CN108502852A - A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting - Google Patents
A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting Download PDFInfo
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- CN108502852A CN108502852A CN201810202991.XA CN201810202991A CN108502852A CN 108502852 A CN108502852 A CN 108502852A CN 201810202991 A CN201810202991 A CN 201810202991A CN 108502852 A CN108502852 A CN 108502852A
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- Prior art keywords
- copper anode
- anode mud
- microwave
- selenium
- distilled water
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- 239000010949 copper Substances 0.000 title claims abstract description 86
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 80
- 239000011669 selenium Substances 0.000 title claims abstract description 56
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 49
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000001180 sulfating effect Effects 0.000 title claims abstract description 19
- 239000012153 distilled water Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000009825 accumulation Methods 0.000 claims abstract description 7
- 238000013019 agitation Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000002893 slag Substances 0.000 claims abstract description 7
- 229910052714 tellurium Inorganic materials 0.000 claims description 8
- 238000007670 refining Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 5
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000002386 leaching Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The present invention relates to a kind of methods that selenium in copper anode mud is recycled in microwave sulfating roasting, belong to non-ferrous metallurgy secondary resource utilization technology field.Copper anode mud is dried fine grinding and obtains copper anode mud powder by the present invention；Under agitation, the concentrated sulfuric acid is added to be uniformly mixed in copper anode mud powder and obtains mixture slurry；Mixture slurry is placed in microwave tube type oven, it is passed through air, 1.5 ~ 3h of microwave calcining is carried out under the conditions of temperature is 350 ~ 650 DEG C and obtains fired slags and tail gas containing selenium, and tail gas containing selenium empties after distilled water A NaOH solution distilled water B tertiary treatment, in Se accumulation to distilled water A.The method that this method uses microwave sulfating roasting has efficient, simple and quick, processing time is short, reduces energy consumption and acid consumes, production cost is low, is conducive to the industrial applications of selenium in copper anode mud.
Description
Technical field
The present invention relates to a kind of methods that selenium in copper anode mud is recycled in microwave sulfating roasting, belong to non-ferrous metallurgy two
Secondary field of resource recovery technique.
Background technology
Copper anode mud is the byproduct generated in electrolytic refining course of copper, and yield accounts for about 1% or so of blister copper amount.2016
About 8,440,000 tons of China's refined copper yield, ten thousand tons of copper anode mud yield about 8-9.The a large amount of rare precious metals being rich in copper anode mud are
The important raw material of cupper smelting comprehensively recovering valuable metal.Wherein selenium, tellurium are contained in copper anode mud with high extraction
The content of the metal of value, wherein selenium is higher, and tellurium is then relatively low.Therefore your dilute resource fully in exploitation copper anode mud is right
Meet the national economic development needs to have extraordinary realistic meaning.
Selenium is a kind of rare and scatter element, and selenium has a wide range of applications field, is not only widely used in chemical industry, metallurgy, building materials, electricity
The industrial departments such as son, and there is important medical value, it is a kind of powerful antioxidant, it is required for human body, in agricultural, medicine
Aspect also has important researching value.Selenium master direction to be applied and ratio：Electronics industry 30%, glass industry 30%, metallurgical work
Industry 10%, health care 8% etc..
Currently, the technique of copper anode mud deselenization includes mainly：Traditional sulfating roasting deselenization method, oxidizing roasting deselenization method,
Soda roasts deselenization method, normal pressure or pressure leaching deselenization method and card dure furnace deselenization method etc..Traditional pyrogenic attack technique pair
Environmental pressure is larger, and energy consumption is big, and precious metal losses are serious；Copper anode mud complicated component, normal pressure or pressure leaching selenium effect are paid no attention to
Think, and acid consumption is big；Card dure furnace deselenization method by after this kind of volatile metal removal of selenium, for Dorr close by the equal melting of other metals
Gold, subsequent processing is complicated, long flow path, while also having and being carried out in conjunction with ore dressing and hydrometallurgy.
Invention content
The problem of existing for the above-mentioned prior art and deficiency, the present invention provide a kind of microwave sulfating roasting recycling copper sun
The method of selenium in the mud of pole.The method that the method for the present invention uses microwave sulfating roasting has efficient, simple and quick, place
The reason time is short, reduces energy consumption and acid consumes, production cost is low, is conducive to the industrial applications of selenium in copper anode mud.
A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting, is as follows：
（1）Fine grinding is dried in copper anode mud and obtains copper anode mud powder；
（2）Under agitation, the concentrated sulfuric acid is added to step（1）It is uniformly mixed in gained copper anode mud powder and obtains mixing slurry
Body；
（3）By step（2）Gained mixture slurry is placed in microwave tube type oven, is passed through air, under the conditions of temperature is 350 ~ 650 DEG C
It carries out 1.5 ~ 3h of microwave calcining and obtains fired slags and tail gas containing selenium, tail gas containing selenium is through distilled water A-NaOH solution-distilled water B three-levels
It is emptied after processing, in Se accumulation to distilled water A；
The step（1）Middle copper anode mud is the copper anode mud generated in electrolytic refining course of copper, by percentage to the quality, copper sun
Contain 0.97 ~ 1.04 % of Cu 9.57 ~ 11.70 %, Se 3.03 ~ 3.25%, Te in the mud of pole；
Further, the step（2）The mass ratio of the middle concentrated sulfuric acid and copper anode mud powder is (0.7 ~ 1):1；
Further, the step（3）Middle microwave calcining power is 300 ~ 800W, and frequency is 2.43 ~ 2.48GHz；
The concentrated sulfuric acid is the pure concentrated sulfuric acid of commercially available analysis, a concentration of 95 ~ 98%；
The beneficial effects of the invention are as follows：
（1）The method of the present invention using the volatility of selenium in copper anode mud can be improved, greatly reduce dosage sour in traditional pyrogenic process and
Loss, and can keep, to the good applicability of raw material, significantly simplifying the technological process of production；
（2）Microwave sulfating roasting copper anode mud, 95 ~ 98% selenium in recyclable copper anode mud；
（3）Microwave sulfating roasting copper anode mud, can make roasting more uniform, and energy consumption and roasting time is greatly reduced, heating
Adequacy and selectivity so that acid consumption be greatly reduced, exhaust gas reduce, it is environmental-friendly.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1：A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting, is as follows：
（1）Fine grinding is dried in copper anode mud and obtains copper anode mud powder；Wherein copper anode mud is to be produced in electrolytic refining course of copper
Raw copper anode mud contains Cu 9.57%, Se 3.25%, Te 0.97% by percentage to the quality in copper anode mud；
（2）Under agitation, the concentrated sulfuric acid is added to step（1）It is uniformly mixed in gained copper anode mud powder and obtains mixing slurry
Body；The mass ratio of the wherein concentrated sulfuric acid and copper anode mud powder is 0.7:1；
（3）By step（2）Gained mixture slurry is placed in microwave tube type oven, is passed through air, is carried out under the conditions of temperature is 350 DEG C
Microwave calcining 2h obtains fired slags and tail gas containing selenium, and tail gas containing selenium is through distilled water A-NaOH solution-distilled water B tertiary treatment heel row
Sky, in Se accumulation to distilled water A；
Microwave calcining power is 800W, frequency 2.45GHz in the present embodiment；
The rate of recovery of selenium is 96.61% in the present embodiment.
Embodiment 2：A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting, is as follows：
（1）Fine grinding is dried in copper anode mud and obtains copper anode mud powder；Wherein copper anode mud is to be produced in electrolytic refining course of copper
Raw copper anode mud contains 1.02 % of Cu 10.35 %, Se 3.03%, Te by percentage to the quality in copper anode mud；
（2）Under agitation, the concentrated sulfuric acid is added to step（1）It is uniformly mixed in gained copper anode mud powder and obtains mixing slurry
Body；The mass ratio of the wherein concentrated sulfuric acid and copper anode mud powder is 0.85:1；
（3）By step（2）Gained mixture slurry is placed in microwave tube type oven, is passed through air, is carried out under the conditions of temperature is 500 DEG C
Microwave calcining 1.5h obtains fired slags and tail gas containing selenium, and tail gas containing selenium is after distilled water A-NaOH solution-distilled water B tertiary treatment
It empties, in Se accumulation to distilled water A；
Microwave calcining power is 300W, frequency 2.43GHz in the present embodiment；
The rate of recovery of selenium is 98.24% in the present embodiment.
Embodiment 3：A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting, is as follows：
（1）Fine grinding is dried in copper anode mud and obtains copper anode mud powder；Wherein copper anode mud is to be produced in electrolytic refining course of copper
Raw copper anode mud contains 1.04 % of Cu 11.70 %, Se 3.14%, Te by percentage to the quality in copper anode mud；
（2）Under agitation, the concentrated sulfuric acid is added to step（1）It is uniformly mixed in gained copper anode mud powder and obtains mixing slurry
Body；The mass ratio of the wherein concentrated sulfuric acid and copper anode mud powder is 0.9:1；
（3）By step（2）Gained mixture slurry is placed in microwave tube type oven, is passed through air, is carried out under the conditions of temperature is 650 DEG C
Microwave calcining 2.5h obtains fired slags and tail gas containing selenium, and tail gas containing selenium is after distilled water A-NaOH solution-distilled water B tertiary treatment
It empties, in Se accumulation to distilled water A；
Microwave calcining power is 500W, frequency 2.46GHz in the present embodiment；
The rate of recovery of selenium is 99.35% in the present embodiment.
Embodiment 4：A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting, is as follows：
（1）Fine grinding is dried in copper anode mud and obtains copper anode mud powder；Wherein copper anode mud is to be produced in electrolytic refining course of copper
Raw copper anode mud contains 1.01 % of Cu 11.36 %, Se 3.18%, Te by percentage to the quality in copper anode mud；
（2）Under agitation, the concentrated sulfuric acid is added to step（1）It is uniformly mixed in gained copper anode mud powder and obtains mixing slurry
Body；The mass ratio of the wherein concentrated sulfuric acid and copper anode mud powder is 1:1；
（3）By step（2）Gained mixture slurry is placed in microwave tube type oven, is passed through air, is carried out under the conditions of temperature is 550 DEG C
Microwave calcining 3h obtains fired slags and tail gas containing selenium, and tail gas containing selenium is through distilled water A-NaOH solution-distilled water B tertiary treatment heel row
Sky, in Se accumulation to distilled water A；
Microwave calcining power is 400W, frequency 2.48GHz in the present embodiment；
The rate of recovery of selenium is 98.36% in the present embodiment.
The specific implementation mode of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Go out various change.
Claims (4)
1. a kind of method of selenium in microwave sulfating roasting recycling copper anode mud, which is characterized in that be as follows：
（1）Fine grinding is dried in copper anode mud and obtains copper anode mud powder；
（2）Under agitation, the concentrated sulfuric acid is added to step（1）It is uniformly mixed in gained copper anode mud powder and obtains mixing slurry
Body；
（3）By step（2）Gained mixture slurry is placed in microwave tube type oven, is passed through air, under the conditions of temperature is 350 ~ 650 DEG C
It carries out 1.5 ~ 3h of microwave calcining and obtains fired slags and tail gas containing selenium, tail gas containing selenium is through distilled water A-NaOH solution-distilled water B three-levels
It is emptied after processing, in Se accumulation to distilled water A.
2. the method that selenium in copper anode mud is recycled in microwave sulfating roasting according to claim 1, it is characterised in that：Step
（1）Middle copper anode mud is that the copper anode mud generated in electrolytic refining course of copper contains Cu by percentage to the quality in copper anode mud
0.97 ~ 1.04 % of 9.57 ~ 11.70 %, Se 3.03 ~ 3.25%, Te.
3. the method that selenium in copper anode mud is recycled in microwave sulfating roasting according to claim 1, it is characterised in that：Step
（2）The mass ratio of the middle concentrated sulfuric acid and copper anode mud powder is (0.7 ~ 1):1.
4. the method that selenium in copper anode mud is recycled in microwave sulfating roasting according to claim 1, it is characterised in that：Step
（3）Middle microwave calcining power is 300 ~ 800W, and frequency is 2.43 ~ 2.48GHz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810202991.XA CN108502852A (en) | 2018-03-13 | 2018-03-13 | A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810202991.XA CN108502852A (en) | 2018-03-13 | 2018-03-13 | A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting |
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| CN108502852A true CN108502852A (en) | 2018-09-07 |
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| CN201810202991.XA Pending CN108502852A (en) | 2018-03-13 | 2018-03-13 | A kind of method that selenium in copper anode mud is recycled in microwave sulfating roasting |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109748249A (en) * | 2019-03-12 | 2019-05-14 | 湖南工业大学 | A method of the oxygen-enriched fluidized bed roasting of the earth of positive pole containing selenium-organic reducing extracts selenium |
| CN113336199A (en) * | 2021-06-10 | 2021-09-03 | 昆明理工大学 | Method for roasting and steaming selenium from copper anode mud |
| CN114990338A (en) * | 2022-05-07 | 2022-09-02 | 江西铜业技术研究院有限公司 | Method for efficiently extracting tin from silver separating residues of copper anode slime |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109748249A (en) * | 2019-03-12 | 2019-05-14 | 湖南工业大学 | A method of the oxygen-enriched fluidized bed roasting of the earth of positive pole containing selenium-organic reducing extracts selenium |
| CN109748249B (en) * | 2019-03-12 | 2022-04-22 | 湖南工业大学 | Method for extracting selenium from selenium-containing anode mud by oxygen-enriched fluidized roasting-organic reduction |
| CN113336199A (en) * | 2021-06-10 | 2021-09-03 | 昆明理工大学 | Method for roasting and steaming selenium from copper anode mud |
| CN114990338A (en) * | 2022-05-07 | 2022-09-02 | 江西铜业技术研究院有限公司 | Method for efficiently extracting tin from silver separating residues of copper anode slime |
| CN114990338B (en) * | 2022-05-07 | 2024-05-31 | 江西铜业技术研究院有限公司 | Method for efficiently extracting tin from silver separating slag of copper anode slime |
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