CN107287429B - A kind of iron content is high, the low electroplating sludge of cupro-nickel content recovery and treatment method - Google Patents
A kind of iron content is high, the low electroplating sludge of cupro-nickel content recovery and treatment method Download PDFInfo
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- CN107287429B CN107287429B CN201710541147.5A CN201710541147A CN107287429B CN 107287429 B CN107287429 B CN 107287429B CN 201710541147 A CN201710541147 A CN 201710541147A CN 107287429 B CN107287429 B CN 107287429B
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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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
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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
- C22B15/0071—Leaching or slurrying with acids or salts thereof 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
- 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
-
- 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
- C22B23/043—Sulfurated 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
- 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
- C22B23/0469—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods by chemical substitution, e.g. by cementation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
A kind of iron content is high, the low electroplating sludge of cupro-nickel content recovery and treatment method, and electroplating sludge is dissolved completely in sulfuric acid solution by (1), and ammonium hydroxide is added to adjust pH=3~4, and agitation and filtration obtains iron hydroxide sludge and Cu2+、Ni2+Based on solution；(2) by iron hydroxide sludge by washing, aqueous is recycled to step (1)；(3) it is precipitated and dissolved in sulfuric acid solution after washing, iron powder reducing is added, ferrous sulfate solution is obtained by filtration, remaining iron powder can be recycled, and solution distillation and concentration, recrystallization, centrifugation are then obtained errous sulfate crystal；(4) iron powder is added in cupro-nickel solution in (1), and successively copper, nickel by powder are obtained and with Fe by replacing, sieving2+Based on solution, and solution enters back into condensing crystallizing in (3) and prepares ferrous sulfate.Present invention process is easily controllable, while realizing that iron resourceization utilizes, has a recovery utilization rate for ensureing other low content metals, and can large-scale production the characteristics of.
Description
Technical field
This application involves the recovery processing technical field of electroplating sludge more particularly to a kind of high content iron, low content cupro-nickels
Electroplating sludge recycling processing method.
Background technology
As " the final state object " after electroplating wastewater precipitation process, the huge sum of money such as Cu, Ni, Zn, Cr, Fe is contained in electroplating sludge
Belong to, ingredient is sufficiently complex, heavy metal is difficult to degrade, and has been put into National Hazard waste register.These in electroplating sludge
Heavy metal has the characteristics that unstable, easy accumulation, is easy to run off, if not dealt carefully with to it, holds very much under external environmental activity
It easily migrates, causes secondary pollution, endangers environment, and then influence human health.
The main methods of electroplating sludge include harmlessness disposing and recycling.From prevention and cure of pollution and resources circulation
From the point of view of utilization, carrying out synthetical recovery to heavy metal resources in electroplating sludge, there is important environment, resource and society to imitate
Benefit.Heavy metal recovery technology includes pyrogenic process and hydrometallurgic recovery, wherein pyrogenic process be limited to of high cost, energy consumption is big, metal recovery rate and
The not high factor of purity.And wet processing relates to leach and detach two big processes for recycling metal in electroplating sludge, leaches
It is mainly soaked using acidleach and alkali, and detaches and mainly pass through chemical precipitation method, reduced separation method, strike etc..
In electroplating sludge, it is many to be related to the research detached containing various metals such as cupro-nickel iron, such as patent
CN200610050002.7 proposes a kind of method recycling valuable metal from electroplating sludge, by being added into acid leaching liquor
Sulfide obtains copper sulfide precipitation and detaches copper, then adjusts pH successively by alkali and successively isolate chromium, iron, nickel and zinc, this method
The copper sulfide of formation inevitably causes secondary pollution in post-processing, while it is useless to produce plating in processing procedure again
Slag does not propose to be further processed method.
Patent CN201510311839.1 provides a kind of method of electroplating sludge comprehensively recovering valuable metal, passes through ammonia
Leaching-acidleach joint leaches metal, is then still the introduction of vulcanized sodium precipitation separation copper, two are equally faced in post-processing
The problem of secondary pollution.
A kind of method that patent CN201410192292.3 provides the recovering copper from electroplating sludge, nickel, iron, first
Adjust acid leaching liquor pH precipitation removal iron, then into cupro-nickel sediment using glycerine separation copper, nickel, this method describe copper,
The separation of three kinds of nickel, iron metals, the glycerine being introduced into reaction rate in weak solution is extremely low, and is likely to result in oxide interface
Solution blackening and after increasing subsequent filtrate intractability, while the introducing of sodium sulphate also results in nickel sulfate product purity in technique
It is not high.
Patent CN201310267803.9 provides a kind of method of the comprehensively recovering valuable metal from electroplating waste mud, equally
It is that metal is successively isolated by acidleach, precipitation, treatment process easily forms the noxious materials such as Cr VI, the sodium carbonate equally introduced
It can influence the purity of final products nickelous carbonate and sodium zincate.
Moreover, the above patent emphasis is that such as Cu, Ni have more valuable metal recycling mostly, and to wherein containing
It is generally only to be handled by simple separation to measure less Fe.The recycling treatment attention rate of iron is general or such as patent publication No.
It is generally only for single specific iron cement described in CN103252340A.And for based on iron, while it including the electricity of other metals
The separation of plating sludge is relatively fewer using then reporting.
Invention content
To overcome the shortcomings of that prior art research, the applicant provide the plating that a kind of iron content is high, cupro-nickel content is low
The recovery and treatment method of sludge.Present invention process is easily controllable, the recovery utilization rate with the other low content metals of guarantee, and energy
The characteristics of enough large-scale productions.
Technical solution of the present invention is as follows：
A kind of iron content is high, the low electroplating sludge of cupro-nickel content recovery and treatment method, it is characterised in that including following step
Suddenly：
(1) electroplating sludge is added in sulfuric acid solution, stirring and dissolving obtains containing Fe3+、Cu2+、Ni2+Solution, add ammonium hydroxide
PH=3~4 are adjusted, standing sedimentation is obtained by filtration hydroxide iron cement and contains Cu2+、Ni2+Filtrate；
(2) hydroxide iron cement is successively clean by 2~3 washings, it washes rear solution and is recycled to step (1)；
(3) rear ferric hydroxide precipitate will be washed in step (2) to be dissolved completely in sulfuric acid solution, excess iron powder room temperature is added and stirs
It mixes, ferrous sulfate solution is obtained by filtration, and filtrate is by that can obtain technical grade sulfuric acid ferrous iron crystal after concentration, recrystallization, centrifugation；
(4) gained Cu in sulfuric acid regulating step (1) is used2+、Ni2+Filtrate makes its pH=1~2, iron powder is added in two portions,
It is filtered after stirring, screening priority obtains irregular near-spherical copper, nickel by powder and contains Fe2+Filtrate, and filtrate press step (3) technique
Prepare ferrous sulfate.
In above-mentioned steps (1), sludge is completely dissolved rear pH value of solution=0.2~1 by 20% sulfuric acid of use quality concentration, dissolving
1~3h of time.
In above-mentioned steps (1), after adjusting pH using ammonium hydroxide under room temperature, solution needs 3~5h of standing sedimentation.
In above-mentioned steps (2), iron hydroxide muddy water is washed：By ferric hydroxide precipitate solid-to-liquid ratio be 1:Under conditions of 1.5~2
Successively mashing washing 2~3 times, each beating time are 2~3h.
In above-mentioned steps (3), 20% sulfuric acid dissolution iron hydroxide sludge of same use quality concentration, the addition of iron powder is
0.5~1 times of the amount of the substance of iron in filtrate.
In above-mentioned steps (4), the iron powder amount being added every time is 1~1.5 times of the amount of the substance of copper or nickel in filtrate.
In above-mentioned steps (4), the sulfuric acid regulation solution pH of use quality a concentration of 80%.
In the electroplating sludge that iron content described above is high, cupro-nickel content is low, iron content is in 10wt% or more, and cupro-nickel content
In 2wt% or less.
The present invention is beneficial to be had technical effect that：
The present invention takes full advantage of the physicochemical properties feature of metal, is tapped a blast furnace first by hydrolytic precipitation separation, then
Copper, nickel by powder are obtained by replacing successively reduction using the difference of redox potential, it is thus achieved that three kinds of metals of cupro-nickel iron
Step by step arithmetic, to solve the problems, such as in such electroplating sludge recycle useful metal.
Compared with patent CN200610050002.7, CN201510311839.1, integrated artistic of the present invention is mild, intermediate nothing
Secondary waste generates, and no longer needs to be handled, will not equally cause secondary pollution.And with patent CN201410192292.3,
CN201310267803.9 is compared, the introducing without other metals and organic solvent outside system in the present invention, before system overall composition
It does not change afterwards, no noxious material and waste water occur, and filtrate eventually enters into distillation and concentration and obtains the sulfuric acid that purity can reach technical grade
Ferrous iron, while the copper of intermediate recycling, the nickel by powder rate of recovery and purity are also very high, can be used as other functional materials such as electrocondution slurry
Raw material, it is simple for process, be widely used, strong operability, the abundant recycling profit that such iron cement is realized in large-scale production can be carried out
With.
Description of the drawings
Fig. 1 is process flow chart provided by the present invention；
Fig. 2 is respectively to obtain the schematic diagram of product ferrous sulfate, copper powder, nickel powder；
Fig. 3 is copper, nickel by powder high power scanning electron microscope (SEM) photograph.
Specific implementation mode
It is specifically to be described to the present invention in conjunction with attached drawing 1 and embodiment below.
Embodiment 1
The electroplating sludge for taking 400kg, is slowly added to the sulfuric acid solution of mass concentration 20%, and stirring and dissolving 1h is measured and leached
The terminal pH=0.4 of liquid is slowly added into ammonium hydroxide and adjusts lysate pH=3, after standing sedimentation 3h press filtration obtain iron hydroxide sludge
With filtrate；Iron hydroxide sludge presses solid-to-liquid ratio 1:1.5 mashing washings, wash 2h every time, the mashing water reuse after washing to plating
Rear hydroxide iron cement is washed in the sulfuric acid solution dissolving of the dissolving of sludge, use quality concentration 20%, adds iron in solution thereto
0.5 times of iron powder of the amount of substance, is stirred at room temperature and ferrous sulfate solution is obtained by filtration, and filtrate concentration, recrystallization, centrifugation finally obtain
Reach technical grade standard ferrous sulfate (purity 87.95%)；And 80% sulphur acid for adjusting pH is added to 1, Xiang Qi in filtrate at normal temperatures
In iron powder is added in two portions, each addition is 1~1.5 times of the amount of the substance of copper or nickel in filtrate, after stirring filter, sieve
Copper powder (purity 98%), nickel powder (purity 97%) successively are obtained, the two rate of recovery is respectively 97.8%, 98%.
Fig. 2 is the schematic diagram for recycling obtained product ferrous sulfate (a), copper powder (b), nickel powder (c), it is seen that
Errous sulfate crystal is light green coloured particles, and particle size distribution is uniform, and the red copper powders formed and grey nickel by powder, powder
Fine and smooth, uniform color has higher porosity and capillarity.And the high power of product copper powder (a), nickel powder (b) is recycled from Fig. 3
Scanning electron microscope (SEM) photograph can be seen that near-spherical pattern is presented in copper, nickel by powder, and measuring correlated performance such as electric conductivity, (the two electricalresistivityρ distinguishes
Reach 16.85n Ω m and 68.25n Ω m, 20 DEG C), apparent density (3.75g/cm3) etc. be substantially better than some irregular shapes
(the two electricalresistivityρ is respectively 24.35n Ω m and 74.68n Ω m to shape Series powder, 20 DEG C；Apparent density 1.25g/cm3)。
Embodiment 2
The electroplating sludge for taking 600kg, is slowly added to the sulfuric acid solution of mass concentration 20%, and stirring and dissolving 2h is measured and leached
The terminal pH=0.7 of liquid is slowly added into ammonium hydroxide and adjusts lysate pH=3.5, after standing sedimentation 4h press filtration obtain iron hydroxide dirt
Mud and filtrate；Iron hydroxide sludge presses solid-to-liquid ratio 1:1.8 mashing washings, wash 2.5h, the mashing water reuse after washing is extremely every time
Rear hydroxide iron cement is washed in the sulfuric acid solution dissolving of the dissolving of electroplating sludge, use quality concentration 20%, is added in solution thereto
0.8 times of iron powder of the amount of the substance of iron, is stirred at room temperature and ferrous sulfate solution is obtained by filtration, and filtrate concentration, recrystallization, centrifugation are final
Technical grade standard ferrous sulfate (purity 91.25%) must be reached；And 80% sulphur acid for adjusting pH is added extremely in filtrate at normal temperatures
1.5, iron powder is added in two portions thereto, each addition is 1~1.5 times of the amount of the substance of copper or nickel in filtrate, after stirring
Filtering, screening successively obtain copper powder (purity 97.8%), nickel powder (purity 98.5%), the two rate of recovery is respectively 99%,
98.9%.
Fig. 2 is the schematic diagram for recycling obtained product ferrous sulfate (a), copper powder (b), nickel powder (c), it is seen that
Errous sulfate crystal is light green coloured particles, and particle size distribution is uniform, and the red copper powders formed and grey nickel by powder, powder
Fine and smooth, uniform color, it is believed that there is higher porosity and capillarity.And recycle product copper powder (a), nickel powder (b) from Fig. 3
High power scanning electron microscope (SEM) photograph can be seen that, copper, nickel by powder present near-spherical pattern, measure correlated performance such as electric conductivity (the two resistance
Rate ρ is respectively 18.75n Ω m and 68.94n Ω m, 20 DEG C), apparent density (4.25g/cm3) etc. be substantially better than some and do not advise
Then (the two electricalresistivityρ is respectively 28.64n Ω m and 78.45n Ω m to shape Series powder, 20 DEG C；Apparent density 1.78g/
cm3)。
Embodiment 3
The electroplating sludge for taking 800kg, is slowly added to the sulfuric acid solution of mass concentration 20%, and stirring and dissolving 3h is measured and leached
The terminal pH=1 of liquid is slowly added into ammonium hydroxide and adjusts lysate pH=4, after standing sedimentation 5h press filtration obtain iron hydroxide sludge with
Filtrate；Iron hydroxide sludge presses solid-to-liquid ratio 1:2 mashing washings, wash 3h, the mashing water reuse after washing to electroplating sludge every time
Dissolving, use quality concentration 20% sulfuric acid solution dissolving washes rear hydroxide iron cement, add the substance of iron in solution thereto
Amount 1.0 times of iron powders, be stirred at room temperature and ferrous sulfate solution be obtained by filtration, filtrate concentration, recrystallization, centrifugation finally obtain and reach
Technical grade standard ferrous sulfate (purity 89.78%)；80% sulphur acid for adjusting pH is added to 2 in filtrate at normal temperatures, is divided to two thereto
Secondary addition iron powder, each addition are 1~1.5 times of the amount of the substance of copper or nickel in filtrate, are filtered after stirring, screening successively obtains
To copper powder (purity 99.2%), nickel powder (purity 98.7%), the two rate of recovery is respectively 98.3%, 99.1%.
Fig. 2 is the schematic diagram for recycling obtained product ferrous sulfate (a), copper powder (b), nickel powder (c), it is seen that
Errous sulfate crystal is light green coloured particles, and particle size distribution is uniform, and the red copper powders formed and grey nickel by powder, powder
Fine and smooth, uniform color, it is believed that there is higher porosity and capillarity.And recycle product copper powder (a), nickel powder (b) from Fig. 3
High power scanning electron microscope (SEM) photograph can be seen that, copper, nickel by powder present near-spherical pattern, measure correlated performance such as electric conductivity (the two resistance
Rate ρ is respectively 19.87n Ω m and 70.16n Ω m, 20 DEG C), apparent density (2.87g/cm3) etc. be substantially better than some and do not advise
Then (the two electricalresistivityρ is respectively 26.38n Ω m and 79.86n Ω m to shape Series powder, 20 DEG C；Apparent density 0.98g/
cm3)。
Claims (4)
1. a kind of iron content is high, the recovery and treatment method of the low electroplating sludge of cupro-nickel content, it is characterised in that include the following steps：
(1) electroplating sludge is added in sulfuric acid solution, stirring and dissolving obtains containing Fe3+、Cu2+、Ni2+Solution, add ammonium hydroxide to adjust
PH=3~4, standing sedimentation are obtained by filtration hydroxide iron cement and contain Cu2+、Ni2+Filtrate；20% sulfuric acid of use quality concentration will
Sludge is completely dissolved rear pH value of solution=0.2~1,1~3h of dissolution time；
(2) hydroxide iron cement is successively clean by 2~3 washings, it washes rear solution and is recycled to step (1)；
(3) rear ferric hydroxide precipitate will be washed in step (2) to be dissolved completely in sulfuric acid solution, iron powder is added and is stirred at room temperature, filters
Ferrous sulfate solution is obtained, and filtrate is by that can obtain technical grade sulfuric acid ferrous iron crystal after concentration, recrystallization, centrifugation；Use quality
20% sulfuric acid dissolution iron hydroxide sludge of concentration, the addition of iron powder are 0.5~1 times of the amount of the substance of iron in solution；
(4) gained in sulfuric acid regulating step (1) is used to contain Cu2+、Ni2+Filtrate, make its pH=1~2, iron powder be added in two portions,
It is filtered after stirring, screening priority obtains irregular near-spherical copper, nickel by powder and contains Fe2+Filtrate, and filtrate press step (3) technique
Prepare ferrous sulfate；The iron powder amount being added every time is 1~1.5 times of the amount of the substance of copper or nickel in filtrate；
In the electroplating sludge that iron content described above is high, cupro-nickel content is low, iron content is in 10wt% or more, and cupro-nickel content exists
2wt% or less.
2. according to the method described in claim 1, it is characterized in that：In above-mentioned steps (1), pH is adjusted using ammonium hydroxide under room temperature
Afterwards, solution needs 3~5h of standing sedimentation.
3. according to the method described in claim 1, it is characterized in that：In above-mentioned steps (2), iron hydroxide muddy water is washed：By hydrogen-oxygen
It is 1 to change iron to be deposited in solid-to-liquid ratio:Successively mashing washing 2~3 times under conditions of 1.5~2, each beating time are 2~3h.
4. according to the method described in claim 1, it is characterized in that：In above-mentioned steps (4), the sulphur of use quality a concentration of 80%
Acid-conditioning solution pH.
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| CN112226618A (en) * | 2020-09-10 | 2021-01-15 | 锡矿山闪星锑业有限责任公司 | Method for recovering copper and nickel from noble antimony by adopting wet replacement method |
| CN112919521B (en) * | 2021-01-22 | 2023-07-11 | 苗婷婷 | Comprehensive utilization method of waste FCC catalyst |
| CN112941314B (en) * | 2021-01-29 | 2022-12-13 | 湖南邦普循环科技有限公司 | Method for separating nickel and iron from nickel-iron alloy and application |
| CN113073204B (en) * | 2021-03-31 | 2023-02-10 | 江西省江铜百泰环保科技有限公司 | Method for recovering copper from low-concentration acidic wastewater |
| CN113106259A (en) * | 2021-04-30 | 2021-07-13 | 佛山经纬纳科环境科技有限公司 | Method for selectively recovering copper from copper-containing sludge by hydrothermal mineralization method |
| CN114772628B (en) * | 2022-04-22 | 2024-02-06 | 盛隆资源再生（无锡）有限公司 | Recovery method of waste etching liquid |
| CN115386730B (en) * | 2022-08-29 | 2023-10-20 | 广东飞南资源利用股份有限公司 | Method for recycling copper and nickel from copper and nickel-containing sludge |
| CN117566978B (en) * | 2024-01-15 | 2024-03-29 | 惠州金茂源环保科技有限公司 | Sludge heavy metal recycling extraction method and system |
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| CN103966446A (en) * | 2014-05-08 | 2014-08-06 | 南京大学 | Method for separating and recovering copper, nickel and iron from electroplating sludge |
| CN106244811B (en) * | 2016-08-24 | 2018-04-06 | 盛隆资源再生（无锡）有限公司 | A kind of recoverying and utilizing method for the electroplating sludge that copper and iron content is low, tin nickel content is high |
| CN106521166B (en) * | 2016-11-29 | 2018-09-18 | 湖南埃格环保科技有限公司 | A method of preparing copper powder and ferrous sulfate using copper-contained sludge wet-leaching solution |
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