CN105925808A - Method for improving grade of by-product sponge cadmium in heptahydrate production - Google Patents
Method for improving grade of by-product sponge cadmium in heptahydrate production Download PDFInfo
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- CN105925808A CN105925808A CN201610271872.0A CN201610271872A CN105925808A CN 105925808 A CN105925808 A CN 105925808A CN 201610271872 A CN201610271872 A CN 201610271872A CN 105925808 A CN105925808 A CN 105925808A
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- filtrate
- cadmium
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- zinc
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Classifications
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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
-
- 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
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for improving the grade of by-product sponge cadmium in heptahydrate production through collected dust soot of pyrometallurgy of lead. The collected dust soot of pyrometallurgy of lead is subject to first-segment neutral leaching, second-segment acid leaching, oxidation iron removing, filtrate impurity removing and purifying filter pressing, and obtained filter residue is the sponge cadmium. Cadmium residue produced through the method can be successfully subject to cake pressing, the appearance of a cadmium cake is beautiful, and the cadmium cake has the metallic luster and is more easily stored and sold.
Description
Technical field
The invention belongs to metallurgical technology field, be specifically related to a kind of flue dust that gathers dust utilizing pyrometallurgical smelting of lead and carry out seven water sulphuric acid
The method improving by-product Spongy Cadmium grade in the production of zinc.
Background technology
At present, lead is smelted based on pyrogenic process, though this technique is more ripe, but production procedure is long, and returning charge is many, needs to consume costliness
Metallurgical coke, containing the element such as zinc, ferrum, stannum, lead, copper, cadmium in the flue dust that gathers dust of pyrometallurgical smelting of lead, directly environment is caused sternly by discharge
Heavily contaminated, and, cause the wasting of resources.The flue dust that gathers dust currently with pyrometallurgical smelting of lead produces the mesh of zinc sulphate heptahydrate cleaning procedure
Be the impurity elements such as Cd, Cu, Pb in order to remove in ZnSO4 solution, ZnSO4 solution that output is refined and side-product sponge
Cadmium, improves the response rate of main metallic zinc the most as far as possible.The principle of purification process is: can with its current potential of replacement ratio more according to metallic zinc
Positive metal ion so that it is changing into metallic state and separate out from solution, zinc then becomes Zn2+ and enters the principle of solution, reaches
The purpose of purification and impurity removal, owing to handled solution is ZnSO4 solution, does not results in new pollution.
At impurity element present in cleaning procedure in addition to Cd, Cu, Pb that content is higher, also moiety content is relatively
Metallic element low, that electromotive force is higher than cadmium, such as Sn etc., together can precipitate with Cd, after causing purification filter pressing when with zinc dust precipitation
Cadmium slag is dilute, and the cadmium cake of compacting is shapeless, thus affects sale and the price of side-product Spongy Cadmium.
Summary of the invention
It is an object of the invention to provide during a kind of zinc sulphate heptahydrate produces the method improving by-product Spongy Cadmium grade, output
Cadmium slag can success cake of press, cadmium cake outward appearance is beautiful, have metallic luster and easily stored sale.
The present invention is attained in that zinc sulphate heptahydrate improves by-product Spongy Cadmium product in producing by the following technical solutions
The method of position, comprises the following steps:
A. one section of neutral leaching
The flue dust that gathers dust of pyrometallurgical smelting of lead is dissolved in water, and adding sulfur acid for adjusting pH value is 4.0-5.0, and temperature is 60-65 DEG C, stirs 20-
40min, separates filtering residue and filtrate；
B. two-stage nitration acidic leaching
Adding sulphuric acid in step a gained filtering residue, regulation pH value is 2.0-3.0, stirs 20-40min, and temperature is 50-60 DEG C of time-division
From filtering residue and filtrate；
C. iron removal by oxidation
Step a merges with gained filtrate in step b, adjusts the temperature to 55-60 DEG C, iron content in detection filtrate, is subsequently adding double
Oxygen water, ferrum is 1:(1.2-1.3 with the mol ratio of hydrogen peroxide), regulation pH value is 3.7-4.0, stirring reaction；Continue interpolation to gather dust
The potassium permanganate of flue dust gross mass 0.5%-0.6%, solution is warming up to 75-85 DEG C, and stirring 20-40min, adjustment pH are 5.0-
6.0, carry out filter pressing when temperature is 60-65 DEG C；
D. filtrate remove impurity
Step c gained filtrate adjusts temperature and is 75-85 DEG C, and regulation pH value is 3.0-5.0, adds flue dust gross mass 2.5-of gathering dust
The zinc powder of 2.7%, separates filtering residue and filtrate；
E. purify
Step d gained filtrate purifies, and adding sulfur acid for adjusting pH value is 3.0-3.5, and temperature is 55-60 DEG C, cadmium in detection filtrate
Content, adds zinc powder, and cadmium is 1:(0.9-1 with the mol ratio of zinc powder), stir 20-30min, detection cadmium content is less than 0.02%
Time, filter pressing, gained filtering residue is Spongy Cadmium.
Filtrate in step b returns step a and carries out secondary neutrality leaching.
Step d gained filtrate adjusts temperature and is 45-50 DEG C, pH value 3.0-3.5, cadmium content in detection filtrate, adds zinc powder
Being (4-5) with the mol ratio of cadmium: 1, stir 20-30min, carry out filter pressing when detection cadmium content is less than 0.002%, filtrate is sulfur
Acid zinc solution.
It is 1.58-1.63 that the concentrated still of solution of zinc sulfate is concentrated into proportion, and then adding acid for adjusting pH value is 4.5 to cool down
Crystallization, goes out liquid with 30 DEG C and enters drier solid-liquid separation.
Zinc powder particle diameter is 325 mesh.
The present invention using technique scheme adjusts temperature in purification and impurity removal step and is 75-85 DEG C, and regulation pH value is
3.0-5.0, adds the zinc powder of flue dust gross mass 2.5-2.7% of gathering dust, and separates filtering residue and filtrate, first content is relatively low, electric
The metallic element Sn that gesture is higher than cadmium removes, it is to avoid when with zinc dust precipitation, Sn together can precipitate with Cd, uses disclosed by the invention
The cadmium slag of method output can success cake of press, cadmium cake outward appearance is beautiful to be had metallic luster and is easier to deposit outer selling.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
As it is shown in figure 1, zinc sulphate heptahydrate improves by-product Spongy Cadmium grade method in producing, comprise the following steps:
A. one section of neutral leaching
The flue dust that gathers dust of pyrometallurgical smelting of lead is dissolved in water, opens blender, add when flue dust proportion reaches 1.45-1.5 and slowly add sulfur
Acid for adjusting pH value is 4.0-5.0, and temperature is 60-65 DEG C, stirs 20-40min, and temperature is down to 60 DEG C, adds the ferrum that detection obtains
The mol ratio of the hydrogen peroxide of content 50%, i.e. ferrum and hydrogen peroxide is 2:1, once except ferrum, stirring reaction 30min, separate filtering residue and
Filtrate；
B. two-stage nitration acidic leaching
Adding sulphuric acid in step a gained filtering residue, regulation pH value is 2.0-3.0, stirs 20-40min, and temperature is 50-60 DEG C of time-division
From filtering residue and filtrate, filtrate returns step a and carries out secondary neutrality leaching；
C. iron removal by oxidation
Step a gained filtrate adjusts the temperature to 55-60 DEG C, opens blower fan and blender, and regulation pH value is 3.7-4.0, then delays
The slow hydrogen peroxide adding excess, iron content in detection filtrate, ferrum is 1:(1.2-1.3 with the mol ratio of hydrogen peroxide), it is added to ferrum and removes
Till Gan Jing, stirring reaction；Continuing to add the potassium permanganate of flue dust gross mass 0.5%-0.6% of gathering dust, solution is warming up to 75-85
DEG C, stirring 20-40min, adjustment pH are 5.0-6.0, carry out filter pressing when temperature is 60-65 DEG C；
D. filtrate remove impurity
Step c gained filtrate adjusts temperature and is 75-85 DEG C, and regulation pH value is 3.0-5.0, according to the data of chemical examination detection, adds
The zinc powder of 325 mesh of flue dust gross mass 2.5-2.7% of gathering dust, separates filtering residue and filtrate；
E. purify
Step d gained filtrate purifies, and adding sulfur acid for adjusting pH value is 3.0-3.5, and temperature is 55-60 DEG C, cadmium in detection filtrate
Content, adds the zinc powder of 325 mesh, and cadmium is 1:(0.9-1 with the mol ratio of zinc powder), stir 20-30min, detection cadmium content is less than
When 0.02%, filter pressing, gained filtering residue is Spongy Cadmium.
Step d gained filtrate adjusts temperature and is 45-50 DEG C, pH value 3.0-3.5, cadmium content in detection filtrate, adds zinc powder
Being (4-5) with the mol ratio of cadmium: 1, stir 20-30min, carry out filter pressing when detection cadmium content is less than 0.002%, filtrate is sulfur
Acid zinc solution.
It is 1.58-1.63 that the concentrated still of solution of zinc sulfate is concentrated into proportion, and then adding acid for adjusting pH value is 4.5 to cool down
Crystallization, goes out liquid with 30 DEG C and enters drier solid-liquid separation, through pulverizing, drying, outer after metering packing sells.
Embodiment 1
Zinc sulphate heptahydrate improves the method for by-product Spongy Cadmium grade in producing, comprise the following steps:
A. one section of neutral leaching
The flue dust that gathers dust of pyrometallurgical smelting of lead is dissolved in water, opens blender, add and when flue dust proportion reaches 1.45, slowly add sulphuric acid tune
Joint pH value is 4.0, and temperature is 60 DEG C, stirs 20min, and temperature is down to 60 DEG C, adds the dioxygen of the iron content 50% that detection obtains
Water, i.e. ferrum are 2:1 with the mol ratio of hydrogen peroxide, once except ferrum, and stirring reaction 30min, separate filtering residue and filtrate；
B. two-stage nitration acidic leaching
Adding sulphuric acid in step a gained filtering residue, regulation pH value is 2.0, stirs 20min, separates filtering residue and filter when temperature is 50 DEG C
Liquid, filtrate returns step a and carries out secondary neutrality leaching；
C. iron removal by oxidation
Step a gained filtrate adjusts the temperature to 55 DEG C, opens blower fan and blender, and regulation pH value is 3.7, is then slowly added into
The hydrogen peroxide of excess, iron content in detection filtrate, the mol ratio of ferrum and hydrogen peroxide is 1:1.2, is added to ferrum except till clean, stirring
Reaction；Continuing to add the potassium permanganate of flue dust gross mass 0.5% of gathering dust, solution is warming up to 75 DEG C, stirs 20min, adjusts pH and is
5.0, carry out filter pressing when temperature is 60 DEG C；
D. filtrate remove impurity
It is 75 DEG C that step c gained filtrate adjusts temperature, and regulation pH value is 3.0, according to the data of chemical examination detection, adds the flue dust that gathers dust
The zinc powder of 325 mesh of gross mass 2.5%, separates filtering residue and filtrate；
E. purify
Step d gained filtrate purifies, and adding sulfur acid for adjusting pH value is 3.0, and temperature is 55 DEG C, cadmium content in detection filtrate, adds
Entering the zinc powder of 325 mesh, cadmium is 1:0.9 with the mol ratio of zinc powder, stirs 20min, when detection cadmium content is less than 0.02%, and filter pressing,
Gained filtering residue is Spongy Cadmium.
Embodiment 2
Zinc sulphate heptahydrate improves the method for by-product Spongy Cadmium grade in producing, comprise the following steps:
A. one section of neutral leaching
The flue dust that gathers dust of pyrometallurgical smelting of lead is dissolved in water, opens blender, add and when flue dust proportion reaches 1.5, slowly add sulphuric acid regulation
PH value is 5.0, and temperature is 65 DEG C, stirs 40min, and temperature is down to 60 DEG C, adds the hydrogen peroxide of the iron content 50% that detection obtains,
I.e. ferrum is 2:1 with the mol ratio of hydrogen peroxide, once except ferrum, and stirring reaction 30min, separate filtering residue and filtrate；
B. two-stage nitration acidic leaching
Adding sulphuric acid in step a gained filtering residue, regulation pH value is 3.0, stirs 40min, separates filtering residue and filter when temperature is 60 DEG C
Liquid, filtrate returns step a and carries out secondary neutrality leaching；
C. iron removal by oxidation
Step a gained filtrate adjusts the temperature to 60 DEG C, opens blower fan and blender, and regulation pH value is 4.0, is then slowly added into
The hydrogen peroxide of amount, iron content in detection filtrate, the mol ratio of ferrum and hydrogen peroxide is 1:1.3, is added to ferrum except till clean, stirring is anti-
Should；Continuing to add the potassium permanganate of flue dust gross mass 0.6% of gathering dust, solution is warming up to 85 DEG C, stirs 40min, adjusts pH and is
6.0, carry out filter pressing when temperature is 65 DEG C；
D. filtrate remove impurity
It is 85 DEG C that step c gained filtrate adjusts temperature, and regulation pH value is 5.0, according to the data of chemical examination detection, adds the flue dust that gathers dust
The zinc powder of 325 mesh of gross mass 2.7%, separates filtering residue and filtrate；
E. purify
Step d gained filtrate purifies, and adding sulfur acid for adjusting pH value is 3.5, and temperature is 60 DEG C, cadmium content in detection filtrate, adds
Entering the zinc powder of 325 mesh, cadmium is 1:1 with the mol ratio of zinc powder, stirs 30min, when detection cadmium content is less than 0.02%, and filter pressing, institute
Obtain filtering residue and be Spongy Cadmium.
Embodiment 3-embodiment 11
Embodiment 3-11 is shown in Table 1 with the difference of embodiment 1, and remaining reaction condition is same as in Example 1.
Table 1
Claims (5)
1. the method improving by-product Spongy Cadmium grade during zinc sulphate heptahydrate produces, it is characterised in that comprise the following steps:
A. one section of neutral leaching
The flue dust that gathers dust of pyrometallurgical smelting of lead is dissolved in water, and adding sulfur acid for adjusting pH value is 4.0-5.0, and temperature is 60-65 DEG C, stirs 20-
40min, separates filtering residue and filtrate；
B. two-stage nitration acidic leaching
Adding sulphuric acid in step a gained filtering residue, regulation pH value is 2.0-3.0, stirs 20-40min, and temperature is 50-60 DEG C of time-division
From filtering residue and filtrate；
C. iron removal by oxidation
Step a merges with step b gained filtrate, adjusts the temperature to 55-60 DEG C, iron content in detection filtrate, is subsequently adding dioxygen
Water, ferrum is 1:(1.2-1.3 with the mol ratio of hydrogen peroxide), regulation pH value is 3.7-4.0, stirring reaction；Continue interpolation to gather dust cigarette
The potassium permanganate of ash gross mass 0.5%-0.6%, solution is warming up to 75-85 DEG C, and stirring 20-40min, adjustment pH are 5.0-6.0, temperature
Filter pressing is carried out when degree is for 60-65 DEG C；
D. filtrate remove impurity
Step c gained filtrate adjusts temperature and is 75-85 DEG C, and regulation pH value is 3.0-5.0, adds flue dust gross mass 2.5-of gathering dust
The zinc powder of 2.7%, separates filtering residue and filtrate；
E. purify
Step d gained filtrate purifies, and adding sulfur acid for adjusting pH value is 3.0-3.5, and temperature is 55-60 DEG C, cadmium in detection filtrate
Content, adds zinc powder, and cadmium is 1:(0.9-1 with the mol ratio of zinc powder), stir 20-30min, when detection cadmium content is less than 0.02%,
Filter pressing, gained filtering residue is Spongy Cadmium.
The method improving by-product Spongy Cadmium grade during the most according to claim 1, zinc sulphate heptahydrate produces, it is characterised in that:
Filtrate in step b returns step a and carries out secondary neutrality leaching.
The method improving by-product Spongy Cadmium grade during the most according to claim 1, zinc sulphate heptahydrate produces, it is characterised in that:
Step d gained filtrate adjusts temperature and is 45-50 DEG C, pH value 3.0-3.5, cadmium content in detection filtrate, and addition zinc powder rubs with cadmium
Your ratio is (4-5): 1, stirs 20-30min, carries out filter pressing when detection cadmium content is less than 0.002%, and filtrate is solution of zinc sulfate.
The method improving by-product Spongy Cadmium grade during the most according to claim 3, zinc sulphate heptahydrate produces, it is characterised in that:
It is 1.58-1.63 that the concentrated still of solution of zinc sulfate is concentrated into proportion, and then adding acid for adjusting pH value is 4.5 to carry out crystallisation by cooling, with
30 DEG C go out liquid and enter drier solid-liquid separation.
The method improving by-product Spongy Cadmium grade during the most according to claim 1, zinc sulphate heptahydrate produces, it is characterised in that:
Zinc powder particle diameter is 325 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610271872.0A CN105925808A (en) | 2016-04-28 | 2016-04-28 | Method for improving grade of by-product sponge cadmium in heptahydrate production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610271872.0A CN105925808A (en) | 2016-04-28 | 2016-04-28 | Method for improving grade of by-product sponge cadmium in heptahydrate production |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709382A (en) * | 2009-12-17 | 2010-05-19 | 新乡超能电源有限公司 | Recovery and comprehensive treatment process of valuable metals in zinciferous materials |
| CN102517455A (en) * | 2011-12-29 | 2012-06-27 | 株洲冶炼集团股份有限公司 | Method for recovering cadmium from copper cadmium residues |
| CN102851509A (en) * | 2012-08-15 | 2013-01-02 | 湖南水口山有色金属集团有限公司 | Method for recovering cadmium from flue dust of bottom-blowing furnace |
| CN104451157A (en) * | 2014-11-25 | 2015-03-25 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method for lead smelting high-cadmium ash and zinc electrolysis wastewater |
-
2016
- 2016-04-28 CN CN201610271872.0A patent/CN105925808A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709382A (en) * | 2009-12-17 | 2010-05-19 | 新乡超能电源有限公司 | Recovery and comprehensive treatment process of valuable metals in zinciferous materials |
| CN102517455A (en) * | 2011-12-29 | 2012-06-27 | 株洲冶炼集团股份有限公司 | Method for recovering cadmium from copper cadmium residues |
| CN102851509A (en) * | 2012-08-15 | 2013-01-02 | 湖南水口山有色金属集团有限公司 | Method for recovering cadmium from flue dust of bottom-blowing furnace |
| CN104451157A (en) * | 2014-11-25 | 2015-03-25 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method for lead smelting high-cadmium ash and zinc electrolysis wastewater |
Non-Patent Citations (1)
| Title |
|---|
| 李冬云: "韶冶电尘提镉工艺和设备的改进研究", 《中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑》 * |
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Application publication date: 20160907 |