtering the acid solution to obtain an indium dissolution solution which has passed through a filter, and is supplied to the indium dissolution solution supply unit.

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