CN106381400A - Efficient enrichment recovery method and system for lead and silver in lead smelting waste - Google Patents
Efficient enrichment recovery method and system for lead and silver in lead smelting waste Download PDFInfo
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- CN106381400A CN106381400A CN201610973648.6A CN201610973648A CN106381400A CN 106381400 A CN106381400 A CN 106381400A CN 201610973648 A CN201610973648 A CN 201610973648A CN 106381400 A CN106381400 A CN 106381400A
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- lead
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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
- C22B7/04—Working-up slag
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
- C22B7/008—Wet processes by an alkaline or ammoniacal 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 an efficient enrichment recovery method and system for lead and silver in lead smelting waste. The method includes the steps that (1) pretreatment is carried out, wherein the lead smelting waste is cooled to 0 DEG C to 5 DEG C, and then the temperature rises to 500 DEG C to 600 DEG C with the speed being 10 DEG C/min; (2) alkaline leaching is carried out, wherein the lead smelting waste and a sodium hydroxide solution are mixed while the lead smelting waste is hot, and alkaline leaching liquid and alkaline leaching slag are obtained; (3) the alkaline leaching liquid is subject to lead precipitating through vulcanization, wherein a sodium sulphide solution is added into the alkaline leaching slag obtained in the step (2) until the lead in the alkaline leaching liquid completely precipitates, and lead concentrate is obtained; and (4) water is added into the alkaline leaching slag obtained in the step (2) for size mixing, then a sodium carbonate solution is added to adjust the pH value to be 10 to 11, then sodium cyanide is added for cyanidation leaching, leaching liquid and leaching slag are obtained, the leaching slag is subject to filter pressing stockpiling, the leaching liquid is subject to purification, deoxygenation and zinc powder replacement, and silver mud is obtained. By means of the efficient enrichment recovery method and system, the treatment method is simple, and efficient recovery enrichment of lead and silver is achieved.
Description
Technical field
The present invention relates to a kind of waste slag treatment method and in particular in a kind of lead melting waste slag lead and silver efficiently concentrating return
Receiving method and system.Belong to lead metallurgical slag processing technology field.
Background technology
Shi Qian big producing country of China, lead yield is sure to occupy the first in the world.Mineral products lead bullion major part is using biography in the world at present
System method sintering-retailoring of blast furnace flow process produces, and has mature and reliable, the features such as flow process is perfect, technical-economic index is preferable,
But, inevitably producing a large amount of waste residues, waste residue still remains a part of lead, if not reclaiming, certainly will cause greatly
Waste.
In addition, the silver on a small quantity containing in waste residue is typically processed by the way of storing up, fail to obtain synthetical recovery, so not
Only cause the wasting of resources, and there is potential impact to environment.
Content of the invention
The purpose of the present invention is for overcoming above-mentioned the deficiencies in the prior art, providing the height of lead and silver in a kind of lead melting waste slag
Effect enriching and recovering method.
The present invention further correspondingly provides the efficiently concentrating recovery system of lead and silver in a kind of lead melting waste slag.
For achieving the above object, the present invention adopts following technical proposals：
The efficiently concentrating recovery method of lead and silver in lead melting waste slag, including step：
(1) pretreatment：Lead melting waste slag is cooled to 0～5 DEG C, is then warming up to 500～600 with the speed of 10 DEG C/min
℃；
(2) alkali leaching：While hot lead melting waste slag is mixed with sodium hydroxide solution, obtain alkali immersion and alkali phase analysis；
(3) the heavy lead of alkali immersion sulfuration：Add sodium sulfide solution in the alkali immersion of step (2) gained, until in alkali immersion
Lead all precipitates, and obtains lead concentrate；
(4) add water in step (2) gained alkali phase analysis and size mixing, add sodium carbonate liquor adjustment pH value to 10～11, so
Add Cyanogran. to carry out Cyanide Leaching afterwards, obtain leachate and leached mud, leached mud filter pressing is stored up, leachate passes through to purify, takes off
Oxygen, zinc dust precipitation are processed, and obtain silver-colored mud.
Preferably, in step (2), lead melting waste slag and the mass volume ratio of sodium hydroxide solution are 1：2～4, sodium hydroxide
The mass concentration of solution is 20%.
Preferably, in step (3), the mass concentration of sodium sulfide solution is 15～20%.
Preferably, the alkali phase analysis after sizing mixing that add water in step (4) account for the 25～30% of gross mass.
Preferably, in step (4), the mass concentration of sodium carbonate liquor is 18%.
Preferably, in the leachate obtaining in step (4), cyaniding sodium content is the 0.15～0.2% of total leachate quality.
Preferably, in step (4), the time of Cyanide Leaching is 24～36 hours.
The efficiently concentrating recovery system of lead and silver in lead melting waste slag, including the pretreatment unit being sequentially connected, alkali process
Device and the first equipment for separating liquid from solid, the liquid outlet of described first equipment for separating liquid from solid and solid outlet, are reclaimed with lead respectively
Device and silver recovery unit connect.
Preferably, described pretreatment unit is stainless steel cauldron.
Preferably, described first equipment for separating liquid from solid is solid-liquid separating machine.
Preferably, described lead retracting device is connected with sodium sulfide solution feed arrangement and the second equipment for separating liquid from solid respectively.
It is further preferred that described second equipment for separating liquid from solid is solid-liquid separating machine.
Preferably, the entrance of described silver recovery unit is connected with sodium carbonate liquor feed arrangement and Cyanogran. feed arrangement respectively
Connect, its outlet is connected with the 3rd equipment for separating liquid from solid.
It is further preferred that described 3rd equipment for separating liquid from solid is solid-liquid separating machine.
It is further preferred that the liquid outlet of described 3rd equipment for separating liquid from solid and solid outlet, respectively with pressure filter and
The silver-colored reaction unit of zinc displacement connects.
Beneficial effects of the present invention：
The pretreatment that lead melting waste slag first is carried out lowering the temperature plus is rapidly heated by the present invention, improves the internal structure of waste residue, makes
Obtain metallic element to be easier to obtain release.Then carry out alkali leaching process while hot, and gained alkali immersion and alkali phase analysis are carried out respectively
Lead reclaims and processes with silver recovery, and processing method is simple it is achieved that the high efficiente callback of lead and silver is enriched with.
After testing, in gained lead concentrate of the present invention the mass content of lead more than 60%, silver the response rate more than 95%.
Brief description
Fig. 1 is the efficiently concentrating recovery system structural representation of the present invention；
Wherein, 1 is pretreatment unit, and 2 is alkali process device, and 3 is the first equipment for separating liquid from solid, and 4 is lead retracting device, 5
For silver recovery unit, 6 is sodium sulfide solution feed arrangement, and 7 is the second equipment for separating liquid from solid, and 8 is sodium carbonate liquor feed arrangement,
9 is Cyanogran. feed arrangement, and 10 is the 3rd equipment for separating liquid from solid, and 11 is pressure filter, and 12 replace silver-colored reaction unit for zinc.
Specific embodiment
The present invention will be further elaborated with reference to the accompanying drawings and examples it should explanation, and the description below is only
It is to explain the present invention, its content is not defined.
Embodiment 1：
The efficiently concentrating recovery method of lead and silver in lead melting waste slag, including step：
(1) pretreatment：Lead melting waste slag is cooled to 0 DEG C, is then warming up to 500 DEG C with the speed of 10 DEG C/min；
(2) alkali leaching：While hot lead melting waste slag is mixed with sodium hydroxide solution, obtain alkali immersion and alkali phase analysis；
(3) the heavy lead of alkali immersion sulfuration：Add sodium sulfide solution in the alkali immersion of step (2) gained, until in alkali immersion
Lead all precipitates, and obtains lead concentrate；
(4) add water in step (2) gained alkali phase analysis and size mixing, add sodium carbonate liquor adjustment pH value to 10, Ran Houjia
Enter Cyanogran. and carry out Cyanide Leaching, obtain leachate and leached mud, leached mud filter pressing is stored up, leachate passes through purification, deoxidation, zinc
Powder substitution is processed, and obtains silver-colored mud.
In step (2), lead melting waste slag and the mass volume ratio of sodium hydroxide solution are 1：2, the quality of sodium hydroxide solution
Concentration is 20%.
In step (3), the mass concentration of sodium sulfide solution is 15%.
The alkali phase analysis after sizing mixing that add water in step (4) account for the 25% of gross mass.
In step (4), the mass concentration of sodium carbonate liquor is 18%.
In the leachate obtaining in step (4), cyaniding sodium content is the 0.15% of total leachate quality.
In step (4), the time of Cyanide Leaching is 24 hours.
As shown in figure 1, in lead melting waste slag lead and silver efficiently concentrating recovery system, include the pretreatment that is sequentially connected and fill
Put 1, alkali process device 2 and the first equipment for separating liquid from solid 3, the liquid outlet of the first equipment for separating liquid from solid 3 and solid outlet, respectively
It is connected with lead retracting device 4 and silver recovery unit 5.
Pretreatment unit 1 is stainless steel cauldron.
First equipment for separating liquid from solid 3 is solid-liquid separating machine.
Lead retracting device 4 is connected with sodium sulfide solution feed arrangement 6 and the second equipment for separating liquid from solid 7 respectively.
Second equipment for separating liquid from solid 7 is solid-liquid separating machine.
The entrance of silver recovery unit 5 is connected with sodium carbonate liquor feed arrangement 8 and Cyanogran. feed arrangement 9 respectively, and it goes out
Mouth is connected with the 3rd equipment for separating liquid from solid 10.
3rd equipment for separating liquid from solid 10 is solid-liquid separating machine.
The liquid outlet of the 3rd equipment for separating liquid from solid 10 and solid outlet, respectively with pressure filter 11 and zinc displacement silver reaction dress
Put 12 connections.
After testing, in step (3) gained lead concentrate the mass content of lead more than 60%, step (4) gained silver recovery
Rate (to be calculated on the basis of the content of silver in lead melting waste slag) more than 95%.
Embodiment 2：
The efficiently concentrating recovery method of lead and silver in lead melting waste slag, including step：
(1) pretreatment：Lead melting waste slag is cooled to 5 DEG C, is then warming up to 600 DEG C with the speed of 10 DEG C/min；
(2) alkali leaching：While hot lead melting waste slag is mixed with sodium hydroxide solution, obtain alkali immersion and alkali phase analysis；
(3) the heavy lead of alkali immersion sulfuration：Add sodium sulfide solution in the alkali immersion of step (2) gained, until in alkali immersion
Lead all precipitates, and obtains lead concentrate；
(4) add water in step (2) gained alkali phase analysis and size mixing, add sodium carbonate liquor adjustment pH value to 11, Ran Houjia
Enter Cyanogran. and carry out Cyanide Leaching, obtain leachate and leached mud, leached mud filter pressing is stored up, leachate passes through purification, deoxidation, zinc
Powder substitution is processed, and obtains silver-colored mud.
In step (2), lead melting waste slag and the mass volume ratio of sodium hydroxide solution are 1：4, the quality of sodium hydroxide solution
Concentration is 20%.
In step (3), the mass concentration of sodium sulfide solution is 20%.
The alkali phase analysis after sizing mixing that add water in step (4) account for the 30% of gross mass.
In step (4), the mass concentration of sodium carbonate liquor is 18%.
In the leachate obtaining in step (4), cyaniding sodium content is the 0.2% of total leachate quality.
In step (4), the time of Cyanide Leaching is 36 hours.
The efficiently concentrating recovery system of lead and silver in lead melting waste slag, with embodiment 1.
After testing, in step (3) gained lead concentrate the mass content of lead more than 60%, step (4) gained silver recovery
Rate (to be calculated on the basis of the content of silver in lead melting waste slag) more than 95%.
Embodiment 3：
The efficiently concentrating recovery method of lead and silver in lead melting waste slag, including step：
(1) pretreatment：Lead melting waste slag is cooled to 5 DEG C, is then warming up to 600 DEG C with the speed of 10 DEG C/min；
(2) alkali leaching：While hot lead melting waste slag is mixed with sodium hydroxide solution, obtain alkali immersion and alkali phase analysis；
(3) the heavy lead of alkali immersion sulfuration：Add sodium sulfide solution in the alkali immersion of step (2) gained, until in alkali immersion
Lead all precipitates, and obtains lead concentrate；
(4) add water in step (2) gained alkali phase analysis and size mixing, add sodium carbonate liquor adjustment pH value to 11, Ran Houjia
Enter Cyanogran. and carry out Cyanide Leaching, obtain leachate and leached mud, leached mud filter pressing is stored up, leachate passes through purification, deoxidation, zinc
Powder substitution is processed, and obtains silver-colored mud.
In step (2), lead melting waste slag and the mass volume ratio of sodium hydroxide solution are 1：4, the quality of sodium hydroxide solution
Concentration is 20%.
In step (3), the mass concentration of sodium sulfide solution is 20%.
The alkali phase analysis after sizing mixing that add water in step (4) account for the 30% of gross mass.
In step (4), the mass concentration of sodium carbonate liquor is 18%.
In the leachate obtaining in step (4), cyaniding sodium content is the 0.2% of total leachate quality.
In step (4), the time of Cyanide Leaching is 36 hours.
The efficiently concentrating recovery system of lead and silver in lead melting waste slag, with embodiment 1.
After testing, in step (3) gained lead concentrate the mass content of lead more than 60%, step (4) gained silver recovery
Rate (to be calculated on the basis of the content of silver in lead melting waste slag) more than 95%.
Embodiment 4：
The efficiently concentrating recovery method of lead and silver in lead melting waste slag, including step：
(1) pretreatment：Lead melting waste slag is cooled to 0 DEG C, is then warming up to 600 DEG C with the speed of 10 DEG C/min；
(2) alkali leaching：While hot lead melting waste slag is mixed with sodium hydroxide solution, obtain alkali immersion and alkali phase analysis；
(3) the heavy lead of alkali immersion sulfuration：Add sodium sulfide solution in the alkali immersion of step (2) gained, until in alkali immersion
Lead all precipitates, and obtains lead concentrate；
(4) add water in step (2) gained alkali phase analysis and size mixing, add sodium carbonate liquor adjustment pH value to 10, Ran Houjia
Enter Cyanogran. and carry out Cyanide Leaching, obtain leachate and leached mud, leached mud filter pressing is stored up, leachate passes through purification, deoxidation, zinc
Powder substitution is processed, and obtains silver-colored mud.
In step (2), lead melting waste slag and the mass volume ratio of sodium hydroxide solution are 1：4, the quality of sodium hydroxide solution
Concentration is 20%.
In step (3), the mass concentration of sodium sulfide solution is 18%.
The alkali phase analysis after sizing mixing that add water in step (4) account for the 30% of gross mass.
In step (4), the mass concentration of sodium carbonate liquor is 18%.
In the leachate obtaining in step (4), cyaniding sodium content is the 0.2% of total leachate quality.
In step (4), the time of Cyanide Leaching is 30 hours.
The efficiently concentrating recovery system of lead and silver in lead melting waste slag, with embodiment 1.
After testing, in step (3) gained lead concentrate the mass content of lead more than 60%, step (4) gained silver recovery
Rate (to be calculated on the basis of the content of silver in lead melting waste slag) more than 95%.
Embodiment 5：
The efficiently concentrating recovery method of lead and silver in lead melting waste slag, including step：
(1) pretreatment：Lead melting waste slag is cooled to 3 DEG C, is then warming up to 550 DEG C with the speed of 10 DEG C/min；
(2) alkali leaching：While hot lead melting waste slag is mixed with sodium hydroxide solution, obtain alkali immersion and alkali phase analysis；
(3) the heavy lead of alkali immersion sulfuration：Add sodium sulfide solution in the alkali immersion of step (2) gained, until in alkali immersion
Lead all precipitates, and obtains lead concentrate；
(4) add water in step (2) gained alkali phase analysis and size mixing, add sodium carbonate liquor adjustment pH value to 10, Ran Houjia
Enter Cyanogran. and carry out Cyanide Leaching, obtain leachate and leached mud, leached mud filter pressing is stored up, leachate passes through purification, deoxidation, zinc
Powder substitution is processed, and obtains silver-colored mud.
In step (2), lead melting waste slag and the mass volume ratio of sodium hydroxide solution are 1：3, the quality of sodium hydroxide solution
Concentration is 20%.
In step (3), the mass concentration of sodium sulfide solution is 18%.
The alkali phase analysis after sizing mixing that add water in step (4) account for the 25～30% of gross mass.
In step (4), the mass concentration of sodium carbonate liquor is 18%.
In the leachate obtaining in step (4), cyaniding sodium content is the 0.15% of total leachate quality.
In step (4), the time of Cyanide Leaching is 32 hours.
The efficiently concentrating recovery system of lead and silver in lead melting waste slag, with embodiment 1.
After testing, in step (3) gained lead concentrate the mass content of lead more than 60%, step (4) gained silver recovery
Rate (to be calculated on the basis of the content of silver in lead melting waste slag) more than 95%.
Although the above-mentioned accompanying drawing that combines is described to the specific embodiment of the present invention, not model is protected to the present invention
The restriction enclosed, on the basis of technical scheme, those skilled in the art do not need to pay creative work and can do
The various modifications going out or deformation are still within protection scope of the present invention.
Claims (8)
1. in lead melting waste slag lead and silver efficiently concentrating recovery method it is characterised in that include step：
(1) pretreatment：Lead melting waste slag is cooled to 0～5 DEG C, is then warming up to 500～600 DEG C with the speed of 10 DEG C/min；
(2) alkali leaching：While hot lead melting waste slag is mixed with sodium hydroxide solution, obtain alkali immersion and alkali phase analysis；
(3) the heavy lead of alkali immersion sulfuration：Add sodium sulfide solution in the alkali immersion of step (2) gained, until the lead in alkali immersion is complete
Portion is precipitated, and obtains lead concentrate；
(4) add water in step (2) gained alkali phase analysis and size mixing, add sodium carbonate liquor adjustment pH value to 10～11, Ran Houjia
Enter Cyanogran. and carry out Cyanide Leaching, obtain leachate and leached mud, leached mud filter pressing is stored up, leachate passes through purification, deoxidation, zinc
Powder substitution is processed, and obtains silver-colored mud.
2. efficiently concentrating recovery method according to claim 1 is it is characterised in that lead melting waste slag and hydrogen in step (2)
The mass volume ratio of sodium hydroxide solution is 1：2～4, the mass concentration of sodium hydroxide solution is 20%.
3. efficiently concentrating recovery method according to claim 1 it is characterised in that in step (3) sodium sulfide solution matter
Amount concentration is 15～20%.
4. efficiently concentrating recovery method according to claim 1 is it is characterised in that the alkali after sizing mixing that adds water in step (4)
Phase analysis account for the 25～30% of gross mass；The mass concentration of sodium carbonate liquor is 18%；In leachate, cyaniding sodium content is total leaching
The 0.15～0.2% of liquid quality；The time of Cyanide Leaching is 24～36 hours.
5. the efficiently concentrating recovery system corresponding to method any one of claim 1 or 4 it is characterised in that include according to
The pretreatment unit of secondary connection, alkali process device and the first equipment for separating liquid from solid, the liquid discharge of described first equipment for separating liquid from solid
Mouth and solid outlet, are connected with lead retracting device and silver recovery unit respectively.
6. efficiently concentrating recovery system according to claim 5 it is characterised in that described lead retracting device respectively with sulfuration
Sodium solution feed arrangement and the second equipment for separating liquid from solid connect.
7. efficiently concentrating recovery system according to claim 5 is it is characterised in that the entrance of described silver recovery unit is distinguished
It is connected with sodium carbonate liquor feed arrangement and Cyanogran. feed arrangement, its outlet is connected with the 3rd equipment for separating liquid from solid.
8. efficiently concentrating recovery system according to claim 7 is it is characterised in that the liquid of described 3rd equipment for separating liquid from solid
Body outlet and solid outlet, are connected with pressure filter and the silver-colored reaction unit of zinc displacement respectively.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610973648.6A CN106381400A (en) | 2016-11-07 | 2016-11-07 | Efficient enrichment recovery method and system for lead and silver in lead smelting waste |
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| CN201610973648.6A CN106381400A (en) | 2016-11-07 | 2016-11-07 | Efficient enrichment recovery method and system for lead and silver in lead smelting waste |
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| CN114959274A (en) * | 2022-06-01 | 2022-08-30 | 紫金铜业有限公司 | Method for efficiently separating valuable elements in lead filter cake |
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| CN110396597A (en) * | 2019-07-19 | 2019-11-01 | 江西铜业集团有限公司 | A kind of selecting smelting combination process of the high efficiency extraction lead bismuth from oxidation cleaning residue |
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| CN114959274B (en) * | 2022-06-01 | 2024-02-13 | 紫金铜业有限公司 | Method for efficiently separating valuable elements in lead filter cake |
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