CN110257633A - It is a kind of to handle wet process zinc abstraction copper-cadmium slag, method of the nickel cobalt slag to prepare copper sponge, Spongy Cadmium simultaneously - Google Patents
It is a kind of to handle wet process zinc abstraction copper-cadmium slag, method of the nickel cobalt slag to prepare copper sponge, Spongy Cadmium simultaneously Download PDFInfo
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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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
- C22B17/00—Obtaining cadmium
- C22B17/04—Obtaining cadmium by wet processes
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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
- C22B7/006—Wet processes
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- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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Abstract
The invention discloses one kind can handle wet process zinc abstraction copper-cadmium slag, method of the nickel cobalt slag to prepare copper sponge, Spongy Cadmium simultaneously, leaching operation is carried out after copper-cadmium slag and nickel cobalt slag are mixed, 40-45 DEG C of temperature, begin acid: 146-155g/l, terminal ph:4-4.5, reaction time: 1.5h.It is separated by solid-liquid separation after reaction by filter press, liquid returns to main system, and solid carries out concentrated acid hot dipping, cobalt, nickel, cadmium are entered into liquid phase, copper enters slag phase, is separated by solid-liquid separation after reaction by filter press, slag is copper sponge, and liquid is by oxygen except high-grade Spongy Cadmiums of techniques output such as iron, zinc dust precipitations.The present invention solve it is lower using cupric, cadmium in the copper-cadmium slag of antimonic salt forward direction purification process output in Zinc Hydrometallurgy Process, it is lower containing cobalt in nickel cobalt slag, and the problem of copper, cadmium can not be recycled.Having many advantages, such as can to prepare simpler copper sponge, Spongy Cadmium, process flow, copper, cadmium direct yield and comprehensive recovery higher for Treatment of Copper, the lower copper-cadmium slag of cadmium amount and nickel cobalt slag simultaneously.
Description
Technical field
The present invention relates to chemical substance separating treatment technical fields, and in particular to one kind is for handling wet process zinc abstraction copper cadmium
The method of slag, nickel cobalt slag to prepare copper sponge, Spongy Cadmium belongs to wet process zinc smelting dreg processing technology field.
Background technique
In wet process zinc metallurgical process, cleaning procedure is frequently with purification by arsenate technique, and there are two types of the techniques: positive antimonic salt is net
Chemical industry skill and reverse purification by arsenate.The advantages of positive purification by arsenate, is that zinc powder consumption is lower, and energy loss is lower.But it uses
Copper, the cadmium content of the copper-cadmium slag of positive purification by arsenate technique output are unstable, and content is lower, and also containing a small amount of in nickel cobalt slag
Copper, cadmium.The method of conventional process copper-cadmium slag and nickel cobalt slag is cumbersome, and copper-cadmium slag, nickel cobalt slag must separate and use different works
Skill is handled.Therefore, copper-cadmium slag and nickel cobalt slag are handled according to traditional treatment process there are process flows tediously long, recycling
The disadvantages of rate is lower.Also result in the copper in nickel cobalt slag, cadmium is unable to comprehensive reutilization, result in waste of resources.In addition, content compared with
Low copper-cadmium slag is difficult to adopt traditional treatment process.
Summary of the invention
The technical problem to be solved by the present invention is in view of the shortcomings of the prior art, provide a kind of simpler process flow, copper,
The direct yield and comprehensive recovery of cadmium be higher, can Treatment of Copper, the lower copper-cadmium slag of cadmium amount, nickel cobalt slag simultaneously, to prepare sponge
The method of copper, Spongy Cadmium.
In order to solve the above technical problems, the present invention adopts the following technical scheme: one kind can handle wet process zinc abstraction copper simultaneously
The method of cadmium slag, nickel cobalt slag to prepare copper sponge, Spongy Cadmium, it is characterised in that: it carries out according to the following steps,
1), the copper-cadmium slag of cupric, cadmium is uniformly mixed with the nickel cobalt slag of cupric, cadmium；
2) operation, control parameter, are leached using electrolysis waste solution are as follows: 40 DEG C -45 DEG C of reaction temperature, begin acid: 146g/l-
155g/l, terminal ph:4-4.5, reaction time: 1.5h, liquid-solid ratio: 3-4:1；
3) after, waste liquid leaches operation separation of solid and liquid, solid phase carries out concentrated acid hot dipping, control parameter are as follows: 90 DEG C of reaction temperature-
96 DEG C, begin acid: 98% concentrated sulfuric acid, acid sludge ratio: 1:3, liquid-solid ratio: 4-7:1, reaction time: 5h, terminal ph:4-4.5；Reaction knot
It is separated by solid-liquid separation after beam, solid phase is copper sponge；
4) after, concentrated acid hot dipping operation is separated by solid-liquid separation, liquid phase carries out oxygen and removes iron, control parameter are as follows: amount of oxygen: according to liquid
4 times of oxygen theoretical amount needed for total iron content, reaction time: 2h in phase；
5) after, being separated by solid-liquid separation except iron reaction operation, liquid phase carries out zinc dust precipitation technique, control parameter are as follows: reaction temperature:
50 DEG C -55 DEG C, the reaction time: 1.5-2h, zinc powder additional amount are 1.2 of zinc powder theoretical amount needed for iron content in liquid phase, cadmium, copper displacement
Times；
6) it is separated by solid-liquid separation after, replacing, solid phase is Spongy Cadmium.
In step 1), used copper-cadmium slag is cupric, the lower copper-cadmium slag of cadmium, content are as follows: copper 1%-10%, cadmium
2%-15%；Nickel cobalt slag is the nickel cobalt slag containing a small amount of copper, cadmium, content are as follows: copper 0.2%-5%, cadmium 1%-6.5%；Copper cadmium
The mixing match of slag and nickel cobalt slag is 1:1.
In step 2), reaction process ph is controlled between 2.5-3, generates a large amount of hydrogen to prevent excessive acid.
In step 1) after mixing by copper-cadmium slag and nickel cobalt slag, mixture is delivered to reaction after using condensed water pulp
Tank is handled.
In step 5), zinc powder adition process is added according to a small amount of multiple mode, especially when zinc powder total amount is more,
Several pieces should be divided into be added portionwise.
The present invention has the following advantages that relative to the method for conventional process copper-cadmium slag, nickel cobalt slag, first, can Treatment of Copper,
The lower copper-cadmium slag of cadmium amount and nickel cobalt slag are allowed to that copper sponge, Spongy Cadmium can be prepared；Second, copper-cadmium slag and nickel cobalt slag can be mixed
Unify processing, simplified process flow, reduces processing cost；The direct yield and synthetical recovery of copper, cadmium can be improved in third
Rate reduces the wasting of resources.
Specific embodiment
It is described further With reference to embodiment:
Embodiment 1, raw material: copper-cadmium slag 10t, nickel cobalt slag 10t.Copper-cadmium slag content: copper 1.6%, cadmium 3.58%, nickel cobalt slag contain
Amount: copper 2.3%, cadmium 5.2%.It carries out according to the following steps,
1), copper-cadmium slag and nickel cobalt slag are uniformly mixed, proportion is 1:1, using being delivered to reactor tank after condensed water pulp；
2) electrolysis waste solution, is added and carries out leaching operation, 40 DEG C -45 DEG C of reaction temperature, begin acid 155g/l, terminal ph:4-
4.5, reaction process ph are controlled between 2.5-3, prevent excessive acid from generating a large amount of hydrogen, the reaction time: 1.5h, liquid-solid ratio: 3:
1.The complete rear separation of solid and liquid of operation is leached, solid phase about 6.1t chemically examines ingredient are as follows: copper 6.5%, cadmium 14%；
3), solid phase carries out concentrated acid hot dipping, control parameter are as follows: 90 DEG C -96 DEG C of reaction temperature, begin acid: 98% concentrated sulfuric acid, acid
Slag ratio: 1:3, liquid-solid ratio: 4:1, reaction time: 5h, terminal ph:4-4.5.It being separated by solid-liquid separation after reaction, solid phase is copper sponge,
About 1.2t, result of laboratory test are as follows: copper 31.3%, cadmium 2.27%.Liquid phase volume about 30m3, result of laboratory test: cadmium 28g/l, copper
0.002g/l；
4), liquid phase carries out oxygen and removes iron, reaction time 2h；
5) zinc powder about 500kg is added in, zinc dust precipitation technique, and zinc powder adding manner is using a small amount of multiple principle, reaction temperature
Degree: 50 DEG C -55 DEG C, the reaction time: about 2h；
6), be separated by solid-liquid separation, solid phase be Spongy Cadmium, about 810kg, result of laboratory test are as follows: cadmium 86%, zinc 8%, other 6%,
Total 100%.
As a result: the direct yield of cadmium is 79.34%, comprehensive recovery 82.5%；The comprehensive recovery of copper is 96.3%.
Embodiment 2, raw material: copper-cadmium slag 10t, nickel cobalt slag 10t.Copper-cadmium slag content: copper 1.9%, cadmium 6.36%, nickel cobalt slag contain
Amount: copper 1.39%, cadmium 4.22%.It carries out according to the following steps,
1), copper-cadmium slag and nickel cobalt slag are uniformly mixed, proportion is 1:1, using being delivered to reactor tank after condensed water pulp；
2) electrolysis waste solution, is added and carries out leaching operation, 40 DEG C -45 DEG C of reaction temperature, begin acid: 155g/l, terminal ph:4-
4.5, reaction process ph are controlled between 2.5-3, prevent excessive acid from generating a large amount of hydrogen, the reaction time: 1.5h, liquid-solid ratio: 4:
1.The complete rear separation of solid and liquid of operation is leached, solid phase about 5.4t chemically examines ingredient are as follows: copper 5.8%, cadmium 14.9%；
3), solid phase carries out concentrated acid hot dipping, control parameter are as follows: 90 DEG C -96 DEG C of reaction temperature, begin acid: 98% concentrated sulfuric acid, acid
Slag ratio: 1:3, liquid-solid ratio: 7:1, reaction time: 5h, terminal ph:4-4.5.It being separated by solid-liquid separation after reaction, solid phase is copper sponge,
About 1t, result of laboratory test are as follows: copper 26.7%, cadmium 2.33%.Liquid phase volume about 32m3, result of laboratory test: cadmium 24.8g/l, copper
0.002g/l；
4), liquid phase carries out oxygen and removes iron, reaction time 2h；
5) zinc powder about 550kg is added in, zinc dust precipitation technique, and zinc powder adding manner is using a small amount of multiple principle, reaction temperature
Degree: 50 DEG C -55 DEG C, the reaction time: about 1.5h；
6) it, is separated by solid-liquid separation.Its solid phase is Spongy Cadmium, about 910kg, result of laboratory test are as follows: cadmium 87%, zinc 9%, other
4%, add up to 100%.
As a result: the direct yield of cadmium: 74.8%, comprehensive recovery are as follows: 80.2%；The comprehensive recovery of copper: 82%.
Embodiment 3, raw material: copper-cadmium slag 10t, nickel cobalt slag 10t.Copper-cadmium slag content: copper 1%, cadmium 15%, nickel cobalt slag content:
Copper 5%, cadmium 1%.It carries out according to the following steps,
1), copper-cadmium slag and nickel cobalt slag are uniformly mixed, proportion is 1:1, using being delivered to reactor tank after condensed water pulp；
2) electrolysis waste solution, is added and carries out leaching operation, 40 DEG C -45 DEG C of reaction temperature, begin acid 150g/l, terminal ph:4-
4.5, reaction process ph are controlled between 2.5-3, prevent excessive acid from generating a large amount of hydrogen, the reaction time: 1.5h, liquid-solid ratio: 4:
1.The complete rear separation of solid and liquid of operation is leached, solid phase about 9.4t chemically examines ingredient are as follows: copper 6.3%, cadmium 17%；
3), solid phase carries out concentrated acid hot dipping, control parameter are as follows: 90 DEG C -96 DEG C of reaction temperature, begin acid: 98% concentrated sulfuric acid, acid
Slag ratio: 1:3, liquid-solid ratio: 5:1, reaction time: 5h, terminal ph:4-4.5.It being separated by solid-liquid separation after reaction, solid phase is copper sponge,
About 1.25t, result of laboratory test are as follows: copper 32.3%, cadmium 3.27%.Liquid phase volume about 47m3, result of laboratory test: cadmium 31g/l, copper
0.003g/l；
4), liquid phase carries out oxygen and removes iron, reaction time 2h；
5) zinc powder about 600kg is added in, zinc dust precipitation technique, and zinc powder adding manner is using a small amount of multiple principle, reaction temperature
Degree: 50 DEG C -55 DEG C, the reaction time: about 2h；
6) it, is separated by solid-liquid separation, solid phase is Spongy Cadmium, about 1260kg, result of laboratory test are as follows: cadmium 89%, zinc 6%, other
5%, add up to 100%.
As a result: the direct yield of cadmium is 82.37%, comprehensive recovery 70.1%；The comprehensive recovery of copper is 91.3%.
Embodiment 4, raw material: copper-cadmium slag 10t, nickel cobalt slag 10t.Copper-cadmium slag content: copper 10%, cadmium 2%, nickel cobalt slag content:
Copper 0.2%, cadmium 6.5%.It carries out according to the following steps,
1), copper-cadmium slag and nickel cobalt slag are uniformly mixed, proportion is 1:1, using being delivered to reactor tank after condensed water pulp；
2) electrolysis waste solution, is added and carries out leaching operation, 40 DEG C -45 DEG C of reaction temperature, begin acid: 155g/l, terminal ph:4-
4.5, reaction process ph are controlled between 2.5-3, prevent excessive acid from generating a large amount of hydrogen, the reaction time: 1.5h, liquid-solid ratio: 4:
1.The complete rear separation of solid and liquid of operation is leached, solid phase about 6.6t chemically examines ingredient are as follows: copper 15.3%, cadmium 12.7%；
3), solid phase carries out concentrated acid hot dipping, control parameter are as follows: 90 DEG C -96 DEG C of reaction temperature, begin acid: 98% concentrated sulfuric acid, acid
Slag ratio: 1:3, liquid-solid ratio: 7:1, reaction time: 5h, terminal ph:4-4.5.It being separated by solid-liquid separation after reaction, solid phase is copper sponge,
About 2.8t, result of laboratory test are as follows: copper 33.5%, cadmium 2.83%.Liquid phase volume about 32m3, result of laboratory test: cadmium 23.6g/l, copper
0.002g/l；
4), liquid phase carries out oxygen and removes iron, reaction time 2h；
5) zinc powder about 906kg is added in, zinc dust precipitation technique, and zinc powder adding manner is using a small amount of multiple principle, reaction temperature
Degree: 50 DEG C -55 DEG C, the reaction time: about 1.5h；
6) it, is separated by solid-liquid separation.Its solid phase is Spongy Cadmium, about 864kg, result of laboratory test are as follows: cadmium 88%, zinc 6%, other
6%, add up to 100%.
As a result: the direct yield of cadmium: 89.4%, comprehensive recovery are as follows: 81.5%；The comprehensive recovery of copper: 89%.
The above has been described in detail, described above, is only a preferred embodiment of the present invention, when cannot
Limit practical range of the invention, i.e., it is all according to the made equivalent changes and modifications of the application range, it should still belong to the present invention and cover model
In enclosing.
Claims (5)
1. one kind can handle wet process zinc abstraction copper-cadmium slag, method of the nickel cobalt slag to prepare Spongy Cadmium, Spongy Cadmium simultaneously, feature exists
In: it carries out according to the following steps,
1), the copper-cadmium slag of cupric, cadmium is uniformly mixed with the nickel cobalt slag of cupric, cadmium；
2) operation, control parameter, are leached using electrolysis waste solution are as follows: 40 DEG C -45 DEG C of reaction temperature, begin acid: 146g/l-155g/
L, terminal ph:4-4.5, reaction time: 1.5h, liquid-solid ratio: 3-4:1；
3) after, waste liquid leaches operation separation of solid and liquid, solid phase carries out concentrated acid hot dipping, control parameter are as follows: 90 DEG C -96 of reaction temperature
DEG C, begin acid: 98% concentrated sulfuric acid, acid sludge ratio: 1:3, liquid-solid ratio: 4-7:1, reaction time: 5h, terminal ph:4-4.5；Reaction terminates
After be separated by solid-liquid separation, solid phase is copper sponge；
4) after, concentrated acid hot dipping operation is separated by solid-liquid separation, liquid phase carries out oxygen and removes iron, control parameter are as follows: amount of oxygen: according in liquid phase
4 times of oxygen theoretical amount needed for total iron content, reaction time: 2h；
5) after, being separated by solid-liquid separation except iron reaction operation, liquid phase carries out zinc dust precipitation technique, control parameter are as follows: reaction temperature: 50
DEG C -55 DEG C, the reaction time: 1.5-2h, zinc powder additional amount are 1.2 of zinc powder theoretical amount needed for iron content in liquid phase, cadmium, copper are replaced
Times；
6) it is separated by solid-liquid separation after, replacing, solid phase is Spongy Cadmium.
2. wet process zinc abstraction copper-cadmium slag, the nickel cobalt slag according to claim 1 of can handling simultaneously is to prepare copper sponge, Spongy Cadmium
Method, it is characterised in that: in step 1), used copper-cadmium slag be cupric, the lower copper-cadmium slag of cadmium, content are as follows: copper
1%-10%, cadmium 2%-15%；Nickel cobalt slag is the nickel cobalt slag containing a small amount of copper, cadmium, content are as follows: copper 0.2%-5%, cadmium 1%-
6.5%；The mixing match of copper-cadmium slag and nickel cobalt slag is 1:1.
3. wet process zinc abstraction copper-cadmium slag, the nickel cobalt slag according to claim 1 of can handling simultaneously is to prepare copper sponge, Spongy Cadmium
Method, it is characterised in that: in step 2), reaction process ph control prevents excessive acid between 2.5-3 and generates a large amount of
Hydrogen.
4. wet process zinc abstraction copper-cadmium slag, the nickel cobalt slag according to claim 1 of can handling simultaneously is to prepare copper sponge, Spongy Cadmium
Method, it is characterised in that: in step 1) after mixing by copper-cadmium slag and nickel cobalt slag, after mixture uses condensed water pulp
Reactor tank is delivered to be handled.
5. wet process zinc abstraction copper-cadmium slag, the nickel cobalt slag according to claim 1 of can handling simultaneously is to prepare copper sponge, Spongy Cadmium
Method, it is characterised in that: in step 5), zinc powder adition process is added according to a small amount of multiple mode.
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| CN201910553545.8A CN110257633B (en) | 2019-06-25 | 2019-06-25 | Method for preparing sponge copper and sponge cadmium by simultaneously treating wet-process zinc smelting copper cadmium slag and nickel cobalt slag |
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| CN201910553545.8A CN110257633B (en) | 2019-06-25 | 2019-06-25 | Method for preparing sponge copper and sponge cadmium by simultaneously treating wet-process zinc smelting copper cadmium slag and nickel cobalt slag |
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Cited By (3)
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| CN110951969A (en) * | 2019-11-08 | 2020-04-03 | 荆门市格林美新材料有限公司 | Method for recovering valuable metals from difficult-to-treat cobalt-nickel-containing tailings |
| CN113005303A (en) * | 2021-03-26 | 2021-06-22 | 陕西锌业有限公司 | Method for extracting cobalt from cadmium-poor high-cobalt liquid |
| CN113969415A (en) * | 2021-09-27 | 2022-01-25 | 贵州省冶金化工研究所 | Method for producing zinc alloy by utilizing copper-cadmium slag electrolysis |
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| CN113969415A (en) * | 2021-09-27 | 2022-01-25 | 贵州省冶金化工研究所 | Method for producing zinc alloy by utilizing copper-cadmium slag electrolysis |
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