CN107299219B - A kind of resource utilization method of electroplating sludge - Google Patents
A kind of resource utilization method of electroplating sludge Download PDFInfo
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- CN107299219B CN107299219B CN201710496929.1A CN201710496929A CN107299219B CN 107299219 B CN107299219 B CN 107299219B CN 201710496929 A CN201710496929 A CN 201710496929A CN 107299219 B CN107299219 B CN 107299219B
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
-
- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
-
- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
-
- 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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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention belongs to solid waste of heavy metal processing technology fields, and in particular, to a kind of resource utilization method of electroplating sludge.The present invention roasts certain time under 950~1250 DEG C of reducing atmosphere, obtains product of roasting and the dedusting ash based on zinc oxide the following steps are included: (1) mixes electroplating sludge and reducing agent；(2) product of roasting is crushed, ore grinding and gravity treatment, obtains copper, iron, Ni alloy powder and chromium-rich tailing；(3) high intensity magnetic separation is carried out to chromium-rich tailing, obtains fine chrome mine；(4) by copper, iron, Ni alloy powder, acidolysis is carried out, obtains copper sponge with iron replacement copper；Then fractional neutralization precipitated iron and nickel again, obtain iron ore concentrate and nickel hydroxide.The present invention realizes iron, chromium, nickel, copper, zinc by reduction roasting, Selectively leaching and precipitating and efficiently separates, and opens up a new way for innoxious, the resource utilization of electroplating sludge.
Description
Technical field
The invention belongs to solid waste of heavy metal processing technology fields, in particular it relates to a kind of resource of electroplating sludge
Change the method for utilizing.
Background technique
Electroplating industry is basic industry important in national economy, and one of current whole world three greatly pollution industry.By
It is enriched Cu in electroplating wastewater, Ni, Cr in electroplating sludge, the harmful heavy metals such as Zn are listed in state key hazardous waste.It is close
Nian Lai, the quantity rapid development of China's electroplating enterprise, and most of electroplating enterprise scale is smaller, equipment is backward, management level is low
Under, cause sludge yield big and complicated component mouth.The method of disposal of electroplating sludge and its research of resource technology have become
One of urgent problem to be solved in China environmental protection work.
Currently, the research of electric plating sludge resource technology focuses primarily upon heavy metal recovery technology both at home and abroad, mainly include
Several routes below:
Lixiviation process: by carrying out Selectively leaching to electroplating sludge, dissolve out heavy metal components therein, so that realizing has
The separation and enrichment of valence metal, extract technology mainly includes that acidleach and ammonia soak two kinds of techniques at present.Lixiviation process have simple process,
The high advantage of metal recovery rate, but generally existing selective relative deviation, the reluctant problem of waste liquid.
Roasting And Leaching method: it first using the impurity in high-temperature roasting pretreating sludge, then is extracted and is roasted with leaching agents such as acid, water
Valuable heavy metal in product, main includes that acid roasting and alkali roast two kinds of techniques.Sour roasting technique enhances reaction process, right
The selectivity of metal still deviation；Alkali roasting technique is high to the rate of recovery of chromium, but can generate Cr VI, and environmental pressure is larger.
Smelting process: smelting process is generally using coal, coke as fuel and reducing substances, supplemented by iron ore, Copper Ores, lime stone etc.
Material, smelting process furnace temperature are mainly used for recycling the Cu and Ni in electroplating sludge, product is matte and thick nickel at l300 DEG C or more.Ice
Copper and thick nickel all can directly be recycled with electrolysis method.Smelting technology only recycles copper and mickel, and comprehensive resource utilization rate is low.
In conclusion electric plating sludge resource is that resource utilization is low, siderochrome is difficult to efficiently separate, mistake using main problem
Journey is seriously polluted.The purpose of optimum economic benefit is utilized and obtained from the right combination of resource, and exploitation electroplating sludge is efficient
Separation technology is of great significance.
Summary of the invention
In view of the above shortcomings of the prior art, the main object of the present invention is to solve ferrochrome cleaning point in electroplating sludge
From, the problems such as process contamination is serious, resource utilization is low, a kind of resource utilization method of electroplating sludge is provided, it is dirty for plating
The comprehensive utilization of mud provides an effective approach.
The resource utilization method of electroplating sludge of the invention is to mix it with reducing agent using electroplating sludge as raw material,
Make zinc oxide reduction simple substance zinc by reduction roasting, enter dedusting ash with flue gas after simple substance zinc distillation-oxidation, obtains zinc production
Product；Realize that copper, nickel, the metallization reduction of iron, chromium oxide do not restore at the same time, roasted product by broken, ore grinding and
Sorting, obtains copper, iron, Ni alloy powder and chromium-rich tailing, and chromium-rich tailing passes through the available fine chrome mine of high intensity magnetic separation, alloy powder
Corresponding product is obtained with precipitating by the way that acid is molten.
The resource utilization method of electroplating sludge of the invention, comprising the following steps:
(1) electroplating sludge and reducing agent are mixed, 1~12h are kept the temperature under 950~1250 DEG C of reducing atmosphere,
Obtain product of roasting and the dedusting ash based on zinc oxide；
(2) product of roasting that step (1) obtains is crushed, ore grinding and sorting, obtain copper, iron, Ni alloy powder and
Chromium-rich tailing；
(3) the chromium-rich tailing for obtaining step (2) carries out high magnetic separation, obtains fine chrome mine；
(4) copper, iron, the Ni alloy powder for obtaining step (2) carries out acidolysis, and reduced iron powder displacement copper is then added, Gu
Copper sponge and filtrate are obtained after liquid separation；
(5) oxidation of divalent iron ion in the filtrate for obtaining step (4) is at trivalent, then fractional neutralization precipitated iron and
Nickel obtains iron ore concentrate and nickel hydroxide.
Method according to the present invention, reducing agent described in step (1) are charcoal, coke, graphite, coal, and preferably coal is made
For reducing agent.
Method according to the present invention, reducing agent dosage described in step (1) be electroplating sludge quality 10wt%~
50wt%.
Method according to the present invention, crushed product size described in step (2) are≤10mm, and grinding fineness is -74 μ
M content accounts for 70% or more.
Method according to the present invention, the high intensity magnetic separation magnetic field strength described in step (3) are 8000~16000 high
This.
Method according to the present invention, acid described in step (4) include: hydrochloric acid, sulfuric acid, nitric acid, one in hydrofluoric acid
Kind or several mixing.
Method according to the present invention, acidolysis temperature described in step (4) they are 25~95 DEG C, the acidolysis time is 30~
300min, it is 10:1~1:1 that acid hydrolysis solution, which consolidates mass ratio,.
Method according to the present invention, oxidation of divalent iron ion method described in step (5) includes air oxidation, ozone
Oxidation, hydrogen peroxide oxidation.
Method according to the present invention, terminal pH is between 3.5-5 for the precipitating of iron oxide described in step (5), hydroxide
It is pH >=9.0 that nickel, which precipitates terminal,.
A kind of resource utilization method of electroplating sludge of the present invention, with existing lixiviation process, Roasting And Leaching method and smelting process
It compares, there is apparent superiority:
(1) present invention recycles zinc oxide by reduction roasting, while realizing the selective metallization reduction of iron, copper, nickel,
The stabilization processes for completing heavy metal shorten the treatment process of electroplating sludge.
(2) present invention sorts to have obtained copper, nickel, ferroalloy powder and chromium-rich tailing by fine grinding, alloy powder and chromium-rich
Tailing has obtained corresponding product after handling respectively, realize iron and chromium efficiently separate and the cleaning of copper and mickel is extracted.
Specific embodiment
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.Unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.It is described to understand the present invention just for the sake of help, it should not be considered as to concrete restriction of the invention.
Typical case's plating sludge chemical composition (wet basis) is as follows
| Ingredient | H2O | Ni | Cu | Fe | Mg | Cr | Zn | Al | Other |
| Content/% | 71.53 | 3.65 | 4.56 | 7.86 | 4.54 | 3.12 | 2.94 | 0.54 | 1.26 |
Embodiment 1
The coal of electroplating sludge and butt 35wt% is mixed, is placed in graphite crucible, 950 DEG C at a temperature of protect
It is cooling after warm 1h, it is collected into dedusting ash containing zinc (ZnO content 85.41%), roasted product (crushed product after broken ore grinding
Granularity is≤10mm, and grinding fineness is that -74 μm of contents account for 70% or more) gravity treatment is carried out, obtaining nickel, iron, copper total content is more than
The rate of recovery of 90% alloy powder, nickel and copper all reaches 95% or more.Gravity tailings recycles fine chrome mine, chromium using intensity magnetic separator
Grade reaches 46.56%, 80% or more the rate of recovery.Copper, iron, nickel alloy powder using 30% hydrochloric acid as leach medium, 95
Under the conditions of DEG C, liquid-solid ratio 1:1 leaches 30min, and leachate obtained copper sponge after iron replacement, then rouse air iron from
Son is oxidized to trivalent, and fractional neutralization precipitates to obtain iron ore concentrate of the TFe grade greater than 62% and purity is more than 90% nickel hydroxide.
Embodiment 2
The graphite of electroplating sludge and butt 10wt% is mixed, is placed in graphite crucible, in 1250 DEG C of temperature
It is cooling after lower heat preservation 12h, it is collected into dedusting ash containing zinc (ZnO content 90.24%), roasted product is (broken after broken ore grinding
Product granularity is≤10mm, and grinding fineness is that -74 μm of contents account for 70% or more) gravity treatment is carried out, it is super to obtain nickel, iron, copper total content
Cross 95% alloy powder, the rate of recovery of nickel and copper all reaches 80% or more.Gravity tailings recycles chromogen using intensity magnetic separator
Mine, chromium grade reach 33.56%, 80% or more the rate of recovery.Copper, iron, nickel alloy powder using 15% sulfuric acid and 15% salt
Acid, which is used as, leaches medium, and under the conditions of 25 DEG C, liquid-solid ratio 10:1 leaches 240min, and leachate has obtained sponge after iron replacement
Copper, then adds hydrogen peroxide ferrous ions oxidation into trivalent, fractional neutralization precipitate to obtain iron ore concentrate of the TFe grade greater than 62% and
Purity is more than 90% nickel hydroxide.
Embodiment 3
The coke of electroplating sludge and butt 20wt% is mixed, is placed in graphite crucible, in 1150 DEG C of temperature
It is cooling after lower heat preservation 4h, it is collected into dedusting ash containing zinc (ZnO content 88.26%), roasted product is (broken after broken ore grinding
Product granularity is≤10mm, and grinding fineness is that -74 μm of contents account for 70% or more) gravity treatment is carried out, it is super to obtain nickel, iron, copper total content
Cross 93% alloy powder, the rate of recovery of nickel and copper all reaches 90% or more.Gravity tailings using intensity magnetic separator recycling fine chrome mine,
Chromium grade reaches 42.25%, and the rate of recovery reaches 85% or more.Nickel, iron, copper alloy powder using 45% nitric acid as leach
Medium, under the conditions of 95 DEG C, liquid-solid ratio 4:1 leaches 120min, and leachate has obtained copper sponge after iron replacement, and then drum is empty
Gas is ferrous ions oxidation at trivalent, and fractional neutralization precipitates to obtain iron ore concentrate of the TFe grade greater than 62% and purity is more than 90%
Nickel hydroxide.
Embodiment 4
The charcoal of electroplating sludge and butt 20wt% is mixed, is placed in graphite crucible, in 1200 DEG C of temperature
It is cooling after lower heat preservation 2h, it is collected into dedusting ash containing zinc (ZnO content 91.34%), roasted product is (broken after broken ore grinding
Product granularity is≤10mm, and grinding fineness is that -74 μm of contents account for 40% or more) gravity treatment is carried out, it is super to obtain nickel, iron, copper total content
Cross 93% alloy powder, the rate of recovery of nickel and copper all reaches 85% or more.Gravity tailings using intensity magnetic separator recycling fine chrome mine,
Chromium grade reaches 43.35%, and the rate of recovery reaches 90% or more.Nickel, iron, copper alloy powder use 15% hydrochloric acid and 3% hydrogen
Fluoric acid, which is used as, leaches medium, and under the conditions of 45 DEG C, liquid-solid ratio 2:1 leaches 120min, and leachate has obtained sponge after iron replacement
Then copper rouses air ferrous ions oxidation into trivalent, fractional neutralization precipitates to obtain iron ore concentrate and purity of the TFe grade greater than 62%
Nickel hydroxide more than 90%.
Certainly, the present invention can also there are many embodiments, without deviating from the spirit and substance of the present invention, are familiar with
Those skilled in the art can disclosure according to the present invention make various corresponding changes and modifications, but these it is corresponding change and
Deformation all should belong to scope of protection of the claims of the invention.
Claims (9)
1. a kind of resource utilization method of electroplating sludge, comprising the following steps:
(1) electroplating sludge and reducing agent are mixed, 1~12h is kept the temperature under 950~1250 DEG C of reducing atmosphere, is obtained
Product of roasting and the dedusting ash based on zinc oxide；
(2) product of roasting that step (1) obtains is crushed, ore grinding and sorting, obtains copper, iron, Ni alloy powder and chromium-rich
Tailing；
(3) the chromium-rich tailing for obtaining step (2) carries out high magnetic separation, obtains fine chrome mine；
(4) copper, iron, the Ni alloy powder for obtaining step (2) carries out acidolysis, and reduced iron powder displacement copper, solid-liquid point is then added
Copper sponge and filtrate are obtained from after；
(5) oxidation of divalent iron ion in the filtrate for obtaining step (4) is at trivalent, and then fractional neutralization precipitated iron and nickel, obtain
To iron ore concentrate and nickel hydroxide.
2. the method according to claim 1, wherein reducing agent described in step (1) be charcoal, coke, graphite,
Coal.
3. the method according to claim 1, wherein reducing agent dosage described in step (1) is dry for electroplating sludge
10wt%~50wt% of matrix amount.
4. the method according to claim 1, wherein crushed product size described in step (2) is≤10mm, mill
Mine fineness is that -74 μm of contents account for 70% or more.
5. the method according to claim 1, wherein high magnetic separation magnetic field strength described in step (3) is 8000
~16000 Gausses.
6. the method according to claim 1, wherein acid described in step (4) include: hydrochloric acid, sulfuric acid, nitric acid,
One of hydrofluoric acid or several mixing.
7. the method according to claim 1, wherein acidolysis temperature described in step (4) be 25~95 DEG C, acidolysis
Time is 30~300min, and it is 10:1~1:1 that acid hydrolysis solution, which consolidates mass ratio,.
8. the method according to claim 1, wherein oxidation of divalent iron ion method described in step (5) includes
Air oxidation, ozone oxidation, hydrogen peroxide oxidation.
9. the method according to claim 1, wherein the precipitating terminal pH of neutralization precipitation iron described in step (5)
Between 3.5-5, nickel hydroxide precipitate terminal is pH >=9.0.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108672714A (en) * | 2018-04-24 | 2018-10-19 | 上海大学 | The method that alloy powder is directly prepared by cold rolling sludge |
| CN109433216A (en) * | 2018-11-07 | 2019-03-08 | 上海大学 | A method of catalyst is prepared using heavy metal sewage sludge fusion and gasification |
| CN111763821B (en) * | 2020-07-23 | 2023-10-24 | 宝武集团环境资源科技有限公司 | Electroplating sludge treatment method and device |
| CN113145304B (en) * | 2021-04-26 | 2023-03-21 | 昆明理工大学 | Method for recovering copper, nickel, zinc, iron and chromium by combining in-situ reduction, vulcanization, floatation, magnetism and electricity of electroplating sludge |
| CN114032395B (en) * | 2021-11-09 | 2023-08-11 | 东华大学 | Method for recovering copper, nickel and chromium in electroplating sludge by using waste cathode carbon as additive through oxidation-reduction two-step method |
| CN114686689B (en) * | 2022-04-11 | 2023-08-25 | 华北理工大学 | Multi-source metallurgical dust treatment method |
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