CN116891949B - Process for recycling three-phase slag produced in wet copper extraction process - Google Patents
Process for recycling three-phase slag produced in wet copper extraction process Download PDFInfo
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- CN116891949B CN116891949B CN202310659291.4A CN202310659291A CN116891949B CN 116891949 B CN116891949 B CN 116891949B CN 202310659291 A CN202310659291 A CN 202310659291A CN 116891949 B CN116891949 B CN 116891949B
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- copper
- phase
- tributyl phosphate
- slag
- extractant
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- 239000010949 copper Substances 0.000 title claims abstract description 91
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 89
- 239000002893 slag Substances 0.000 title claims abstract description 44
- 238000000605 extraction Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title claims abstract description 11
- 239000012071 phase Substances 0.000 claims abstract description 66
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000012074 organic phase Substances 0.000 claims abstract description 27
- 239000007790 solid phase Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 10
- FZENGILVLUJGJX-NSCUHMNNSA-N (E)-acetaldehyde oxime Chemical compound C\C=N\O FZENGILVLUJGJX-NSCUHMNNSA-N 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 2
- 238000005363 electrowinning Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 12
- 239000000839 emulsion Substances 0.000 abstract description 7
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001431 copper ion Inorganic materials 0.000 abstract description 4
- 238000009833 condensation Methods 0.000 abstract description 3
- 229910000365 copper sulfate Inorganic materials 0.000 abstract description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000008346 aqueous phase Substances 0.000 description 5
- 238000002329 infrared spectrum Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- 230000001804 emulsifying effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052627 muscovite Inorganic materials 0.000 description 3
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a process for recycling three-phase slag produced in a wet copper extraction process, which comprises the steps of firstly mixing tributyl phosphate and three-phase slag, and stirring for one time to enable extractant organic phase and emulsion phase in the three-phase slag to enter tributyl phosphate; then standing and separating to obtain a water phase containing copper ions, an organic phase containing an extractant and tributyl phosphate and a solid phase containing copper; and finally, distilling and separating the extractant and the tributyl phosphate from the mixed organic phase by adopting a rotary evaporation-condensation mode, so as to realize the recycling of the tributyl phosphate and the resource utilization of copper in the three-phase slag. The pretreatment of chemical analysis of the substances is realized by separating three-phase slag into an organic phase containing copper extractant, a water phase containing copper sulfate and a solid phase containing copper through physical extraction; tributyl phosphate is selected as a physical extractant, and the repeated utilization of the tributyl phosphate is realized by an evaporation-condensation method, so that the method has the advantages of high efficiency, cleanness, short flow and the like.
Description
Technical Field
The invention relates to the technical field of chemical smelting treatment, in particular to a recycling process for three-phase slag generated in a wet copper extraction process.
Background
In copper extraction processes, an emulsion layer (dirt) or a third phase tends to form between the organic and aqueous phases for a variety of reasons. The solvent extraction interface emulsification often causes adverse effects such as increased extraction production cost, unsmooth process, environmental pollution and the like, and the generation of an emulsifying layer (dirt) or a third phase can not only prevent the interaction between an organic phase and a water phase in the extraction process and influence the balance of copper ions between the two phases and the recovery rate of copper, but also cause the loss of an organic extractant due to the entrainment effect of the third phase and directly influence the unit consumption of the extractant. In order to solve the problem, a centrifugal device or a filter pressing device is generally adopted in the industry to separate three-phase substances, so that the entrained copper extractant and the emulsified slag are separated, but the obtained three-phase slag still contains 25% -30% of the extractant and has higher copper content. The consumption of the copper extractant after the treatment by the method is still 9 kg/t.Cu, and how to further reduce the consumption of the copper extractant is one of the problems of the current industry. The reason for combining the generation of three-phase substances is that iron ions in copper oxide ores are high, the aldoxime extractant is oxidized to cause emulsification, and suspended substances formed by silicon-containing substances in leaching liquid cause emulsification. Three-phase material generation is caused by material fluctuation, and the material is difficult to select, so that recovery of extractant and copper from three-phase slag is an effective method. Meanwhile, the three-phase slag contains both organic phases such as copper extractant and copper-containing inorganic phases, so that the hazardous waste slag produced by copper smelting at present can be piled up only in a hazardous waste warehouse or is entrusted to be disposed of by an external unit, the cost is high, and the great resource waste is caused. Therefore, the resource utilization of the three-phase slag has great practical significance for the copper extraction industry.
Disclosure of Invention
Aiming at the problems that the three-phase slag produced in the copper smelting and extracting process is difficult to treat and difficult to recycle, the invention provides a process which is simpler in process, high in efficiency, clean, environment-friendly and short in flow and can recycle the three-phase slag produced in the wet copper extracting process.
In order to solve the technical problems, the invention adopts the following technical scheme: a process for recycling three-phase slag produced in a wet copper extraction process is characterized by comprising the following steps of: the method comprises the following steps:
Step 1: mixing and stirring the three-phase slag and tributyl phosphate for physical extraction, wherein the control conditions are as follows: the mass ratio of tributyl phosphate to the three-phase slag is 2:1, and the stirring time is 2h at normal temperature. Standing and separating for 1h after the physical extraction is finished to obtain a mixed organic phase, a copper-containing water phase and a copper-containing solid phase;
step 2: and (3) placing the mixed organic phase obtained in the step (1) into a rotary evaporator, and performing reduced pressure distillation to obtain the copper extractant and tributyl phosphate. The control conditions are as follows: 6 to 6.5kPa, the temperature is 65 ℃ to 70 ℃, and the volume ratio of distillate to distilled liquid is 2.2:1;
Step 3: returning the distillate with the main component of tributyl phosphate obtained in the step 2 to the step 1, mixing with the new tributyl phosphate, and continuing to serve as an extractant for physical extraction;
in the step 1, the three-phase slag is three-phase slag dangerous slag obtained by using aldoxime and ketoxime copper extractant in the wet copper extraction process, and emulsifying the extractant to form three-phase substances due to more impurities in the leaching liquid extraction process, and then performing mechanical separation (after filter pressing and centrifugation).
In the step 1, the main component of the copper-containing water phase is CuSO 4 solution, cu is 44.6-46.84g/L, fe is 2.36-3.38g/L, and the copper-containing water phase can be directly returned to a leaching liquid storage tank for carrying out the next step of electrodepositing copper.
In step 1, the copper-containing solid phase contains 21.6-22.42% copper and 0.25-0.36% iron, and the slag can be directly sold.
The invention has the advantages that: 1. because the organic and inorganic mixture in the three-phase slag cannot be directly analyzed and tested, the three-phase slag can be separated into an organic phase containing copper extractant, a water phase containing copper sulfate and a solid phase containing copper through physical extraction, so that the pretreatment of chemical analysis of the substances is realized;
2. Tributyl phosphate is selected as a physical extractant, and the repeated utilization of the tributyl phosphate is realized by an evaporation-condensation method, so that the method is a recyclable, clean and environment-friendly method. The tributyl phosphate, ketoxime and aldoxime extractant are used to be miscible and insoluble in copper sulfate solution, so that three-phase separation can be realized. In addition, the boiling point of tributyl phosphate is 180-183 deg.c under normal pressure, and the boiling point of ketoxime and aldoxime copper extractant is 466.2 deg.c under normal pressure, so that the separation of the two matters may be realized via distillation.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a FTIR spectrum of an organic phase and TBP, from which it is known that the infrared spectrum of the organic phase is consistent with that of tributyl phosphate, and that a symmetrical stretching vibration absorption peak of phosphate group (PO 4) appears at 1022.17cm -1, and that after an emulsion is dissolved by TBP, an extractant enters into TBP to form an organic phase;
FIG. 3 shows an X-ray diffraction pattern of a copper-containing solid phase, from which it is seen that copper in the solid phase is predominantly in the form of CuSO 4（H2 O) and other impurities are predominantly muscovite. Therefore, the water phase copper, the solid phase copper and the extractant in the three-phase slag are effectively separated after physical extraction.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying figures 1-3:
Example 1: weighing 200g of three-phase slag dangerous waste residue obtained by using aldoxime and ketoxime copper extractant in the wet copper extraction process and emulsifying the extractant to form three-phase substances due to more impurities in the leaching liquid extraction process and then carrying out mechanical separation (after filter pressing and centrifugation), wherein the steps are as follows:
Step 1: mixing and stirring the three-phase slag and tributyl phosphate for physical extraction, wherein the control conditions are as follows: the mass ratio of tributyl phosphate to the three-phase slag is 2:1, and the stirring time is 2h at normal temperature. Standing and separating for 1h after the physical extraction is finished to obtain a mixed organic phase, a copper-containing water phase and a copper-containing solid phase;
Step 2: and (3) placing the mixed organic phase obtained in the step (1) into a rotary evaporator, and performing reduced pressure distillation to obtain the copper extractant and tributyl phosphate. The control conditions are as follows: 6.5kPa, the temperature is 65 ℃, and the volume ratio of distillate to distilled liquid is 2.2:1;
Step 3: returning the distillate with the main component of tributyl phosphate obtained in the step 2 to the step 1, mixing with the new tributyl phosphate, and continuing to serve as an extractant for physical extraction;
Results: the infrared diagram of the obtained organic phase and tributyl phosphate is shown in fig. 2, the copper-containing aqueous phase composition is shown in the following table 1, and the copper-containing solid phase composition is shown in the following tables 2 and 3:
As can be seen from Table 1, copper in the copper-containing aqueous phase is 46.84g/L, which is equivalent to the concentration of copper ions in the copper electrolyte, and metallic copper can be produced by electrodeposition after mixing with the copper electrolyte. Copper-containing 22.42% of the copper-containing solid phase, and FIG. 2 shows an infrared spectrum of an organic phase in the emulsion and TBP, wherein the infrared spectrum of the organic phase is consistent with that of tributyl phosphate, and a symmetrical stretching vibration absorption peak of a phosphate group (PO 4) appears at 1022.17cm -1. After the emulsion is dissolved by TBP, the extractant enters TBP to form an organic phase. From the diffraction pattern of fig. 3, copper in the solid phase is mainly in the form of CuSO 4（H2 O), and other impurities are mainly muscovite. Therefore, the water phase copper, the solid phase copper and the extractant in the three-phase slag are effectively separated after physical extraction.
Example 2: weighing 100g of three-phase slag dangerous waste residues obtained by using aldoxime and ketoxime copper extractants in the wet copper extraction process to emulsify the extractants into three-phase substances due to more impurities in the extraction leaching process and then carrying out mechanical separation (after filter pressing and centrifugation), wherein the steps are as follows:
Step 1: mixing and stirring the three-phase slag and tributyl phosphate for physical extraction, wherein the control conditions are as follows: the mass ratio of tributyl phosphate to the three-phase slag is 2:1, and the stirring time is 2h at normal temperature. Standing and separating for 1h after the physical extraction is finished to obtain a mixed organic phase, a copper-containing water phase and a copper-containing solid phase;
Step 2: and (3) placing the mixed organic phase obtained in the step (1) into a rotary evaporator, and performing reduced pressure distillation to obtain the copper extractant and tributyl phosphate. The control conditions are as follows: 6kPa, the temperature is 70 ℃, and the volume ratio of distillate to distilled liquid is 2.2:1;
Step 3: returning the distillate with the main component of tributyl phosphate obtained in the step 2 to the step 1, mixing with the new tributyl phosphate, and continuing to serve as an extractant for physical extraction;
Results: the resulting organic phase and tributyl phosphate infrared plot is shown in FIG. 2, the copper-containing aqueous phase composition is shown in Table 3 below, and the copper-containing solid phase composition is shown in Table 4 below and FIG. 3 below:
as is clear from Table 2, the copper-containing aqueous phase had a copper content of 44.6g/L, which was equivalent to the copper ion content of the copper electrolyte, and the copper electrolyte was mixed with copper to prepare metallic copper by electrodeposition. The copper-containing solid phase contains 21.6% of copper, and FIG. 2 shows an infrared spectrum of an organic phase and TBP in the emulsion, wherein the infrared spectrum of the organic phase is consistent with that of tributyl phosphate, and a symmetrical telescopic vibration absorption peak of a phosphate group (PO 4) appears at 1022.17cm -1. After the emulsion is dissolved by TBP, the extractant enters TBP to form an organic phase. From the diffraction pattern of fig. 3, copper in the solid phase is mainly in the form of CuSO 4（H2 O), and other impurities are mainly muscovite. Therefore, the water phase copper, the solid phase copper and the extractant in the three-phase slag are effectively separated after physical extraction.
The foregoing detailed description of the application has been presented for purposes of illustration and description, but is not intended to limit the scope of the application, i.e., the application is not limited to the details shown and described.
Claims (5)
1. The process for recycling the three-phase slag produced in the wet copper extraction process is characterized in that the three-phase slag produced in the wet copper extraction process is three-phase dangerous slag obtained by using aldoxime and ketoxime copper extractants to emulsify the extractants due to more impurities in the leaching liquid extraction process and then carrying out mechanical separation, and the process comprises the following steps: the method comprises the following steps:
step 1: mixing and stirring the three-phase slag and tributyl phosphate for physical extraction, and standing and separating after the physical extraction is completed to obtain a mixed organic phase, a copper-containing water phase and a copper-containing solid phase;
step 2: placing the mixed organic phase obtained in the step 1 into a rotary evaporator, and performing reduced pressure distillation to obtain a copper extractant and tributyl phosphate;
step 3: and (3) returning the distillate with the main component of tributyl phosphate obtained in the step (2) to the step (1) to be mixed with new tributyl phosphate, and then continuously taking the mixture as an extractant for physical extraction.
2. The process for recycling three-phase slag generated in the wet copper extraction process according to claim 1, wherein the process comprises the following steps: the control conditions for physical extraction in step 1 are: the mass ratio of tributyl phosphate to the three-phase slag is 2:1, the stirring time is 2h at normal temperature, and the three-phase slag is subjected to standing separation for 1h after the physical extraction is completed.
3. The process for recycling three-phase slag generated in the wet copper extraction process according to claim 1, wherein the process comprises the following steps: the main component of the copper-containing water phase is CuSO 4 solution, the Cu content is 44.6-46.84g/L, the Fe content is 2.36-3.38g/L, and the copper-containing water phase can be directly returned to a leaching liquid storage tank for carrying out the next copper electrowinning.
4. The process for recycling three-phase slag generated in the wet copper extraction process according to claim 1, wherein the process comprises the following steps: the copper-containing solid phase contains 21.6-22.42% of copper and 0.25-0.36% of iron.
5. The process for recycling three-phase slag generated in the wet copper extraction process according to claim 1, wherein the process comprises the following steps: in step 1, the conditions for performing reduced pressure distillation are as follows: 6-6.5kPa, the temperature is 65-70 ℃, and the volume ratio of distillate to distilled liquid is 2.2:1.
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| CN202310659291.4A CN116891949B (en) | 2023-06-06 | 2023-06-06 | Process for recycling three-phase slag produced in wet copper extraction process |
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| CN202310659291.4A CN116891949B (en) | 2023-06-06 | 2023-06-06 | Process for recycling three-phase slag produced in wet copper extraction process |
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| CN116891949B true CN116891949B (en) | 2024-05-03 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996025525A1 (en) * | 1995-02-16 | 1996-08-22 | Henkel Corporation | Modifiers for aldoxime extractant of metal values |
| JP2009167452A (en) * | 2008-01-15 | 2009-07-30 | Sumitomo Metal Mining Co Ltd | Solvent extraction method for aqueous solution of chloride |
| CN107557581A (en) * | 2017-07-20 | 2018-01-09 | 陈飙 | A kind of method that copper is reclaimed from acidic waste etching liquid |
| CN109179756A (en) * | 2018-09-26 | 2019-01-11 | 衢州华友钴新材料有限公司 | A kind for the treatment of process purifying SS from hydrometallurgy cobalt copper solution |
| CN216935042U (en) * | 2022-01-19 | 2022-07-12 | 西部矿业股份有限公司 | Copper smelting extraction three-phase slag filtering device |
-
2023
- 2023-06-06 CN CN202310659291.4A patent/CN116891949B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996025525A1 (en) * | 1995-02-16 | 1996-08-22 | Henkel Corporation | Modifiers for aldoxime extractant of metal values |
| JP2009167452A (en) * | 2008-01-15 | 2009-07-30 | Sumitomo Metal Mining Co Ltd | Solvent extraction method for aqueous solution of chloride |
| CN107557581A (en) * | 2017-07-20 | 2018-01-09 | 陈飙 | A kind of method that copper is reclaimed from acidic waste etching liquid |
| CN109179756A (en) * | 2018-09-26 | 2019-01-11 | 衢州华友钴新材料有限公司 | A kind for the treatment of process purifying SS from hydrometallurgy cobalt copper solution |
| CN216935042U (en) * | 2022-01-19 | 2022-07-12 | 西部矿业股份有限公司 | Copper smelting extraction three-phase slag filtering device |
Non-Patent Citations (1)
| Title |
|---|
| 溶剂萃取在处理含铜溶液中的应用;黄卉;;昆明冶金高等专科学校学报(01);75-77 * |
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