CN104451157A - Comprehensive recovery method for lead smelting high-cadmium ash and zinc electrolysis wastewater - Google Patents
Comprehensive recovery method for lead smelting high-cadmium ash and zinc electrolysis wastewater Download PDFInfo
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- CN104451157A CN104451157A CN201410685559.2A CN201410685559A CN104451157A CN 104451157 A CN104451157 A CN 104451157A CN 201410685559 A CN201410685559 A CN 201410685559A CN 104451157 A CN104451157 A CN 104451157A
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- leaching
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- zinc electrolysis
- cadmium
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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
Abstract
The invention discloses a comprehensive recovery method for lead smelting high-cadmium ash and zinc electrolysis wastewater. The method comprises the following steps: washing with alkali, leaching, flocculating to remove arsenic, displacing, briquetting, casting and distilling, wherein the alkali washing step is ultrasonically carried out, and the used alkali is a mixture of sodium hydroxide, pure alkali or potassium hydroxide and pure alkali; the leaching step comprises two-stage leaching substeps, and a used leaching agent is the zinc electrolysis wastewater or mixed liquid of the zinc electrolysis wastewater and two-stage leaching liquid; in the flocculating arsenic removal step, a flocculating agent-ferrous sulfate heptahydrate and an oxidant-hydrogen peroxide are added for removing arsenic in the leaching liquid when the first-stage leaching process is to be finished. The method is high in comprehensive utilization rate, relatively low in recovery cost and high in cadmium and zinc recovery rate.
Description
Technical field
The present invention relates to a kind of method of refuse hydrometallurgy, particularly a kind of comprehensive recovering process refining plumbous high cadmium cigarette ash and zinc electrolysis waste water.
Background technology
In plumbous smelting process, lead ore concentrate is through melting operation, and the flue dust of output to gather dust the cigarette ash collected through electricity, when lower containing cadmium in cigarette ash, returns to feed circuit batching; When cadmium content in cigarette ash is more than 8%, cigarette ash is opened a way out lead system, and cigarette ash is now called the plumbous high cadmium cigarette ash of refining.Refine usually containing valuable metals such as lead, cadmium and zinc in plumbous high cadmium cigarette ash, simultaneously also containing harmful element F, Cl.
The processing mode of the plumbous high cadmium cigarette ash of current refining has: (1) stores up, and what this was serious pollutes environment, and causes the huge wasting of resources and financial loss.(2) refine plumbous high cadmium cigarette ash diluted acid leaching together with rotary kiln flue dust, it is plumbous that acid leaching residue send lead system to reclaim, and pickling liquor is incorporated to the calcining leach liquor of zinc abstraction system, adopts common process to reclaim cadmium, output cadmium ingot in zinc abstraction system; Although this method has reclaimed valuable metal lead, cadmium and zinc in the plumbous high cadmium cigarette ash of refining, the rate of recovery of zinc cadmium is not high, and harmful element F, Cl major part enters Zn system, adds the cost of de-F, Cl in zinc production process.(3) refine plumbous high cadmium cigarette ash and sulfurization roasting can make cadmium in addition enrichment through melting, the intermediates sulfur compound simultaneously obtained is little, and directly use sulfuric acid leaching, the rate of recovery of cadmium is higher.But this method belongs to pyrogenic process process, environmental pollution is comparatively large, and zinc is not recycled simultaneously.
In zinc metallurgical process, need carry out weak acid immersion and cleaning to the cathode plate surface foreign material of Zinc electrolysis, the water produced after cleaning negative plate is called zinc electrolysis waste water.General in zinc electrolysis waste water is 10 ~ 30g/L containing zinc, and sulfur acid is 10 ~ 20g/L.The processing mode of current zinc electrolysis waste water has: (1), according to Zn system volumetric balance, a part returns Zn system, and supplement the partial water loss in zinc metallurgical process, another part is incorporated to Sewage treatment systems.This method increases zinc abstraction factory externally discharged waste water amount, increases cost of sewage disposal, wastes resource simultaneously.(2) first to use in alkali and acid in zinc electrolysis waste water, then reclaim zinc wherein with extraction process.Though this method has reclaimed the zinc in zinc electrolysis waste water, the rate of recovery of zinc is lower, and acid is not utilized.
Therefore, prior art can not adapt to the valuable metal such as comprehensive recovery of lead, cadmium and zinc from the plumbous high cadmium cigarette ash of refining and zinc electrolysis waste water, and utilize the acid in zinc electrolysis waste water, the how valuable metal such as plumbous, the cadmium of high efficiente callback and zinc to make full use of acid in waste water, effectively reduce production cost be again the difficult problem needing to be explored further from waste and waste water.
Summary of the invention
The object of the present invention is to provide a kind of comprehensive recovering process refining plumbous high cadmium cigarette ash and zinc electrolysis waste water, it can in alkali cleaning under Ultrasonic Conditions, remove F, Cl of in the plumbous high cadmium cigarette ash of refining more than 96%, make the acid in zinc electrolysis waste water make full use of in refining plumbous high cadmium cigarette ash leaching, zinc recovery reaches 98%, and the cadmium rate of recovery is more than 85%.
Technical scheme of the present invention is:
Refine the comprehensive recovering process of plumbous high cadmium cigarette ash and zinc electrolysis waste water: comprise the steps such as alkali cleaning, leaching, flocculation dearsenification, displacement, pressure group, casting mold, distillation, it is characterized in that:
A. described caustic scrubbing step carries out alkali cleaning to the plumbous high cadmium cigarette ash of refining under hyperacoustic condition, the mixture that the alkali that alkali cleaning uses is sodium hydroxide+soda ash or potassium hydroxide+soda ash;
B. described leaching step leaches alkali cleaning slag, is divided into one section to leach and two sections of leaching steps, the mixed solution that the leaching agent of use is zinc electrolysis waste water or zinc electrolysis waste water+two sections of leach liquors;
C. described flocculation dearsenification step is when leaching close to terminal for one section, adds flocculation agent iron vitriol and oxidant hydrogen peroxide and removes arsenic in one section of leach liquor.
Preferably, described caustic scrubbing step is that alkali cleaning temperature can be carried out under 0 ~ 100 DEG C of condition, but preferred alkali cleaning temperature is 60 ~ 85 DEG C, carry out under Ultrasonic Conditions in alkaline cleaning procedure, and according to the suitable preferably ultrasonic intensity of the kind of raw material, production efficiency is the preferred single factor of ultrasonic intensity.
Preferably, described one section of extraction temperature leached is 65 ~ 90 DEG C, and leaching agent is the mixed solution of zinc electrolysis waste water and two sections of leach liquors, and leaching terminal pH is 3 ~ 4.
Preferably, described two sections of leaching agents leached are zinc electrolysis waste water, and temperature is 80 ~ 95 DEG C, and extraction time is 2 ~ 4h, and leaching terminal point control pH is 0.5 ~ 1.
Preferably, described flocculation dearsenification step is when leaching close to terminal for one section, adds 5 ~ 10g iron vitriol, and slowly add hydrogen peroxide by often liter of leach liquor.
Further, smelt through lead the lead reclaimed wherein after the leached mud washing of described two sections of leaching step gained, displaced liquid reclaims zinc wherein through zinc abstraction.
Beneficial effect of the present invention is as follows:
Plumbous for refining high cadmium cigarette ash is first carried out alkali cleaning existing under hyperacoustic condition by the present invention, make the decreasing ratio of F, Cl in the plumbous high cadmium cigarette ash of refining more than 96%, ensure that and use zinc electrolysis waste water to leach the content of F, Cl content in the leach liquor of the plumbous high cadmium cigarette ash of refining lower than F, Cl in zinc electrolyte, thus reduce the cost recovery that cadmium displaced liquid returns zinc in Zn system.
Alkali cleaning slag is leached and flocculation dearsenification through two suboptimization, ensure that the cadmium rate of recovery in the plumbous high cadmium cigarette ash of refining reaches 85%, reduce the content of impurity in alkali cleaning slag leach liquor, improve the grade of cadmium in thick cadmium.
Use zinc electrolysis waste water to leach alkali cleaning slag, take full advantage of the acid in zinc electrolysis waste water and reclaimed the zinc in zinc electrolysis waste water and the plumbous high cadmium cigarette ash of refining, the rate of recovery of zinc reaches 98%.
The leached mud of alkali cleaning slag returns Zn system, and the lead refined in plumbous high cadmium cigarette ash obtains recovery.Thus the lead, cadmium and the zinc that reach in the synthetical recovery plumbous high cadmium cigarette ash of refining and zinc electrolysis waste water, and successfully make use of the acid in zinc electrolysis waste water, reduce production cost.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
The invention provides by the alkali cleaning to the plumbous high cadmium cigarette ash of refining, the step such as leaching, flocculation dearsenification, displacement, pressure group, casting mold, distillation of alkali cleaning slag and zinc electrolysis waste water, is separated and reclaims the valuable metals such as lead, cadmium and zinc respectively, and make full use of the method for sulfuric acid.
In the alkaline cleaning procedure of the plumbous high cadmium cigarette ash of refining, the mass percent of material and ultrasonic intensity in the sodium hydroxide+soda ash of alkali cleaning liquid-solid ratio, alkali cleaning time, alkali cleaning or the mixture of potassium hydroxide+soda ash, to improve the efficiency of de-F, Cl and to reduce premised on production cost.
In the leaching process of the plumbous high cadmium cigarette ash of refining, leach liquid-solid ratio, make the volume ratio of the mixed solution of zinc electrolysis waste water+two sections of leach liquors that leaching agent uses, premised on the rate of recovery reducing production cost and raising zinc and cadmium.
In flocculation dearsenification step, in order to improve the quality of one section of leach liquor, i.e. lead impurity element, arsenic equal size in the thick cadmium of intermediates, can use usually known adding material, and the adding premised on the leaching yield of the quality not reducing by one section of leach liquor and zinc cadmium of adding material.
Embodiment 1:
With the method process plumbous high cadmium cigarette ash of refining of the present invention and zinc electrolysis waste water, refine the mass percentage content of the main component of plumbous high cadmium cigarette ash for (%): Pb:53.96, Zn:13.25, Cd:10.64, the mass concentration of the main component of zinc electrolysis waste water is respectively (g/L): H
2sO
4: 18.27, Zn:13.42, treatment step is:
Add water on request, the mixture of potassium hydroxide+soda ash prepares alkaline wash, after being warmed up to 60 DEG C, under stirring more sufficient situation, add the plumbous high cadmium cigarette ash of refining, and open ultrasonic wave, ultrasonic frequency is 20HZ, after alkali cleaning terminates, and the terminal pH=9 of solution, the alkali cleaning time is 60 minutes, alkali cleaning liquid-solid ratio=8, measure and the decreasing ratio that the decreasing ratio calculating F is 96.37%, Cl is 98.13%.
With the mixed solution of zinc electrolysis waste water+two sections of leach liquors for leaching agent, carry out one section of leaching to alkali cleaning slag, extraction temperature is 65 DEG C, and the pH leaching terminal is 3.Leach terminal, in one section of leach liquor, add 5g iron vitriol by often liter of leach liquor, and slowly add hydrogen peroxide.Flocculation is after dearsenification completes, and the mass concentration of the impurity such as plumbous in dearsenification liquid, iron and arsenic is less than 0.01g/L.
With zinc electrolysis waste water for leaching agent, carry out two sections of leachings to one section of leached mud, extraction temperature is 80 DEG C, and extraction time is 2h, and the pH leaching terminal is 0.5.
By the method process, the leaching yield of zinc and cadmium reaches 98.36% and 90.18% respectively, and the plumbous mass percentage content in two sections of leached muds is 63.27%, is more conducive to plumbous recovery of smelting.
Embodiment 2:
With the method process plumbous high cadmium cigarette ash of refining of the present invention and zinc electrolysis waste water, refine the mass percentage content of the main component of plumbous high cadmium cigarette ash for (%): Pb:48.61, Zn:15.54, Cd:9.49, the mass concentration of the main component of zinc electrolysis waste water is respectively (g/L): H
2sO
4: 15.62, Zn:25.11, treatment step is:
Add water on request, the mixture of potassium hydroxide+soda ash prepares alkaline wash, after being warmed up to 70 DEG C, under stirring more sufficient situation, add the plumbous high cadmium cigarette ash of refining, and open ultrasonic wave, ultrasonic frequency is 30HZ, after alkali cleaning terminates, the terminal pH=10 of solution, the alkali cleaning time is 90 minutes, and alkali cleaning liquid-solid ratio=6, after alkali cleaning terminates, to measure and the decreasing ratio that the decreasing ratio calculating F is 96.85%, Cl is 98.74%.
With the mixed solution of zinc electrolysis waste water+two sections of leach liquors for leaching agent, carry out one section of leaching to alkali cleaning slag, extraction temperature is 75 DEG C, and the pH leaching terminal is 3.5.Leach terminal, in one section of leach liquor, add 8g iron vitriol by often liter of leach liquor, and slowly add hydrogen peroxide.Flocculation is after dearsenification completes, and the mass concentration of the impurity such as plumbous in dearsenification liquid, iron and arsenic is less than 0.01g/L.
With zinc electrolysis waste water for leaching agent, carry out two sections of leachings to one section of leached mud, extraction temperature is 90 DEG C, and extraction time is 3h, and the pH leaching terminal is 0.8.
By the method process, the leaching yield of zinc and cadmium reaches 98.80% and 89.84% respectively, and the plumbous mass percentage content in two sections of leached muds is 60.25%, is more conducive to plumbous recovery of smelting.
Embodiment 3:
With the method process plumbous high cadmium cigarette ash of refining of the present invention and zinc electrolysis waste water, refine the mass percentage content of the main component of plumbous high cadmium cigarette ash for (%): Pb:51.17, Zn:15.38, Cd:10.81, the mass concentration of the main component of zinc electrolysis waste water is respectively (g/L): H
2sO
4: 14.55, Zn:28.24, treatment step is:
Add water on request, the mixture of potassium hydroxide+soda ash prepares alkaline wash, after being warmed up to 85 DEG C, under stirring more sufficient situation, add the plumbous high cadmium cigarette ash of refining, and open ultrasonic wave, ultrasonic frequency is 50HZ, after alkali cleaning terminates, the terminal pH=11 of solution, the alkali cleaning time is 120 minutes, and alkali cleaning liquid-solid ratio=3, after alkali cleaning terminates, to measure and the decreasing ratio that the decreasing ratio calculating F is 97.06%, Cl is 98.35%.
With the mixed solution of zinc electrolysis waste water+two sections of leach liquors for leaching agent, carry out one section of leaching to alkali cleaning slag, extraction temperature is 90 DEG C, and the pH leaching terminal is 4.Leach terminal, in one section of leach liquor, add 10g iron vitriol by often liter of leach liquor, and slowly add hydrogen peroxide.Flocculation is after dearsenification completes, and the mass concentration of the impurity such as plumbous in dearsenification liquid, iron and arsenic is less than 0.01g/L.
With zinc electrolysis waste water for leaching agent, carry out two sections of leachings to one section of leached mud, extraction temperature is 95 DEG C, and extraction time is 4h, and the pH leaching terminal is 1.
By the method process, the leaching yield of zinc and cadmium reaches 98.36% and 88.60% respectively, and the plumbous mass percentage content in two sections of leached muds is 64.08%, is more conducive to plumbous recovery of smelting.
The valuable material of the present invention in the synthetical recovery plumbous high cadmium cigarette ash of refining and zinc electrolysis waste water, simply and efficiently can remove F, the Cl in the plumbous high cadmium cigarette ash of refining, and be separated and reclaim lead, cadmium and zinc efficiently, make full use of the acid in zinc electrolysis waste water simultaneously, in environmental protection and resource reutilization, industrial application has remarkable advantage.
The present invention, including but not limited to above-mentioned embodiment, as long as have employed the processing method that alkali cleaning under Ultrasonic Conditions takes off F, Cl and one section of leaching rear flocculation dearsenification step, namely belongs to protection scope of the present invention.
Claims (6)
1. refine a comprehensive recovering process for plumbous high cadmium cigarette ash and zinc electrolysis waste water, comprise the steps such as alkali cleaning, leaching, flocculation dearsenification, displacement, pressure group, casting mold, distillation, it is characterized in that:
A. described caustic scrubbing step carries out alkali cleaning to the plumbous high cadmium cigarette ash of refining under hyperacoustic condition, the mixture that the alkali that alkali cleaning uses is sodium hydroxide+soda ash or potassium hydroxide+soda ash;
B. described leaching step leaches alkali cleaning slag, is divided into one section to leach and two sections of leachings, the mixed solution that the leaching agent of use is zinc electrolysis waste water or zinc electrolysis waste water+two sections of leach liquors;
C. described flocculation dearsenification step is when leaching close to terminal for one section, adds flocculation agent iron vitriol and oxidant hydrogen peroxide and removes arsenic in one section of leach liquor.
2. a kind of comprehensive recovering process refining plumbous high cadmium cigarette ash and zinc electrolysis waste water according to claim 1, it is characterized in that: the caustic scrubbing step of the plumbous high cadmium cigarette ash of described refining is that alkali cleaning temperature is carried out under the condition of 0 ~ 100 DEG C, but preferred alkali cleaning temperature is 60 ~ 85 DEG C, carries out in alkaline cleaning procedure under Ultrasonic Conditions.
3. a kind of comprehensive recovering process refining plumbous high cadmium cigarette ash and zinc electrolysis waste water according to claim 1, it is characterized in that: described one section of extraction temperature leached is 65 ~ 90 DEG C, leaching agent is the mixed solution of zinc electrolysis waste water and two sections of leach liquors, and leaching terminal pH is 3 ~ 4.
4. a kind of comprehensive recovering process refining plumbous high cadmium cigarette ash and zinc electrolysis waste water according to claim 1, it is characterized in that: described two sections of leaching agents leached are zinc electrolysis waste water, temperature is 80 ~ 95 DEG C, and extraction time is 2 ~ 4h, and leaching terminal point control pH is 0.5 ~ 1.
5. a kind of comprehensive recovering process refining plumbous high cadmium cigarette ash and zinc electrolysis waste water according to claim 1, it is characterized in that: described flocculation dearsenification step is carried out close to during terminal one section of leaching, add 5 ~ 10g iron vitriol by often liter of leach liquor, and slowly add hydrogen peroxide.
6. a kind of comprehensive recovering process refining plumbous high cadmium cigarette ash and zinc electrolysis waste water according to claim 1, it is characterized in that: smelt through lead the lead reclaimed wherein after the leached mud washing of described two sections of leaching step gained, displaced liquid reclaims zinc wherein through zinc abstraction.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105925808A (en) * | 2016-04-28 | 2016-09-07 | 河南金利金铅集团有限公司 | Method for improving grade of by-product sponge cadmium in heptahydrate production |
| JP2019512606A (en) * | 2016-03-24 | 2019-05-16 | イー．ヴイ．エイチ． エス．アール．エル． | Method of processing used cathode ray tube |
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Application publication date: 20150325 |