CN114622099A - Comprehensive recovery and safe disposal method for high-arsenic material in copper smelting - Google Patents
Comprehensive recovery and safe disposal method for high-arsenic material in copper smelting Download PDFInfo
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- CN114622099A CN114622099A CN202210262882.3A CN202210262882A CN114622099A CN 114622099 A CN114622099 A CN 114622099A CN 202210262882 A CN202210262882 A CN 202210262882A CN 114622099 A CN114622099 A CN 114622099A
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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
- C22B7/02—Working-up flue dust
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
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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
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
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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
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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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
- C22B7/007—Wet processes by acid leaching
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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
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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Abstract
The invention discloses a comprehensive recovery and safe disposal method of a high-arsenic material in copper smelting, which comprises the following steps: step one, obtaining high-arsenic soot generated in copper smelting; secondly, adding alkali liquor and oxygen into the high-arsenic soot for pressure alkali leaching; step three, filtering to obtain leaching slag and leaching liquid; adding excessive calcium oxide into the leachate to generate calcium arsenate, and then sequentially drying, pelletizing and reducing to obtain metal arsenic and calcium oxide; and step five, performing acid leaching on the leachate by using excessive sulfuric acid to obtain a copper sulfate and zinc sulfate mixed solution and lead-bismuth slag. By designing different alkali liquor concentrations, solid-to-liquid ratios, oxygen partial pressures and the like, the leaching efficiency of arsenic and other metals in the high-arsenic soot is effectively improved, the arsenic and other metals are fully recovered, the pollution of the arsenic to the environment is effectively avoided, and the resource recovery is fully performed.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of arsenic treatment, in particular to a comprehensive recovery and safe disposal method of a high-arsenic material in copper smelting.
[ background of the invention ]
Copper is a non-ferrous metal which is very closely related to human beings, has rich natural resources and excellent electrical conductivity, thermal conductivity, ductility, corrosion resistance and wear resistance, and is widely applied to the fields of electric power, electronics, energy, petrochemicals, machinery, metallurgy, traffic, light industry, emerging industries and the like.
Arsenic is one of the main associated elements in copper ore, and although arsenic minerals are inhibited to the greatest extent in the ore dressing process and enter tailings, part of arsenic enters a smelting system along with copper concentrate. Moreover, the arsenic content in copper ore is increasing with the consumption of high quality resources. Arsenic is widely distributed in a copper smelting system, almost all intermediate products contain arsenic, and the arsenic is enriched in materials such as soot and the like through a complex smelting impurity removal process. Arsenic compounds are highly toxic and if not handled properly, the toxicity is released and poses a significant threat to the environment and human health. Such arsenic contamination incidents occur mostly in mining areas or in smelters centrally. At present, materials such as high-arsenic soot and the like can only be stockpiled in many smelting plants due to high treatment difficulty and high cost, but the stockpiling method cannot solve the practical problem.
[ summary of the invention ]
In order to solve the technical problems, the invention discloses a comprehensive recovery and safe disposal method of a high-arsenic material in copper smelting. By designing different alkali liquor concentrations, solid-to-liquid ratios, oxygen partial pressures and the like, the leaching efficiency of arsenic and other metals in the high-arsenic soot is effectively improved, the arsenic and other metals are fully recovered, the pollution of the arsenic to the environment is effectively avoided, and the resource recovery is fully performed.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a comprehensive recovery and safe disposal method of high-arsenic materials in copper smelting comprises the following steps:
step one, obtaining high-arsenic soot generated in copper smelting;
secondly, adding alkali liquor and oxygen into the high-arsenic soot for pressure alkali leaching;
step three, filtering to obtain leaching slag and leaching liquid;
step four, adding excessive calcium oxide into the leachate to generate calcium arsenate, and then sequentially drying, pelletizing and reducing to obtain metal arsenic and calcium oxide;
step five, performing acid leaching on the leachate by using excessive sulfuric acid to obtain a mixed solution of copper sulfate and zinc sulfate and lead-bismuth slag;
step six, extracting and separating the mixed solution of copper sulfate and zinc sulfate to obtain copper sulfate and zinc sulfate, and carrying out copper electrodeposition on the copper sulfate to obtain metal copper and sulfuric acid; the zinc sulfate reacts with excess sodium carbonate to produce a basic zinc carbonate precipitate and a sodium sulfate solution.
In the second step, in the process of pressurized alkaline leaching, the alkali liquor is NaOH solution, the liquid-solid ratio is 10:1ml/g, and the concentration of NaOH in the NaOH solution is 60 g/L.
In the second step, the temperature is 150 ℃, the oxygen partial pressure is 0.8MPa, and the alkaline leaching is performed for 1 h.
In a further improvement, in the fourth step, metallic arsenic is obtained by vacuum reduction.
In a further improvement, the lead-bismuth slag is recovered by a fire method.
By designing different alkali liquor concentrations, solid-to-liquid ratios, oxygen partial pressures and the like, the leaching efficiency of arsenic and other metals in the high-arsenic soot is effectively improved, the arsenic and other metals are fully recovered, the pollution of the arsenic to the environment is effectively avoided, and the resource recovery is fully performed.
[ description of the drawings ]
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention to its proper form. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is the effect of NaOH concentration on leaching rate at a liquid-to-solid ratio of 6: 1;
FIG. 3 is the effect of NaOH concentration on leaching rate at a liquid-to-solid ratio of 8: 1;
FIG. 4 is the effect of NaOH concentration on leaching rate at a liquid-to-solid ratio of 10: 1;
FIG. 5 is a graph showing the effect of alkaline leaching time on leaching rate;
FIG. 6 is the effect of temperature on leaching rate;
FIG. 7 is a graph showing the effect of oxygen partial pressure on leaching rate.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
(1) Influence of NaOH concentration and liquid-to-solid ratio
The fixed soot amount was 100g, the stirring speed was 200rpm, the leaching time was 2 hours, the temperature was 110 ℃, the oxygen partial pressure was 0.5MPa, and the leaching rates of As, Zn, Cu and Pb were examined at different NaOH concentrations and liquid-solid ratios, and the results are shown in fig. 2 to 4.
As can be seen from FIGS. 2 to 4, increasing the NaOH concentration and the liquid-solid ratio all have different degrees of promotion effects on As, Zn, Cu and Pb leaching. When the liquid-solid ratio is 6:1, the concentration of NaOH is increased from 40g/L to 100g/L, the leaching rate of As is increased from 66.53% to 90.30%, the leaching rates of Zn, Cu and Pb are also increased, and when the concentration of NaOH is 80g/L, a better selective leaching effect can be obtained. When the liquid-solid ratio is increased to 8:1, the leaching rate of As reaches 84.82% when the concentration of NaOH reaches 60g/L, and the leaching rates of Zn, Cu and Pb are respectively 5.23%,
1.69 percent and 1.52 percent, the leaching rates of Zn and Pb are obviously increased by increasing the concentration of NaOH, and ideal selective separation is difficult to achieve. When the liquid-solid ratio is increased to 10:1 and the NaOH concentration reaches 60g/L, the leaching rate of As reaches 89.17%, and the leaching rates of Zn, Cu and Pb at this time are 7.96%, 2.17% and 6.26%, respectively, although increasing the NaOH concentration helps leaching of arsenic, Zn, Cu and Pb are also leached. From the viewpoint of improving the effect of separating As from Zn, Cu and Pb, the liquid-solid ratio was 10:1, and the NaOH concentration was 60g/L As appropriate, and the leaching rates of As, Zn, Cu and Pb were 89.17%, 7.96%, 2.17% and 6.26%, respectively.
(2) Effect of Leaching time
The amount of the fixed soot used was 100g, the stirring speed was 200rpm, the NaOH concentration was 60g/L, the liquid-solid ratio was 10:1, the temperature was 110 ℃ and the oxygen partial pressure was 0.5MPa, and the results of examining the leaching rates of As, Zn, Cu and Pb at different times are shown in FIG. 5.
The results show that the alkaline leaching dearsenification reaction proceeds faster. After reacting for 1h, the leaching rate of As reaches more than 88 percent; and then, the reaction time is continuously prolonged, the fluctuation range of the As leaching rate is small, but the leaching rate of Zn is slightly increased. From the comprehensive consideration of improving the working efficiency, reducing the production cost, increasing the leaching rate of As, and the like, the optimal leaching time is determined to be 1h, and the leaching rates of As, Zn, Cu and Pb are respectively 89.27%, 3.50%, 2.16% and 8.37%.
(3) Influence of temperature
The fixed soot dosage of 100g, the stirring speed of 200rpm, the NaOH concentration of 60g/L, the liquid-solid ratio of 10:1, the leaching time of 1h and the oxygen partial pressure of 0.5MPa, and the leaching rates of As, Zn, Cu and Pb at different temperatures are examined, and the results are shown in FIG. 6.
The test results show that an increase in temperature favors the leaching reaction. When the leaching temperature is increased from 90 ℃ to 150 ℃, the leaching rate of As is quickly increased from 86.15% to 94.45%, and the temperature is continuously increased, so that the leaching rate of As is not obviously increased; the leaching rate of Pb has small increase along with the temperature rise, and the leaching rates of Cu and Zn are always in a lower range. Comprehensively considering the aspects of energy consumption, As leaching rate and the like, the optimal leaching temperature is determined to be 150 ℃, and the leaching rates of As, Zn, Cu and Pb are respectively 94.45 percent and 7.02 percent at the time,
4.03% and 11.27%.
(4) Influence of oxygen partial pressure
The fixed soot dosage is 100g, the stirring speed is 200rpm, the NaOH concentration is 60g/L, the liquid-solid ratio is 10:1, the leaching time is 1h, the temperature is 150 ℃, the leaching rates of As, Zn, Cu and Pb under different oxygen partial pressure conditions are examined, and the result is shown in FIG. 7.
As is clear from FIG. 7, the leaching rate of As slightly increased with the increase in oxygen partial pressure, and stabilized at 94% or more at oxygen partial pressure >0.6 MPa. The leaching rate of Pb tends to decrease with the increase of the oxygen partial pressure, when the oxygen partial pressure is
When the pressure is 0.8MPa, the leaching rate is 8.07 percent, and the leaching rate is reduced by about 9 percent compared with the leaching rate when the oxygen partial pressure is 0.2 MPa. The leaching rates of Cu and Zn are kept stable along with the change of the oxygen partial pressure. Therefore, 0.8MPa was selected As the optimum oxygen partial pressure, at which the leaching rates of As, Zn, Cu and Pb were 94.37%, 5.13%, 3.86% and 8.07%, respectively.
According to the alkaline leaching condition test, the optimal small test conditions are as follows: the concentration of NaOH is 60g/L, the liquid-solid ratio is 10:1, the reaction time is 1h, the reaction temperature is 150 ℃, and the oxygen partial pressure is 0.8 MPa.
(5) Comprehensive condition test
400g of soot was used for a comprehensive condition test under the conditions of 60g/L NaOH concentration, 10:1 liquid-solid ratio, 1h reaction time, 150 ℃ reaction temperature, 0.8MPa oxygen partial pressure, and the test results are shown in tables 2-9. As shown in the table, the leaching rate of As in the oxygen pressure alkaline leaching process can reach 94.57%, while the leaching rates of Pb, Zn, Cu and Bi are respectively 5.48%, 7.39%, 2.52% and 0.14%, so that the ideal selective arsenic removal effect can be achieved, and a small amount of lead and zinc in the leaching solution can be removed by an oxidation precipitation or a sulfide precipitation method.
TABLE 1 test results of soot oxygen pressure alkaline leaching comprehensive conditions
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any simple modification, equivalent change and modification made by those skilled in the art according to the technical spirit of the present invention without departing from the technical scope of the present invention are all within the scope of the present invention.
Claims (5)
1. A comprehensive recovery and safe disposal method of high-arsenic materials in copper smelting is characterized by comprising the following steps:
step one, obtaining high-arsenic soot generated in copper smelting;
secondly, adding alkali liquor and oxygen into the high-arsenic soot for pressure alkali leaching;
step three, filtering to obtain leaching slag and leaching liquid;
adding excessive calcium oxide into the leachate to generate calcium arsenate, and then sequentially drying, pelletizing and reducing to obtain metal arsenic and calcium oxide;
step five, performing acid leaching on the leachate by using excessive sulfuric acid to obtain a copper sulfate and zinc sulfate mixed solution and lead-bismuth slag;
step six, extracting and separating the mixed solution of copper sulfate and zinc sulfate to obtain copper sulfate and zinc sulfate, and carrying out copper electrodeposition on the copper sulfate to obtain metal copper and sulfuric acid; the zinc sulfate reacts with excess sodium carbonate to produce a basic zinc carbonate precipitate and a sodium sulfate solution.
2. The method for comprehensively recovering and safely disposing the high-arsenic material in the copper smelting process as claimed in claim 1, wherein in the second step, in the pressure alkaline leaching process, the alkali liquor is NaOH solution, the liquid-solid ratio is 10:1ml/g, and the concentration of NaOH in the NaOH solution is 60 g/L.
3. The method for comprehensively recovering and safely disposing the high-arsenic material in the copper smelting process as claimed in claim 1, wherein in the second step, the temperature is 150 ℃, the oxygen partial pressure is 0.8MPa, and the alkaline leaching is performed for 1 h.
4. The method for comprehensively recovering and safely disposing the high-arsenic material in the copper smelting process as claimed in claim 1, wherein in the fourth step, the metallic arsenic is obtained by vacuum reduction.
5. The method for comprehensively recovering and safely disposing the high-arsenic material in the copper smelting process as claimed in claim 1, wherein the lead-bismuth slag is recovered by a fire-feeding method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210262882.3A CN114622099A (en) | 2022-03-17 | 2022-03-17 | Comprehensive recovery and safe disposal method for high-arsenic material in copper smelting |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11199231A (en) * | 1997-12-26 | 1999-07-27 | Nippon Mining & Metals Co Ltd | Production of calcium arsenate |
| JP2007297243A (en) * | 2006-04-28 | 2007-11-15 | Dowa Holdings Co Ltd | Arsenic-containing material treatment method |
| CN102212701A (en) * | 2011-05-31 | 2011-10-12 | 江西南城鑫业环保处置有限公司 | Method for recovering metallic copper and zinc from copper smelting ash |
| CN103255289A (en) * | 2013-05-22 | 2013-08-21 | 昆明理工大学 | Method for removing arsenic matte by alkaline leaching at oxygen pressure and recovering arsenic |
| CN105567978A (en) * | 2016-01-28 | 2016-05-11 | 浙江新时代中能循环科技有限公司 | Method for recycling copper, zinc, cobalt and nickel from various kinds of nonferrous metal containing waste |
| CN106555058A (en) * | 2016-10-29 | 2017-04-05 | 郴州市金贵银业股份有限公司 | A kind of technique for processing high arsenic-and copper-bearing material |
| CN106756058A (en) * | 2016-12-21 | 2017-05-31 | 中南大学 | A kind of dearsenification from arsenic-containing smoke dust and its method for solidification |
| CN106834705A (en) * | 2016-11-18 | 2017-06-13 | 河南中原黄金冶炼厂有限责任公司 | A kind of method of copper smelting by pyrometallurgy white cigarette dust resources comprehensive utilization |
| CN106893864A (en) * | 2017-03-24 | 2017-06-27 | 中南大学 | A kind of method that arsenic is reclaimed in the mud from black copper |
| CN107338454A (en) * | 2017-07-19 | 2017-11-10 | 中南大学 | A kind of method that copper and arsenic are reclaimed from white metal |
-
2022
- 2022-03-17 CN CN202210262882.3A patent/CN114622099A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11199231A (en) * | 1997-12-26 | 1999-07-27 | Nippon Mining & Metals Co Ltd | Production of calcium arsenate |
| JP2007297243A (en) * | 2006-04-28 | 2007-11-15 | Dowa Holdings Co Ltd | Arsenic-containing material treatment method |
| CN102212701A (en) * | 2011-05-31 | 2011-10-12 | 江西南城鑫业环保处置有限公司 | Method for recovering metallic copper and zinc from copper smelting ash |
| CN103255289A (en) * | 2013-05-22 | 2013-08-21 | 昆明理工大学 | Method for removing arsenic matte by alkaline leaching at oxygen pressure and recovering arsenic |
| CN105567978A (en) * | 2016-01-28 | 2016-05-11 | 浙江新时代中能循环科技有限公司 | Method for recycling copper, zinc, cobalt and nickel from various kinds of nonferrous metal containing waste |
| CN106555058A (en) * | 2016-10-29 | 2017-04-05 | 郴州市金贵银业股份有限公司 | A kind of technique for processing high arsenic-and copper-bearing material |
| CN106834705A (en) * | 2016-11-18 | 2017-06-13 | 河南中原黄金冶炼厂有限责任公司 | A kind of method of copper smelting by pyrometallurgy white cigarette dust resources comprehensive utilization |
| CN106756058A (en) * | 2016-12-21 | 2017-05-31 | 中南大学 | A kind of dearsenification from arsenic-containing smoke dust and its method for solidification |
| CN106893864A (en) * | 2017-03-24 | 2017-06-27 | 中南大学 | A kind of method that arsenic is reclaimed in the mud from black copper |
| CN107338454A (en) * | 2017-07-19 | 2017-11-10 | 中南大学 | A kind of method that copper and arsenic are reclaimed from white metal |
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