CN108251651B - method for separating zinc-cadmium-lead alloy materials from copper-cadmium slag and nickel-cobalt slag generated in zinc smelting process - Google Patents
method for separating zinc-cadmium-lead alloy materials from copper-cadmium slag and nickel-cobalt slag generated in zinc smelting process Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
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- C22B5/00—General methods of reducing to metals
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Abstract
the invention discloses a method for separating zinc-cadmium-lead alloy materials from copper-cadmium slag and nickel-cobalt slag generated in a zinc smelting process, which comprises the steps of adding coal dust and alkaline earth metal oxide into the copper-cadmium slag, the nickel-cobalt slag or a mixture of the copper-cadmium slag and the nickel-cobalt slag, carrying out vacuum distillation after the mixture is pelletized, starting heating at the distillation temperature of 900-1200 ℃ under the distillation pressure of below 200Pa, then carrying out heat preservation for 0.5-10 hours, collecting distillate obtained by distillation, namely the lead, zinc and cadmium alloy materials, and collecting distillation residues, namely copper, nickel, cobalt and the like. The invention realizes the separation of lead, zinc and cadmium from copper, nickel and cobalt in copper-cadmium slag and nickel-cobalt slag by utilizing the vapor pressure difference of lead, zinc and cadmium from copper, nickel and cobalt in the copper-cadmium slag and the nickel-cobalt slag at different temperatures. In the distillation process, a large amount of lead, zinc and cadmium can be separated out, and the residues in the distillation residues are copper, nickel and cobalt, so that the primary separation of metals in the copper-cadmium residues and the nickel-cobalt residues is realized. The method has the advantages of convenient operation, high energy utilization rate and heating efficiency, safety, sanitation and no pollution.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of zinc metallurgy, relates to preliminary separation of copper-cadmium slag and nickel-cobalt slag generated in a zinc smelting process, and particularly relates to a method for separating a zinc-cadmium-lead alloy material from the copper-cadmium slag and the nickel-cobalt slag generated in the zinc smelting process.
[ background of the invention ]
the zinc hydrometallurgy is a main method for zinc extraction metallurgy, and the zinc hydrometallurgy mainly comprises the following working procedures: roasting zinc concentrate, leaching calcine sulfuric acid solution, purifying zinc sulfate solution, and electrodepositing the purified zinc sulfate solution to produce metal zinc. The zinc sulfate leaching solution usually contains impurity metals such as copper, cadmium, nickel, cobalt and the like, and the removal method of the metals mainly adopts a zinc powder reduction method, because the removal conditions of copper, cadmium and nickel and cobalt are different, the removal method of the four metals is generally carried out in two steps, copper, cadmium slag and nickel and cobalt slag are correspondingly produced, and because the raw material components of zinc concentrate and the purification conditions of zinc sulfate are different, the compositions of the copper, cadmium slag and the nickel and cobalt slag produced by different manufacturers are also different. The general composition of the copper cadmium slag and the nickel cobalt slag is shown in table 1:
TABLE 1
| Name (R) | 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％ |
The zinc in the copper-cadmium slag and the nickel-cobalt slag mainly exists in a metal form, and a small amount of zinc sulfate exists; iron exists mainly in the form of ferric hydroxide; cobalt, lead, nickel, cadmium and the like exist mainly in a metal form except that a small part exists in a sulfate form; manganese is present in the form of manganese sulphate.
At present, the two kinds of slag are mainly treated by wet leaching, separation and recovery, namely, the slag is selectively leached by acid or ammonium solution, and then metal in the slag is separated and recovered from the solution by adopting various methods. The patent 'a recovery method of copper-cadmium slag' (201410174714.4) discloses a recovery method of copper-cadmium slag, which mainly comprises the following process flows: leaching copper-cadmium slag, primary replacement, pressing cakes, making liquid from overflow slurry, secondary replacement, pressing cakes to obtain crude cadmium, reducing and smelting the crude cadmium, and continuously carrying out vacuum distillation on the refined cadmium to produce the refined cadmium. The problems of the above method are: the process is long, waste liquid and waste residue containing heavy metals are generated in the processes of leaching, separation and the like, and the waste liquid and the waste residue can cause environmental pollution.
[ summary of the invention ]
Based on the problems in the prior art, the invention provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in the zinc smelting process, and the method can solve the problems of multiple processes, long process, low metal recovery rate and large pollutant generation amount in the prior art, and effectively separate most of metals in the copper, cadmium slag and the nickel, cobalt slag.
In order to solve the technical problem, the application adopts the following technical scheme:
a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process comprises the steps of adding coal powder and alkaline earth metal oxide powder into raw materials, fully mixing to form a mixture, pressing the mixture into balls, then carrying out vacuum distillation on the pressed mixture, wherein the distillation temperature is 900-1200 ℃, the heat preservation time is 0.5-10 hours, cooling after the distillation is finished, and collecting distillate obtained by the distillation in the cooling process, wherein the distillate is the zinc, cadmium and lead alloy materials;
The raw materials are copper-cadmium slag, nickel-cobalt slag or a mixture of the copper-cadmium slag and the nickel-cobalt slag, and the mass ratio range of the raw materials, the coal powder and the alkaline earth metal oxide powder is as follows: the raw material, coal powder and alkaline earth metal oxide powder are 100 to (0.5-50).
when the mixture after the ball pressing is subjected to vacuum distillation, the pressure is not higher than 200 Pa.
The copper-cadmium slag and the nickel-cobalt slag are purification slag which is produced in a zinc sulfate purification process in a zinc hydrometallurgy process and is used for respectively purifying copper, cadmium and nickel and cobalt; or cadmium-containing slag produced in the cadmium smelting process and zinc-containing slag produced in the zinc smelting process.
The residue left after distillation is a mixture containing copper, nickel, cobalt, iron and manganese.
the coal powder is raw coal powder, coke powder or semi coke powder.
The alkaline earth metal oxide powder is quicklime powder, dolomite powder or limestone powder.
The mixture after the pressing of the pellets was subjected to vacuum distillation in a vacuum distillation furnace.
Compared with the prior art, the invention has the following beneficial effects:
The method of the invention utilizes the vapor pressure difference of zinc, lead and cadmium in the raw material and copper, nickel, cobalt and other metals in the raw material at different temperatures to realize the separation of the zinc, lead and cadmium in the raw material and the copper, nickel, manganese and other metals in the raw material, and the purpose of adding the coal powder and the alkaline earth metal oxide powder is to ensure that the lead and zinc existing in the form of sulfate in the raw material is easier to reduce, lead and zinc existing in the form of sulfate are converted into metal states to be volatilized and distilled, thereby improving the distillation recovery rate of the lead and the zinc. During the distillation process, a large amount of zinc, lead and cadmium can be distilled and volatilized, and the zinc, lead and cadmium in the distillate are enriched, so that the subsequent distillate and the distillation residue can be further separated conveniently. The method has the advantages of convenient operation, high energy utilization rate and heating efficiency, safety, sanitation and no pollution. The zinc, lead and cadmium concentrate obtained by the method mainly exists in a metal state, the subsequent separation process is simple, and the method has the characteristics of high enrichment speed and high production efficiency. The method for separating the metal in the slag has the characteristics of short flow, short period, high efficiency and high comprehensive utilization rate of resources, and can greatly improve the separation and extraction efficiency of the metal in the slag. The method of the invention can obtain lead, zinc and cadmium with the volatilization rate of more than 98 percent.
[ detailed description ] embodiments
The present invention will be described in further detail with reference to examples.
When the method for separating the zinc-cadmium-lead alloy material from the copper-cadmium slag and the nickel-cobalt slag generated in the zinc smelting process is implemented, the mixture or the mixture of the copper-cadmium slag and the nickel-cobalt slag is/are independently used as a raw material, the coal powder and the alkaline earth metal oxide powder are added into the raw material according to the proportion, and the mass ratio range of the raw material, the coal powder and the alkaline earth metal oxide powder is as follows: mixing the mixture of powdered coal and alkaline earth metal oxide powder to obtain mixture, pressing the mixture into balls, adding the mixture into vacuum distillation furnace, vacuumizing the vacuum distillation furnace until the pressure in the vacuum distillation furnace is below 200Pa, heating the vacuum distillation furnace, wherein the distillation temperature in the vacuum distillation furnace is 900-1200 ℃, then preserving heat for 0.5-10 hours, cooling after the distillation is finished, and in the cooling process, and collecting distillate obtained by distillation, wherein the distillate is a zinc, cadmium and lead alloy material, and the distillation residue is a mixed material containing copper, nickel, cobalt, iron and manganese, so that the primary separation of main components in the copper-cadmium slag, the nickel-cobalt slag or the mixed material of the copper-cadmium slag and the nickel-cobalt slag is realized. The zinc, cadmium and lead alloy obtained by preliminary distillation and separation can be further separated and purified to obtain single metal. The distillation residue can further separate copper, nickel, cobalt and the like.
the copper-cadmium slag and the nickel-cobalt slag are the purification slag produced in the zinc sulfate purification process of zinc hydrometallurgy and used for purifying copper, cadmium, nickel and cobalt; or cadmium-containing slag produced in the cadmium smelting process and zinc-containing slag produced in the zinc smelting process; the coal powder is raw coal powder, coke powder or semi-coke powder; the alkaline earth metal oxide powder is quicklime powder, dolomite powder or limestone powder.
The principle of the invention is that most metals in the copper-cadmium slag and the nickel-cobalt slag exist in the form of metal or alloy, a small amount of metal sulfate exists, and volatile components in the copper-cadmium slag and the nickel-cobalt slag are separated by utilizing the property according to the difference of vapor pressure of the metals in the slag in the heating process and the rule of reduction decomposition of the metal sulfate.
The present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention fall within the protection scope of the present invention. The present invention will be described in further detail with reference to examples.
In the following examples, the copper-cadmium slag and the nickel-cobalt slag are produced from the zinc sulfate solution purification process in the zinc hydrometallurgy process. Or cadmium-containing slag produced in the cadmium smelting process and zinc-containing slag produced in the zinc smelting process.
Example 1:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with the materials according to the mass ratio of the copper-cadmium slag, the coal powder and the quicklime of 100: 0.5, the materials are uniformly mixed and pressed into balls under the pressure of 24MPa by a ball press machine to prepare the copper-cadmium alloy materialPlacing the mixture pellets in a graphite crucible, putting the mixture pellets in a vacuum distillation furnace, starting a vacuum pump to enable the pressure in the vacuum furnace to reach below 200Pa, starting heating, keeping the temperature for 5 hours when the temperature is 1000 ℃, breaking the vacuum after cooling to the normal temperature after the temperature is kept, and collecting distillate obtained by distillation, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.8%, 99.2% and 99.8%.
Example 2:
this embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with the pulverized coal and the quicklime powder (mass ratio) is 100: 50, the mixture is uniformly mixed and then pressed into pellets under the pressure of 24MPa by a ball press to prepare pellets with the diameter of 10mm, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 5 hours when the temperature reaches 1000 ℃, the vacuum is broken after the temperature is kept and is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
and weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.8%, 99.5% and 99.8%.
Example 3:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with the pulverized coal and the quicklime powder (mass ratio) is 100: 0.5, the mixture is uniformly mixed and then pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating is started, the temperature is kept for 0.5 hour when the temperature is 900 ℃, the temperature is reduced to the normal temperature after the temperature is kept, vacuum is broken, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
and weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 72.8%, 79.5% and 79.8%.
Example 4:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with the pulverized coal and the quicklime powder (mass ratio) is 100: 50, the mixture is uniformly mixed and then pressed into pellets under the pressure of 24MPa by a ball press to prepare pellets with the diameter of 10mm, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 10 hours when the temperature reaches 1200 ℃, the vacuum is broken after the temperature is kept and is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.9%, 99.9% and 99.9%.
Example 5:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of nickel cobalt slag is dried at 100 ℃, the dried nickel cobalt slag is mixed with the raw materials according to the mass ratio of the nickel cobalt slag, the coal powder and the quicklime powder being 100: 25, the mixture is uniformly mixed and then pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 5 hours when the temperature is 1000 ℃, the vacuum is broken after the temperature is kept to be reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.5%, 99.2% and 99.8%.
Example 6:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of nickel-cobalt slag is dried at 100 ℃, the dried nickel-cobalt slag is mixed with the pulverized coal and the quicklime powder according to the mass ratio of 100: 0.5, the mixture is uniformly mixed and then pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum distillation furnace reaches below 200Pa, the heating is started, the temperature is kept for 0.5 hour when the temperature is 900 ℃, the vacuum is broken after the temperature is kept to be reduced to the normal temperature after the temperature is kept, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
and weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 79.5%, 79.2% and 79.8%.
Example 7:
this embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of nickel cobalt slag is dried at 100 ℃, the dried nickel cobalt slag is mixed with the materials according to the mass ratio of the nickel cobalt slag, the coal powder and the quicklime powder being 100: 50, the materials are uniformly mixed and then pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 10 hours when the temperature is up to 1200 ℃, the vacuum is broken after the temperature is kept and the temperature is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.7%, 99.5% and 99.8%.
Example 8:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of nickel-cobalt slag is dried at 100 ℃, the dried nickel-cobalt slag is mixed with the pulverized coal and the quicklime powder according to the mass ratio of 100: 0.5, the mixture is uniformly mixed and then pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 10 hours when the temperature reaches 1200 ℃, the vacuum is broken after the temperature is kept and the temperature is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.4%, 99.6% and 99.7%.
example 9:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: respectively taking nickel cobalt slag and copper cadmium slag dried at 100 ℃, mixing the two slag according to the mass ratio of 1: 1, mixing the mixed slag according to the mass ratio of the mixed slag to coal powder to quicklime powder (the mass ratio) is 100: 0.5, uniformly mixing the ingredients, pressing the mixture into pellets with the diameter of 10mm by using a ball press under the pressure of 24MPa, putting the pellets into a graphite crucible, putting the pellets into a vacuum distillation furnace, starting a vacuum pump to ensure that the pressure in the vacuum furnace reaches below 200Pa, starting heating, keeping the temperature for 0.5 hour when the temperature is 900 ℃, reducing the temperature to the normal temperature after the temperature is kept, breaking the vacuum, and collecting distillate obtained by distillation, namely the separated lead-zinc-cadmium alloy material.
and weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 78.5%, 78.2% and 78.8%.
example 10:
this embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: respectively taking nickel cobalt slag and copper cadmium slag dried at 100 ℃, mixing the two slag according to the mass ratio of 1: 1, blending the mixed slag according to the mass ratio of the mixed slag to coal powder to quicklime powder (the mass ratio) is 100: 25, uniformly mixing the blended slag, pressing the mixture into pellets with the diameter of 10mm by using a ball press under the pressure of 24MPa, putting the pellets into a graphite crucible, putting the graphite crucible into a vacuum distillation furnace, starting a vacuum pump to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating, keeping the temperature for 5 hours when the temperature is 1000 ℃, breaking the vacuum after cooling to the normal temperature after keeping the temperature, and collecting distillate obtained by distillation, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 89.5%, 89.2% and 89.8%.
Example 11:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: respectively taking nickel cobalt slag and copper cadmium slag dried at 100 ℃, mixing the two slag according to the mass ratio of 1: 1, blending the mixed slag according to the mass ratio of the mixed slag to coal powder to quicklime powder (the mass ratio) is 100: 50, uniformly mixing the blended slag, pressing the mixture into pellets with the diameter of 10mm by using a ball press under the pressure of 24MPa, putting the pellets into a graphite crucible, putting the graphite crucible into a vacuum distillation furnace, starting a vacuum pump to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating, keeping the temperature for 10 hours when the temperature is 1200 ℃, breaking the vacuum after the temperature is kept, cooling to the normal temperature, collecting distillate obtained by distillation, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.8%, 99.7% and 99.8%.
example 12:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with blue carbon powder and quicklime according to the mass ratio of 100: 0.5, the mixture is pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa after being uniformly mixed, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating is started until the temperature reaches 1000 ℃, the temperature is kept for 5 hours, the vacuum is broken after the temperature is kept and the temperature is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.6%, 99% and 99.5%.
Example 13:
this embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with coke powder and calcium oxide according to the mass ratio of 100: 0.5, the mixture is pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa after being uniformly mixed, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating is started, the temperature is kept for 5 hours when the temperature reaches 1000 ℃, the vacuum is broken after the temperature is kept and the temperature is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
and weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.8%, 99.2% and 99.8%.
Example 14:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with the pulverized coal and the limestone powder according to the mass ratio of 100: 0.5, the mixture is pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa after being uniformly mixed, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 5 hours when the temperature reaches 1000 ℃, the vacuum is broken after the temperature is kept and the temperature is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.2%, 99.2% and 99.8%.
Example 15:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of copper-cadmium slag is dried at 100 ℃, the dried copper-cadmium slag is mixed with the pulverized coal and dolomite powder according to the mass ratio of 100: 0.5, the mixture is pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa after being uniformly mixed, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating is started until the temperature reaches 1000 ℃, the temperature is kept for 5 hours, the vacuum is broken after the temperature is kept and the temperature is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.2%, 99.1% and 99.2%.
Example 16:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of nickel cobalt slag is dried at 100 ℃, the dried nickel cobalt slag is mixed with the coke powder and the quicklime powder according to the mass ratio of 100: 25, the mixture is pressed into pellets with the diameter of 10mm by a ball press machine under the pressure of 24MPa after being uniformly mixed, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 5 hours when the temperature is 1000 ℃, the vacuum is broken after the temperature is kept to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.2%, 99.1% and 99.8%.
example 17:
this embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of nickel cobalt slag is dried at 100 ℃, the dried nickel cobalt slag is mixed with the blue carbon powder and the quicklime powder according to the mass ratio of 100: 25, the mixture is uniformly mixed and then pressed into pellets with the diameter of 10mm by a ball press under the pressure of 24MPa, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum furnace reaches below 200Pa, the heating is started, the temperature is kept for 5 hours when the temperature reaches 1000 ℃, the vacuum is broken after the temperature is kept and the temperature is reduced to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.4%, 99.2% and 99.7%.
example 18:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: 0.5kg of nickel cobalt slag is dried at 100 ℃, the dried nickel cobalt slag is mixed with the cobalt slag, the semi-coke powder and the dolomite powder (mass ratio) is 100: 25, the mixture is uniformly mixed and then pressed into pellets under the pressure of 24MPa by a ball press to prepare pellets with the diameter of 10mm, the pellets of the mixture are placed in a graphite crucible and put in a vacuum distillation furnace, a vacuum pump is started to ensure that the pressure in the vacuum distillation furnace reaches below 200Pa, the heating is started, the temperature is kept for 5 hours when the temperature is 1000 ℃, the vacuum is broken after the temperature is kept to the normal temperature, and distillate obtained by distillation is collected, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 99.3%, 99.1% and 99.5%.
Example 19:
this embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: respectively taking nickel cobalt slag and copper cadmium slag dried at 100 ℃, mixing the two slag according to the mass ratio of 1: 1, blending the mixed slag according to the mass ratio of the mixed slag to coke powder to quicklime powder (mass ratio) of 100: 25, uniformly mixing the blended slag, pressing the mixture into pellets with the diameter of 10mm by using a ball press under the pressure of 24MPa, putting the pellets into a graphite crucible, putting the pellets into a vacuum distillation furnace, starting a vacuum pump to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating, keeping the temperature for 5 hours when the temperature is 1000 ℃, breaking the vacuum after the temperature is kept, cooling to the normal temperature, collecting distillate obtained by distillation, namely the separated zinc lead cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 89.6%, 89.8% and 89.5%.
Example 20:
this embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: respectively taking nickel cobalt slag and copper cadmium slag dried at 100 ℃, mixing the two slag according to the mass ratio of 1: 1, blending the mixed slag according to the mass ratio of the mixed slag to blue carbon powder to quicklime powder (mass ratio) of 100: 25, uniformly mixing the blended slag, pressing the mixture into pellets with the diameter of 10mm by using a ball press under the pressure of 24MPa, putting the pellets into a graphite crucible, putting the pellets into a vacuum distillation furnace, starting a vacuum pump to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating, keeping the temperature for 5 hours when the temperature is 1000 ℃, breaking the vacuum after the temperature is kept, cooling to the normal temperature, collecting distillate obtained by distillation, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 89.6%, 89.8% and 89.5%.
Example 21:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: respectively taking nickel cobalt slag and copper cadmium slag dried at 100 ℃, mixing the two slag according to the mass ratio of 1: 1, blending the mixed slag according to the mass ratio of the mixed slag to blue carbon powder to limestone powder (the mass ratio) is 100: 25, uniformly mixing the blended slag, pressing the mixture into pellets with the diameter of 10mm by using a ball press under the pressure of 24MPa, putting the pellets into a graphite crucible, putting the pellets into a vacuum distillation furnace, starting a vacuum pump to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating, keeping the temperature for 5 hours when the temperature is 1000 ℃, breaking the vacuum after the temperature is kept, cooling to the normal temperature, collecting distillate obtained by distillation, namely the separated zinc lead cadmium alloy material.
and weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 89.6%, 89.6% and 89.4%.
example 22:
This embodiment provides a method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process, which specifically comprises the following steps: respectively taking nickel cobalt slag and copper cadmium slag dried at 100 ℃, mixing the two kinds of slag according to the mass ratio of 1: 1, burdening the mixed slag according to the mass ratio of the mixed slag to blue carbon powder to dolomite powder (the mass ratio) of 100: 25, uniformly mixing the burdening and the mixing, pressing the mixture into pellets with the diameter of 10mm by using a ball press under the pressure of 24MPa, putting the pellets into a graphite crucible, putting the pellets into a vacuum distillation furnace, starting a vacuum pump to ensure that the pressure in the vacuum furnace reaches below 200Pa, heating, keeping the temperature for 5 hours when the temperature is 1000 ℃, breaking the vacuum after the temperature is reduced to the normal temperature after the temperature is kept, and collecting distillate obtained by distillation, namely the separated lead-zinc-cadmium alloy material.
And weighing the distillation residues, analyzing the contents of lead, zinc and cadmium in the distillation residues, and calculating the volatilization rates of lead, zinc and cadmium, wherein the volatilization rates of lead, zinc and cadmium after distillation respectively reach 89.4%, 89.5% and 89.3%.
Claims (5)
1. A method for separating zinc, cadmium and lead alloy materials from copper, cadmium slag and nickel, cobalt slag generated in a zinc smelting process is characterized in that coal powder and alkaline earth metal oxide powder are added into raw materials and are fully mixed to form a mixture, the mixture is pressed into balls, then the mixture after being pressed into balls is subjected to vacuum distillation, the distillation temperature is 1000 ℃, the heat preservation time is 5 hours, the temperature is reduced after the distillation is finished, distillate obtained by the distillation is collected in the temperature reduction process, and the distillate is the zinc, cadmium and lead alloy material;
The raw materials are copper-cadmium slag, nickel-cobalt slag or a mixture of the copper-cadmium slag and the nickel-cobalt slag, and the mass ratio of the raw materials, the coal powder and the alkaline earth metal oxide powder is as follows: the raw materials, the coal powder and the alkaline earth metal oxide powder are 100: 0.5; or the raw materials, the coal powder and the alkaline earth metal oxide powder are 100: 25;
The copper-cadmium slag and the nickel-cobalt slag are purification slag which is produced in a zinc sulfate purification process in a zinc hydrometallurgy process and is used for respectively purifying copper, cadmium and nickel and cobalt; or cadmium-containing slag produced in the cadmium smelting process and zinc-containing slag produced in the zinc smelting process;
The alkaline earth metal oxide powder is dolomite powder or limestone powder;
When pressing the balls, a ball press is adopted to press the balls under the pressure of 24 MPa.
2. The method for separating the zinc-cadmium-lead alloy material from the copper-cadmium slag and the nickel-cobalt slag generated in the zinc smelting process as claimed in claim 1, wherein the pressure of the mixture after the ball pressing is not higher than 200Pa when the mixture is subjected to vacuum distillation.
3. the method for separating the zinc-cadmium-lead alloy material from the copper-cadmium slag and the nickel-cobalt slag generated in the zinc smelting process as claimed in claim 1, wherein the residue left after distillation is a mixed material containing copper, nickel, cobalt, iron and manganese.
4. The method for separating the zinc-cadmium-lead alloy material from the copper-cadmium slag and the nickel-cobalt slag generated in the zinc smelting process according to claim 1, wherein the coal powder is raw coal powder, coke powder or semi-coke powder.
5. The method for separating the zinc-cadmium-lead alloy material from the copper-cadmium slag and the nickel-cobalt slag generated in the zinc smelting process as claimed in claim 1, wherein the mixture after the ball pressing is subjected to vacuum distillation in a vacuum distillation furnace.
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| CN109576505A (en) * | 2018-12-20 | 2019-04-05 | 北京矿冶科技集团有限公司 | A kind of method that zinc cobalt efficiently separates |
| 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 |
| CN113969355B (en) * | 2021-09-27 | 2023-05-09 | 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 utilizing organic cobalt slag |
| CN114182097B (en) * | 2021-12-08 | 2024-03-12 | 西安建筑科技大学 | Method for cooperatively recycling copper-zinc-containing oxide and zinc sulfide |
| CN114457236B (en) * | 2021-12-16 | 2023-01-24 | 中南大学 | Separation and purification device for metal waste residues and separation and purification method for cobalt oxide residues |
| CN114774681B (en) * | 2022-04-26 | 2024-02-13 | 东北大学 | Recycling method of zinc-containing ash |
| CN115011797A (en) * | 2022-06-07 | 2022-09-06 | 湖北大江环保科技股份有限公司 | Method for smelting copper by using vacuum distillation equipment |
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