CN110550611A - Method for efficiently leaching tellurium from copper separating slag of copper anode slime enhanced by external field effect - Google Patents
Method for efficiently leaching tellurium from copper separating slag of copper anode slime enhanced by external field effect Download PDFInfo
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- CN110550611A CN110550611A CN201910990544.XA CN201910990544A CN110550611A CN 110550611 A CN110550611 A CN 110550611A CN 201910990544 A CN201910990544 A CN 201910990544A CN 110550611 A CN110550611 A CN 110550611A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
Abstract
the invention relates to a non-ferrous metal hydrometallurgy technology, in particular to a method for efficiently leaching tellurium from copper anode slime separated copper slag strengthened by an external field effect. The invention comprises the following steps: grinding the copper slag raw material; mixing sodium hydroxide as leaching agent and sodium chlorate as oxidant with the material to obtain mixed material liquid; placing the mixed material liquid on an ultrasonic-microwave synergistic reaction workstation, setting ultrasonic power and microwave power parameters, and continuously stirring according to a certain liquid-solid ratio under the reinforcing action of ultrasonic waves or microwaves or ultrasonic-microwaves synergistic external fields to carry out leaching reaction; and taking out the solution obtained in the previous step, leaching at normal pressure, discharging, carrying out suction filtration on the obtained solution, and carrying out suction filtration to obtain the tellurium-containing leaching solution. The method utilizes external field ultrasonic waves and microwaves to assist in strong oxidation leaching, has the characteristics of short treatment time, high leaching speed, low energy consumption and the like, can destroy the structure of the copper separating slag, realizes the high-efficiency leaching of tellurium under normal pressure, and improves the tellurium leaching rate by 26-35%.
Description
Technical Field
The invention relates to a nonferrous metal hydrometallurgy technology, in particular to a method for efficiently leaching tellurium from copper separating slag of copper anode slime strengthened by an external field effect, which efficiently leaches valuable metal Te from the copper separating slag, thereby improving the leaching rate of tellurium.
background
tellurium is a rare-earth element, and the abundance of tellurium is the smallest of metals and non-metals (the average abundance is 6 multiplied by 10 -6%), tellurium exists in copper anode slime in the form of compounds such as Cu 2 Te, Ag 2 Te, Au 2 Te, PbTe and TeO 2, tellurium and the compounds thereof are widely used for (1) producing cadmium telluride thin-film solar cells, (2) improving the machinability of steel as an alloy additive, (3) improving the machinability of copper alloy without reducing the conductivity as a trace additive, and (4) as a vulcanizing agent, a rubber processing accelerator and a catalyst component for synthetic fiber production.
Most recoverable tellurium in the world is associated with minerals such as copper, gold and the like, and the main source for industrially producing tellurium is anode mud generated in the electrolytic refining process of copper and lead. In the copper electrolytic refining process, copper on the anode and base metal with more negative potential dissolve into the solution, and potential correction metal does not dissolve and fall into the bottom of the tank to become copper anode mud. The method comprises the following basic steps of extracting Te based on the hydrometallurgy technical principle: crushing the copper separating residue, ball milling, leaching, purifying, neutralizing, calcining, alkali dissolving and electrodepositing to obtain high-purity tellurium, wherein the tellurium enters the solution in the process, and then the tellurium is separated and recovered from the solution.
the copper separating slag contains a large amount of rare elements, the existing extraction process is complex, the tellurium leaching rate is low and is difficult to be increased by 70%, and the reaction time is long.
Disclosure of Invention
The invention aims to provide a method for efficiently leaching tellurium from copper separation slag of copper anode slime reinforced by an external field effect. The method can leach at low temperature and normal pressure, reduce energy consumption and shorten leaching time, the leaching time of the copper-separating slag is reduced from the current 90-120min to 14-44 min, the treatment capacity is large, the tellurium leaching rate is high, other valuable metals are concentrated, and comprehensive recovery is facilitated.
The invention comprises the following steps:
Step 1, grinding a copper slag raw material;
step 2, mixing sodium hydroxide serving as a leaching solution and sodium chlorate serving as an oxidant with the raw materials in the step 1 to prepare a mixed material liquid;
Step 3, placing the mixed material liquid obtained in the step 2 on an ultrasonic-microwave synergistic reaction workstation (existing equipment), setting ultrasonic power and microwave power parameters, and continuously stirring the mixed material liquid according to a certain liquid-solid ratio under the reinforcing action of ultrasonic waves or microwaves or an external field of ultrasonic-microwave synergy to carry out leaching reaction;
step 4, taking out the solution obtained in the step 3, leaching for 1-30min at normal pressure, discharging, carrying out suction filtration on the obtained solution, and carrying out suction filtration to obtain a tellurium-containing leaching solution;
The concentration of the sodium hydroxide in the step 2 is 0.4-1.4mol/L, and the addition amount of the sodium chlorate is 0.8-1.5 times of the actual addition amount of the copper slag raw material;
In the step 3, the ultrasonic power is 0-500W, the microwave power is 0-700W, and the liquid-solid ratio is 4-10: 1.
Grinding the raw materials of the copper slag in the step 1 to be more than 200 meshes.
The stirring speed in the step 3 is 100-300 r/min.
The copper slag in the step 1 comprises the following main components in percentage by mass: pb: 15-16.06%, Ag: 14-14.9%, Ba: 14-16.43%, Sn: 8-9.02%, Te: 3-3.64%, Cu: 2 to 2.88 percent.
The principle of the invention is as follows: the mixed liquid is placed in the ultrasonic-microwave synergistic reaction work, and (1) under the action of ultrasonic waves, mass and heat transfer are accelerated, so that a surface film of the copper separating slag is damaged to a certain extent, the particle surfaces of the copper separating slag are exposed, and the solid-liquid reaction is promoted. Meanwhile, the phenomenon of 'turbulent flow' occurs in the solution, a large amount of 'micro bubbles' are generated to form a cavitation effect, and the diffusion resistance and the reaction activation energy are reduced; (2) under the action of microwaves, the microwave heating converts electromagnetic energy into heat energy, the heat energy is closely related to the polarization property of molecules in the copper separation slag, the polarized molecules with positive and negative poles are orderly arranged in a magnetic field, the direction of the magnetic field is changed, and the polarized molecules continuously rotate at high speed, so that heat is generated. The method can rapidly heat the solution, promote the leaching reaction, improve the leaching rate of tellurium in the metallurgical process, reduce the reaction time, reduce the amount of waste gas, waste residue and waste liquid compared with the traditional wet metallurgy, and is favorable for environmental protection. Due to the characteristics of microwaves and ultrasonic waves, the method has higher utilization value than the traditional hydrometallurgy.
The main chemical reaction equation of the invention is as follows:
3TeO2+6OH-+ClO3 -＝3TeO4 2-+3H2O+Cl-；
3Pb5TeO7+36OH-+ClO3 -＝3TeO4 2-+15PbO2 2-+Cl-+18H2O。
The method utilizes external field ultrasonic waves and microwaves to assist in strong oxidation leaching, has the characteristics of short treatment time, high leaching speed, low energy consumption and the like, can destroy the structure of the copper separation slag, realizes the high-efficiency leaching of tellurium under normal pressure, and can improve the tellurium leaching rate by 26-35 percent as shown in Table 2.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The chemical composition of the copper-separating slag used in the examples of the present invention is shown in the following table 1:
TABLE 1 composition table of raw materials of copper slag
| element(s) | Cu | Ag | Ba | Pb | Te | Sn |
| content (wt.) | 2.88％ | 14.9％ | 16.43％ | 16.06％ | 3.64％ | 8.83％ |
。
example 1:
Step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
Step 2, mixing 1mol/L sodium hydroxide solution and 8g sodium chlorate to prepare mixed feed liquid;
and 3, placing the mixed material liquid obtained in the step 2 in an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the ultrasonic power to be 150W and the liquid-solid ratio to be 9:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 150r/min and under the reaction condition of 30 min.
and 4, taking out the solution obtained in the step 3, leaching at normal pressure for 20min, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 87.98%.
example 2:
Step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
Step 2, mixing sodium hydroxide solution with the concentration of 1.2mol/L and 12g of sodium chlorate to prepare mixed feed liquid;
and 3, placing the mixed material liquid obtained in the step 2 in an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the microwave power to be 700W and the liquid-solid ratio to be 10:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 300r/min and under the reaction condition of 240 s.
And 4, taking out the solution obtained in the step 3, leaching at normal pressure for 20min, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 91.08%.
Example 3:
Step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
Step 2, mixing 1mol/L sodium hydroxide solution and 15g sodium chlorate to prepare mixed feed liquid;
and 3, placing the mixed material liquid obtained in the step 2 in an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the ultrasonic power to be 300W and the microwave power to be 300W and controlling the liquid-solid ratio to be 8:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 300r/min and under the reaction condition of 10 min.
And 4, taking out the solution obtained in the step 3, leaching for 20min at normal pressure, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 90.67%.
Example 4:
step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
Step 2, mixing 0.8mol/L sodium hydroxide solution and 10g sodium chlorate to prepare mixed feed liquid;
and 3, placing the mixed material liquid obtained in the step 2 in an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the ultrasonic power to be 150W and the microwave power to be 450W and controlling the liquid-solid ratio to be 9:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 300r/min and under the reaction condition of 5 min.
and 4, taking out the solution obtained in the step 3, leaching for 20min at normal pressure, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 93.29%.
Example 5:
step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
Step 2, mixing 1.2mol/L sodium hydroxide solution and 15g sodium chlorate to prepare mixed feed liquid;
And 3, placing the mixed material liquid obtained in the step 2 in an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the ultrasonic power to be 450W and the microwave power to be 150W and controlling the liquid-solid ratio to be 9:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 300r/min and under the reaction condition of 15 min.
And 4, taking out the solution obtained in the step 3, leaching for 20min at normal pressure, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 88.3%.
Example 6:
step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
Step 2, mixing 0.6mol/L sodium hydroxide solution and 12g sodium chlorate to prepare mixed feed liquid;
and 3, placing the mixed material liquid obtained in the step 2 in an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the ultrasonic power to be 300W and the microwave power to be 300W and controlling the liquid-solid ratio to be 7:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 300r/min and under the reaction condition of 18.41 min.
And 4, taking out the solution obtained in the step 3, leaching at normal pressure for 20min, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 86.2%.
Example 7:
step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
Step 2, mixing 1.4mol/L sodium hydroxide solution and 15g sodium chlorate to prepare mixed feed liquid;
And 3, placing the mixed material liquid obtained in the step 2 in an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the ultrasonic power to be 150W and the microwave power to be 150W and controlling the liquid-solid ratio to be 9:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 300r/min and under the reaction condition of 5 min.
And 4, taking out the solution obtained in the step 3, leaching at normal pressure for 20min, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 95.3%.
example 8 (comparative experiment):
taking copper anode slime copper-separating residue in a 250mL beaker, pouring 1.2mol/L sodium hydroxide solution according to a liquid-solid ratio of 9:1 (optimal), placing the mixture in a water bath dry pot, starting stirring, slowly adding oxidant sodium chlorate, sealing the opening of the beaker by a plastic film, starting timing, leaching for 2h under normal pressure, taking down the film after leaching reaction is finished, and filtering, wherein the leaching rate of tellurium is only 59.98% by chemical analysis.
TABLE 2 comparison of the process parameters and leach rates for the inventive and comparative examples
| examples | ultrasonic power/w | microwave power/w | leaching time/min | Tellurium leaching rate/%) |
| 1 | 150 | 0 | 50 | 88 |
| 2 | 0 | 700 | 24 | 91.1 |
| 3 | 300 | 300 | 30 | 90.7 |
| 4 | 150 | 450 | 25 | 93.3 |
| 5 | 450 | 150 | 35 | 88.3 |
| 6 | 300 | 300 | 38 | 86.2 |
| 7 | 150 | 150 | 25 | 95.3 |
| conventional methods | 0 | 0 | 120 | 59.9 |
As can be seen from Table 2, compared with the traditional hydrometallurgy, the method disclosed by the invention has the advantages that the reaction time is greatly shortened and the leaching rate of tellurium is remarkably improved by researching the strong oxidation of tellurium in copper slag under the alkaline condition through the cooperation of the ultrasonic wave and the microwave.
Claims (6)
1. A method for efficiently leaching tellurium from copper separating slag of copper anode slime strengthened by external field action is characterized by comprising the following steps:
Step 1, grinding a copper slag raw material;
step 2, mixing sodium hydroxide serving as a leaching solution and sodium chlorate serving as an oxidant with the raw materials in the step 1 to prepare a mixed material liquid;
Step 3, placing the mixed material liquid obtained in the step 2 on an ultrasonic-microwave synergistic reaction workstation, setting ultrasonic power and microwave power parameters, and continuously stirring according to a certain liquid-solid ratio under the reinforcing action of ultrasonic waves or microwaves or an ultrasonic-microwave synergistic external field to carry out leaching reaction;
Step 4, taking out the solution obtained in the step 3, leaching for 1-30min at normal pressure, discharging, carrying out suction filtration on the obtained solution, and carrying out suction filtration to obtain a tellurium-containing leaching solution;
The concentration of the sodium hydroxide in the step 2 is 0.4-1.4mol/L, and the addition amount of the sodium chlorate is 0.8-1.5 times of the actual addition amount of the copper slag raw material;
In the step 3, the ultrasonic power is 0-500W, the microwave power is 0-700W, and the liquid-solid ratio is 4-10: 1.
2. The method for efficiently leaching tellurium from copper separation slag of copper anode slime reinforced by external field action as claimed in claim 1, which is characterized in that the main chemical reactions are as follows:
3TeO2+6OH-+ClO3 -＝3TeO4 2-+3H2O+Cl-；
3Pb5TeO7+36OH-+ClO3 -＝3TeO4 2-+15PbO2 2-+Cl-+18H2O。
3. The method for efficiently leaching tellurium from copper separation slag of copper anode slime strengthened by external field action as claimed in claim 1, which is characterized in that: grinding the raw materials of the copper slag in the step 1 to be more than 200 meshes.
4. the method for efficiently leaching tellurium from copper-separated slag of external field enhanced copper anode slime as claimed in claim 1, wherein the stirring speed in step 3 is 100-300 r/min.
5. the method for efficiently leaching tellurium from copper separation slag of external field effect reinforced copper anode slime as claimed in claim 1, wherein the mass percentages of the main components of the copper separation slag in step 1 are as follows: pb: 15-16.06%, Ag: 14-14.9%, Ba: 14-16.43%, Sn: 8-9.02%, Te: 3-3.64%, Cu: 2 to 2.88 percent.
6. the method for efficiently leaching tellurium from copper separation slag of copper anode slime strengthened by external field effect as claimed in claim 1, which is characterized by comprising the following steps:
step 1, grinding 10g of copper slag raw materials to more than 200 meshes;
step 2, mixing 1.4mol/L sodium hydroxide solution and 15g sodium chlorate to prepare mixed feed liquid;
Step 3, placing the mixed material liquid obtained in the step 2 on an ultrasonic-microwave synergistic reaction workstation, setting basic parameters of the ultrasonic-microwave synergistic reaction workstation, controlling the ultrasonic power to be 150W, the microwave power to be 150W and the liquid-solid ratio to be 9:1, starting a stirrer, and carrying out leaching reaction at the stirring speed of 300r/min and under the reaction condition of 5 min;
and 4, taking out the solution obtained in the step 3, leaching for 20min at normal pressure, discharging, and performing suction filtration to obtain a tellurium-containing leaching solution, wherein the tellurium leaching rate is 95.3%.
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| CN112961990A (en) * | 2021-02-01 | 2021-06-15 | 昆明理工大学 | Method for extracting platinum, palladium and gold from copper anode mud by ultrasonic enhanced ozone |
| CN113373314A (en) * | 2021-06-17 | 2021-09-10 | 安徽工业大学 | Method for efficiently recycling scattered metal tellurium from cuprous telluride residues |
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