CN114906824A - Short-process lead-selenium separation method for lead filter cake - Google Patents
Short-process lead-selenium separation method for lead filter cake Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000012065 filter cake Substances 0.000 title claims abstract description 32
- 238000000926 separation method Methods 0.000 title claims abstract description 23
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 title abstract description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 56
- 239000011669 selenium Substances 0.000 claims abstract description 56
- 239000002893 slag Substances 0.000 claims abstract description 26
- 238000004821 distillation Methods 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 13
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052802 copper Inorganic materials 0.000 abstract description 8
- 239000010949 copper Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 7
- 229910052737 gold Inorganic materials 0.000 abstract description 7
- 239000010931 gold Substances 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 7
- 229910052797 bismuth Inorganic materials 0.000 abstract description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011133 lead Substances 0.000 abstract description 6
- 239000004332 silver Substances 0.000 abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 10
- 239000003546 flue gas Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 230000019635 sulfation Effects 0.000 description 2
- 238000005670 sulfation reaction Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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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
- C01B19/004—Oxides; Hydroxides
-
- 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
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/023—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
-
- 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
-
- 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
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
-
- 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
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a short-process lead-selenium separation method for lead filter cakes, which utilizes the difference of saturated vapor pressure of different substances under the vacuum condition and considers the difference of salt decomposition temperature and substance volatilization temperature at the same time to realize high-efficiency separation of selenium in the lead filter cakes under the vacuum distillation condition, the volatilized selenium vapor can be condensed and collected to obtain crude selenium products, and lead, copper, bismuth, gold and silver are effectively enriched in distillation bottom slag. The grade of the crude selenium product obtained by the method is more than 95 percent, and the crude selenium product can be directly sold or returned to the existing selenium recovery system for further refining, so the method has considerable benefit. The selenium content in the bottom slag obtained by the method can be reduced to be below 0.5%, and gold, silver, lead, bismuth and the like are enriched in the bottom slag, so that the sale valuation coefficient can be further improved. The method has short flow and is easy to realize.
Description
Technical Field
The invention relates to the technical field of metal smelting, in particular to a short-process lead-selenium separation method for lead filter cakes.
Background
When the pyrometallurgical copper smelting flue gas is used for preparing acid, the soot is washed by dynamic waves to obtain relatively pure sulfur dioxide flue gas, and the slag obtained by filtering is called a lead filter cake. The lead filter cake is black solid, the main components of the lead filter cake comprise copper, selenium, lead and arsenic, and a small amount of gold, silver, bismuth, tellurium and the like, wherein most of selenium exists in the form of selenium dioxide in the oxidation smelting process, enters a flue gas washing tower along with sulfur dioxide flue gas, and then forms H after being dissolved in water in the washing tower 2 SeO 3 Then is coated with SO 2 Reducing the selenium into metal selenium, and reacting with Au, Ag, Cu, Te and other elements in the smoke to generate corresponding alloy compounds. At present, because the components of the lead filter cake are complex and the treatment difficulty is relatively high, a plurality of factories do not treat or only simply treat the lead filter cake and then sell the lead filter cake for related enterprises to recover part of metals which are usually soldIn the process, only metals such as gold, silver, copper, lead, bismuth and the like are priced, and selenium is not priced, so that resource waste is caused, and the economic benefit is directly influenced.
At present, a plurality of technologies for recovering selenium from selenium-containing materials exist, and a sulfation roasting method is adopted as a mainstream process. The sulfation roasting method is to mix seleniferous acid mud with concentrated sulfuric acid and then roast the mixture in a rotary kiln to oxidize selenium into volatile SeO 2 And recovered as crude selenium. The method has the advantages of low roasting temperature, high selenium recovery rate and the like, but has the defects of quick corrosion of equipment, long auxiliary process, serious environmental pollution and prominent arsenic dispersion problem.
CN102583264 discloses a method for leaching selenium in acid mud by using sodium sulfite, which uses a pressure leaching process, and has the advantages of high leaching temperature, large equipment investment and high cost. The research of selenium enrichment by a dressing and smelting method can enrich acid mud containing 0.1 to 0.3 percent of selenium to about 1 percent, but does not relate to an extraction process.
CN109055719A discloses a method for recovering valuable metals from selenium-containing acid mud, which mainly comprises the steps of low-temperature roasting, two-stage acid leaching, sodium sulfite reduction and iron powder reduction, and high-mercury smoke dust, lead slag, crude selenium-grade sponge copper and the like are respectively obtained. In the low-temperature roasting process, selenium is easy to oxidize and volatilize into smoke dust, so that the recovery rate of selenium is influenced; the solution after selenium reduction is replaced by iron powder to recover copper, new impurities can be brought to a system, the solution cannot be recycled, and meanwhile, a large amount of slag can be generated in the wastewater treatment process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a short-flow lead-selenium separation method for lead filter cakes, which takes vacuum distillation as a means, separates and recovers selenium in the lead filter cakes in a short flow, effectively improves the resource utilization rate and improves the economic benefits of enterprises.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for separating lead and selenium from lead filter cakes in a short process comprises the following specific steps:
A. washing with water: mixing the lead filter cake with water, stirring and reacting at normal temperature to dissolve soluble sulfate and free acid in the lead filter cake;
B. and (3) drying: b, performing liquid-solid separation on the ore pulp finally obtained in the step A, and drying the solid obtained by the liquid-solid separation in a vacuum drying oven to prevent the crude selenium from being oxidized due to moisture brought in the subsequent vacuum distillation process;
C. and (3) distillation: and D, putting the solid obtained after drying in the step B into a vacuum distillation furnace for distillation to obtain lead-enriched bottom slag and a crude selenium product.
Further, in the step A, the liquid-solid ratio L/g of the lead filter cake to water is 3-5:1, and the reaction time is 0.5-1.5h under stirring.
Further, in step B, the solid was dried to a moisture < 0.1%.
Further, in the step B, the drying temperature is 60-110 ℃ and the drying time is 4-12 h.
Further, in the step C, in the distillation, the vacuum degree is 5-10Pa, the distillation temperature is 250-400 ℃, and the distillation time is 3-5 h.
The invention has the beneficial effects that: the grade of the crude selenium product obtained by the method is more than 95 percent, and the crude selenium product can be directly sold or returned to the existing selenium recovery system for further refining, so the method has considerable benefit. The selenium content in the bottom slag obtained by the method can be reduced to be below 0.5%, and gold, silver, lead, bismuth and the like are enriched in the bottom slag, so that the selling pricing coefficient is further improved. The method has short flow and is easy to realize.
Drawings
FIG. 1 is a schematic flow chart of the method of examples 1 to 5 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that the present embodiment is based on the technical solution, and the detailed implementation and the specific operation process are provided, but the protection scope of the present invention is not limited to the present embodiment.
Embodiments 1 to 5 provide an application example of a short-process lead-selenium separation method for lead filter cakes, where the lead filter cakes are from a copper smelting flue gas washing section, selenium content is in a range of 4% to 15%, part of selenium exists in a simple substance form, and part of selenium exists in compound forms of AgxSey, AuxSey, CuxSey, and the like, and meanwhile, due to high sulfuric acid concentration of a dynamic wave washing liquid, a large amount of sulfate exists in the lead filter cakes, phase components are complex, and ideal separation effect cannot be achieved by conventional method treatment.
As shown in fig. 1, the method of this embodiment 1-5 is based on the existence state of the main elements in the lead filter cake, and utilizes the difference of saturated vapor pressures of different substances under vacuum conditions, and considers the difference of the salt decomposition temperature and the substance volatilization temperature, so as to realize the high-efficiency separation of selenium in the lead filter cake under vacuum distillation conditions, the volatilized selenium vapor can be condensed and collected to obtain a crude selenium product, lead, copper, bismuth, gold, and silver are effectively enriched in the distillation bottom slag, and the economic and social benefits are significant.
Example 1
1kg of lead filter cake containing Au10.15g/t, Ag1685.36g/t, Pb46.62%, Bi1.05%, Se4.79% and Hg0.29% is placed in a beaker, water is added according to the liquid-solid ratio L/g3:1, and the mixture is stirred and reacted for 1h at normal temperature. After liquid-solid separation, the obtained solid is dried in a vacuum drying oven at 60 ℃ for 12h, and the final solid contains 0.08% of water and 90.3% of slag. The liquid obtained by the liquid-solid separation can return to the dynamic wave washing section for flue gas washing. And (3) placing 300g of the dried solid in a vacuum distillation furnace, heating when the vacuum degree is 8Pa, and carrying out distillation reaction at 400 ℃ for 3h to obtain 262.5g of bottom slag, wherein the bottom slag contains 59.70% of lead and 0.05% of selenium. 16.3g of crude selenium product is obtained, and the selenium content is 95.11 percent.
Example 2:
1kg of lead filter cake containing Au10.15g/t, Ag1685.36g/t, Pb46.62%, Bi1.05%, Se4.79% and Hg0.29% is placed in a beaker, water is added according to the liquid-solid ratio L/g5:1, and the mixture is stirred and reacted for 0.5h at normal temperature. After liquid-solid separation, the obtained solid is dried in a vacuum drying oven at 110 ℃ for 4 hours, the water content of the final solid is 0.07 percent, and the slag rate is 88.5 percent. The liquid obtained by the liquid-solid separation can return to the dynamic wave washing section for flue gas washing. And (3) placing 300g of the dried solid in a vacuum distillation furnace, heating when the vacuum degree is 5Pa, and carrying out distillation reaction at 250 ℃ for 5h to obtain 275.8g of bottom slag, wherein the bottom slag contains 56.95% of lead and 0.25% of selenium. 15.7g of crude selenium product with the selenium content of 96.64 percent is obtained.
Example 3:
1kg of lead filter cake containing Au10.15g/t, Ag1685.36g/t, Pb46.62%, Bi1.05%, Se4.79% and Hg0.29% is placed in a beaker, water is added according to the liquid-solid ratio L/g4:1, and the mixture is stirred and reacted for 1.5h at normal temperature. After liquid-solid separation, the obtained solid was dried in a vacuum oven at 100 ℃ for 5 hours, and the final solid contained 0.07% of water and 89.6% of slag. The liquid obtained by the liquid-solid separation can return to the dynamic wave washing section for flue gas washing. And (3) placing 300g of the dried solid in a vacuum distillation furnace, heating when the vacuum degree reaches 10Pa, and carrying out distillation reaction at 350 ℃ for 4h to obtain 270.3g of bottom slag, wherein the bottom slag contains 57.75% of lead and 0.11% of selenium. 16.1g of crude selenium product is obtained, and the content of selenium is 95.35 percent.
Example 4:
1kg of lead filter cake containing Au6.00g/t, Ag774.08g/t, Pb55.02%, Bi1.10%, Se6.48% and Hg0.72% is placed in a beaker, water is added according to the liquid-solid ratio L/g4:1, and the mixture is stirred and reacted for 1.5 hours at normal temperature. After liquid-solid separation, the obtained solid was dried in a vacuum oven at 100 ℃ for 5 hours, and the final solid contained 0.07% of water and 91.4% of slag. The liquid obtained by the liquid-solid separation can return to the dynamic wave washing section for flue gas washing. And (3) placing 300g of the dried solid in a vacuum distillation furnace, heating when the vacuum degree reaches 10Pa, and carrying out distillation reaction at 350 ℃ for 4h to obtain 264.6g of bottom slag, wherein the bottom slag contains 65.4% of lead and 0.15% of selenium. 21.7g of crude selenium product is obtained, and the selenium content is 95.04%.
Example 5:
1kg of lead filter cake containing 20.1g/t of Au20.1g/t, Ag387.08g/t, Pb36.98%, Bi11.21%, Se14.52% and Hg0.57% is placed in a beaker, water is added according to the liquid-solid ratio L/g4:1, and the mixture is stirred and reacted for 1.5h at normal temperature. After liquid-solid separation, the obtained solid is dried for 5 hours in a vacuum drying oven at 100 ℃, and the final solid contains 0.07 percent of water and 90.8 percent of slag. The liquid obtained by the liquid-solid separation can return to the dynamic wave washing section for flue gas washing. And (3) placing 300g of the dried solid in a vacuum distillation furnace, heating when the vacuum degree reaches 10Pa, and carrying out distillation reaction at 350 ℃ for 4h to obtain 233.2g of bottom slag, wherein the slag contains 51.39% of lead and 0.18% of selenium. 54.5g of crude selenium product is obtained, and the selenium content is 95.66%.
The lead filter cake treatment results of the methods of examples 1-5 are shown in table 1.
TABLE 1
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.
Claims (5)
1. A method for separating lead and selenium from lead filter cakes in a short process is characterized by comprising the following specific steps:
A. washing with water: mixing the lead filter cake with water, stirring and reacting at normal temperature to dissolve soluble sulfate and free acid in the lead filter cake;
B. and (3) drying: b, performing liquid-solid separation on the ore pulp finally obtained in the step A, and drying the solid obtained by the liquid-solid separation in a vacuum drying oven to prevent the crude selenium from being oxidized due to moisture brought in the subsequent vacuum distillation process;
C. and (3) distillation: and D, putting the solid obtained after drying in the step B into a vacuum distillation furnace for distillation to obtain lead-enriched bottom slag and a crude selenium product.
2. The method according to claim 1, wherein in the step A, the liquid-solid ratio L/g of the lead filter cake to the water is 3-5:1, and the stirring reaction time is 0.5-1.5 h.
3. The process according to claim 1, wherein in step B, the solid is dried to a moisture content of < 0.1%.
4. The method according to claim 1, wherein in step B, the drying temperature is 60-110 ℃ and the drying time is 4-12 h.
5. The method according to claim 1, wherein in the step C, the vacuum degree in the distillation is 5-10Pa, the distillation temperature is 250-400 ℃, and the distillation time is 3-5 h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779790A (en) * | 2016-04-12 | 2016-07-20 | 永兴佳盛有色金属再生利用有限责任公司 | Method for removing lead and purifying bismuth from lead-bismuth material through vacuum distillation |
| CN106946233A (en) * | 2017-04-18 | 2017-07-14 | 昆明鼎邦科技股份有限公司 | A kind of method of impure selenium material vacuum Refining |
| CN113832350A (en) * | 2021-09-10 | 2021-12-24 | 紫金矿业集团股份有限公司 | Short-process zinc-cobalt separation method for zinc smelting cobalt slag |
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- 2022-06-01 CN CN202210617668.5A patent/CN114906824A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779790A (en) * | 2016-04-12 | 2016-07-20 | 永兴佳盛有色金属再生利用有限责任公司 | Method for removing lead and purifying bismuth from lead-bismuth material through vacuum distillation |
| CN106946233A (en) * | 2017-04-18 | 2017-07-14 | 昆明鼎邦科技股份有限公司 | A kind of method of impure selenium material vacuum Refining |
| CN113832350A (en) * | 2021-09-10 | 2021-12-24 | 紫金矿业集团股份有限公司 | Short-process zinc-cobalt separation method for zinc smelting cobalt slag |
Non-Patent Citations (1)
| Title |
|---|
| 李栋等: "硒资源及其提取技术研究进展", 有色金属科学与工程, vol. 2018, no. 1, pages 504 - 23 * |
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