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Extracting indium from indium containing materials
I. Overview
China's factories use P204 organic solvent extraction method to extract indium from smelting intermediates. The advantages are:
(1) P204 has good selectivity to indium and can extract indium from a mixture containing very low indium.
(2) The extraction enrichment rate is up to 100 times or more.
(3) The process is simple, the operation is continuous, and it is easy to realize automation.
(4) The extraction recovery rate of indium is as high as 96% to 99%.
Recovered starting material indium zinc refining tank from the shaft intermediate product has
1. Indium zinc oxide produced by coke
During the coking process, indium is volatilized with hydrocarbons into zinc oxide (containing 0.1% to 0.2% of indium and 50% to 60% of zinc). It is the largest amount of raw materials in the vertical tank zinc smelting process, and contains a high grade of indium, accounting for 70% to 80% of the total indium recovery.
2. Cadmium system acid immersion liquid
The cadmium-containing raw material contains 0.01% to 0.008% of indium which is hydrolyzed at the end of the immersion, and enters the acid leaching solution during acid leaching.
3. Indium-containing crude lead by -product of zinc rectification process
Zinc distillation, high boiling point metal column eluted into the lead furnace, separated by liquation, indium enriched in the bottom of the crude lead, indium containing up to 0.5% to 1.2%.
The method of manufacturing the extract solution differs depending on the raw materials. The indium-containing zinc oxide is subjected to acid leaching, sinking silicon, and filtered to obtain a raw liquid, and the cadmium acid immersion liquid is subjected to sinking silicon and filtered to obtain an extract liquid. For the indium-containing crude lead, it is selected to be melted, blasted at a temperature of 750-800 ° C, so that indium is indium oxide into the scum, crushed and sieved by a ball mill , and the obtained powdery indium oxide is leached with dilute sulfuric acid to obtain sulfuric acid. The indium solution is combined with the zinc oxide silicon-filtered liquid.
Figure 1 is an example of a process for recovering indium from a vertical tank zinc smelting intermediate.
Figure 1 Process for recovering indium from vertical tank zinc smelting intermediates
Second, raw materials
Table 1 shows an example of an indium containing intermediate component of zinc smelting in a vertical tank.
Table 1 Examples of indium containing intermediates in vertical tank zinc smelting
Material name
In
Zn
Fe
Pb
Cd
Cu
As
Bi
Sn
SiO 2
Indium zinc oxide, %
0.1 to 0.2
50~60
0.63
1.86
1.5
0.15
0.03
0.08
Cadmium leaching solution, g/L
0.04~0.06
50~60
15~18
25
0.1
2.5
0.2
Crude crude lead, %
0.5 to 1.2
1 to 3
0.05
96
0.02
0.32
0.05
Third, technical operating conditions
(1) Preparation of feed liquid
1. Zinc oxide leaching
The leaching can be carried out in a mechanical agitation tank, using a period of acidic leaching, and the end point contains 20-30 g/L of acid. The main component of zinc oxide is soluble metal oxide, which is easily soluble in dilute sulfuric acid solution. The leaching rate is very high, and the slag rate is only 1% to 5%. Therefore, the right leaching is about 10 cycles and then slag is discharged once. Examples of operating conditions for zinc oxide leaching techniques are as follows:
temperature
85～95°C
Liquid to solid ratio
(5~6): 1
Acid
150～160g/L
Final acid
20~30g/L
Leaching time
2~3h
Clarification time
3~4h
2, sinking silicon
Zinc oxide leaching solution and cadmium acid leaching solution contain higher silica (SiO 2 ) and have a wide fluctuation range. In practice, when the stock solution contains more than 0.5 g/L of silica, a third phase is produced during the extraction. At the same time, the stock solution needs to maintain a high acidity during the extraction process, otherwise the partition coefficient of copper and cadmium in the extraction is significantly decreased; silica is easy to form a colloid which is not easy to precipitate in an acidic solution, so it is necessary to add animal gelatin silicon. The solution contains Si1～3g/L, and the addition of 0.1～0.3g/L can reduce the silica to below 0.5g/L. The operating conditions of the sinking silicon technology are as follows:
Temperature 70～80°C
Adding glue amount 10% to 12% of SiO 2 content
Stir for 1~2h, precipitate for 3~4h
3, filter
The solution after sinking with silicon was filtered using a corundum filter. Its technical operating conditions are:
Filtration speed 0.8~1m 3 /(m 2 ·h)
Pressure 0.2～0.3MPa
Temperature 50～60°C Backflushing pressure 0.3～0.5MPa
4, crude lead oxidation
Indium-containing crude lead in the cast iron melt pot, stirring air into the drum oxide, indium oxide and the metal impurities into the dross, and separating the lead enriched. At the same time, the refined lead containing about 0.1% BiO is produced. Usually, the blasting is 5-6 hours, the oxidation of indium is complete, the residual indium of the lead liquid is 0.001% to 0.002%, and the scum rate is 25% to 30%. Therefore, the slag is repeatedly blasted 4 to 5 times per pot, The scum is finely ground by a ball mill, sieved with a 0.42 mm sieve, and the lead particles are returned to the reoxidation. Examples of operating conditions for oxidation technology are as follows:
Temperature 750 ~ 800 ° C blast pressure 0.2 ~ 0.3MPa
Blast time 5~6h Scum rate 25%~30%
Operating cycle 7~8h
Table 2 shows examples of scum and refined lead components.
Table 2 Scum and refined lead composition, %
project
In
Zn
Cu
Fe
Bi
Sn
As
Cd
Pb
Scum 1
1.57
4.65
0.002
0.4
0.06
0.46
micro-
87.9
Scum 2
3.3
6.5
0.38
micro-
0.29
micro-
92.5
Refined lead
0.002
0.001
0.001
0.1
0.001
0.001
0.0005
99.82
5, scum leaching
The indium-containing oxidized dross is leached with dilute sulfuric acid to convert indium into indium sulfate into the solution. Examples of technical operating conditions for leaching are as follows:
Temperature 85～90°C Liquid-solid ratio (5～6):1
Starting acid 110～120g/L final acid 20～30g/L
In order to maximize the indium into the solution, it is generally required to carry out leaching 2 to 3 times, and the liquid-solid ratio of the second leaching can be reduced to (2 to 3):1, and the final slag contains 0.05% or less of indium.
6, cadmium acid immersion liquid sinking silicon
The main components (g/L) of the cadmium acid immersion liquid are: Zn 70 to 90; Cd 20 to 30; In 0.1 to 0.5; Fe 5 to 10; SiO 2 0.2 to 0.6; and H 2 SO 4 20 to 30.
The sinking operating conditions of this solution are the same as those for zinc oxide, but should be extracted separately to return the raffinate to the cadmium system.
(2) Solvent extraction
It is extracted with P 204 organic solvent to make indium enter the organic phase; the heavy metal impurities are removed by acid washing, and then stripped with hydrochloric acid to obtain a higher concentration of indium chloride. The enrichment ratio of indium can reach 100 to 300 times.
P 204 extractant chemical name is di-2-phosphoric acid group, are acidic extraction, molecular weight 322, a bulk density of 0.9694 ~ 0.97g / cm 3, a viscosity of 25.92 cps, Pale yellow oily liquid, transparent, almost odorless, soluble in benzene, petroleum, coal, oil, organic solvents. The solubility in water was 0.012 g/L; in 1 mol sulfuric acid it was 0.017 g/L.
P 204 is usually diluted with 3 to 4 times of No. 200 kerosene to reduce its viscosity and density, and it is easy to stratify with water. 200 Kerosene density 0.78g / cm 3, the chemical components of a mixture of alkanes C 13 ~ 15, there should not dilute the presence of hydrocarbons.
1, extraction
Examples of operating conditions for extraction techniques are as follows:
Extractant P 204 : kerosene 1: 2 ~ 4 O / A1: 15;
Temperature 20～30°C The temperature of the raw liquid into the stirring chamber is 10m 3 /(m 2 ·h);
Precipitate stratified flow rate 1.84m 3 /(m 2 ·h) raffinate residual indium <0.001g / L;
The indium extraction rate is >97%.
Table 3 shows examples of the components of the extract stock solution and the raffinate.
Table 3 Extracting stock solution and raffinate components, g/L
project
In
Cd
Zn
As
Extraction stock solution
0.1
9.45
54.1
2.25
Raffinate
0.001
9.45
55.1
2.24
2, acid
Part of the heavy metal ions in the organic phase can be removed by flushing with dilute sulfuric acid. The technical operating conditions are as follows:
Pickling solution containing sulfuric acid 80 ~ 100g / L O / A = 5: 1
Operating temperature 20～30°C Organic phase flow rate 0.42m 3 /(m 2 ·h)
3, anti-collection
The washed organic phase was back-extracted with concentrated hydrochloric acid to obtain an InCl 3 solution. An example of its technical operating conditions is as follows:
Stripping agent hydrochloric acid concentration 6mol/L O/A=5:1
Operating temperature 20～30°C Organic phase flow rate 0.42m 3 /(m 2 ·h)
The example of the Huludao zinc plant extraction is as follows:
Extraction, pickling and stripping are carried out in the same tank extraction tank. The extraction tank is divided into 10 grades, of which 4 grades are extracted, 3 grades are pickled, and 3 grades are stripped. The aqueous phase and the organic phase are countercurrently extracted, and the agitator rotation speed is 600-650 r/min, and the extraction process is shown in FIG.
Figure 2 Indium extraction process
(three) replacement
Replaced with an indium zinc plate InCl 3 solution required in a closed vessel and has ventilation is performed, the negative pressure holding operation, arsenic prevent hydrogen from escaping during the reaction. An example of the operating conditions of the replacement technique is as follows:
Acidity 3~4mol Replacement temperature 50～60°C
Replacement time 4~5h After replacement, the solution contains indium <0.01g/L
(4) Pressing smelting
The deposited sponge indium was replaced by water for 3 to 4 times, and pressed into a dough by a hydraulic press (the agglomerated pressure was greater than 1.5 MPa). The agglomerates smelt the ingot under the protection of liquid caustic soda. The melting temperature is 350 to 450 °C. Table 4 is an example of smelting crude indium components.
Table 4 Melting of crude indium, %
Serial number
In
Zn
As
Cu
Bi
Fe
Sn
Pb
T1
Cd
1
99.5
0.03
0.0005
0.017
0.0032
0.015
0.14
0.24
0.0016
0.01
2
99.6
0.01
0.0005
0.011
0.001
0.031
0.17
0.16
0.005
0.018
(5) Crude indium electrolysis
1. Plate manufacturing
The crude indium is melted and cast into an anode under the protection of glycerin, and the outer layer is coated with two layers of analytical filter paper, and then the silk bag is pressed to prevent the anode mud from falling into the electrolyte during electrolysis. The electrolyzed finished indium is melted under the protection of glycerin and cast into a 1 mm thick sheet, which is the cathode.
2, electrolyte manufacturing
The indium was dissolved in analytically pure sulfuric acid, and NaCl and animal glue were added to prepare the following components: In 80 to 100 g/L, NaCl 80 to 100 g/L, animal glue 0.5 to 1 g/L, and pH 2 to 3.
3. Electrolysis
Electrolytic technical conditions: temperature 20 ~ 30 ° C; current density 60 ~ 80A / m 2 ; cell voltage 0.25 ~ 0.3V, the same pole center distance 4mm, electrolysis cycle 6 ~ 7d, current efficiency greater than 96%, residual rate 45% ~ 50%, electrolytic recovery rate > 95%.
The electro-indium needs to be subjected to secondary electrolysis, and its operating conditions are the same as once. Table 5 shows an example of the cathode quality of the secondary electrolysis.
Table 5 precipitated cathode mass, %
Serial number
In
Ag
Cu
Al
Fe
Sn
Pb
T1
Cd
1
99.96
0.0001
0.0001
0.0001
0.0001
0.00063
0.00063
0.016
0.02
2
99.95
0.0001
0.0001
0.0001
0.0001
0.00063
0.00063
0.021
0.02
3
99.95
0.0001
0.0001
0.0001
0.0001
0.00063
0.00063
0.023
0.02
4
99.94
0.0001
0.0001
0.0001
0.0001
0.00063
0.00063
0.034
0.02
(6) Indium refining
Indium is high in antimony and cadmium and must be removed by chemical methods. The technical operating conditions are as follows:
1, in addition to cadmium
The temperature is 170-180 ° C, glycerol: indium = 1:10; mechanical stirring, the amount of KI added is 2 to 3 times the amount of cadmium, and the time is 1.5 to 2.0 h/time. Due to the difference in the amount of cadmium, it can be repeated 2 or 3 times according to the analysis.
2, except é“Š
After the cadmium was kept at a temperature of 170 to 180 ° C, glycerin:indium = 1: (5 to 6), hydrogen chloride gas was passed for about 30 minutes and mechanically stirred.
Table 6 shows examples of refined indium quality after refining.
Serial number
In
As
Cu
Al
Fe
Sn
Pb
T1
Cd
1
99.994
0.0001
0.0001
0.0001
0.0001
0.0007
0.00063
0.0011
0.001
2
99.994
0.0001
0.0001
0.0001
0.0001
0.0007
0.00063
0.0012
0.001
3
99.994
0.0001
0.0001
0.0001
0.0001
0.0007
0.00063
0.0010
0.001
Fourth, technical and economic indicators
(1) Example of recovery rate of indium in each process, %
Leaching 92 ~ 96 replacement 96 ~ 98 extraction 95 ~ 97 stripping 98 ~ 99 smelting 92 ~ 93 pickling 95 ~ 97 electrolysis 95 ~ 96.
(II) Example of raw material consumption of indium production (kg/kg indium)
Industrial hydrochloric acid 310～330 zinc plate (99.99%) 4～5
Industrial sulfuric acid 300～320 glycerin 2.4～3
Industrial caustic soda 2.5~3 filter paper 2 sheets/kg indium
Analysis of pure sulfuric acid 0.01 ~ 0.02 steam 2000 ~ 3000
P 204 0.8～1 Electricity 100～110kW·h
No. 200 kerosene 2.4~3
Fifth, the main equipment selection
(1) Leaching trough
The use of steel-lined granite in the leaching tank is better, and the selection calculation can refer to the formula.
N=V (t/24V has )
Where V-day treatment of pulp or dissolved amount, m3;
V has - the effective volume of the selected tank, m 3 , which is 0.85 to 0.9 of the groove geometry volume;
T-operation cycle, h, leaching takes 8, purification takes 4 to 6, one replacement takes 30 to 40 minutes, and secondary replacement takes 40 to 50 minutes.
(2) Extraction tank
Indium extraction generally uses a square box type extraction tank, and each single stage extraction tank is divided into a mixing chamber and a clarification chamber. The effective volume of the clarification chamber is four times that of the mixing chamber. The number of stages of the extraction tank can be determined according to experimental numbers, generally using three-stage or four-stage extraction, three-stage acid washing and three-stage stripping, and the total number is nine or ten. The flow rate of the stock solution in the mixing chamber is 10-12 m 3 /(m 2 ·h), the residence time is 4-5 min, and the stirring speed is 600-650 r/min.
1, the side length of the single-stage extraction mixing chamber L
Q-day treatment of the amount of raw liquid, m 3 ;
V-mixing chamber stock flow rate, m 3 /(m 2 ·h)
2. The effective height of the extraction tank h
h=[Qt/(24×60×l 2 )]m
The amount of Q-day treated raw liquid in the formula, m3;
T-stock solution residence time in the mixing chamber, min;
l-The length of the mixing chamber is m.
3. The total height of the extraction tank is 1.5 times the effective height.
4, calculation examples
The indium-containing stock solution was treated daily for 24 m 3 to find the main size of the extraction tank.
H=1.5×0.75=1.13m, take 1.15m
The effective volume of the clarification chamber is 4 times that of the mixing chamber, which yields:
Total extraction tank width
W=5l=5×0.3=1.5m
The number of extraction stages is calculated in ten steps, and the total length of the extraction tank is obtained.
L=10l=10×0.3=3m
The main dimensions of the extraction tank are calculated by calculation as shown in Fig. 3.
Figure 3 shows the main dimensions of the extraction tank
(3) Electrolyzer
The calculation of the electrolytic cell is the same as that of the general electrolytic refining tank. The following is an example of an electrolytic cell with an annual output of 700 to 800 kg of indium.
The size of the electrolytic cell is 190×380×265mm, and the material is 8～10mm thick plastic or plexiglass. The number is 16 and divided into 2 groups according to the first and second electrolysis, 8 in each group. The anode size of 170 × 210mm, a thickness 6mm, the outer edge of the plate lugs to the distance of 35mm, so the total height of 240mm anode, each anode weight 2.4 ~ 2.5kg, 7 blocks per slot, a stainless steel cathode 1mm thick titanium plate The size is slightly larger than the anode.
Sixth, configuration reference map
Figure 4 shows an example of a flat layout of indium production.
Figure 4 Indium production workshop plane configuration example
1—leaching tank; 2—storage tank; 3— graphite cooler; 4—ventilation pipeline; 5—plate frame filter press;
6-lead leaching tank; 7-vacuum conveying device; 8-extracting tank; 9-low-level storage tank;
10 - filtrate intermediate tank; 11 - suction filter; 12 - mud tank; 13 - pump; 14 - lifter;
15-slag chute; 16-oxidation furnace; 17-air compressor; 18-cylinder sieve; 19-ball mill;
20-displacement tank; 21-neutralization tank; 22-electrolysis chamber; 23-ion exchange column
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