CN113462898B - Oxygen pressure leaching zinc smelting purification impurity removal process - Google Patents
Oxygen pressure leaching zinc smelting purification impurity removal process Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B17/00—Obtaining cadmium
- C22B17/04—Obtaining cadmium by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
- C22B23/0469—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods by chemical substitution, e.g. by cementation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a novel oxygen pressure leaching zinc smelting purification impurity removal process, which comprises the steps of firstly adding electrolytic waste liquid into iron-removed liquid to adjust the pH value of the solution, then adding second-stage purification slag, and controlling reaction conditions to produce first-stage purification slag and first-stage purification liquid. And adding the electrolytic waste liquid and the zinc powder into the first-stage purified liquid to produce a second-stage purified liquid and second-stage purified slag, returning the second-stage purified slag to the liquid after iron removal as a purifying agent, and feeding the second-stage purified liquid into a third-stage purifying tank to remove residual cadmium. The process returns the second-stage purification slag to the first-stage purification to be used as a purifying agent for the first-stage purification operation, can reduce the unit consumption of zinc powder and the amount of slag generated by purification, reduces the production cost, facilitates the comprehensive treatment of downstream procedures, and has the advantages of low addition of zinc powder, thorough purification and impurity removal and the like.
Description
Technical Field
The invention relates to the technical field of chemical metallurgy treatment, in particular to a process for smelting, purifying and removing impurities by using oxygen pressure leaching zinc in the field of wet metallurgy.
Background
The oxygen pressure leaching process is to react zinc concentrate in an oxygen pressure leaching kettle to generate zinc sulfate solution and sulfur simple substance, and the produced sulfur is more convenient to store and transport than sulfuric acid produced by the traditional process, so the oxygen pressure leaching process slowly becomes the mainstream of zinc smelting. However, the leachate produced by oxygen pressure leaching has certain difference from the traditional roasting leachate, especially in the aspects of ionic valence state and the like. And (3) producing iron-removed liquid after iron removal from leachate produced by oxygen pressure leaching, wherein the valence states of Zn, Cd, Co, Ni and the like in the iron-removed liquid are different from those of the traditional iron-removed liquid. The traditional process comprises a forward antimonate purification process and a reverse antimonate purification process, wherein the forward antimonate purification process is to add zinc powder to produce a first section of purification slag, namely copper-cadmium slag, in a first section of purification process, and add zinc powder, copper sulfate and antimonate to produce a second section of purification slag, namely nickel-cobalt slag, in a second section of purification process. Reverse antimonate purification is to remove nickel and cobalt in one stage and produce nickel and cobalt slag, and remove copper and cadmium in the second stage and produce copper and cadmium slag. The unit consumption of zinc powder in the traditional purification process is high, the average level in the industry is 60kg of zinc powder/t.Zn, and meanwhile, the amount of added antimonate can influence the downstream electrodeposition. In the traditional process, the pH value of the deironing liquid is 5.0-5.2, then the temperature is controlled to be 55-60 ℃ by cooling through a cooling tower, zinc powder is added according to 8-12 times of the content of cadmium and copper in the liquid, and the reaction time is 1-1.5. The obtained first-stage purification slag contains 36.8-45% of zinc, 5.6-6.2% of copper, 10.6-12% of cadmium and about 0.08% of cobalt. The obtained second-stage purification slag contains 58.26% of zinc, wherein the proportion of simple substance zinc is 80%, cadmium is 2-4%, and cobalt is 0.2-0.3%. The high proportion of the simple substance zinc in the second-stage purification slag results in large consumption of zinc powder in the purification process, and the obtained first-stage purification slag and second-stage purification slag need to be separately and independently treated to recover zinc, copper and cadmium therein.
In order to reduce the unit consumption of zinc powder and produce high-quality purified liquid, and avoid the influence on electrodeposition, the development of a new technology for smelting, purifying and removing impurities of zinc by oxygen pressure leaching has great practical significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel oxygen pressure leaching zinc smelting purification impurity removal process which has the advantages of simple process, less unit consumption of zinc powder and lower cost, can effectively reduce the impurities of copper, cadmium, cobalt and nickel in the solution and can avoid the influence on downstream electrodeposition caused by adding antimony salt.
In order to solve the technical problems, the invention adopts the following technical scheme: a novel oxygen pressure leaching zinc smelting purification impurity removal process is characterized in that: the method comprises the following steps:
step 1: adding the electrolytic waste liquid into the liquid after iron removal, and adjusting the pH value of the solution to 4.5-4.8; then adding the second-stage purification slag, controlling the reaction temperature to be 60-65 ℃ and the reaction time to be 1.5-2 h; after the reaction is finished, carrying out solid-liquid separation to obtain a first-stage purified liquid and a first-stage purified slag. In the traditional process, the pH value of the deironing liquid is 5.0-5.2, then the temperature is controlled to be 55-60 ℃ by cooling through a cooling tower, zinc powder is added according to 8-12 times of the content of cadmium and copper in the liquid, and the reaction time is 1-1.5. Compared with the prior art, the method has the advantages that zinc powder is not added in the first-stage purification, the zinc powder is replaced by adding the second-stage purification slag, and the qualified first-stage purification solution is replaced by utilizing the excessive zinc powder in the second-stage slag.
Step 2: pumping the first-stage purification liquid obtained in the step 1 to a first-stage purification tank, adding electrolytic waste liquid to adjust the pH value to 4.8-5.0, adding zinc powder, wherein the adding amount of the zinc powder is 300 times of the cobalt content, controlling the reaction temperature to be 80-85 ℃, and reacting for 2-2.5 hours; and after the reaction is finished, carrying out solid-liquid separation to obtain second-stage purification slag and second-stage purification liquid. The pH value of the traditional process is 5.0-5.2, the reaction temperature is 85-90 ℃, and the reaction time is 2.5-3 h.
And step 3: pumping the two-stage purified liquid obtained in the step (2) to a three-stage purifying tank, adding zinc powder, wherein the adding amount of the zinc powder is 8-12 times of the cadmium content, the reaction temperature is 65-75 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain three-stage purified slag and three-stage purified liquid; and conveying the three sections of purified liquid to an electrolysis process for electrolyzing zinc, combining the three sections of purified slag and the first section of purified slag, and conveying the combined three sections of purified slag and the first section of purified slag to a comprehensive recovery process for recovering copper, cadmium and cobalt.
In step 1, the liquid after iron removal is the liquid after iron removal produced by the leaching solution produced by the oxygen pressure leaching process and the goethite iron removal method, and the pH value is about 5.0.
In the step 2, all the second-stage purification slag produced by the second-stage purification is returned to the first-stage purification to be used as a purifying agent in the first-stage purification process.
The electrolytic waste liquid in the step 1 contains H + ：165-175g/L、Zn 2+ ：50-55g/L。
The two-stage purification slag in the step 1 and the step 2 is two-stage purification slag obtained by a reverse antimony salt purification method, namely nickel-cobalt slag, the main component of which is excessive zinc powder, the content of simple substance zinc is 50-56%, cadmium is 4-6%, cobalt is 0.05-0.07%, and lead is 10-15%.
The first-stage purifying liquid in the step 1 contains Zn 2+ ：140-165g/L、Cu 2+ ＜0.0005g/L、 Cd 2+ Less than 0.1g/L, Co, 10-16 g/L. Of course, the above data may vary depending on the content of valuable metals in the ore; the main components of the first stage purification slag comprise: 17-23% of Zn, 3-5% of Pb, 7-13% of Cu and 7-13% of Cd.
The component of the two-stage purifying liquid in the step 2 comprises Zn 2+ ：145-165g/L、Cu 2+ ＜0.0005g/L、 Cd 2+ ：0.001-0.004g/L、Co＜0.0005g/L。
The three-stage purification slag in the step 3 contains 15-20% of zinc and can also contain trace cadmium.
The three-stage purification solution in the step 3 contains Zn 2+ :145-165g/L、Cu 2+ ＜0.0005g/L、Cd 2+ ＜ 0.001g/L、Co＜0.0005g/L。
Compared with the traditional purification and impurity removal process, the process has the following advantages:
firstly, the second-stage purification slag is completely returned to the first-stage purification to be used as a first-stage purification purifying agent, and then the zinc powder of the traditional purification impurity removal process is replaced, so that the adding amount of the zinc powder is effectively reduced. The control parameters of the invention are combined, and the ion activity is utilized to control the reaction of nickel and cobalt in the second-stage purification slag and sulfuric acid in the iron-removed liquid in the reaction to enter the first-stage purification liquid again;
before adding the second-stage purification slag and the zinc powder, the pH of the solution is adjusted by using the electrolytic waste liquid, and the acidity is lower after the adjustment, so that the zinc powder and the second-stage purification slag are more favorable for the replacement reaction with elements such as copper, cadmium, cobalt, nickel and the like in the solution;
thirdly, the first-stage purification slag produced by the process contains copper, cadmium, cobalt and nickel, so that the metals such as copper, cadmium, cobalt and the like can be conveniently and comprehensively recovered in the subsequent process, and the copper, cadmium, cobalt and nickel slag can be simultaneously treated.
Fourthly, the electrolytic waste liquid is added in the two-stage purification process, the zinc powder is added, and the addition of activators such as copper sulfate, antimonite and the like in the traditional process is avoided by controlling parameters, so that the subsequent influence on electrodeposition is avoided.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further illustrated by the following specific examples in conjunction with figure 1:
example 1: the components of the liquid after iron removal by oxygen pressure leaching are as follows:
| element(s) | Zn | Cu | Cd | Co |
| Content (g/L) | 145 | 0.27 | 1.12 | 0.014 |
The method comprises the following steps:
step 1: adding the waste electrolyte to the solution (150 m) after iron removal 3 ) Adjusting the pH value of the solution to 4.5; then adding two-stage purification slag, controlling the reaction temperature at 60 ℃ and the reaction time at 2 h; after the reaction is finished, carrying out solid-liquid separation to obtain a first-stage purified liquid and a first-stage purified slag;
and 2, step: pumping the first section of purified liquid obtained in the step 1 to a first section of purifying tank, adding the electrolytic waste liquid to adjust the pH value to 5.0, adding zinc powder, wherein the adding amount of the zinc powder is 300 times (namely 630kg) of the cobalt content, controlling the reaction temperature to be 85 ℃, and reacting for 2 hours; after the reaction is finished, carrying out solid-liquid separation to obtain second-stage purification slag and second-stage purification liquid;
and 3, step 3: pumping the second-stage purified liquid obtained in the step 2 to a third-stage purifying tank, and adding zinc powder, wherein the adding amount of the zinc powder is 8 times (namely 1.344t) of the cadmium content (the adding amount is converted into 0.004g/L of cadmium after secondary purification); the reaction temperature is 70 ℃, and after the reaction is finished, solid-liquid separation is carried out to obtain three-stage purification slag and three-stage purification liquid. And conveying the three sections of purified liquid to an electrolysis process for electrolyzing zinc, combining the three sections of purified slag and the first section of purified slag, and conveying the combined three sections of purified slag and the first section of purified slag to a comprehensive recovery process for recovering copper, cadmium and cobalt.
As a result: the main components of the first-stage purification slag and the third-stage purification liquid produced by the process are as follows:
| element(s) | Zn | Cu | Cd | Co |
| First stage purification residue content (%) | 32.9 | 5.46 | 10.6 | 0.073 |
| Three-stage purification liquid content (g/L) | 148 | 0.00047 | 0.0009 | 0.00043 |
The impurity contents of copper, cadmium and cobalt in the produced three-stage purifying liquid all meet the electrodeposition requirement. The removal rate is [1- (Me content in the three-stage purified liquid/Me content in the liquid after iron removal by oxygen pressure leaching) ]. 100%, and Me represents the metal content. Wherein the removal rate of copper is 99.8%, the removal rate of cadmium is 99.9%, and the removal rate of cobalt is 96.9%.
Example 2: the components of the liquid after iron removal by oxygen pressure leaching are as follows:
| element(s) | Zn | Cu | Cd | Co |
| Content (g/L) | 145.5 | 0.23 | 1.15 | 0.016 |
The method comprises the following steps:
step 1: adding the waste electrolyte into the solution (100 m) after iron removal 3 ) Adjusting the pH value of the solution to 4.8; then adding two-stage purification slag, controlling the reaction temperature to 64 ℃ and the reaction time to 1.5 h; after the reaction is finished, carrying out solid-liquid separation to obtain a first-stage purified liquid and a first-stage purified slag;
step 2: pumping the first section of purified liquid obtained in the step 1 to a first section of purifying tank, adding the electrolytic waste liquid to adjust the pH value to 4.8, adding zinc powder, wherein the adding amount of the zinc powder is 300 times (480kg) of the cobalt content, controlling the reaction temperature to be 85 ℃, and the reaction time to be 2.5 hours; after the reaction is finished, carrying out solid-liquid separation to obtain second-stage purification slag and second-stage purification liquid;
and step 3: pumping the second-stage purified liquid obtained in the step 2 to a third-stage purifying tank, and adding zinc powder, wherein the adding amount of the zinc powder is 12 times of the cadmium content (1380 kg); the reaction temperature is 70 ℃, and after the reaction is finished, solid-liquid separation is carried out to obtain three-stage purification slag and three-stage purification liquid. And conveying the three sections of purified liquid to an electrolysis process for electrolyzing zinc, combining the three sections of purified slag and the first section of purified slag, and conveying the combined three sections of purified slag and the first section of purified slag to a comprehensive recovery process for recovering copper, cadmium and cobalt.
As a result: the main components of the first-stage purification slag and the third-stage purification liquid produced by the process are as follows:
| element(s) | Zn | Cu | Cd | Co |
| First stage purification residue content (%) | 34.2 | 6.48 | 9.46 | 0.066 |
| Three-stage purification liquid content (g/L) | 148.6 | 0.00067 | 0.00085 | 0.00023 |
The impurity contents of copper, cadmium and cobalt in the produced three-stage purifying liquid all meet the electrodeposition requirement. The removal rate is [1- (Me content in the three-stage purified liquid/Me content in the liquid after iron removal by oxygen pressure leaching) ]. 100%, and Me represents the metal content. Wherein the removal rate of copper is 99.7%, the removal rate of cadmium is 99.9% and the removal rate of cobalt is 98.5%.
While the invention has been described in detail in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
Claims (9)
1. A zinc oxygen pressure leaching smelting purification impurity removal process is characterized in that: the method comprises the following steps:
step 1: adding the electrolytic waste liquid into the liquid after iron removal, and adjusting the pH value of the solution to 4.5-4.8; then adding the second-stage purification slag, controlling the reaction temperature to be 60-65 ℃ and the reaction time to be 1.5-2 h; after the reaction is finished, carrying out solid-liquid separation to obtain a first-stage purified liquid and a first-stage purified slag;
step 2: pumping the first section of purified liquid obtained in the step 1 to a first section of purifying tank, adding electrolytic waste liquid to adjust the pH value to 4.8-5.0, adding zinc powder, wherein the adding amount of the zinc powder is 300 times of the cobalt content, controlling the reaction temperature to be 80-85 ℃, and the reaction time to be 2-2.5 h; after the reaction is finished, carrying out solid-liquid separation to obtain second-stage purification slag and second-stage purification liquid; the electrolytic waste liquid contains H + ：165-175g/L、Zn 2+ ：50-55g/L；
And step 3: pumping the second-stage purified liquid obtained in the step 2 to a third-stage purifying tank, adding zinc powder, wherein the adding amount of the zinc powder is 8-12 times of the cadmium content, the reaction temperature is 65-75 ℃, and after the reaction is finished, carrying out solid-liquid separation to obtain third-stage purified slag and third-stage purified liquid; and conveying the three sections of purified liquid to an electrolysis process for electrolyzing zinc, combining the three sections of purified slag and the first section of purified slag, and conveying the combined three sections of purified slag and the first section of purified slag to a comprehensive recovery process for recovering copper, cadmium and cobalt.
2. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: in step 1, the liquid after iron removal is the liquid after iron removal produced by the leaching solution produced by the oxygen pressure leaching process and the goethite iron removal method, and the pH value is about 5.0.
3. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: in the step 2, all the second-stage purification slag produced by the second-stage purification is returned to the first-stage purification to be used as a purifying agent in the first-stage purification process.
4. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: the two-stage purification slag in the step 1 and the step 2 is two-stage purification slag obtained by a reverse antimonate purification method, namely nickel-cobalt slag, the main component of which is excessive zinc powder, the content of simple substance zinc is 50-56%, cadmium is 4-6%, cobalt is 0.05-0.07%, and lead is 10-15%.
5. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: the first-stage purifying liquid in the step 1 contains Zn 2+ ：140-165g/L、Cu 2+ ＜0.0005g/L、Cd 2+ ＜0.1g/L、Co:10-16g/L。
6. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: the main components of the first stage purification slag in the step 1 comprise: 17-23% of Zn, 3-5% of Pb, 7-13% of Cu and 7-13% of Cd.
7. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: the component of the two-stage purifying liquid in the step 2 comprises Zn 2+ ：145-165g/L、Cu 2+ ＜0.0005g/L、Cd 2+ ：0.001-0.004g/L、Co＜0.0005g/L。
8. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: the three-stage purification slag in the step 3 contains 15-20% of zinc.
9. The oxygen pressure leaching zinc smelting purification impurity removal process according to claim 1, characterized in that: the three-stage purification liquid in the step 3 comprises Zn2 +/145-165 g/L, Cu2+ < 0.0005g/L, Cd2+ < 0.001g/L, Co < 0.0005 g/L.
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| JP2002285253A (en) * | 2001-03-28 | 2002-10-03 | Dowa Mining Co Ltd | Method for leaching zinc concentrate |
| JP2004292901A (en) * | 2003-03-27 | 2004-10-21 | Dowa Mining Co Ltd | Leaching method for zinc concentrate |
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| CN106893872A (en) * | 2016-12-27 | 2017-06-27 | 河南豫光锌业有限公司 | A kind of method of zinc hydrometallurgy deeply purifying and removing cobalt |
| CN112501452A (en) * | 2020-11-05 | 2021-03-16 | 矿冶科技集团有限公司 | Method for purifying zinc mineral material leaching solution |
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| JP2002285253A (en) * | 2001-03-28 | 2002-10-03 | Dowa Mining Co Ltd | Method for leaching zinc concentrate |
| JP2004292901A (en) * | 2003-03-27 | 2004-10-21 | Dowa Mining Co Ltd | Leaching method for zinc concentrate |
| CN106244813A (en) * | 2016-08-29 | 2016-12-21 | 江西铜业股份有限公司 | A kind of zinc abstraction nickel cobalt slag recoverying and utilizing method |
| CN106893872A (en) * | 2016-12-27 | 2017-06-27 | 河南豫光锌业有限公司 | A kind of method of zinc hydrometallurgy deeply purifying and removing cobalt |
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