CN109439916A - A kind of method of the wet-treating containing cadmium fumes - Google Patents
A kind of method of the wet-treating containing cadmium fumes Download PDFInfo
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- CN109439916A CN109439916A CN201811418578.3A CN201811418578A CN109439916A CN 109439916 A CN109439916 A CN 109439916A CN 201811418578 A CN201811418578 A CN 201811418578A CN 109439916 A CN109439916 A CN 109439916A
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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
- C22B7/02—Working-up flue dust
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
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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
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin 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
- C22B7/007—Wet processes by acid leaching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
A kind of method of the wet-treating containing cadmium fumes will contain cadmium fumes with dilute sulfuric acid and carry out oxygen leaching, and leachate is cadmium sulfate solution, and the Tin concentrate that cadmium is as removed after filtering is washed with water in leached mud；Zincification powder substitution obtains Spongy Cadmium product and displaced liquid after cadmium sulfate solution is purified arsenic removal；Displaced liquid is used to produce basic zinc carbonate.The present invention can make to efficiently separate containing the cadmium in cadmium fumes, form cadmium in tin smelting system and open a way, while can also output Spongy Cadmium product.
Description
Technical field
The invention belongs to noxious fume processing technology fields in hydrometallurgy and Chemical Manufacture, and in particular to containing cadmium fumes
Processing method.
Background technique
In tin smelting process, cadmium was not opened a way, was just constantly recycled in systems, enrichment, to form one kind containing cadmium 5
~15%, it is stanniferous 30~60% contain cadmium fumes.Tin, the cadmium of this flue dust largely exist with oxide form, part cadmium
Exist with oxide morphology.Method is mainly the following to such processing containing cadmium fumes both at home and abroad:
(1) pyrometallurgical smelting: pyrometallurgy of zinc factory can high cadmium zinc of the output containing cadmium 15~30% or 5.6~20.8% or so.
High boiling impurity generally being separated with rectifying column, pure cadmium being made, then adding sodium hydroxide carries out basic refining and obtains 99.995%
Pure cadmium.
(2) wet process: it is chiefly used in handling roasted dust of zinc, the cadmium-containing solution obtained by sulfuric acid leaching flue dust under normal pressure, by net
After eliminating arsenic, iron, goes out Spongy Cadmium with zinc dust precipitation and be subject to the process that pure cadmium is produced in founding refining.Process flow includes cadmium slag
The processes such as leaching, solution purification, displacement, Spongy Cadmium founding and refining.But in the presence of cadmium is with oxide morphology, under normal pressure instead
Answer cadmium leaching rate not high, it is difficult to and other valuable metals efficiently separate.
(3) combination method mentions cadmium: combination method, which mentions cadmium, will contain cadmium fumes by the enrichment of roasting removing impurities, dilute sulfuric acid leaching, oxidation water
After releasing de-iron arsenic, zinc dust precipitation obtain Spongy Cadmium, pressurize agglomerating, caustic soda covered in casting iron pan and casts thick cadmium ingot, essence is added
Refine Refining output cadmium ingot in tower.
Above method, the leaching of cadmium are all to be reacted under normal pressure, and in the presence of cadmium is with oxide morphology, cadmium is difficult to
It leaches.
Summary of the invention
It is an object of the invention to solve above-mentioned the deficiencies in the prior art, provide it is a kind of can make it is effective containing the cadmium in cadmium fumes
Separation, make cadmium tin smelting system formed open a way, while can also output Spongy Cadmium product method of the wet-treating containing cadmium fumes.
The purpose of the present invention is achieved through the following technical solutions:
A kind of method of the wet-treating containing cadmium fumes, processing method are as follows:
(1) cadmium leaches: will contain cadmium fumes with dilute sulfuric acid and carry out oxygen leaching, leachate is cadmium sulfate solution, and leached mud is used
It is the Tin concentrate for removing cadmium after water washing filtering；
(2) solution purification and displacement cadmium: cadmium sulfate solution purifies arsenic removal, and scavenging solution zincification powder substitution obtains Spongy Cadmium production
Product and displaced liquid；
(3) it recycles zinc: displaced liquid being used to produce basic zinc carbonate.
The cadmium fumes of the present invention that contain are that cadmium exists with sulfide and oxide form, tin is with smelting existing for oxide form
Flue dust is refined, flue dust contains cadmium 5~20%, stanniferous 30~60%.
Oxygen leaching described in step (1) of the present invention, dilute sulfuric acid and the liquid-solid ratio containing cadmium fumes are 3~12: 1, initial acid
40~200g/L of concentration, 90~150 DEG C of reaction temperature, the reaction time 2~6 hours, reaction pressure was 1~2MPa, obtained sulphur
Sour cadmium solution 10~50g/L containing cadmium.
Cadmium sulfate solution described in step (2) of the present invention purifies arsenic removal, is the addition mass concentration 50 into cadmium sulfate solution
~80% milk of lime adjusts pH value of solution 5~5.4, removes the arsenic in cadmium sulfate solution, is purified liquid；Weight is added in scavenging solution
The zinc dust precipitation that amount is 0.6~0.8 times of cadmium total amount in solution obtains Spongy Cadmium product and displaced liquid.
Recycling zinc described in step (3) of the present invention is that 2.6~3.0 times of zinc total amount are added in solution into displaced liquid
Bicarbonate ammonia-sinking zinc, produces to obtain basic zinc carbonate.It recycles liquid after the heavy zinc of zinc and returns and leached for cadmium or leached mud is washed
It washs.
The invention has the following advantages:
1, wet-treating of the invention is that in a high pressure reaction kettle, the oxygen leaching carried out using oxygen as oxidant is anti-
It answers, can leach with cadmium existing for oxide morphology, cadmium is entered in solution with cadmium sulfate, and tin enters slag with stannic oxide, is realized effective
Cadmium separation and tin.
2, the present invention will contain after cadmium fumes leach with dilute sulfuric acid, and zincification powder substitution can be obtained the purified arsenic removal of leachate again
Spongy Cadmium product, it is simple for process.
3, containing cadmium fumes after leaching, for cadmium leaching rate up to 95% or more, tin enters slag rate 99.9%, final leached mud (tin
Concentrate) contain cadmium within 1%, realize the open circuit of cadmium in tin smelting system.
4, output Spongy Cadmium product, basic zinc carbonate and leached mud (Tin concentrate) in leaching treatment technique containing cadmium fumes,
Solution realize closed cycle, either wash water still sink zinc after liquid all can return to use, leached mud (Tin concentrate) can return to tin smelting
Refining system, no discharging of waste liquid, energy conservation and environmental protection.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention be suitable for processing cadmium with sulfide and oxide form exist and tin is to smelt cigarette existing for oxide form
Dirt, flue dust contain cadmium 5~20%, stanniferous 30~60%.
Embodiment 1
A kind of method of the wet-treating containing cadmium fumes, as shown in Figure 1, processing method is as follows:
(1) cadmium leaches: will contain cadmium fumes with dilute sulfuric acid and carry out oxygen leaching, dilute sulfuric acid and the liquid-solid ratio containing cadmium fumes are 3
~12: 1,40~200g/L of initial acid, 90~150 DEG C of reaction temperature, the reaction time 2~6 hours, reaction pressure be 1~
2MPa.Obtained leachate is the cadmium sulfate solution of 10~50g/L containing cadmium, and leached mud as removes cadmium after filtering is washed with water
Tin concentrate；
(2) solution purification and displacement cadmium: the milk of lime adjusting that mass concentration 50~80% is added into cadmium sulfate solution is molten
Milk of lime is added into cadmium sulfate solution for liquid pH5~5.4, removes the arsenic in cadmium sulfate solution, is purified liquid；In scavenging solution
The zinc dust precipitation that weight is 0.6~0.8 times of cadmium total amount in solution is added and obtains Spongy Cadmium product and displaced liquid；
(3) it recycles zinc: being the bicarbonate ammonia-sinking zinc for adding 2.6~3.0 times of zinc total amount in solution into displaced liquid, produce
Basic zinc carbonate is obtained, liquid is returned for cadmium leaching or the washing of leached mud after recycling the heavy zinc of zinc.
Embodiment 2
A kind of method of the wet-treating containing cadmium fumes, processing method are as follows:
(1) cadmium 8.9% will be contained, stanniferous 44.1% 500g containing cadmium fumes is leached, leaching condition: sulfuric acid using dilute sulfuric acid
Initial acidity 100g/L, liquid-solid ratio 6:1,90~100 DEG C of reaction temperature, reaction process leads to oxygen, and kettle pressure is 1MPa, reaction time 4
Hour, the cadmium sulfate solution and 362g leached mud of 2.85L 15g/L containing cadmium is obtained, leached mud is contained after filtering is washed with water
The Tin concentrate (Cd residual 0.21%, basic to remove) of Sn60.5%；
(2) milk of lime that mass concentration 80% is added into cadmium sulfate solution adjusts pH value of solution 5.1, by cadmium sulfate solution plus
Milk of lime arsenic removal, the time 1 hour, obtains the cadmium sulfate solution of 2.86L 14.8g/L containing cadmium by 50~60 DEG C of arsenic removal temperature after arsenic removal
That is scavenging solution；
(3) zinc powder that weight is 0.7 times of cadmium total amount in solution is added into scavenging solution to be replaced, in 40~50 DEG C of temperature
Under, it replaces 1 hour, obtains displaced liquid and the Spongy Cadmium containing cadmium 60~80%, Spongy Cadmium obtains cadmium cake through hydraulic press briquetting；
(4) ammonium hydrogen carbonate that weight is 2.8 times of zinc total amount in solution is added into displaced liquid to be precipitated, 40~50
It at a temperature of DEG C, reacts 1 hour, obtains liquid and basic zinc carbonate after heavy zinc.Liquid is returned after heavy zinc washs for leached mud.
Embodiment 3
A kind of method of the wet-treating containing cadmium fumes, processing method are as follows:
(1) cadmium 7%, stanniferous 45% 500g containing cadmium fumes, using dilute sulfuric acid pressure leaching, leaching condition: initially will be contained
Acidity 60g/L, liquid-solid ratio 5:1,120~130 DEG C of reaction temperature, reaction process leads to oxygen, and kettle pressure is 1.2MPa, and the reaction time 4 is small
When, the cadmium sulfate solution and 370g leached mud of 2.36L 13.5g/L containing cadmium is obtained, leached mud is contained after filtering is washed with water
Sn60.5%, the Tin concentrate for remaining Cd 0.38%；
(2) milk of lime that mass concentration 50% is added into cadmium sulfate solution adjusts pH value of solution 5~5.2, temperature 50~60
DEG C, the time 1 hour, the cadmium sulfate solution of 2.35L 10.4g/L containing cadmium is obtained after arsenic removal；
(3) scavenging solution is replaced with the zinc powder that weight is 0.6 times of cadmium total amount in solution, at a temperature of 40~50 DEG C,
Displacement 1 hour, obtains displaced liquid and the Spongy Cadmium containing cadmium 60~80%, Spongy Cadmium obtains cadmium cake through hydraulic press briquetting；
(4) displaced liquid is precipitated with the ammonium hydrogen carbonate that weight is 3.0 times of zinc total amount in solution, in 40~50 DEG C of temperature
It under degree, reacts 1 hour, obtains liquid and basic zinc carbonate after heavy zinc.Liquid, which returns, after heavy zinc is used for pressure leaching.
Embodiment 4
A kind of method of the wet-treating containing cadmium fumes, processing method are as follows:
(1) cadmium 5.01% will be contained, stanniferous 59.89% 500g containing cadmium fumes leaches item using dilute sulfuric acid pressure leaching
Part: initial acidity 40g/L, liquid-solid ratio 12:1,140~150 DEG C of reaction temperature, reaction process leads to oxygen, and kettle pressure is 2MPa, when reaction
Between 2 hours, obtain the cadmium sulfate solution and 364g leached mud of 2.32L 18g/L containing cadmium, leached mud is washed with water to be obtained by filtration contains
Sn60.3%, the Tin concentrate for remaining Cd 0.35%；
(2) into cadmium sulfate solution be added mass concentration 65% milk of lime adjust pH value of solution 5.4,50~60 DEG C of temperature,
Time 1 hour, the cadmium sulfate solution of 2.34L 17.8g/L containing cadmium is obtained after arsenic removal；
(3) scavenging solution is replaced with the zinc powder that weight is 0.8 times of cadmium total amount in solution, at a temperature of 40~50 DEG C,
Displacement 1 hour, obtains displaced liquid and the Spongy Cadmium containing cadmium 60~80%, Spongy Cadmium obtains cadmium cake through hydraulic press briquetting；
(4) displaced liquid is precipitated with the ammonium hydrogen carbonate that weight is 2.6 times of zinc total amount in solution, in 40~50 DEG C of temperature
It under degree, reacts 1 hour, obtains liquid and basic zinc carbonate after heavy zinc.Liquid, which returns, after heavy zinc is used for pressure leaching.
Embodiment 5
A kind of method of the wet-treating containing cadmium fumes, processing method are as follows:
(1) cadmium 19.98% will be contained, stanniferous 30.12% 500g containing cadmium fumes leaches item using dilute sulfuric acid pressure leaching
Part: initial acidity 200g/L, liquid-solid ratio 3:1,130~140 DEG C of reaction temperature, reaction process leads to oxygen, and kettle pressure is 1MPa, when reaction
Between 6 hours, obtain 2.35L 14g/L containing cadmium cadmium sulfate solution and 372g leached mud containing Sn60.2%, Cd 0.5%；
(2) by cadmium sulfate solution in (1) add mass concentration 55% milk of lime adjust pH value of solution 5.3,50~60 DEG C of temperature,
Time 1 hour, the cadmium sulfate solution of 2.36L 48.8g/L containing cadmium is obtained after arsenic removal；
(3) scavenging solution is replaced with the zinc powder that weight is 0.65 times of cadmium total amount in solution, at a temperature of 40~50 DEG C,
Displacement 1 hour, obtains displaced liquid and the Spongy Cadmium containing cadmium 60~80%, Spongy Cadmium obtains cadmium cake through hydraulic press briquetting；
(4) displaced liquid is precipitated with the ammonium hydrogen carbonate that weight is 2.7 times of zinc total amount in solution, in 40~50 DEG C of temperature
It under degree, reacts 1 hour, obtains liquid and basic zinc carbonate after heavy zinc.Liquid is returned for washing leached mud after heavy zinc.
Unless otherwise indicated, each percentage composition numerical value occurred in the present invention is mass percent.
The present invention is to realize the separation of tin cadmium, and containing the method that cadmium fumes use oxygen leaching, cadmium enters liquid with cadmium sulfate, and tin is by oxygen
Chemical conversion stannic oxide enters slag, has efficiently separated containing the cadmium in cadmium fumes, leachate uses zinc dust precipitation solution after except iron arsenic
In cadmium obtain Spongy Cadmium, so that cadmium is opened a way and is recycled from tin smelting system, the Tin concentrate of output returns to tin smelting system.
Claims (6)
1. a kind of method of wet-treating containing cadmium fumes, which is characterized in that processing method is as follows:
(1) cadmium leaches: will contain cadmium fumes with dilute sulfuric acid and carry out oxygen leaching, leachate is cadmium sulfate solution, and leached mud is washed with water
Washing is the Tin concentrate for removing cadmium after filtering；
(2) solution purification and displacement cadmium: cadmium sulfate solution purify arsenic removal, scavenging solution zincification powder substitution i.e. obtain Spongy Cadmium product and
Displaced liquid；
(3) it recycles zinc: displaced liquid being used to produce basic zinc carbonate.
2. method of a kind of wet-treating containing cadmium fumes according to claim 1, which is characterized in that described to be containing cadmium fumes
Cadmium exists with sulfide and oxide form, tin is with smelting smoke dust existing for oxide form, and flue dust is containing cadmium 5~20%, stanniferous
30~60%.
3. method of a kind of wet-treating containing cadmium fumes according to claim 1 or 2, which is characterized in that above-mentioned steps (1)
The oxygen leaching, dilute sulfuric acid and the liquid-solid ratio containing cadmium fumes are 3~12: 1,40~200g/L of initial acid, reaction temperature
90~150 DEG C of degree, the reaction time 2~6 hours, reaction pressure was 1~2MPa, obtained cadmium sulfate solution 10~50g/L containing cadmium.
4. method of a kind of wet-treating containing cadmium fumes according to claim 1 or 2, which is characterized in that above-mentioned steps (2)
The cadmium sulfate solution purifies arsenic removal, is the milk of lime adjusting solution that mass concentration 50~80% is added into cadmium sulfate solution
PH5~5.4 remove the arsenic in cadmium sulfate solution, are purified liquid；It is cadmium total amount 0.6 in solution that weight is added into scavenging solution
~0.8 times of zinc dust precipitation obtains Spongy Cadmium product and displaced liquid.
5. method of a kind of wet-treating containing cadmium fumes according to claim 1 or 2, which is characterized in that above-mentioned steps (3)
The recycling zinc is that 2.6~3.0 times of zinc total amount of ammonium hydrogen carbonate is produced to obtain alkali formula carbon in addition solution into displaced liquid
Sour zinc.
6. method of a kind of wet-treating containing cadmium fumes according to claim 5, which is characterized in that after the heavy zinc for recycling zinc
Liquid is returned for cadmium leaching or the washing of leached mud.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699547A (en) * | 2019-08-23 | 2020-01-17 | 白银有色集团股份有限公司 | Method for recovering zinc and cadmium from waste alkaline residues |
| CN112320994A (en) * | 2020-08-13 | 2021-02-05 | 郴州雄风环保科技有限公司 | Method for treating high-arsenic high-cadmium wastewater |
| CN114134330A (en) * | 2021-12-20 | 2022-03-04 | 昆明冶金研究院有限公司 | Method for recovering cadmium from high-cadmium smoke dust |
| CN114480856A (en) * | 2021-12-15 | 2022-05-13 | 云南驰宏锌锗股份有限公司 | Method for recovering cadmium from high-cadmium smoke dust |
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Application publication date: 20190308 |