CN109517980A - A kind of method of synthetical recovery Copper in Electroplating Sludge nickel - Google Patents
A kind of method of synthetical recovery Copper in Electroplating Sludge nickel Download PDFInfo
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- CN109517980A CN109517980A CN201811456085.9A CN201811456085A CN109517980A CN 109517980 A CN109517980 A CN 109517980A CN 201811456085 A CN201811456085 A CN 201811456085A CN 109517980 A CN109517980 A CN 109517980A
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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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/2406—Binding; Briquetting ; Granulating pelletizing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/002—Inorganic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/012—Organic compounds containing sulfur
-
- 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
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/16—Sintering; Agglomerating
-
- 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
- C22B15/0002—Preliminary treatment
- C22B15/001—Preliminary treatment with modification of the copper constituent
- C22B15/0013—Preliminary treatment with modification of the copper constituent by roasting
- C22B15/0017—Sulfating or sulfiding roasting
-
- 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
- C22B23/005—Preliminary treatment of ores, e.g. by roasting or by the Krupp-Renn process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/04—Frothers
-
- 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 present invention relates to danger solid waste environmental protection treatment and resource regeneration field, a kind of method for specifically disclosing electroplating sludge processing recycling cupro-nickel.Method provided by the invention is first by electroplating sludge and sulfidation roasting additive mixed pelletizing, obtain green pellets, then green pellets is dry, be placed in 800~1200 DEG C at a temperature of sulfidation roasting, then it is that -0.045mm accounts for 60~80% that roasted product, which is milled to granularity, obtains ore grinding ore pulp；Flotation, isolated cupro-nickel bulk concentrate are carried out to ore grinding ore pulp, flotation tailing is harmless tailings, and it is that -0.037mm accounts for 90~95% that cupro-nickel bulk concentrate, which is regrinded to granularity, and flotation respectively obtains copper concentrate product and nickel ore concentrate product.Method provided by the invention handles electroplating sludge by sulfidation roasting and flotation, can synthetical recovery cupro-nickel valuable element therein, obtain copper concentrate and nickel ore concentrate respectively, the content of beary metal of flotation tailings significantly reduces, and Leaching is lower than relevant national standard.
Description
Technical field
The present invention relates to hazardous waste processing and resource regeneration technical fields, handle back more particularly to a kind of electroplating sludge
The method for receiving cupro-nickel.
Background technique
Electroplating sludge refers to the generated sediment containing various heavy during electroplating wastewater processing, these sediments
Moisture content is high, and wherein heavy metal components thermal stability is high and easy to migrate, easily causes secondary pollution.1998, China will be electroplated
Sludge is included in " National Hazard waste register " as typical case；" the hazardous waste business licence management method implemented in 2004
(2013 revision) " strict regulations have been formulated to the collection, storage and disposition etc. of electroplating sludge, to prevent electroplating sludge secondary
The generation of pollution.
There are numerous studies, the research in terms for the treatment of sludge is concentrated mainly on the technology of related electroplating sludge processing in recent years
In terms of the technologies such as the solidification of heavy metal element and stabilisation, try hard to realize the innoxious of toxic heavy metal element.But from
From the point of view of metal resource recycles, electroplating sludge is a kind of material that valuable metal element grade is relatively high in fact, often
The valuable metal element seen includes copper, nickel, chromium and zinc etc..But since these valuable metal elements are mostly with the oxide of high degree of dispersion
Form exists, and therefore, it is difficult to be enriched with by conventional means.It is current that the technique that aspect is studied is recycled in relation to valuable metal element
Core is concentrated mainly under the leaching-out technique system of non-ferrous metal, such as ammonium hydroxide lixiviation process, sulfuric acid leaching etc., in process flow
On the problems such as there are at high cost, process is complicated, operating efficiency is low.Therefore, it is also desirable to which the resource technology to electroplating sludge carries out
Research, to propose that practicability is good, processing method of good economy performance, to meet the market demand.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of methods of synthetical recovery Copper in Electroplating Sludge nickel, pass through sulphur
Change roasting and flotation handle electroplating sludge, can synthetical recovery cupro-nickel valuable element therein, obtain copper concentrate and nickel essence respectively
The content of beary metal of mine, flotation tailings significantly reduces, and Leaching is lower than relevant national standard.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of synthetical recovery Copper in Electroplating Sludge nickel
Method, including but not limited to following steps:
S1: electroplating sludge being mixed with sulfidation roasting additive, pelletizing, obtains green pellets, and the particle size range of green pellets is 8
~10mm, the sulfidation roasting additive are made of vulcanizing agent, flux, fluxing agent and reducing agent, the vulcanizing agent be pyrite,
The combination of any one or more of vulcanized sodium and sulphur, the flux are quartz and/or aluminium oxide, and the fluxing agent is borax
And/or sodium metasilicate, the reducing agent are anthracite；
S2: the green pellets is dry, sulphur at a temperature of the green pellets after drying process is then placed in 800~1200 DEG C
Change 60~120min of roasting, then natural cooling, obtains roasted product；
S3: it is -2mm that the roasted product, which is crushed to granularity, later under 60~65% ore milling concentration, after broken
Roasted product be milled to granularity be -0.045mm account for 60~80%, obtain ore grinding ore pulp；
S4: flotation is carried out to ore grinding ore pulp, isolated cupro-nickel bulk concentrate, flotation tailing is harmless tailings, when flotation
The flotation agent added into ore grinding ore pulp is made of regulator I, collecting agent and foaming agent, and the regulator I is lime and/or sulphur
Sour copper, the collecting agent are butyl xanthate and/or butylamine black powder, and the foaming agent is No. two flotation oils；
S5: it is that -0.037mm accounts for 90~95% that obtained cupro-nickel bulk concentrate, which is regrinded to granularity, obtains cupro-nickel bulk concentrate
Ore pulp is added regulator II into the copper-nickel bulk concentrate ore pulp and carries out copper moulding flotation, respectively obtains copper concentrate product
With nickel ore concentrate product, regulator II is sodium sulfite and/or vulcanized sodium.
It is further preferred that obtained the copper-nickel bulk concentrate ore pulp first carries out flotation removal of impurities, adjustment is added again later
Agent II carries out copper moulding flotation, and the impurity thing that flotation cleans is harmless tailings.To obtained cupro-nickel bulk concentrate ore pulp
Flotation removal of impurities is first carried out, carries out copper moulding flotation again later, the copper concentrate product that can be improved and nickel ore concentrate product
Grade, and improve the separative efficiency of copper moulding flotation.
Preferably, in step S1, the dosage of the vulcanizing agent is the sum of contained copper and mickel element molal quantity in electroplating sludge
2~3 times.
Preferably, in step S1, the dosage of the flux is the 10~30% of electroplating sludge dry weight.
Preferably, in step S1, the fluxing agent dosage is the 1~3% of electroplating sludge dry weight.
Preferably, in step S1, the reducing agent dosage is the 5~20% of electroplating sludge dry weight.
Preferably, in step S4, the dosage of the regulator I is that electroplating sludge per ton (dry weight) adds 200~2000g,
The dosage of the collecting agent is that electroplating sludge per ton (dry weight) adds 150~500g, and the dosage of the foaming agent is plating per ton
Sludge (dry weight) adds 50~150g.
Preferably, in step S5, the dosage of the regulator II be electroplating sludge per ton (dry weight) addition 1500~
3000g。
Preferably, in step S4, ore grinding flotation of ore pulp technique uses multistage flotation, including 1~2 roughing flotation, 1~2
Secondary flotation is scanned selected with 2~3 flotation.Situation is sorted depending on practical, roughing flotation, flotation are scanned and the selected number of segment of flotation
It makes the appropriate adjustments.
Preferably, in step S5, copper moulding floatation process uses multistage flotation, including 1~2 roughing flotation, 1~2
Secondary flotation is scanned selected with 3~4 flotation.Situation is sorted depending on practical, roughing flotation, flotation are scanned and the selected number of segment of flotation
It makes the appropriate adjustments.
Wherein, No. two flotation oils namely 2# oil.
The method of synthetical recovery Copper in Electroplating Sludge nickel provided by the invention first adds electroplating sludge and sulfidation roasting
The particle size range of agent mixing, pelletizing, obtained green pellets is 8~10mm, can accelerate rate of drying in the particle size range, and
And reaction contact area is big when sulfidation roasting, keeps reaction more thorough, improves the rate of recovery of valuable element, dry later, high temperature sulphur
Change roasting, sulfidation roasting additive is made of vulcanizing agent, flux, fluxing agent and reducing agent.The vulcanizing agent is pyrite, vulcanization
The combination of any one or more of sodium and sulphur, the flux are quartz and/or aluminium oxide, the fluxing agent be borax and/
Or sodium metasilicate, the reducing agent are anthracite.In high temperature vulcanized roasting process, vulcanizing agent is made as sulphur source, predominantly vulcanization
Industry provides element sulphur, generates the sulfide mineral of valuable metal；Flux is primarily to improve the flowing in sintering process between substance
Property, so that the valuable metal of fine grain teeth cloth is released effectively and participate in vulcanization reaction, reaches the mesh that valuable metal is separated with impurity
's；Fluxing agent is mainly used for reducing the fusion temperature of calcining matter, improves roasting efficiency；Reducing agent is that also Primordial Qi is provided for roasting
Atmosphere guarantees that the sulfur product of valuable metal is not oxidized.After roasting, the copper, nickel in electroplating sludge are by original oxide shape
Formula is changed into sulphided form, can carry out FLOTATION SEPARATION using method for floating.It is -2mm that roasted product, which is crushed to granularity, it
Afterwards under 60~65% ore milling concentration, it is that -0.045mm accounts for 60~80% that broken roasted product, which is milled to granularity, is obtained
Granular mass percentage in ore grinding ore pulp namely ore grinding ore pulp less than 0.045mm partial size accounts for 60~80%, produces according to roasting
Product carry out embedding cloth structural analysis, and under the grinding condition, copper, nickel sulfide and harmless tailing in roasted product have been basically reached
Complete solution from carrying out flotation, isolated cupro-nickel bulk concentrate, flotation tailing is harmless tailings later.Obtained cupro-nickel mixing essence
It is that -0.037mm accounts for 90~95% that mine, which is regrinded to granularity, obtains cupro-nickel bulk concentrate ore pulp, under the grinding condition, cupro-nickel mixing
Copper in concentrate, nickel sulfide basically reaches will be completely dissociated, and flotation is carried out later, in regulator sodium sulfite and/or vulcanized sodium
Under the action of, respectively obtain copper concentrate product and nickel ore concentrate product.It is added in floatation process, regulator is to reinforce collecting
Agent valuable metal sulfide surface absorption, or inhibit collecting agent impure mineral surface absorption, and then promoted collecting agent
In the efficiency of mineral surfaces selective absorption, collecting agent is the hydrophobicity in order to improve valuable metal sulfide, and then is made valuable
Metal realizes enrichment in flotation froth product, and foaming agent forms stable foam to reduce the surface tension of flotation pulp
Layer promotes flotation efficiency.
The method of synthetical recovery Copper in Electroplating Sludge nickel provided by the invention, mainly for electroplating sludge be cupric, nickel
Content is all larger than 1% electroplate factory's waste liquid solidification sediment, and the copper grade of copper concentrate obtained by final process is greater than 16%, copper recycling
Rate is greater than 60%；The nickel grade of nickel ore concentrate is greater than 8%, and nickel recovery is greater than 60%；Copper and mickel content is below in tailings
0.5%, Leaching is lower than " hazardous waste judging standard " (GB5085.3-2007) leaching characteristic identification standard value.
The method of synthetical recovery Copper in Electroplating Sludge nickel provided by the invention is for the first time using sulfidation roasting and flotation as technology
Core handles electroplating sludge, can synthetical recovery cupro-nickel valuable element therein, and obtain copper concentrate and nickel ore concentrate respectively；Technique
Process is reasonable, wider to the adaptability of raw material, and electroplate factory's waste liquid solidification sediment that cupric, nickel content are all larger than 1% can be located
Reason, and be not related to Leaching of Heavy Metals technology, be easier to implement and manipulate, economic feasibility is high, has good industrial prospect；Phase
As former state to electroplating sludge, the content of beary metal of tailings significantly reduces, and Leaching is lower than relevant national standard, and environmental benefit is prominent
Out.
Specific embodiment
The technical scheme of the invention is described in detail through specific implementation examples.
Embodiment 1
Process object is the electroplating sludge of Guangdong Jiangmen electroplate factory, and wherein the mass percentage content of copper and mickel is respectively
2.48% and 1.59%, electroplating sludge is handled using following technique, and copper, nickel are recycled:
(1) electroplating sludge is taken to mix with sulfidation roasting additive, pelletizing obtains green pellets, and sulfidation roasting additive is by sulphur
Agent, flux, fluxing agent and reducing agent composition, vulcanizing agent are pyrite, and flux is quartz, and fluxing agent is borax, and reducing agent is
Anthracite, the dosage of vulcanizing agent are 2 times of the sum of contained copper and mickel element molal quantity in electroplating sludge, and the dosage of flux is plating
The 25% of mud dry weight, fluxing agent dosage are the 1% of electroplating sludge dry weight, and reducing agent dosage is the 20% of electroplating sludge dry weight；
(2) after green pellets is dry, sulfidation roasting 100min obtains roasted product after natural cooling at 1000 DEG C；
(3) roasted product is crushed to granularity is -2mm (i.e. granularity is less than 2mm), then under 60% ore milling concentration,
It is that -0.045mm accounts for 80% that broken roasted product, which is milled to granularity, obtains ore grinding ore pulp；
(4) regulator lime and copper sulphate, collecting agent butyl xanthate and butylamine black powder are sequentially added into ore grinding ore pulp, are risen
No. two flotation oils of infusion, the dosage of regulator is that electroplating sludge per ton (calculating by dry weight, similarly hereinafter) adds 1100g, specifically, stone
The dosage of ash is that electroplating sludge per ton adds 1000g, and the dosage of copper sulphate is that electroplating sludge per ton adds 100g, the use of collecting agent
Amount is that electroplating sludge per ton adds 300g, specifically, the dosage of butyl xanthate is that electroplating sludge per ton adds 200g, butylamine black powder
Dosage be that electroplating sludge per ton adds 100g, the dosage of foaming agent is that electroplating sludge per ton adds 100g, and successively addition finishes
Afterwards, stirring action 30 minutes, then flotation, floatation process are used multistage flotation, are specifically swept using 1 roughing flotation, 2 flotation
Choosing and the selected technique of 3 flotation, isolated cupro-nickel bulk concentrate, flotation tailing are harmless tailings；
(5) by cupro-nickel bulk concentrate be finely ground to granularity be -0.037mm account for 95%, then be added regulator sodium sulfite and
Vulcanized sodium, the dosage of regulator is that electroplating sludge per ton adds 1500g, specifically, the dosage of sodium sulfite is that plating per ton is dirty
Mud adds 500g, and the dosage of vulcanized sodium is that electroplating sludge per ton adds 1000g, after addition, stirring action 30 minutes, then
Flotation, floatation process use multistage flotation, specifically scan the technique selected with 3 flotation using 1 roughing flotation, 1 flotation,
Isolated copper concentrate product and nickel ore concentrate product.
Copper concentrate product is 9.16% with respect to the yield of the dry original sample of electroplating sludge, and the grade of copper and mickel is respectively
20.49% and 3.16%, the rate of recovery of copper and mickel is respectively 75.68% and 18.20%；Nickel ore concentrate product is dry with respect to electroplating sludge
The yield of dry original sample is 12.14%, and the grade difference nickel of copper and mickel is 2.23% and 9.46%, and the rate of recovery of copper and mickel is respectively
10.92% and 72.23%；Tailings is 110.47% with respect to the yield of the dry original sample of electroplating sludge, copper, nickel content be respectively
0.30% and 0.14%.
Embodiment 2
Process object is the electroplating sludge of Foshan electroplate factory, and wherein the mass percentage content of copper and mickel is respectively
5.16% and 3.37%, electroplating sludge is handled using following technique, and copper, nickel are recycled:
(1) electroplating sludge is taken to mix with sulfidation roasting additive, pelletizing obtains green pellets, and sulfidation roasting additive is by sulphur
Agent, flux, fluxing agent and reducing agent composition, vulcanizing agent are the mixture (quality of pyrite and sulphur of pyrite and sulphur
Than for 3: 1), flux be quartz and aluminium oxide mixture (quartz and aluminium oxide mass ratio be 2: 1), fluxing agent be borax and
The mixture (mass ratio of borax and sodium metasilicate is 1: 1) of sodium metasilicate, reducing agent are anthracite, and the dosage of vulcanizing agent is that plating is dirty
3 times of the sum of contained copper and mickel element molal quantity in mud, the dosage of flux are the 30% of electroplating sludge dry weight, and fluxing agent dosage is
The 2% of electroplating sludge dry weight, reducing agent dosage are the 10% of electroplating sludge dry weight；
(2) after green pellets is dry, sulfidation roasting 120min obtains roasted product after natural cooling at 800 DEG C；
(3) roasted product is crushed to granularity is -2mm (i.e. granularity is less than 2mm), then under 65% ore milling concentration,
It is that -0.045mm accounts for 60% that broken roasted product, which is milled to granularity, obtains ore grinding ore pulp；
(4) regulator lime and copper sulphate, collecting agent butyl xanthate are sequentially added into ore grinding ore pulp, foaming agent two floating
Choosing oil, the dosage of regulator is that electroplating sludge per ton (calculating by dry weight, similarly hereinafter) adds 1700g, specifically, the dosage of lime is
Electroplating sludge per ton adds 1500g, and the dosage of copper sulphate is that electroplating sludge per ton adds 200g, and the dosage of collecting agent is electricity per ton
It plates sludge and adds 400g, the dosage of foaming agent is that electroplating sludge per ton adds 150g, and after successively adding, stirring action 40 divides
Clock, then flotation, floatation process use multistage flotation, are specifically scanned using 1 roughing flotation, 1 flotation selected with 2 flotation
Technique, isolated cupro-nickel bulk concentrate, flotation tailing be harmless tailings；
(5) cupro-nickel bulk concentrate is finely ground to granularity is that -0.037mm accounts for 90%, then to obtained cupro-nickel bulk concentrate
Ore pulp first carries out flotation removal of impurities, and the impurity thing that flotation cleans is harmless tailings, is added and adjusts into the ore pulp after flotation removal of impurities
Whole dose of sodium sulfite and vulcanized sodium, the dosage of regulator is that electroplating sludge per ton adds 3000g, specifically, the use of sodium sulfite
Amount is that electroplating sludge per ton adds 1000g, and the dosage of vulcanized sodium is that electroplating sludge per ton adds 2000g, after addition, stirring
Effect 20 minutes, then flotation, floatation process are used multistage flotation, are specifically scanned and 3 times using 1 roughing flotation, 2 flotation
The selected technique of flotation, isolated copper concentrate product and nickel ore concentrate product.
Copper concentrate product is 16.04% with respect to the yield of the dry original sample of electroplating sludge, and the grade of copper and mickel is respectively
26.47% and 3.25%, the rate of recovery of copper and mickel is respectively 82.28% and 15.47%；Nickel ore concentrate product is dry with respect to electroplating sludge
The yield of dry original sample is 18.21%, and the grade difference nickel of copper and mickel is 2.44% and 14.22%, and the rate of recovery of copper and mickel is distinguished
For 8.61% and 76.84%；Tailings is 107.14% with respect to the yield of the dry original sample of electroplating sludge, copper, nickel content be respectively
0.44% and 0.24%.
Embodiment 3
Process object is the electroplating sludge of Ningbo of Zhejiang electroplate factory, and wherein the mass percentage content of copper and mickel is respectively
2.87% and 3.05%, electroplating sludge is handled using following technique, and copper, nickel are recycled:
(1) electroplating sludge is taken to mix with sulfidation roasting additive, pelletizing obtains green pellets, and sulfidation roasting additive is by sulphur
Agent, flux, fluxing agent and reducing agent composition, vulcanizing agent are mixture (pyrite and the vulcanized sodium of pyrite and vulcanized sodium
Mass ratio is 1: 1), flux is the mixture (mass ratio of quartz and aluminium oxide is 1: 1) of quartz and aluminium oxide, and fluxing agent is boron
The mixture (mass ratio of borax and sodium metasilicate is 1: 2) of sand and sodium metasilicate, reducing agent is anthracite, and the dosage of vulcanizing agent is electricity
3 times for plating the sum of contained copper and mickel element molal quantity in sludge, the dosage of flux are the 10% of electroplating sludge dry weight, and fluxing agent is used
Amount is the 3% of electroplating sludge dry weight, and reducing agent dosage is the 5% of electroplating sludge dry weight；
(2) after green pellets is dry, sulfidation roasting 60min obtains roasted product after natural cooling at 1200 DEG C；
(3) roasted product is crushed to granularity is -2mm (i.e. granularity is less than 2mm), then under 62% ore milling concentration,
It is that -0.045mm accounts for 70% that broken roasted product, which is milled to granularity, obtains ore grinding ore pulp；
(4) regulator lime, collecting agent butyl xanthate and butylamine black powder are sequentially added into ore grinding ore pulp, foaming agent two
Flotation oil, the dosage of regulator are that electroplating sludge per ton (calculating by dry weight, similarly hereinafter) adds 2000g, and the dosage of collecting agent is every
Ton electroplating sludge adds 500g, specifically, the dosage of butyl xanthate is that electroplating sludge per ton adds 400g, the dosage of butylamine black powder
100g is added for electroplating sludge per ton, the dosage of foaming agent is that electroplating sludge per ton adds 150g, after successively adding, stirring
Effect 20 minutes, then flotation, floatation process are used multistage flotation, are specifically scanned and 2 times using 1 roughing flotation, 2 flotation
The selected technique of flotation, isolated cupro-nickel bulk concentrate, flotation tailing are harmless tailings；
(5) cupro-nickel bulk concentrate is finely ground to granularity is that -0.037mm accounts for 92%, then to obtained cupro-nickel bulk concentrate
Ore pulp first carries out flotation removal of impurities, and the impurity thing that flotation cleans is harmless tailings, is added and adjusts into the ore pulp after flotation removal of impurities
Whole dose of sodium sulfite and vulcanized sodium, the dosage of regulator is that electroplating sludge per ton adds 2300g, specifically, the use of sodium sulfite
Amount is that electroplating sludge per ton adds 800g, and the dosage of vulcanized sodium is that electroplating sludge per ton adds 1500g, after addition, stirring
Effect 20 minutes, then flotation, floatation process are used multistage flotation, are specifically scanned and 4 times using 1 roughing flotation, 1 flotation
The selected technique of flotation, isolated copper concentrate product and nickel ore concentrate product.
Copper concentrate product is 10.13% with respect to the yield of the dry original sample of electroplating sludge, and the grade of copper and mickel is respectively
23.48% and 3.34%, the rate of recovery of copper and mickel is respectively 82.88% and 11.09%；Nickel ore concentrate product is dry with respect to electroplating sludge
The yield of dry original sample is 16.51%, and the grade difference nickel of copper and mickel is 1.52% and 14.72%, and the rate of recovery of copper and mickel is distinguished
For 8.74% and 79.68%；Tailings is 109.41% with respect to the yield of the dry original sample of electroplating sludge, copper, nickel content be respectively
0.22% and 0.26%.
Embodiment 4
Process object is the electroplating sludge of electroplate factory, Anhui Chizhou City, and wherein the mass percentage content of copper and mickel is respectively
1.14% and 1.06%, electroplating sludge is handled using following technique, and copper, nickel are recycled:
(1) electroplating sludge is taken to mix with sulfidation roasting additive, pelletizing obtains green pellets, and sulfidation roasting additive is by sulphur
Agent, flux, fluxing agent and reducing agent composition, vulcanizing agent are mixture (pyrite and the vulcanized sodium of pyrite and vulcanized sodium
Mass ratio is 1: 1), flux is aluminium oxide, and fluxing agent is sodium metasilicate, and reducing agent is anthracite, and the dosage of vulcanizing agent is that plating is dirty
2 times of the sum of contained copper and mickel element molal quantity in mud, the dosage of flux are the 20% of electroplating sludge dry weight, and fluxing agent dosage is
The 3% of electroplating sludge dry weight, reducing agent dosage are the 5% of electroplating sludge dry weight；
(2) after green pellets is dry, sulfidation roasting 120min obtains roasted product after natural cooling at 900 DEG C；
(3) roasted product is crushed to granularity is -2mm (i.e. granularity is less than 2mm), then under 60% ore milling concentration,
It is that -0.045mm accounts for 75% that broken roasted product, which is milled to granularity, obtains ore grinding ore pulp；
(4) regulator lime and copper sulphate, collecting agent butyl xanthate are sequentially added into ore grinding ore pulp, foaming agent two floating
Choosing oil, the dosage of regulator is that electroplating sludge per ton (calculating by dry weight, similarly hereinafter) adds 550g, specifically, the dosage of lime is
Electroplating sludge per ton adds 500g, and the dosage of copper sulphate is that electroplating sludge per ton adds 50g, and the dosage of collecting agent is plating per ton
Sludge adds 150g, and the dosage of foaming agent is that electroplating sludge per ton adds 50g, after successively adding, stirring action 40 minutes,
Then flotation, floatation process use multistage flotation, are specifically scanned using 1 roughing flotation, 1 flotation selected with 2 flotation
Technique, isolated cupro-nickel bulk concentrate, flotation tailing are harmless tailings；
(5) cupro-nickel bulk concentrate is finely ground to granularity is that -0.037mm accounts for 95%, then to obtained cupro-nickel bulk concentrate
Ore pulp first carries out flotation removal of impurities, and the impurity thing that flotation cleans is harmless tailings, is added and adjusts into the ore pulp after flotation removal of impurities
Whole dose of sodium sulfite and vulcanized sodium, the dosage of regulator is that electroplating sludge per ton adds 1500g, specifically, the use of sodium sulfite
Amount is that electroplating sludge per ton adds 500g, and the dosage of vulcanized sodium is that electroplating sludge per ton adds 1000g, after addition, stirring
Effect 20 minutes, then flotation, floatation process are used multistage flotation, are specifically scanned and 3 times using 1 roughing flotation, 1 flotation
The selected technique of flotation, isolated copper concentrate product and nickel ore concentrate product.
Copper concentrate product is 4.85% with respect to the yield of the dry original sample of electroplating sludge, and the grade of copper and mickel is respectively
16.57% and 1.94%, the rate of recovery of copper and mickel is respectively 70.50% and 8.88%；Nickel ore concentrate product is dry with respect to electroplating sludge
The yield of dry original sample is 9.12%, and the grade difference nickel of copper and mickel is 1.72% and 8.17%, and the rate of recovery of copper and mickel is respectively
13.76% and 70.29%；Tailings is 105.63% with respect to the yield of the dry original sample of electroplating sludge, copper, nickel content be respectively
0.17% and 0.21%.
Embodiment 5
Process object is the electroplating sludge of Guangdong Huizhou electroplate factory, and wherein the mass percentage content of copper and mickel is respectively
2.14% and 2.37%, electroplating sludge is handled using following technique, and copper, nickel are recycled:
(1) electroplating sludge is taken to mix with sulfidation roasting additive, pelletizing obtains green pellets, and sulfidation roasting additive is by sulphur
Agent, flux, fluxing agent and reducing agent composition, vulcanizing agent are mixture (pyrite, vulcanization of pyrite, sulphur and vulcanized sodium
The mass ratio of sodium and sulphur is 2: 2: 1), flux is quartz, and fluxing agent is sodium metasilicate, and reducing agent is anthracite, the use of vulcanizing agent
Amount is 2 times of the sum of contained copper and mickel element molal quantity in electroplating sludge, and the dosage of flux is the 15% of electroplating sludge dry weight, is helped
Flux dosage is the 1% of electroplating sludge dry weight, and reducing agent dosage is the 8% of electroplating sludge dry weight；
(2) after green pellets is dry, sulfidation roasting 60min obtains roasted product after natural cooling at 1200 DEG C；
(3) roasted product is crushed to granularity is -2mm (i.e. granularity be less than 2mm), then 62.5% ore milling concentration
Under, it is that -0.045mm accounts for 65% that broken roasted product, which is milled to granularity, obtains ore grinding ore pulp；
(4) regulator lime and copper sulphate, collecting agent butylamine black powder are sequentially added into ore grinding ore pulp, foaming agent two floating
Choosing oil, the dosage of regulator is that electroplating sludge per ton (calculating by dry weight, similarly hereinafter) adds 220g, specifically, the dosage of lime is
Electroplating sludge per ton adds 120g, and the dosage of copper sulphate is that electroplating sludge per ton adds 100g, and the dosage of collecting agent is electricity per ton
It plates sludge and adds 300g, the dosage of foaming agent is that electroplating sludge per ton adds 100g, and after successively adding, stirring action 40 divides
Clock, then flotation, floatation process use multistage flotation, are specifically scanned using 1 roughing flotation, 1 flotation selected with 3 flotation
Technique, isolated cupro-nickel bulk concentrate, flotation tailing be harmless tailings；
(5) cupro-nickel bulk concentrate is finely ground to granularity is that -0.037mm accounts for 90%, then to obtained cupro-nickel bulk concentrate
Ore pulp first carries out flotation removal of impurities, and the impurity thing that flotation cleans is harmless tailings, is added and adjusts into the ore pulp after flotation removal of impurities
Whole dose of sodium sulfite and vulcanized sodium, the dosage of regulator is that electroplating sludge per ton adds 2300g, specifically, the use of sodium sulfite
Amount is that electroplating sludge per ton adds 800g, and the dosage of vulcanized sodium is that electroplating sludge per ton adds 1500g, after addition, stirring
Effect 20 minutes, then flotation, floatation process are used multistage flotation, are specifically scanned and 3 times using 1 roughing flotation, 1 flotation
The selected technique of flotation, isolated copper concentrate product and nickel ore concentrate product.
Copper concentrate product is 7.19% with respect to the yield of the dry original sample of electroplating sludge, and the grade of copper and mickel is respectively
22.89% and 3.34%, the rate of recovery of copper and mickel is respectively 76.91% and 10.13%；Nickel ore concentrate product is dry with respect to electroplating sludge
The yield of dry original sample is 14.10%, and the grade difference nickel of copper and mickel is 2.34% and 12.11%, and the rate of recovery of copper and mickel is distinguished
For 15.42% and 72.05%；Tailings is 98.46% with respect to the yield of the dry original sample of electroplating sludge, copper, nickel content be respectively
0.17% and 0.43%.
Harmless tailings obtained to above-described embodiment 1-5 is according to " hazardous waste judging standard " (GB5085.3-2007)
The tailings toxic leaching test standard of execution is detected, and as a result see the table below shown, it is seen that tailings obtained by above-described embodiment
Leaching is below standard requirements.
Each embodiment tailings toxicity leaches result (unit: mg/L)
Illustrated by above embodiments, method provided by the invention can carry out harmless treatment to electroplating sludge, and return
Cupro-nickel valuable element therein is received, the copper grade of copper concentrate obtained by final process is greater than 16%, and copper recovery is greater than 60%；Nickel essence
The nickel grade of mine is greater than 8%, and nickel recovery is greater than 60%；Copper and mickel content is below 0.5% in tailings, and Leaching is lower than
" hazardous waste judging standard " (GB5085.3-2007) leaching characteristic identification standard value.
Claims (10)
1. a kind of method of synthetical recovery Copper in Electroplating Sludge nickel, which is characterized in that comprising steps of
S1: electroplating sludge being mixed with sulfidation roasting additive, pelletizing, obtains green pellets, and the particle size range of green pellets is 8~
10mm, the sulfidation roasting additive are made of vulcanizing agent, flux, fluxing agent and reducing agent, and the vulcanizing agent is pyrite, sulphur
Change the combination of any one or more of sodium and sulphur, the flux is quartz and/or aluminium oxide, and the fluxing agent is borax
And/or sodium metasilicate, the reducing agent are anthracite；
S2: the green pellets is dry, vulcanize roasting at a temperature of the green pellets after drying process is then placed in 800~1200 DEG C
60~120min is burnt, then natural cooling, obtains roasted product；
S3: it is -2mm that the roasted product, which is crushed to granularity, later under 60~65% ore milling concentration, by broken roasting
Burning product to be milled to granularity is that -0.045mm accounts for 60~80%, obtains ore grinding ore pulp；
S4: flotation, isolated cupro-nickel bulk concentrate are carried out to ore grinding ore pulp, flotation tailing is harmless tailings, to mill when flotation
The flotation agent added in mine ore pulp is made of regulator I, collecting agent and foaming agent, and the regulator I is lime and/or sulfuric acid
Copper, the collecting agent are butyl xanthate and/or butylamine black powder, and the foaming agent is No. two flotation oils；
S5: it is that -0.037mm accounts for 90~95% that obtained cupro-nickel bulk concentrate, which is regrinded to granularity, obtains cupro-nickel bulk concentrate ore pulp,
Regulator II is added into the copper-nickel bulk concentrate ore pulp and carries out copper moulding flotation, respectively obtains copper concentrate product and nickel essence
Mineral products, regulator II are sodium sulfite and/or vulcanized sodium.
2. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 1, which is characterized in that the obtained copper
Nickel bulk concentrate ore pulp first carries out flotation removal of impurities, adds regulator II again later and carries out copper moulding flotation, flotation cleans to obtain
Impurity thing be harmless tailings.
3. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 1 or 2, which is characterized in that in step S1,
The dosage of the vulcanizing agent is 2~3 times of the sum of contained copper and mickel element molal quantity in electroplating sludge.
4. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 3, which is characterized in that in step S1, institute
The dosage for stating flux is the 10~30% of electroplating sludge dry weight.
5. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 4, which is characterized in that in step S1, institute
State 1~3% that fluxing agent dosage is electroplating sludge dry weight.
6. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 5, which is characterized in that in step S1, institute
State 5~20% that reducing agent dosage is electroplating sludge dry weight.
7. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 6, which is characterized in that in step S4, institute
The dosage for stating regulator I is that electroplating sludge per ton adds 200~2000g, and the dosage of the collecting agent is that electroplating sludge per ton adds
Add 150~500g, the dosage of the foaming agent is that electroplating sludge per ton adds 50~150g.
8. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 7, which is characterized in that in step S5, institute
The dosage for stating regulator II is that electroplating sludge per ton adds 1500~3000g.
9. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 8, which is characterized in that in step S4, mill
Mine flotation of ore pulp technique use multistage flotation, including 1~2 roughing flotation, 1~2 flotation scan it is selected with 2~3 flotation.
10. the method for synthetical recovery Copper in Electroplating Sludge nickel according to claim 9, which is characterized in that in step S5, copper
Nickel separating flotation technique use multistage flotation, including 1~2 roughing flotation, 1~2 flotation scan it is selected with 3~4 flotation.
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| CN111500865A (en) * | 2020-05-06 | 2020-08-07 | 杭州临安兴旺电镀有限公司 | Method for recycling heavy metals in electroplating sludge |
| CN113145304A (en) * | 2021-04-26 | 2021-07-23 | 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 |
| CN113477404A (en) * | 2021-07-06 | 2021-10-08 | 中南大学 | Method for efficiently recovering copper-nickel metal from nickel smelting slag |
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