CN108251651A - A kind of method of separation of Zinc cadmium metal material in copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag - Google Patents
A kind of method of separation of Zinc cadmium metal material in copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag Download PDFInfo
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- CN108251651A CN108251651A CN201810138604.0A CN201810138604A CN108251651A CN 108251651 A CN108251651 A CN 108251651A CN 201810138604 A CN201810138604 A CN 201810138604A CN 108251651 A CN108251651 A CN 108251651A
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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
- C22B7/04—Working-up slag
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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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
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Abstract
The invention discloses a kind of methods of separation of Zinc cadmium metal material in copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag, by the mixture of copper-cadmium slag, nickel cobalt slag or copper-cadmium slag and nickel cobalt slag supplying coal dust and alkaline earth oxide, it is evaporated in vacuo after mixture ball, distillation pressure is below 200Pa, it begins to warm up, vapo(u)rizing temperature is 900 DEG C~1200 DEG C, then keeps the temperature 0.5~10 hour, it is lead, zinc, cadmium alloy material to collect the distillate that distillation obtains, and bottoms are copper, nickel, cobalt etc..The present invention realizes that lead in copper-cadmium slag and nickel cobalt slag, zinc, cadmium and copper, nickel, cobalt detach using vapour pressure difference in different temperatures of lead in copper-cadmium slag and nickel cobalt slag, zinc, cadmium and copper, nickel, cobalt.A large amount of lead, zinc, cadmium can be separated in distillation process, and residue is copper, nickel, cobalt in bottoms, realizes the initial gross separation of copper-cadmium slag and nickel cobalt metal in the dreg.This method is easy to operate, and energy utilization rate and the efficiency of heating surface are high, and safety and sanitation are pollution-free.
Description
【Technical field】
The invention belongs to zinc field of metallurgy, are related to the initial gross separation of the copper-cadmium slag and nickel cobalt slag of the generation of zinc metallurgy process, specifically
It is related to a kind of method of separation of Zinc cadmium metal material in copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag.
【Background technology】
Zinc hydrometallurgy is the main method of zinc Extraction metallurgy, and the process of zinc hydrometallurgy mainly has:Sulfuric acid, calcining sulphur
Acid solution leaches, Purification of zinc sulfate solution, solution of zinc sulfate electrodeposition output metallic zinc after purification.Usually contain in zinc sulfate leaching liquid
There are the foreign metals such as copper, cadmium, nickel, cobalt, and the minimizing technology of these metals mainly uses zinc powder reduction method, due to copper cadmium and nickel
The removal condition of cobalt is different, and the method for the removal of these four general metals is carried out in two steps, corresponding output copper-cadmium slag and nickel cobalt
Slag, because zinc concentrate material composition and zinc sulfate purification condition are different, the copper-cadmium slag of different manufacturers output and the composition of nickel cobalt slag
It is variant.The general ingredient of copper-cadmium slag and nickel cobalt slag is shown in Table 1:
Table 1
Title | Zn | Cd | Co | Pb | Mn | Fe | Ni | Cu | H2O |
Copper-cadmium slag | 41.9% | 16.08% | 0.021% | / | 0.09% | 0.013% | / | 8.63% | 44.2% |
Nickel cobalt slag | 45-60% | 1-2% | 0.05-0.1% | 1-2% | 0.1-0.5% | 0.2-0.5% | 0.02-0.05% | / | 10-40% |
Zinc mainly exists with metal form in copper-cadmium slag and nickel cobalt slag, exists on a small quantity with sulfuric acid zinc fraction;Iron is mainly with hydrogen
Iron oxide exists;Cobalt, lead, nickel, cadmium etc. mainly exist in addition to fraction exists in the form of sulfate with metal form;
Manganese exists in the form of manganese sulfate.
At present the main processing mode of both the above slag for wet-leaching, separation, recycling, i.e., with acid or ammonium salt solution to slag into
Row Selectively leaching then separates and recovers metal therein using a variety of methods from solution.A kind of patent " copper-cadmium slag
Recovery method " (201410174714.4) disclose a kind of recovery method of copper-cadmium slag, technical process is:Copper-cadmium slag
Leaching-primary displacement-cake of press-overflow slurry liquid making-twice replaced-cake of press obtains thick cadmium-thick cadmium reduction melting-pure cadmium continuous vacuum
Distillation production pure cadmium.The problem of above method is:Technique is tediously long, and can be generated containing heavy metal in processes such as leaching, separation
Waste liquid and waste residue, waste liquid and waste residue can cause environmental pollution.
【Invention content】
Based on problems of the prior art, the present invention proposes a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt
The method of separation of Zinc cadmium metal material in slag, the present invention can solve that process in the prior art is more, and technique is tediously long, metal recovery
The problem of rate is low, pollutant yield is big, and realize most of metal in copper-cadmium slag and nickel cobalt slag and efficiently separate.
In order to solve the above-mentioned technical problem, the application, which adopts the following technical scheme that, is achieved:
A kind of method of separation of Zinc cadmium metal material in copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag, into raw material
Coal dust and alkaline earth metallic oxide powder end are added in, is thoroughly mixed to form mixture, pressure ball is carried out to mixture, it then will be after pressure ball
Mixture be evaporated in vacuo, vapo(u)rizing temperature be 900 DEG C~1200 DEG C, soaking time be 0.5~10 hour, after distillation
Cool down, in temperature-fall period, collect the distillate that distillation obtains, distillate is zinc cadmium metal material;
Mixture of the raw material for copper-cadmium slag, nickel cobalt slag or copper-cadmium slag and nickel cobalt slag, raw material, coal dust and alkaline-earth metal oxygen
Quality proportioning between compound powder is ranging from:Raw material: coal dust: alkaline earth metallic oxide powder end=100: (0.5-50): (0.5-
50)。
When mixture after pressure ball is evaporated in vacuo, pressure is not higher than 200Pa.
The difference purifying copper cadmium and nickel cobalt of copper-cadmium slag and nickel cobalt slag for zinc sulfate cleaning procedure output in Zinc hydrometallurgy process
The purification slag of output;Or to smelt the slag containing cadmium of cadmium process output and the residues containing zinc of Zinc smelting process output.
Residual residue after distillation is the mixed material for including copper, nickel, cobalt, iron and manganese.
Coal dust is raw coal powder, coke powder or semi-coke powder.
Alkaline earth metallic oxide powder end is calcium lime powder, dolomite dust or agstone.
Mixture after pressure ball is evaporated in vacuo in vacuum distillation furnace.
Compared with prior art, the present invention has the advantages that:
The method of the present invention is in different temperatures using the metals such as copper, nickel and cobalt in zinc, lead and the cadmium and raw material in raw material
When vapour pressure difference realize that zinc in raw material, lead and cadmium are detached with the metals such as copper, nickel and manganese in raw material, add in coal dust and alkali
The purpose of soil metal oxide powder is to make to be more easy to restore with lead existing for sulphate form and zinc in raw material, makes sulfate form
Existing lead and zinc are changed into metallic state and distillation of volatilizing, and improve the distillation recovery rate of lead zinc.In distillation process a large amount of zinc,
Lead and cadmium can be distilled volatilization, zinc, lead and cadmium enrichment in distillate, convenient in subsequent distillate and bottoms metal into
One step detaches.The method of the present invention is easy to operate, and energy utilization rate and the efficiency of heating surface are high, and safety and sanitation are pollution-free.The side of the present invention
The zinc of method acquisition, lead, cadmium enriched substance, mainly exist with metallic state, and later separation process is simple, and this method has enrichment speed
The characteristics of degree is fast, production efficiency is high.The metal in slag is detached by the method for the present invention, short with flow, the period is short, efficiency
The characteristics of height, comprehensive resource utilization rate is high, can greatly improve the separation and Extraction efficiency of metal in the dreg.Method using the present invention
The volatility of lead, zinc, cadmium can be obtained more than 98%.
【Specific embodiment】
The particular content of the present invention is described in more detail with reference to embodiments.
The method of separation of Zinc cadmium metal material is in reality in the copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag of the present invention
Shi Shi by mixture of copper-cadmium slag and nickel cobalt slag or both separately as raw material, is incorporated coal dust and alkaline earth in proportion in the feed
Metal oxide powder, the quality proportioning between raw material, coal dust and alkaline earth metallic oxide powder end is ranging from:Raw material: coal dust: alkali
Soil metal oxide powder=100: (0.5-50): (0.5-50) will be mixed into the mixing at coal dust and alkaline earth metallic oxide powder end
Material is sufficiently mixed, and obtains mixture, then by mixture pressure ball, then adds in the mixture after pressure ball in vacuum distillation furnace, right
Stove evacuation is evaporated in vacuo, until furnace pressure is evaporated in vacuo in 200Pa hereinafter, starting to stove heat is evaporated in vacuo, vacuum is steamed
Vapo(u)rizing temperature in furnace is 900 DEG C~1200 DEG C, is then kept the temperature, and soaking time is 0.5~10 hour, is dropped after distillation
Temperature in temperature-fall period, collects the distillate that distillation obtains, and distillate is zinc, cadmium and metal material, and distillation residual residue is
Cupric, nickel, cobalt, iron and manganese mixed material, so far, realize copper-cadmium slag, nickel cobalt slag or copper-cadmium slag and nickel cobalt slag mixed material
The initial gross separation of middle main component.Zinc, cadmium and the metal that predistillation separation obtains can do further separating-purifying, obtain
Single metal.Bottoms can further detach copper therein, nickel and cobalt etc..
The copper-cadmium slag and nickel cobalt slag of the present invention is the purifying copper of zinc hydrometallurgy zinc sulfate cleaning procedure output, cadmium, nickel, cobalt produce
The purification slag gone out;Or to smelt the slag containing cadmium of cadmium process output and the residues containing zinc of Zinc smelting process output;Coal dust for raw coal powder,
Coke powder or semi-coke powder;Alkaline earth metallic oxide powder end is calcium lime powder, dolomite dust or agstone.
The principle of the present invention is, in copper-cadmium slag and nickel cobalt slag, most of metal exists in the form of metal or alloy,
There is least a portion of metal sulfate, according to the difference of metal in the dreg vapour pressure in heating process, metal sulfate reduction decomposition
Rule, component volatile in copper-cadmium slag and nickel cobalt slag is detached using this property.
Above-mentioned technical proposal is deferred to, specific embodiments of the present invention are given below, it should be noted that not office of the invention
It is limited to specific examples below, all equivalents done on the basis of technical scheme each fall within the protection model of the present invention
It encloses.The present invention is described in further details with reference to embodiment.
It should be noted that in following embodiments, it is net that copper-cadmium slag and nickel cobalt slag originate from Zinc Hydrometallurgy Process solution of zinc sulfate
Chemical industry sequence.It can also be replaced using the slag containing cadmium of cadmium smelting process generation and the wash slag of Zinc smelting process output.
Embodiment 1:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag: coal in 100 DEG C of drying, the copper-cadmium slag after drying
Powder: quick lime (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press under 24MPa pressure
Pressure ball is madePelletizing, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, open vacuum pump,
So that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, it is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, after heat preservation
Vacuum breaker after room temperature is cooled to, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.8%, 99.2% and 99.8%.
Embodiment 2:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag: coal in 100 DEG C of drying, the copper-cadmium slag after drying
Powder: calcium lime powder (mass ratio)=100: 50: 50 carries out dispensing, and dispensing is after mixing using ball press under 24MPa pressure
The pelletizing of φ 10mm is made in pressure ball, and mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum pump,
So that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, it is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, after heat preservation
Vacuum breaker after room temperature is cooled to, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.8%, 99.5% and 99.8%.
Embodiment 3:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag: coal in 100 DEG C of drying, the copper-cadmium slag after drying
Powder: calcium lime powder (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 0.5 hour during 900 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 72.8%, 79.5% and 79.8%.
Embodiment 4:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag: coal in 100 DEG C of drying, the copper-cadmium slag after drying
Powder: calcium lime powder (mass ratio)=100: 50: 50 carries out dispensing, and dispensing is after mixing using ball press under 24MPa pressure
The pelletizing of φ 10mm is made in pressure ball, and mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum pump,
So that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, it is heated to keeping the temperature 10 hours during 1200 DEG C of temperature, heat preservation terminates
After be cooled to vacuum breaker after room temperature, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.9%, 99.9% and 99.9%.
Embodiment 5:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg nickel cobalts slag is taken to press nickel cobalt slag: coal in 100 DEG C of drying, the nickel cobalt slag after drying
Powder: calcium lime powder (mass ratio)=100: 25: 25 carries out dispensing, and dispensing is after mixing using ball press under 24MPa pressure
The pelletizing of φ 10mm is made in pressure ball, and mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum pump,
So that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, it is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, after heat preservation
Vacuum breaker after room temperature is cooled to, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.5%, 99.2% and 99.8%.
Embodiment 6:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg nickel cobalts slag is taken to press nickel cobalt slag: coal in 100 DEG C of drying, the nickel cobalt slag after drying
Powder: calcium lime powder (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 0.5 hour during 900 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 79.5%, 79.2% and 79.8%.
Embodiment 7:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg nickel cobalts slag is taken to press nickel cobalt slag: coal in 100 DEG C of drying, the nickel cobalt slag after drying
Powder: calcium lime powder (mass ratio)=100: 50: 50 carries out dispensing, and dispensing is after mixing using ball press under 24MPa pressure
The pelletizing of φ 10mm is made in pressure ball, and mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum pump,
So that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, it is heated to keeping the temperature 10 hours during 1200 DEG C of temperature, heat preservation terminates
After be cooled to vacuum breaker after room temperature, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.7%, 99.5% and 99.8%.
Embodiment 8:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg nickel cobalts slag is taken to press nickel cobalt slag: coal in 100 DEG C of drying, the nickel cobalt slag after drying
Powder: calcium lime powder (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 10 hours during 1200 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.4%, 99.6% and 99.7%.
Embodiment 9:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:It learns from else's experience respectively 100 DEG C nickel cobalt slag and copper-cadmium slag after drying, two kinds of slags press 1: 1 (quality
Than) mixed mixing slag, mixing slag presses mixing slag: coal dust: calcium lime powder (mass ratio)=100: 0.5: 0.5 carries out dispensing,
Dispensing using ball press pressure ball under 24MPa pressure, is made the pelletizing of φ 10mm, mixture pelletizing is placed in stone after mixing
It is put into vacuum distillation furnace in black crucible, opens vacuum pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and adds
0.5 hour is kept the temperature during heat to 900 DEG C of temperature, vacuum breaker after room temperature is cooled to after heat preservation, collects the distillate that distillation obtains
The lead Zn-Cd alloy material as isolated.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 78.5%, 78.2% and 78.8%.
Embodiment 10:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:It learns from else's experience respectively 100 DEG C nickel cobalt slag and copper-cadmium slag after drying, two kinds of slags press 1: 1 (quality
Than) mixed mixing slag, mixing slag presses mixing slag: coal dust: calcium lime powder (mass ratio)=100: 25: 25 carries out dispensing, matches
Material using ball press pressure ball under 24MPa pressure, is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite after mixing
It is put into vacuum distillation furnace in crucible, opens vacuum pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, heating
5 hours are kept the temperature to during 1000 DEG C of temperature, vacuum breaker after room temperature is cooled to after heat preservation, collecting the distillate that distillation obtains is
The lead Zn-Cd alloy material isolated.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 89.5%, 89.2% and 89.8%.
Embodiment 11:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:It learns from else's experience respectively 100 DEG C nickel cobalt slag and copper-cadmium slag after drying, two kinds of slags press 1: 1 (quality
Than) mixed mixing slag, mixing slag presses mixing slag: coal dust: calcium lime powder (mass ratio)=100: 50: 50 carries out dispensing, matches
Material using ball press pressure ball under 24MPa pressure, is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite after mixing
It is put into vacuum distillation furnace in crucible, opens vacuum pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, heating
10 hours are kept the temperature to during 1200 DEG C of temperature, vacuum breaker after room temperature is cooled to after heat preservation, collecting the distillate that distillation obtains is
For the lead Zn-Cd alloy material isolated.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.8%, 99.7% and 99.8%.
Embodiment 12:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag in 100 DEG C of drying, the copper-cadmium slag after drying: blue
Powdered carbon: quick lime (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.6%, 99% and 99.5%.
Embodiment 13:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag in 100 DEG C of drying, the copper-cadmium slag after drying: burnt
Powder: quick lime (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press under 24MPa pressure
The pelletizing of φ 10mm is made in pressure ball, and mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum pump,
So that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, it is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, after heat preservation
Vacuum breaker after room temperature is cooled to, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.8%, 99.2% and 99.8%.
Embodiment 14:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag: coal in 100 DEG C of drying, the copper-cadmium slag after drying
Powder: agstone (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.2%, 99.2% and 99.8%.
Embodiment 15:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg copper-cadmium slags is taken to press copper-cadmium slag: coal in 100 DEG C of drying, the copper-cadmium slag after drying
Powder: dolomite dust (mass ratio)=100: 0.5: 0.5 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.2%, 99.1% and 99.2%.
Embodiment 16:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg nickel cobalts slag is taken to press nickel cobalt slag in 100 DEG C of drying, the nickel cobalt slag after drying: burnt
Powder: calcium lime powder (mass ratio)=100: 25: 25 carries out dispensing, and dispensing is after mixing using ball press under 24MPa pressure
The pelletizing of φ 10mm is made in pressure ball, and mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum pump,
So that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, it is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, after heat preservation
Vacuum breaker after room temperature is cooled to, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.2%, 99.1% and 99.8%.
Embodiment 17:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg nickel cobalts slag is taken to press nickel cobalt slag in 100 DEG C of drying, the nickel cobalt slag after drying: blue
Powdered carbon: calcium lime powder (mass ratio)=100: 25: 25 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.4%, 99.2% and 99.7%.
Embodiment 18:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:0.5kg nickel cobalts slag is taken to press nickel cobalt slag in 100 DEG C of drying, the nickel cobalt slag after drying: blue
Powdered carbon: dolomite dust (mass ratio)=100: 25: 25 carries out dispensing, and dispensing is after mixing using ball press in 24MPa pressure
Lower pressure ball is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite crucible and is put into vacuum distillation furnace, opens vacuum
Pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and is heated to keeping the temperature 5 hours during 1000 DEG C of temperature, heat preservation knot
Vacuum breaker after room temperature is cooled to after beam, it is the lead Zn-Cd alloy material isolated to collect the distillate that distillation obtains.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 99.3%, 99.1% and 99.5%.
Embodiment 19:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:It learns from else's experience respectively 100 DEG C nickel cobalt slag and copper-cadmium slag after drying, two kinds of slags press 1: 1 (quality
Than) mixed mixing slag, mixing slag presses mixing slag: coke powder: calcium lime powder (mass ratio)=100: 25: 25 carries out dispensing, matches
Material using ball press pressure ball under 24MPa pressure, is made the pelletizing of φ 10mm, mixture pelletizing is placed in graphite after mixing
It is put into vacuum distillation furnace in crucible, opens vacuum pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, heating
5 hours are kept the temperature to during 1000 DEG C of temperature, vacuum breaker after room temperature is cooled to after heat preservation, collecting the distillate that distillation obtains is
The lead Zn-Cd alloy material isolated.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 89.6%, 89.8% and 89.5%.
Embodiment 20:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:It learns from else's experience respectively 100 DEG C nickel cobalt slag and copper-cadmium slag after drying, two kinds of slags press 1: 1 (quality
Than) mixed mixing slag, mixing slag presses mixing slag: semi-coke powder: calcium lime powder (mass ratio)=100: 25: 25 carries out dispensing,
Dispensing using ball press pressure ball under 24MPa pressure, is made the pelletizing of φ 10mm, mixture pelletizing is placed in stone after mixing
It is put into vacuum distillation furnace in black crucible, opens vacuum pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and adds
5 hours are kept the temperature during heat to 1000 DEG C of temperature, vacuum breaker after room temperature is cooled to after heat preservation, collecting the distillate that distillation obtains is
For the lead Zn-Cd alloy material isolated.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 89.6%, 89.8% and 89.5%.
Embodiment 21:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:It learns from else's experience respectively 100 DEG C nickel cobalt slag and copper-cadmium slag after drying, two kinds of slags press 1: 1 (quality
Than) mixed mixing slag, mixing slag presses mixing slag: semi-coke powder: agstone (mass ratio)=100: 25: 25 carries out dispensing,
Dispensing using ball press pressure ball under 24MPa pressure, is made the pelletizing of φ 10mm, mixture pelletizing is placed in stone after mixing
It is put into vacuum distillation furnace in black crucible, opens vacuum pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and adds
5 hours are kept the temperature during heat to 1000 DEG C of temperature, vacuum breaker after room temperature is cooled to after heat preservation, collecting the distillate that distillation obtains is
For the lead Zn-Cd alloy material isolated.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 89.6%, 89.6% and 89.4%.
Embodiment 22:
The present embodiment provides separation of Zinc cadmium metal material in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
Method, the detailed process of this method are:It learns from else's experience respectively 100 DEG C nickel cobalt slag and copper-cadmium slag after drying, two kinds of slags press 1: 1 (quality
Than) mixed mixing slag, mixing slag presses mixing slag: semi-coke powder: dolomite dust (mass ratio)=100: 25: 25 carries out dispensing,
Dispensing using ball press pressure ball under 24MPa pressure, is made the pelletizing of φ 10mm, mixture pelletizing is placed in stone after mixing
It is put into vacuum distillation furnace in black crucible, opens vacuum pump so that vacuum furnace pressure reaches 200Pa hereinafter, beginning to warm up, and adds
5 hours are kept the temperature during heat to 1000 DEG C of temperature, vacuum breaker after room temperature is cooled to after heat preservation, collecting the distillate that distillation obtains is
For the lead Zn-Cd alloy material isolated.
It weighed, analyzed to bottoms the content of lead therein, zinc, cadmium, the volatility of lead zinc cadmium is calculated, by steaming
The volatility for evaporating rear lead, zinc and cadmium respectively reaches 89.4%, 89.5% and 89.3%.
Claims (7)
1. the method for separation of Zinc cadmium metal material, feature exist in a kind of copper-cadmium slag generated from zinc metallurgy process and nickel cobalt slag
In, coal dust and alkaline earth metallic oxide powder end are added in into raw material, is thoroughly mixed to form mixture, pressure ball is carried out to mixture,
Then the mixture after pressure ball is evaporated in vacuo, vapo(u)rizing temperature is 900 DEG C~1200 DEG C, and soaking time is small for 0.5~10
When, cool down after distillation, in temperature-fall period, collect the distillate that distillation obtains, distillate is zinc cadmium metal material;
Mixture of the raw material for copper-cadmium slag, nickel cobalt slag or copper-cadmium slag and nickel cobalt slag, raw material, coal dust and alkaline earth oxide
Quality proportioning between powder is:Raw material: coal dust: alkaline earth metallic oxide powder end=100: (0.5-50): (0.5-50).
2. separation of Zinc cadmium metal object in a kind of copper-cadmium slag generated from zinc metallurgy process according to claim 1 and nickel cobalt slag
The method of material, which is characterized in that when the mixture after pressure ball is evaporated in vacuo, pressure is not higher than 200Pa.
3. separation of Zinc cadmium metal object in a kind of copper-cadmium slag generated from zinc metallurgy process according to claim 1 and nickel cobalt slag
The method of material, which is characterized in that copper-cadmium slag and nickel cobalt slag are net for the difference of zinc sulfate cleaning procedure output in Zinc hydrometallurgy process
Change copper cadmium and the purification slag of nickel cobalt output;Or for smelt cadmium process output slag containing cadmium and Zinc smelting process output contain zinc
Slag.
4. separation of Zinc cadmium metal object in a kind of copper-cadmium slag generated from zinc metallurgy process according to claim 1 and nickel cobalt slag
The method of material, which is characterized in that the residual residue after distillation is the mixed material for including copper, nickel, cobalt, iron and manganese.
5. separation of Zinc cadmium metal object in a kind of copper-cadmium slag generated from zinc metallurgy process according to claim 1 and nickel cobalt slag
The method of material, which is characterized in that coal dust is raw coal powder, coke powder or semi-coke powder.
6. separation of Zinc cadmium metal object in a kind of copper-cadmium slag generated from zinc metallurgy process according to claim 1 and nickel cobalt slag
The method of material, which is characterized in that alkaline earth metallic oxide powder end is calcium lime powder, dolomite dust or agstone.
7. separation of Zinc cadmium metal object in a kind of copper-cadmium slag generated from zinc metallurgy process according to claim 1 and nickel cobalt slag
The method of material, which is characterized in that the mixture after pressure ball is evaporated in vacuo in vacuum distillation furnace.
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CN114774681A (en) * | 2022-04-26 | 2022-07-22 | 东北大学 | Recycling method of zinc-containing soot |
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CN113969355A (en) * | 2021-09-27 | 2022-01-25 | 铜陵有色设计研究院有限责任公司 | Short-process preparation process for preparing zinc-cadmium alloy by using organic cobalt slag |
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