CN107217145A - A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic - Google Patents
A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic Download PDFInfo
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- CN107217145A CN107217145A CN201611125653.8A CN201611125653A CN107217145A CN 107217145 A CN107217145 A CN 107217145A CN 201611125653 A CN201611125653 A CN 201611125653A CN 107217145 A CN107217145 A CN 107217145A
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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
- C22B7/001—Dry processes
-
- 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
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
-
- 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
-
- 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
-
- 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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention relates to the technical field of metal smelt, a kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic is disclosed.This method comprises the following steps：S1. after drying by copper anode mud and be scattered, it is well mixed with solid reductant, electrical heating reduction distillation goes out lead, antimony, bismuth selenium tellurium, arsenic vaporizer in vacuum drying oven, is left the residue containing gold, silver and bronze；S2. flue dust is passed through multi-stage condensing device group, controls the thermograde of multi-stage condensing device group so that lead, antimony, bismuth selenium tellurium, arsenic are condensed in different condensers in flue dust, respectively obtain lead, antimony, bismuth selenium tellurium, arsenic.Copper anode mud is evaporated in vacuo this method and fractional condensaion two-step method carries out separation lead antimony bismuth selen-tellurjum arsenic, and clearance is high, and the purity of regenerant is high, and technique is simple, does not discharge sulfur dioxide, environmentally safe.
Description
Technical field
The present invention relates to the technical field of metal smelt, more particularly to a kind of copper anode mud vacuum reduction takes off lead antimony
The method of bismuth selen-tellurjum arsenic.
Background technology
Copper anode mud falls within the pureed plasma of cell bottom when being electrolytical refined copper, mainly in anode crude metal not
It is dissolved in the impurity and metal composition to be refined of electrolyte.Generally grey, granularity is about 100~200 mesh.Wherein each component
It is many to exist with valuable and metal values, sulfide, selen-tellurjum compound, oxide, elemental sulfur and basic salt form, it can return
It is incorporated as refining the raw material of gold, silver, lead, antimony, bismuth selenium tellurium, arsenic etc..For example, can be reclaimed by the earth of positive pole of electrolytical refined copper
Copper, and extract gold, silver, selenium, tellurium etc..
At present, copper anode mud processing is broadly divided into pyrogenic attack and wet-treating two-mode.It is larger many using fire
Method technique.Copper anode mud thermal process is generally comprised:Pretreatment → reduction melting → point silver-colored processing → gold and silver electrolysis.Wherein：1)
Pretreatment:The main day of the process is decopper(ing) and other impurity, in order to subsequent treatment, 2) it is basic in gold and silver electrolysis industry
It is similar, and 3) reduction melting+point silver processing:But there are various handling process, be also the master of copper anode mud smelting process therefore
Body portion, has crucial effect for the economic and technical norms of whole technique.
Chinese invention patent application number CN201510893020.0 discloses one kind and reclaimed from copper anode mud flotation tailing
The method of valuable metal, floats side mine tailing by copper anode mud first and obtains reduzate by reduction melting, then by reduzate
Precious metals containing lead is obtained by aoxidizing blowing and containing As and Sb flue dust, is separated by staged vacuum distillation to obtain lead bismuth alloy and copper
Electrum.But one comes that the copper anode mud impurity that flotation obtains is more, and the content requirement that gold and silver is obtained to reduction melting is higher, also
The impurity that former melting is obtained is more, is unfavorable for the vacuum distillation in later stage, two come reduction melting generation waste it is more, it is necessary to increase
The floating side facility of smelting slag, so as to increase investment and operating cost.The disclosure of Chinese invention patent application number 201610435882.3
A kind of high impurity copper ANODE SLIME TREATMENT new technology, comprises the following steps：(1) copper anode mud progress sulfating roasting is removed
Selenium, leaching decopper(ing)；(2) side-blown converter reduction melting：Slag former, reducing agent are added to sulfating roasting except the copper after selenium decopper(ing)
Be uniformly mixed so as to obtain in the earth of positive pole mixed material melted, slag making and reduction reaction formation flue gas, the scum silica frost on upper strata and lower floor it is molten
Body shape precious metals containing lead；(3) it is evaporated in vacuo；(4) gold and silver electrolysis and lead bismuth are reclaimed：Dore metal is put into intermediate frequency furnace, silver-colored sun is cast into
Pole plate carries out silver-colored electrolysis, and lead bismuth alloy is cast into the laggard quadrat of stereotype is electrolysed.The various complexity of processing step of the patent, need through
Smithcraft is reclaimed in persulfuric acid salinization, side-blown converter melting, the Dore metal of generation complicated, the cycle length of material residue subsequent treatment,
The low shortcoming of utilization rate of equipment and installations.And selenium method is removed using concentrated sulfuric acid decopper(ing), after being mixed and stirred with the excessive concentrated sulfuric acid and copper anode mud, in sulphur
Acidizing fired rotary kiln oxidation Decomposition, sulphation, which is decomposed, produces substantial amounts of form waste gas of sulfur dioxide, and environmental pollution is big.
The content of the invention
The technical problem to be solved in the present invention is to overcome drawbacks described above to take off lead antimony there is provided a kind of copper anode mud vacuum reduction
The method of bismuth selen-tellurjum arsenic.
The present invention is achieved through the following technical solutions：
A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic, comprises the following steps：
S1. after drying by copper anode mud and be scattered, it is well mixed with solid reductant, electrical heating reduction is steamed in vacuum drying oven
Lead, antimony, bismuth selenium tellurium, arsenic vaporizer are distillated, is left the residue containing gold, silver and bronze；
S2. vaporizer is passed through multi-stage condensing device group, controls the thermograde of multi-stage condensing device group so that in vaporizer
Lead, antimony, bismuth selenium tellurium, arsenic are condensed in different condensers, respectively obtain lead, antimony, bismuth selenium tellurium and arsenic.
The present invention by be evaporated in vacuo metal with it is nonmetallic, heat different material vapour pressure under vacuo not to the utmost using material
It is identical to be separated, it is not quite similar carry out condensation separation using different material fusing point.
Preferably, the solid reductant is carbon or carbonaceous material.Preferably, the solid reductant is coal, charcoal
Or activated carbon.
Preferably, the quality of the solid reductant is the 0.5%~1.5% of copper anode mud quality.It is further preferred that
The quality of the solid reductant is the 1% of copper anode mud quality.
Preferably, the vacuum of the vacuum drying oven is 2~10Pa；The temperature in vacuum furnace is 1300~1400 DEG C.Further
Preferably, the vacuum of the vacuum drying oven is 8Pa；The temperature in vacuum furnace is 1350 DEG C.
Preferably, the electrical heating distillation time in vacuum drying oven is 5~7 hours.It is further preferred that the electricity in vacuum drying oven adds
The thermal distillation time is 6 hours.
Preferably, the vaporizer is directly passed through multi-stage condensing device group from vacuum drying oven.
Preferably, the multi-stage condensing device group includes 6 interconnected condensers, the temperature of the condenser by height to
It is low to be followed successively by 600 DEG C~550 DEG C, 430 DEG C~380 DEG C, 350 DEG C~340 DEG C, 310 DEG C~290 DEG C, 260 DEG C~240 DEG C and 190
DEG C~170 DEG C.
It is further preferred that the multi-stage condensing device group includes 6 interconnected condensers, the temperature of the condenser
580 DEG C, 400 DEG C, 355 DEG C, 300 DEG C, 250 DEG C and 180 DEG C are followed successively by from high to low.
Compared with now with technology, the invention has the advantages that：
The present invention by copper anode mud is evaporated in vacuo and fractional condensaion two-step method carry out separate lead antimony bismuth selen-tellurjum arsenic,
The materials such as residue and lead, antimony, bismuth selenium tellurium, arsenic with the gold, silver and bronze that obtain high content.
The method of the present invention needs not move through grey blow moulding, greatly alleviates numerous and diverse technique, it is to avoid volume of smoke and
Poisonous tail gas pollution on the environment, while also increasing the rate of recovery of the materials such as lead, antimony, bismuth selenium tellurium, arsenic.
The method of the present invention needs not move through sulfating roasting except selenium and leaches decopper(ing), it is to avoid very complicated process, drop
Low cost, and can simple and effective recovery selenium and copper, while avoiding producing substantial amounts of sulfur dioxide gas, pollute environment.
The method of the present invention is by vacuum drying oven direct electro heating reducing process, and workshop need not set chimney, production technology
Environmental protection.
The thermal efficiency of the present invention is high, and energy-conserving and environment-protective, technological process is short, and occupation area of equipment is small, easily realizes that industry is automatic
Change, safety in production is saved greatly production cost.
The present invention can directly obtain the crude product of the simple substance such as lead, antimony, bismuth selenium tellurium, arsenic, production efficiency from copper anode mud
Height, simple production process.
Embodiment
The present invention is further illustrated with reference to specific embodiment.Unless stated otherwise, used in the embodiment of the present invention
Raw material and method are this area routinely raw material purchased in market and conventional use of method.
Embodiment 1
A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic, comprises the following steps：
S1. after drying by copper anode mud and be scattered, 1000kg copper anode mud is taken to be mixed with 5kg solid reductant coal
Uniformly, electrical heating reduction distillation goes out lead, antimony, bismuth selenium tellurium, arsenic vaporizer in vacuum drying oven, is left the residue containing gold, silver and bronze.Its
In, the vacuum of vacuum drying oven is 2Pa, and the temperature in vacuum furnace is 1400 DEG C, and the electrical heating reduction distillation time in vacuum drying oven is small for 5
When.
S2. vaporizer is passed through multi-stage condensing device group, vaporizer is directly passed through multi-stage condensing device group from vacuum drying oven, controlled
The thermograde of multi-stage condensing device group so that lead, antimony, bismuth selenium tellurium, arsenic are condensed in different condensers in flue dust, respectively
To lead, antimony, bismuth selenium tellurium, arsenic.Wherein, multi-stage condensing device group includes 6 interconnected condensers, and the temperature of condenser is by height
600 DEG C, 430 DEG C, 350 DEG C, 310 DEG C, 260 DEG C and 190 DEG C are followed successively by low.
The content of each component in copper anode mud and residue is detected according to this area conventional method, clearance is calculated.Detection is cold
The lead of condenser recovery, antimony, bismuth selenium tellurium, the purity of arsenic.Testing result is shown in Table 1, detects the tail discharged by the outlet flue of condenser
Gas, testing result is shown without sulfur dioxide.
Embodiment 2
A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic, comprises the following steps：
S1. after drying by copper anode mud and be scattered, 1000kg copper anode mud and 10kg solid reductant coal is taken to mix
Close uniform, electrical heating reduction distillation goes out lead, antimony, bismuth selenium tellurium, arsenic vaporizer in vacuum drying oven, be left the residue containing gold, silver and bronze.
Wherein, the vacuum of vacuum drying oven is 8Pa, and the temperature in vacuum furnace is 1350 DEG C, and the electrical heating reduction distillation time in vacuum drying oven is 6
Hour.
S2. vaporizer is passed through multi-stage condensing device group, vaporizer is directly passed through multi-stage condensing device group from vacuum drying oven, controlled
The thermograde of multi-stage condensing device group so that lead, antimony, bismuth selenium tellurium, arsenic are condensed in different condensers in flue dust, respectively
To lead, antimony, bismuth selenium tellurium, arsenic.Wherein, multi-stage condensing device group includes 6 interconnected condensers, and the temperature of condenser is by height
580 DEG C, 400 DEG C, 355 DEG C, 300 DEG C, 250 DEG C and 180 DEG C are followed successively by low.
The content of each component in copper anode mud and residue is detected according to this area conventional method, clearance is calculated.Detection is cold
The lead of condenser recovery, antimony, bismuth selenium tellurium, the purity of arsenic.Testing result is shown in Table 1, detects the tail discharged by the outlet flue of condenser
Gas, testing result is shown without sulfur dioxide.
Embodiment 3
A kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic, comprises the following steps：
S1. after drying by copper anode mud and be scattered, 1000kg copper anode mud and 15kg solid reductant charcoal is taken to mix
Close uniform, electrical heating reduction distillation goes out lead, antimony, bismuth selenium tellurium, arsenic vaporizer in vacuum drying oven, be left the residue containing gold, silver and bronze.
Wherein, the vacuum of vacuum drying oven is 10Pa, and the temperature in vacuum furnace is 1300 DEG C, and the electrical heating reduction distillation time in vacuum drying oven is
7 hours.
S2. vaporizer is passed through multi-stage condensing device group, vaporizer is directly passed through multi-stage condensing device group from vacuum drying oven, controlled
The thermograde of multi-stage condensing device group so that lead, antimony, bismuth selenium tellurium, arsenic are condensed in different condensers in flue dust, respectively
To lead, antimony, bismuth selenium tellurium, arsenic.Wherein, multi-stage condensing device group includes 6 interconnected condensers, and the temperature of condenser is by height
550 DEG C, 380 DEG C, 340 DEG C, 290 DEG C, 240 DEG C and 170 DEG C are followed successively by low.
The content of each component in copper anode mud and residue is detected according to this area conventional method, clearance is calculated.Detection is cold
The lead of condenser recovery, antimony, bismuth selenium tellurium, the purity of arsenic.Testing result is shown in Table 1, detects the tail discharged by the outlet flue of condenser
Gas, testing result is shown without sulfur dioxide.
Table 1
As shown in Table 1, method of the invention can effectively remove lead, antimony, bismuth selenium tellurium and the arsenic in copper anode mud, and reclaim
To the crude product of leaded, antimony, bismuth selenium tellurium and arsenic simple substance.
Claims (8)
1. a kind of method that copper anode mud vacuum reduction takes off lead antimony bismuth selen-tellurjum arsenic, it is characterised in that comprise the following steps：
S1. after drying by copper anode mud and be scattered, it is well mixed with solid reductant, the electrical heating reduction distillation in vacuum drying oven
Go out lead, antimony, bismuth selenium tellurium, arsenic vaporizer, be left the residue containing gold, silver and bronze；
S2. vaporizer is passed through multi-stage condensing device group, controls the thermograde of multi-stage condensing device group so that lead in vaporizer,
Antimony, bismuth selenium tellurium, arsenic are condensed in different condensers, respectively obtain lead, antimony, bismuth selenium tellurium and arsenic.
2. copper anode mud vacuum reduction takes off the method for lead antimony bismuth selen-tellurjum arsenic according to claim 1, it is characterised in that described solid
Body reducing agent is carbon or carbonaceous material.
3. copper anode mud vacuum reduction takes off the method for lead antimony bismuth selen-tellurjum arsenic according to claim 1, it is characterised in that described solid
The quality of body reducing agent is the 0.5% ~ 1.5% of copper anode mud quality.
4. copper anode mud vacuum reduction takes off the method for lead antimony bismuth selen-tellurjum arsenic according to claim 1, it is characterised in that described true
The vacuum of empty stove is 2 ~ 10Pa；The temperature in vacuum furnace is 1300 ~ 1400 DEG C.
5. copper anode mud vacuum reduction takes off the method for lead antimony bismuth selen-tellurjum arsenic according to claim 1, it is characterised in that vacuum drying oven
The interior electrical heating reduction distillation time is 5 ~ 7 hours.
6. copper anode mud vacuum reduction takes off the method for lead antimony bismuth selen-tellurjum arsenic according to claim 1, it is characterised in that the vapour
Compound is directly passed through multi-stage condensing device group from vacuum drying oven.
7. copper anode mud vacuum reduction takes off the method for lead antimony bismuth selen-tellurjum arsenic according to claim 1, it is characterised in that described many
Level condenser group includes 6 interconnected condensers, the temperature of the condenser be followed successively by from high to low 600 DEG C ~ 550 DEG C,
430 DEG C ~ 380 DEG C, 350 DEG C ~ 340 DEG C, 310 DEG C ~ 290 DEG C, 260 DEG C ~ 240 DEG C and 190 DEG C ~ 170 DEG C.
8. copper anode mud vacuum reduction takes off the method for lead antimony bismuth selen-tellurjum arsenic according to claim 7, it is characterised in that described many
Level condenser group includes 6 interconnected condensers, the temperature of the condenser be followed successively by from high to low 580 DEG C, 400 DEG C,
355 DEG C, 300 DEG C, 250 DEG C and 180 DEG C.
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| CN108285983A (en) * | 2018-03-13 | 2018-07-17 | 昆明理工大学 | A kind of equipment and its application process of arsenic lead mixed vapour fractional condensaion |
| CN108913905A (en) * | 2018-07-20 | 2018-11-30 | 芜湖新瑟安智能科技有限公司 | A kind of anode mud with high As and Pb processing recovery method |
| CN109536712A (en) * | 2018-11-14 | 2019-03-29 | 昆明理工大学 | A method of it being simple and efficient recycling copper and tellurium from copper tellurium slag |
| CN109734059A (en) * | 2019-03-12 | 2019-05-10 | 湖南工业大学 | A method of selenium and removal of impurities are extracted in hydrogenation from copper anode mud |
| CN111187912A (en) * | 2020-02-05 | 2020-05-22 | 铜仁学院 | Method for treating soldering tin electrolysis anode mud |
| CN111607708A (en) * | 2020-07-14 | 2020-09-01 | 湖南金马冶金技术开发有限公司 | Continuous vacuum distillation dearsenification process and system for high-arsenic alloy |
| CN112143896A (en) * | 2020-08-26 | 2020-12-29 | 昆明理工大学 | Method for recovering tellurium and bismuth from bismuth telluride waste |
| CN112609078A (en) * | 2020-12-15 | 2021-04-06 | 河南中原黄金冶炼厂有限责任公司 | Novel process for treating copper anode mud |
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| CN114920208A (en) * | 2022-04-24 | 2022-08-19 | 中南大学 | Method for efficiently separating tellurium or tellurium and selenium from tellurium-containing material |
| CN114959274A (en) * | 2022-06-01 | 2022-08-30 | 紫金铜业有限公司 | Method for efficiently separating valuable elements in lead filter cake |
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| CN108285983A (en) * | 2018-03-13 | 2018-07-17 | 昆明理工大学 | A kind of equipment and its application process of arsenic lead mixed vapour fractional condensaion |
| CN108913905A (en) * | 2018-07-20 | 2018-11-30 | 芜湖新瑟安智能科技有限公司 | A kind of anode mud with high As and Pb processing recovery method |
| CN109536712A (en) * | 2018-11-14 | 2019-03-29 | 昆明理工大学 | A method of it being simple and efficient recycling copper and tellurium from copper tellurium slag |
| CN109536712B (en) * | 2018-11-14 | 2020-07-17 | 昆明理工大学 | Method for simply and efficiently recovering copper and tellurium from copper-tellurium slag |
| CN109734059A (en) * | 2019-03-12 | 2019-05-10 | 湖南工业大学 | A method of selenium and removal of impurities are extracted in hydrogenation from copper anode mud |
| CN111187912A (en) * | 2020-02-05 | 2020-05-22 | 铜仁学院 | Method for treating soldering tin electrolysis anode mud |
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Application publication date: 20170929 |