CN107354488A - Treatment method of final copper-removing solution - Google Patents
Treatment method of final copper-removing solution Download PDFInfo
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- CN107354488A CN107354488A CN201710369838.1A CN201710369838A CN107354488A CN 107354488 A CN107354488 A CN 107354488A CN 201710369838 A CN201710369838 A CN 201710369838A CN 107354488 A CN107354488 A CN 107354488A
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- nickel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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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
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for treating a final copper-removing solution, which adopts oxalic acid as a nickel-precipitating agent of a raw material of the final copper-removing solution, and the specific process is that the oxalic acid is added into the final copper-removing solution purified by copper electrolyte, wherein the final copper-removing solution comprises the following main components in percentage by weight: 10-30g/L of nickel, 0.1-0.6 g/L of copper and 130-400g/L of free acid, wherein the nickel precipitation reagent is combined with nickel ions in the final decoppering solution through heating and stirring reaction to form nickel oxalate precipitation insoluble in dilute sulfuric acid, the nickel oxalate precipitation with the nickel content of 20-40% is obtained through filtration, and meanwhile, a dilute sulfuric acid solution without foreign impurities is obtained, wherein the acid concentration of the dilute sulfuric acid solution is equivalent to that of the free acid in the initial copper electrolysis solution, and the dilute sulfuric acid solution can be directly returned to a copper electrolysis system for recycling.
Description
Technical field
The present invention relates to metallurgical waste water recycling field, and in particular to one kind is whole with heavy nickel chemicals treatment decopper(ing)
The method that liquid and recovery prepare nickel salt and dilution heat of sulfuric acid.
Background technology
Decopper(ing) end liquid is during cupric electrolysis produces tough cathode, and the partial electrolyte stoste distributed is by purification dearsenification antimony
The solution obtained after bismuth, electrodeposition decopper(ing), the typically nickeliferous 10-30g/L of the solution, copper 0.1-0.6 g/L, free acid 130-400g/
L.Such as certain Tong Ye companies potroom needs decopper(ing) end liquid about 8000m3 to be processed every year, its decopper(ing) end liquid composition complete analysis
Average content（Unit g/L）For：Cu 0.38, Pb 0.0065, Zn 1.12, Fe 1.12, Sb 0.077, Bi 0.095, Ni
20.28, As 0.74, H2SO4263.84.Due to the nickel ion containing excess in the decopper(ing) end liquid liquid, followed if directly returning to electrolysis
Ring use can influence the quality of tough cathode, therefore the solution generally requires and carries out nickel removal processing, makes the nickel in decopper(ing) end liquid dense
Degree drops to below 10g/L, to meet electrolyte configuration requirement.
The method of prior art processing decopper(ing) end liquid is evaporation concentration method mostly, i.e., by 40 DEG C of left sides by the way of electricity evaporates
Right decopper(ing) end liquid is heated to 170 DEG C, and decopper(ing) end liquid is concentrated into 1100g/L containing acid, makes the solubility of nickel sulfate reduce, and analyses
Go out to obtain unformed nickel sulfate.This method typically needs to be electrolysed because the electric evaporization process power consumption for producing crude nickle sulphate is larger
In liquid nickel content reach capacity concentration when, inborn ability stream part decopper(ing) end liquid carry out nickel removal processing.Its production technology is certain to extract
The decopper(ing) end liquid of volume is pumped up to head tank, enters electric heating concentration tank, the control of electrical heating evaporating temperature by head tank continuous self-flowing
At 170 DEG C or so, solution about 1100g/L containing acid after evaporation, water cooling crystallization tank is flowed into by closed overflow connecting tube, through supercooling
But, the process operations such as crystallization, filtering, separation, finally give crude nickle sulphate product.It is big to there is power consumption in actual production
（Power consumption reaches 32000kwh/t during heating）, situations such as temperature operation is whard to control in evaporator, cause that production cost is high, equipment
Corrode heavier, energy resource consumption is higher, environmental pollution is larger, financial cost is higher, production efficiency is low, nickel sulfate output capacity is low etc.
Problem.
The content of the invention
The problem of present invention exists for prior art, there is provided one kind is with heavy nickel chemicals treatment decopper(ing) end liquid and reclaims preparation
The method of nickel salt and dilution heat of sulfuric acid, solve the problems, such as decopper(ing) end liquid recycling, and nickel ion content can be obtained and existed
Below 10g/L meets the dilution heat of sulfuric acid of electrolyte configuration requirement, while the nickeliferous nickel salt product up to 20-40% is prepared.
To meet above-mentioned purpose, the technical solution used in the present invention is：
A kind of processing method of decopper(ing) end liquid, using heavy nickel medicament of the oxalic acid as decopper(ing) end liquid raw material, concrete technology is by grass
Acid is added in the decopper(ing) end liquid after cleaning copper electrolyte, and the Contents of Main Components of wherein decopper(ing) end liquid is：Nickel 10-30g/L, copper
0.1-0.6 g/L, free acid 130-400g/L, heated stirring reaction make heavy nickel reagent be combined with the nickel ion in decopper(ing) end liquid
The oxalic acid nickel salt precipitation insoluble in dilute sulfuric acid is formed, is precipitated by being filtrated to get the oxalic acid nickel salt that nickel content is 20-40%, and together
When do not brought into the dilution heat of sulfuric acid of exogenous impurity, the wherein acid concentration of dilution heat of sulfuric acid is dissociated with cupric electrolysis initial soln
Acid concentration is suitable, can directly return to copper electrolysis system recycling.
Preferably, methods described comprises the following steps that：
（1）Experiment raw material：
Decopper(ing) end liquid is acid nickel sulfate solution of the copper electrolyte after electrodeposition decopper(ing), and its Contents of Main Components is：Nickel 10-
30g/L, copper 0.1-0.6 g/L, free acid 130-400g/L；
Oxalic acid；
Polyacrylamide flocculant；
（2）Specific steps：
A, decopper(ing) end liquid is added in acid tolerance response container, solution temperature is maintained at 20-100 DEG C；
B, oxalic acid is added in above-mentioned solution, oxalic acid addition is every liter of decopper(ing) end liquid 20-60g, is then stirred, stir speed (S.S.) is
120-180r/min, stirring reaction 1-4h, make dissolving oxalic acid and generate nickel oxalate with the nickel ion reaction of solution；
C, when temperature is 20-60 DEG C, the polyacrylamide flocculant that mass concentration is 1-2%, polyacrylamide flocculant are added
Dosage is 0.1-50mg/L, and stirring reaction 0.1-1h makes it well mixed, then stands 10-36h, nickel oxalate sediment is sunk
Drop is complete；
D, above-mentioned reaction solution is separated by filtration, sediment rinsing, the oxalic acid nickel salt that drying to obtain nickel content is 20-40%, mistake
Solution after filter is dilution heat of sulfuric acid, and obtained dilution heat of sulfuric acid Contents of Main Components is：Cu≤0.2g/L, Pb≤0.003g/
L, Zn≤0.02g/L, Fe≤0.05g/L, Sb≤0.055g/L, Bi≤0.08g/L, Ni≤8g/L, As≤0.8g/L, H2SO4：
130-400g/L, the solution does not bring exogenous impurity into, and acid concentration is suitable with free acid concentration in cupric electrolysis initial soln, can be straight
Connect and return to copper electrolysis system recycling.
Preferably, the oxalic acid is anhydrous oxalic acid（Molecular formula is H2C2O4）Powder or two oxalic acid hydrates（Molecular formula is
H2C2O4•2H2O）Crystallization.
Beneficial effects of the present invention are：Pass through oxalic acid treatment decopper(ing) end liquid, i.e. acid of the copper electrolyte after electrodeposition decopper(ing)
Property nickel sulfate solution, the removal efficiency of nickel reaches more than 60% in processed decopper(ing) end liquid, the technique letter of its oxalic acid treatment decopper(ing) end liquid
It is single, decopper(ing) end liquid Feedstock treating can be greatly lowered and reclaim the cost of nickel, three wastes produce；Dilution heat of sulfuric acid after processing
The content of exogenous impurity and nickel is not brought into 10 below g/L, and acid concentration is the same as free acid concentration phase in cupric electrolysis initial soln
When, can directly return copper electrolysis system recycling, to industrial wastewater recycling, save the energy, effectively prevent pollution have
It is of great importance.
Embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1：
（1）Raw material：Heavy nickel medicament used is anhydrous oxalic acid reagent.Decopper(ing) end liquid used is derived from silver Nonferrous Metals Group company copper
The decopper(ing) end liquid of industry company scene output, its Contents of Main Components（g/L）：Cu ：0.38, Pb：0.0065, Zn：1.12 Fe：
1.12 Sb：0.077, Bi：0.095, Ni：20.28 As：0.74, H2SO4：263.84.
（2）Implementation：Decopper(ing) end liquid 100ml is taken to be put into beaker, reinforcing body oxalic acid powder 5g is then molten by 20 DEG C
Liquid is heated to 70 DEG C and is stirred, stir speed (S.S.) 130r/min, insulation reaction 1h, is then cooled to 60 DEG C, adds quality
Concentration is 1% polyacrylamide flocculant, and polyacrylamide flocculant dosage is 2mg, continues to stir 0.1h, makes its mixing
Uniformly, 15h is then stood, makes the sedimentation of nickel oxalate sediment complete, is then again separated by filtration solution.Sediment is through rinsing, doing
Dry to obtain nickel oxalate salt 4.3g, the solution after filtering is dilution heat of sulfuric acid 115ml.
（3）Result of the test：Through sample presentation assay, the solid oxalic acid nickel of gained is nickeliferous 29.6%, copper 0.04%.Gained it is dilute
Sulfuric acid solution main component is（g/L）：Cu：0.02, Pb：0.0020, Zn：0.013, Fe：0.045, Sb：0.050, Bi：
0.070, Ni：4.88 As：0.60, H2SO4：285.21.The removal efficiency of nickel is 74.73% in processed solution.
Embodiment 2：
（1）Raw material：Heavy nickel medicament used is two oxalic acid hydrate reagents.Decopper(ing) end liquid used is derived from silver Nonferrous Metals Group company
Tong Ye companies, its Contents of Main Components is the same as embodiment 1.
（2）Implementation：Above-mentioned decopper(ing) end liquid 600ml is taken to be put into beaker, the oxalic acid hydrate powder 24.0g of reinforcing body two,
Then 20 DEG C of solution is heated 60 DEG C and stirred, stir speed (S.S.) 150r/min, insulation reaction 2h, be then cooled to 50 DEG C,
The polyacrylamide flocculant that mass concentration is 2% is added, polyacrylamide flocculant dosage is 3mg, continues to stir 0.1h,
Make it well mixed, then stand 18h, make the sedimentation of nickel oxalate sediment complete, be then again separated by filtration solution.Sediment passes through
Rinsing, drying to obtain solid oxalic acid nickel by powder 28.65g, the solution after filtering is dilution heat of sulfuric acid 615ml.
（3）Result of the test：Through sample presentation assay, the solid oxalic acid nickel of gained is nickeliferous 28.65%, copper 0.25%.Gained
Dilution heat of sulfuric acid main component is（g/L）：Cu：0.19, Pb：0.0022, Zn：0.014, Fe：0.049, Sb：0.053, Bi：
0.075, Ni：6.37 As：0.68, H2SO4：271.68.The removal efficiency of nickel is 67.8% in processed solution.
Embodiment 3
（1）Raw material：Heavy nickel medicament used is oxalic acid reagent.Decopper(ing) end liquid used is the solution after the dilution of embodiment 1, its
Contents of Main Components is：Ni 10g/L, Cu 0.15 g/L, the g/L of free acid 130.
（2）Implementation：Decopper(ing) end liquid 100ml is taken to be put into beaker, reinforcing body oxalic acid powder 2.0g, then by 20 DEG C
Solution is heated to 80 DEG C and stirred, stir speed (S.S.) 150r/min, insulation reaction 3h, is then cooled to 40 DEG C, and it is dense to add quality
The polyacrylamide flocculant for 1% is spent, polyacrylamide flocculant dosage is 10mg, continues to stir 0.1h, makes its mixing equal
It is even, 18h is then stood, makes the sedimentation of nickel oxalate sediment complete, is then again separated by filtration solution.Sediment is through rinsing, drying
Nickel oxalate salt 1.8g is obtained, the solution after filtering is dilution heat of sulfuric acid 110ml.
（3）Result of the test：Through sample presentation assay, the solid oxalic acid nickel of gained is nickeliferous 34%, copper 0.02%.Dilute sulphur of gained
Acid solution main component is（g/L）：Cu：0.015, Pb：0.0018, Zn：0.012, Fe：0.044, Sb：0.049, Bi：0.073,
Ni：3.5, As：0.67, H2SO4：283.51.The removal efficiency of nickel is 61.5% in processed solution.
Embodiment 4
（1）Raw material：Heavy nickel medicament used is oxalic acid reagent.Decopper(ing) end liquid used is the solution after the concentration of embodiment 1, its
Contents of Main Components is：Ni 30g/L, Cu 0.6 g/L, free acid 395g/L.
（2）Implementation：Take decopper(ing) end liquid 100ml to be put into beaker, the oxalic acid hydrate powder 6.0g of reinforcing body two, then will
20 DEG C of solution is heated to 80 DEG C and stirred, stir speed (S.S.) 150r/min, insulation reaction 3h, is then cooled to 40 DEG C, adds
Mass concentration is 1% polyacrylamide flocculant, and polyacrylamide flocculant dosage is 10mg, continues to stir 1h, makes it mixed
Close uniformly, then stand 20h, make the sedimentation of nickel oxalate sediment complete, be then again separated by filtration solution.Sediment through rinsing,
Drying to obtain oxalic acid nickel salt 4.5g, the solution after filtering are dilution heat of sulfuric acid 110ml.
（3）Result of the test：Through sample presentation assay, the solid oxalic acid nickel of gained is nickeliferous 38.3%, copper 0.04%.Gained it is dilute
Sulfuric acid solution main component is（g/L）：Cu：0.016, Pb：0.0021, Zn：0.011, Fe：0.047, Sb：0.051, Bi：
0.074, Ni：7.5, As：0.61, H2SO4：275.69.The removal efficiency of nickel is 72.5% in processed solution.
Claims (3)
- A kind of 1. processing method of decopper(ing) end liquid, it is characterised in that：Using heavy nickel medicament of the oxalic acid as decopper(ing) end liquid raw material, tool To be added to oxalic acid in the decopper(ing) end liquid after cleaning copper electrolyte, the Contents of Main Components of wherein decopper(ing) end liquid is body technology： Nickel 10-30g/L, copper 0.1-0.6 g/L, free acid 130-400g/L, heated stirring reaction make heavy nickel reagent and decopper(ing) end liquid In nickel ion combine to form insoluble in dilute sulfuric acid oxalic acid nickel salt precipitation, by be filtrated to get nickel content be 20-40% oxalic acid Nickel salt precipitates, and is not brought into the dilution heat of sulfuric acid of exogenous impurity simultaneously, the same cupric electrolysis of acid concentration of wherein dilution heat of sulfuric acid Free acid concentration is suitable in initial soln, can directly return to copper electrolysis system recycling.
- 2. the processing method of a kind of decopper(ing) end liquid according to claim 1, it is characterised in that comprise the following steps that：（1）Experiment raw material：Decopper(ing) end liquid is acid nickel sulfate solution of the copper electrolyte after electrodeposition decopper(ing), and its Contents of Main Components is：Nickel 10- 30g/L, copper 0.1-0.6 g/L, free acid 130-400g/L；Oxalic acid；Polyacrylamide flocculant；（2）Specific steps：A, decopper(ing) end liquid is added in acid tolerance response container, solution temperature is maintained at 20-100 DEG C；B, oxalic acid is added in above-mentioned solution, oxalic acid addition is every liter of decopper(ing) end liquid 20-60g, is then stirred, stir speed (S.S.) is 120-180r/min, stirring reaction 1-4h, make dissolving oxalic acid and generate nickel oxalate with the nickel ion reaction of solution；C, when temperature is 20-60 DEG C, the polyacrylamide flocculant that mass concentration is 1-2%, polyacrylamide flocculant are added Dosage is 0.1-50mg/L, and stirring reaction 0.1-1h makes it well mixed, then stands 10-36h, nickel oxalate sediment is sunk Drop is complete；D, above-mentioned reaction solution is separated by filtration, sediment rinsing, the oxalic acid nickel salt that drying to obtain nickel content is 20-40%, mistake Solution after filter is dilution heat of sulfuric acid, and obtained dilution heat of sulfuric acid Contents of Main Components is：Cu≤0.2g/L, Pb≤0.003g/ L, Zn≤0.02g/L, Fe≤0.05g/L, Sb≤0.055g/L, Bi≤0.08g/L, Ni≤8g/L, As≤0.8g/L, H2SO4： 130-400g/L, the solution does not bring exogenous impurity into, and acid concentration is suitable with free acid concentration in cupric electrolysis initial soln, can be straight Connect and return to copper electrolysis system recycling.
- A kind of 3. processing method of decopper(ing) end liquid according to claim 1 or 2, it is characterised in that：The oxalic acid is anhydrous Oxalic acid powder or the crystallization of two oxalic acid hydrates.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710369838.1A CN107354488A (en) | 2017-05-23 | 2017-05-23 | Treatment method of final copper-removing solution |
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| CN201710369838.1A CN107354488A (en) | 2017-05-23 | 2017-05-23 | Treatment method of final copper-removing solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453225A (en) * | 2019-08-29 | 2019-11-15 | 深圳市祺鑫天正环保科技有限公司 | The processing method of acidic etching waste liquid |
| CN112030195A (en) * | 2020-09-02 | 2020-12-04 | 湖南工程学院 | Process for deeply removing oxalic acid |
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| CN101837464A (en) * | 2009-08-28 | 2010-09-22 | 上海九鼎粉体材料有限公司 | Metal nickel powder and preparation method thereof |
| CN105523621A (en) * | 2016-01-29 | 2016-04-27 | 中南大学 | Method for improving sludge settling property in copper-containing wastewater treatment process |
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2017
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837464A (en) * | 2009-08-28 | 2010-09-22 | 上海九鼎粉体材料有限公司 | Metal nickel powder and preparation method thereof |
| CN105523621A (en) * | 2016-01-29 | 2016-04-27 | 中南大学 | Method for improving sludge settling property in copper-containing wastewater treatment process |
Non-Patent Citations (2)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453225A (en) * | 2019-08-29 | 2019-11-15 | 深圳市祺鑫天正环保科技有限公司 | The processing method of acidic etching waste liquid |
| CN110453225B (en) * | 2019-08-29 | 2021-07-30 | 深圳市祺鑫环保科技有限公司 | Method for treating acidic waste etching solution |
| CN112030195A (en) * | 2020-09-02 | 2020-12-04 | 湖南工程学院 | Process for deeply removing oxalic acid |
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Application publication date: 20171117 |