CN108570559A - A method of the depth vulcanization separation cupro-nickel arsenic from high acid solution - Google Patents
A method of the depth vulcanization separation cupro-nickel arsenic from high acid solution Download PDFInfo
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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
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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
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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Abstract
A kind of method of the present invention depth from high acid solution vulcanization separation cupro-nickel arsenic, this method flow detach arsenic, copper, nickel in high acid solution, preferably realizes copper, arsenic, nickel and efficiently separates.The beneficial effects of the present invention are：The new process is by repeatedly vulcanizing decopper(ing), dearsenification, it is with obvious effects, 2 vulcanizations of peracid, it obtains the low pozzuolite copper ashes of high-copper and returns copper production system, it obtains low copper arsenic filter cake and returns white arsenic production system recycling arsenic, the effective inefficient cycle for overcoming copper arsenic, copper, arsenic gets utilization, oxidation pre-treatment is carried out to liquid after vulcanization and avoids the problem of membrane diffusion blocks up film, diffusion recovery acid can return the leaching of black copper mud, recycle nickel and acid therein, spread raffinate reduces containing acid, vulcanize conducive to depth again, overcome the extreme enrichment of sodium ion in N-process, problem is lost in the mechanical entrapment of nickel, final rich nickel liquid is obtained since cupric arsenic is low, recycling nickel cost substantially reduces, since not new solid waste generates, economic benefit and social benefit are apparent.
Description
Technical field
The method of depth that the present invention relates to a kind of from high acid solution vulcanization separation cupro-nickel arsenic, especially adapt to from containing peracid,
The method that copper, nickel, arsenic are detached in the nickeliferous solution of high arsenic, high-copper, entire process resource maximize the use, and vulcanization obtains high-copper
Low arsenic slag returns copper production system, vulcanizes low copper arsenic filter cake production white arsenic, and the acid and nickel spread in recovery acid is recycled utilization, expands
It dissipates raffinate and is conducive to production nickel series of products in next step.
Background technology
Currently, copper waste electrolyte needs open a way processing decopper(ing), arsenic, acid both at home and abroad, while maximal efficiency improves the recycling of nickel
No matter rate, tradition removing arsenic, copper method use substep electrodeposition or directly vulcanization to neutralize, and consumption alkali is high, and obtained copper arsenic slag is tight with nickel
Heavy less than enrichment is efficiently separated, the loss of nickel is big, is directly diffused dialysis, and recovery acid is unfavorable for returning and is since copper arsenic is high
System uses.
Existing recycling nickel method major defect：Diffusion raffinate directly neutralizes sodium ion and is extremely enriched with, copper arsenic Copper in Slag arsenic
It is close, it is unfavorable for recycling copper and arsenic, needs repeatedly decopper(ing), dearsenification, cause inefficient cycle, and be not thorough, as extraction nickel
Raw material, long flow path, alkaline consumption is big, complex procedures, and the rate of recovery of nickel is had a greatly reduced quality.
How alkaline consumption is reduced, obtains low arsenic, the low high-quality nickel bearing raw material of copper high-grade, while reducing the machinery of intermediate material nickel
Be lost it is significant, reduce wastewater treatment capacity, greatly improve the rate of recovery of nickel.
Invention content
A kind of purpose of the method for the vulcanization of the depth from high acid solution separation cupro-nickel arsenic of the present invention is for electrolysis or thick sulphur
In sour copper production process, exist recycling nickel during, separate open high concentration copper, arsenic, acid problem, in certain peracid condition
Preferential 2 vulcanization substeps decopper(ing), dearsenification down, 2 times rich nickel liquid carries out membrane diffusion again after peroxidating, and recovery acid can return black copper
Mud leaching system is solved the problems, such as that the loss of membrane diffusion part of nickel and direct neutralizing acid are returned and is interfered using sodium ion, spread
After raffinate revulcanization, copper arsenic removes ratio more thoroughly, and rich nickel scavenging solution can be used as the quality raw materials of extraction nickel product.
To achieve the above object, the present invention takes following technical scheme：One kind depth vulcanization separation copper from high acid solution
The method of nickel arsenic, this method specifically include following steps：
Step 1：Depth concentration is carried out from high acid solution by pending, thick copper sulphate is obtained and returns copper production system, crystallized
Mother liquor；
Step 2：The crystalline mother solution that obtains handled by step 1 is subjected to 1 vulcanization decopper(ing), 1 time obtained vulcanization decopper(ing) richness nickel
Liquid；
Step 3：The 1 vulcanization decopper(ing) richness nickel liquid that step 2 processing obtains is subjected to 2 vulcanization dearsenifications：Obtain 2 rich nickel liquid raffinates
With low copper arsenic filter cake, obtained low copper arsenic filter cake returns white arsenic production system；
Step 4：By obtained after step process 2 rich nickel liquid raffinates, oxidation reaction is carried out to 2 rich nickel liquid raffinates, is obtained
To oxidation solution return membrane diffusion system；
Step 5：Aoxidize Liquid film diffusion：Membrane diffusion is carried out to the oxidation solution that step 4 obtains, obtained low nickel recovery acid returns black copper
Mud leaching system, diffusion raffinate send 3 depth vulcanization removing impurities in next step；
Step 6：Spread 3 case depth removing impurities of raffinate：To the diffusion raffinate auto-vulcanization depth decopper(ing) arsenic that step 5 obtains, stir
It mixes 2 hours, obtained vulcanized slag returns white arsenic production system, quality raw materials of the scavenging solution as extraction nickel.
Further, the high acid solution in the step 1 is containing liquid, black copper in being restored for waste electrolyte concentrate, arsenious acid
Mud or thick cupric sulphate crystal mother liquor.
Further, 1 vulcanization is carried out to condensing crystallizing mother liquor in the step 2：According to generation copper sulfide theoretical amount
1-3 times of sulphur mole carries out.
Further, liquid carries out 2 vulcanization dearsenifications after 1 vulcanization in the step 3：According to the 1- for generating arsenones theoretical amount
5 times of sulphur moles carry out, and copper is further vulcanized.
Further, in the step 4 oxidant of oxidation reaction addition, according to amount of solution weight ratio be added 0.1-
3%, the oxidant is at least one of hydrogen peroxide, potassium permanganate, sodium chlorate, sodium hypochlorite or ferric trichloride；
Further, oxidated solution is diffused dialysis depickling in the step 5：It is diffused and oozes according to water/feed liquid 1.1-1.5/1
Analysis, acid recovering rate are more than 80%, and diffusion raffinate is conducive to production nickel series of products in next step, and recovery acid cupric arsenic is relatively low, recovery acid
Black copper mud leaching acid is returned, wherein nickel is further recycled.
Further, in the step 6, raffinate is spread to rich nickel, is carried out 3 times（2.8 times of sulphur/arsenic mole=theoretical amount）Vulcanization,
Temperature control room temperature, obtain 3 vulcanized slags and return arsenic production system, wherein cupric 3.25%, contain arsenic 8.91%, nickeliferous 0.67%, return arsenic
Production system, 3 rich nickel liquid 0.001g/L containing arsenic, cupric 0.001g/L, 25.73 g/L containing acid, nickeliferous 50.89g/L send next
Walk nickel product abstraction process.
The beneficial effects of the invention are as follows：This method obtains low ambrose alloy slag and returns copper into 1 vulcanization decopper(ing), 2 vulcanization dearsenifications is crossed
Production system obtains arsenic filter cake and returns white arsenic production system, and copper arsenic resource obtains maximum reasonable, acid is recycled using membrane diffusion,
Since cupric, arsenic, sodium are low, black copper mud can be returned and leach recovery acid and part of nickel；
A kind of method that the vulcanization of the depth from high acid solution detaches copper, nickel, arsenic as described above, by membrane diffusion raffinate depth sulphur
Change, copper arsenic is thoroughly removed, and obtained rich nickel solution can be used as the quality raw materials of production nickel product.
Nickel detaches more thoroughly with copper arsenic, and resource obtains maximum reasonable utilization, non-secondary pollution.
Description of the drawings
Fig. 1 is a kind of flow chart of the method for the vulcanization of the depth from high acid solution separation cupro-nickel arsenic of the present invention.
Specific implementation mode
Technical scheme of the present invention is described further below in conjunction with the accompanying drawings.
As shown in Figure 1, a kind of method of the vulcanization of the depth from high acid solution separation cupro-nickel arsenic of the present invention, this method are specifically wrapped
Include following steps：
Step 1：Depth concentration is carried out from high acid solution by pending, thick copper sulphate is obtained and returns copper production system, crystallized
Mother liquor；
Step 2：The crystalline mother solution that obtains handled by step 1 is subjected to 1 vulcanization decopper(ing), 1 time obtained vulcanization decopper(ing) richness nickel
Liquid；
Step 3：The 1 vulcanization decopper(ing) richness nickel liquid that step 2 processing obtains is subjected to 2 vulcanization dearsenifications：Obtain 2 rich nickel liquid raffinates
With low copper arsenic filter cake, obtained low copper arsenic filter cake returns white arsenic production system；
Step 4：By obtained after step process 2 rich nickel liquid raffinates, oxidation reaction is carried out to 2 rich nickel liquid raffinates, is obtained
To oxidation solution return membrane diffusion system；
Step 5：Aoxidize Liquid film diffusion：Membrane diffusion is carried out to the oxidation solution that step 4 obtains, obtained low nickel recovery acid returns black copper
Mud leaching system, diffusion raffinate send 3 depth vulcanization removing impurities in next step；
Step 6：Spread 3 case depth removing impurities of raffinate：To the diffusion raffinate auto-vulcanization depth decopper(ing) arsenic that step 5 obtains, stir
It mixes 2 hours, obtained vulcanized slag returns white arsenic production system, quality raw materials of the scavenging solution as extraction nickel.
Further, the high acid solution in the step 1 is containing liquid, black copper in being restored for waste electrolyte concentrate, arsenious acid
Mud or thick cupric sulphate crystal mother liquor.
Further, 1 vulcanization is carried out to condensing crystallizing mother liquor in the step 2：According to generation copper sulfide theoretical amount
1-3 times of sulphur mole carries out.
Further, liquid carries out 2 vulcanization dearsenifications after 1 vulcanization in the step 3：According to the 1- for generating arsenones theoretical amount
5 times of sulphur moles carry out, and copper is further vulcanized.
Further, in the step 4 oxidant of oxidation reaction addition, according to amount of solution weight ratio be added 0.1-
3%, the oxidant is at least one of hydrogen peroxide, potassium permanganate, sodium chlorate, sodium hypochlorite or ferric trichloride；
Further, oxidated solution is diffused dialysis depickling in the step 5：It is diffused and oozes according to water/feed liquid 1.1-1.5/1
Analysis, acid recovering rate are more than 80%, and diffusion raffinate is conducive to production nickel series of products in next step, and recovery acid cupric arsenic is relatively low, recovery acid
Black copper mud leaching acid is returned, wherein nickel is further recycled.
Further, in the step 6, raffinate is spread to rich nickel, is carried out 3 times（2.8 times of sulphur/arsenic mole=theoretical amount）Vulcanization,
Temperature control room temperature, obtain 3 vulcanized slags and return arsenic production system, wherein cupric 3.25%, contain arsenic 8.91%, nickeliferous 0.67%, return arsenic
Production system, 3 rich nickel liquid 0.001g/L containing arsenic, cupric 0.001g/L, 25.73 g/L containing acid, nickeliferous 50.89g/L send next
Walk nickel product abstraction process.
Embodiment 1：
A method of the depth vulcanization separation cupro-nickel arsenic from high acid solution,
Liquid 39.67g/L containing arsenic, cupric 28.43g/L in taking 200L arsenious acid to restore, 180 .89g/L, nickeliferous 25.23g/L containing acid
Solution carries out depth concentration, obtains thick copper sulphate and returns copper sulphate production system, crystalline mother solution 119.67g/L containing arsenic, cupric
34.43g/L, 380 .89g/L containing acid, nickeliferous 65.23g/L crystalline mother solutions carry out 1 time（2.3 times of sulphur/copper mole=theoretical amount）Sulphur
To change, temperature controls room temperature, vulcanizes Copper in Slag 48.25%, contains arsenic 9.11%, and nickeliferous 2.79%, return copper production system, liquid after 1 vulcanization
65.29g/L containing arsenic, cupric 3.43g/L are obtained, the 1 rich nickel liquid of 278.56 g/L containing acid, nickeliferous 60.72g/L.
The new method carries out 2 vulcanizations to 48L1 rich nickel liquid（3.4 times of sulphur/arsenic mole=theoretical amount）Vulcanize dearsenification,
Temperature controls room temperature, obtains 2 low copper vulcanization arsenic filter cakes, wherein cupric 2.25%, contains arsenic 58.91%, and nickeliferous 1.93%, return white arsenic
Production system, 2 rich nickel liquid 4.38g/L containing arsenic, cupric 0.53g/L, 246.36 g/L containing acid, nickeliferous 56.65g/L are sent in next step
Carry out oxidation processes.
45L vulcanization dearsenification liquid is aoxidized, adds 1% weight ratio hydrogen peroxide, stirring at normal temperature aoxidizes 2 hours, spare.
Membrane diffusion is carried out after being diluted to oxidation solution, is carried out according to water/feed liquid=1.1/1, acid is recycled and returns the processing of black copper mud
System, rich nickel spread raffinate, 2.68g/L containing arsenic, cupric 0.37g/L, and 36.36 g/L containing acid, nickeliferous 51.54g/L are sent in next step
Carry out 3 case depth dearsenifications, decopper(ing)s.
Raffinate is spread to rich nickel, is carried out 3 times（2.8 times of sulphur/arsenic mole=theoretical amount）Vulcanization, temperature control room temperature, obtain 3
Secondary vulcanized slag returns arsenic production system, wherein cupric 3.25%, contains arsenic 8.91%, and nickeliferous 0.67%, return arsenic production system, 3 rich nickel liquid
0.001g/L containing arsenic, cupric 0.001g/L, 25.73 g/L containing acid, nickeliferous 50.89g/L send next step nickel product abstraction process.
Embodiment 2：
A method of the depth vulcanization separation cupro-nickel arsenic from high acid solution,
Take black copper mud 39.67g/L containing arsenic, the cupric 28.43g/L of 200L, 180 .89g/L containing acid, nickeliferous 25.23g/L solution into
Row depth concentrates, and obtains thick copper sulphate and returns copper sulphate production system, crystalline mother solution 119.67g/L containing arsenic, cupric 34.43g/L contains
380 .89g/L of acid, nickeliferous 65.23g/L crystalline mother solutions carry out 1 time（2.3 times of sulphur/copper mole=theoretical amount）Vulcanization, temperature control
Room temperature vulcanizes Copper in Slag 48.25%, contains arsenic 9.11%, and nickeliferous 2.79%, return copper production system, liquid obtains containing arsenic after 1 vulcanization
65.29g/L, cupric 3.43g/L, the 1 rich nickel liquid of 278.56 g/L containing acid, nickeliferous 60.72g/L.
2 vulcanizations are carried out to 48L1 rich nickel liquid（3.4 times of sulphur/arsenic mole=theoretical amount）Vulcanize dearsenification, temperature control is normal
Temperature obtains 2 low copper vulcanization arsenic filter cakes, wherein cupric 2.25%, contains arsenic 58.91%, and nickeliferous 1.93%, return white arsenic production system, 2
Secondary richness nickel liquid 4.38g/L containing arsenic, cupric 0.53g/L, 246.36 g/L containing acid, nickeliferous 56.65g/L are sent to carry out at oxidation in next step
Reason.
45L vulcanization dearsenification liquid is aoxidized, adds 1% weight ratio hydrogen peroxide, stirring at normal temperature aoxidizes 2 hours, spare.
Membrane diffusion is carried out after being diluted to oxidation solution, is carried out according to water/feed liquid=1.1/1, acid is recycled and returns the processing of black copper mud
System, rich nickel spread raffinate, 2.68g/L containing arsenic, cupric 0.37g/L, and 36.36 g/L containing acid, nickeliferous 51.54g/L are sent in next step
Carry out 3 case depth dearsenifications, decopper(ing)s.
Raffinate is spread to rich nickel, is carried out 3 times（2.8 times of sulphur/arsenic mole=theoretical amount）Vulcanization, temperature control room temperature, obtain 3
Secondary vulcanized slag returns arsenic production system, wherein cupric 3.25%, contains arsenic 8.91%, and nickeliferous 0.67%, return arsenic production system, 3 rich nickel liquid
0.001g/L containing arsenic, cupric 0.001g/L, 25.73 g/L containing acid, nickeliferous 50.89g/L send next step nickel product abstraction process.
One embodiment of the present invention has been described in detail above, it but is not meant to the scope of the present invention
Limitation, content is only the preferred embodiment of the present invention, should not be construed as limiting the practical range of the present invention.Fan Yiben
All the changes and improvements etc. made by patent application range, should all still fall within the scope of the patent of the present invention.
Claims (7)
1. a kind of method of the vulcanization of the depth from high acid solution separation cupro-nickel arsenic, which is characterized in that this method specifically includes following
Step：
Step 1：Depth concentration is carried out from high acid solution by pending, thick copper sulphate is obtained and returns copper production system, crystallized
Mother liquor；
Step 2：The crystalline mother solution that obtains handled by step 1 is subjected to 1 vulcanization decopper(ing), 1 time obtained vulcanization decopper(ing) richness nickel
Liquid；
Step 3：The 1 vulcanization decopper(ing) richness nickel liquid that step 2 processing obtains is subjected to 2 vulcanization dearsenifications：Obtain 2 rich nickel liquid raffinates
With low copper arsenic filter cake, obtained low copper arsenic filter cake returns white arsenic production system；
Step 4：By obtained after step process 2 rich nickel liquid raffinates, oxidation reaction is carried out to 2 rich nickel liquid raffinates, is obtained
To oxidation solution return membrane diffusion system；
Step 5：Aoxidize Liquid film diffusion：Membrane diffusion is carried out to the oxidation solution that step 4 obtains, obtained low nickel recovery acid returns black copper
Mud leaching system, diffusion raffinate send 3 depth vulcanization removing impurities in next step；
Step 6：Spread 3 case depth removing impurities of raffinate：To the diffusion raffinate auto-vulcanization depth decopper(ing) arsenic that step 5 obtains, stir
It mixes 2 hours, obtained vulcanized slag returns white arsenic production system, quality raw materials of the scavenging solution as extraction nickel.
2. according to the method described in claim 1, it is characterized in that, the high acid solution in the step 1 concentrates for waste electrolyte
Liquid, black copper mud or thick cupric sulphate crystal mother liquor in liquid, arsenious acid reduction.
3. according to the method described in claim 1, it is characterized in that, carrying out 1 sulphur to condensing crystallizing mother liquor in the step 2
Change：It is carried out according to 1-3 times of sulphur mole for generating copper sulfide theoretical amount.
4. according to the method described in claim 1, it is characterized in that, 2 vulcanizations of liquid progress are de- after 1 vulcanization in the step 3
Arsenic：It is carried out according to 1-5 times of sulphur mole for generating arsenones theoretical amount, copper is further vulcanized.
5. according to the method described in claim 1, it is characterized in that, in the step 4 oxidant of oxidation reaction addition,
0.1-3% is added according to the weight ratio of amount of solution, the oxidant is hydrogen peroxide, potassium permanganate, sodium chlorate, sodium hypochlorite or three
At least one of iron chloride.
6. according to the method described in claim 1, it is characterized in that, oxidated solution is diffused dialysis depickling in the step 5：
It is diffused dialysis according to water/feed liquid 1.1-1.5/1, acid recovering rate is more than 80%, and diffusion raffinate is conducive to production nickel series in next step
Product, recovery acid cupric arsenic is relatively low, and recovery acid returns black copper mud leaching acid, and wherein nickel is further recycled.
7. according to the method described in claim 1, it is characterized in that, in the step 6, raffinate is spread to rich nickel, is carried out 3 times
（2.8 times of sulphur/arsenic mole=theoretical amount）Vulcanization, temperature control room temperature, obtain 3 vulcanized slags and return arsenic production system, wherein cupric
3.25%, contain arsenic 8.91%, nickeliferous 0.67%, return arsenic production system, 3 rich nickel liquid 0.001g/L containing arsenic, cupric 0.001g/L contain
Acid 25.73 g/L, nickeliferous 50.89g/L send next step nickel product abstraction process.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110283999A (en) * | 2019-07-02 | 2019-09-27 | 株洲三特环保节能股份有限公司 | A kind of processing method of waste solution of copper electrolysis |
| CN110669932A (en) * | 2019-09-25 | 2020-01-10 | 中南大学 | Method for comprehensively utilizing copper electrolyte purification resources |
| CN113667828A (en) * | 2021-09-06 | 2021-11-19 | 长沙有色冶金设计研究院有限公司 | Method for comprehensively recovering valuable metals and arsenic trioxide from copper ash and arsenic sulfide slag |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105439355A (en) * | 2015-12-28 | 2016-03-30 | 中南大学 | Polluted acid resource recovery and advanced treatment method and device |
| CN105603190A (en) * | 2015-12-28 | 2016-05-25 | 中南大学 | Method for purifying and recovering valuable metal by copper electrolyte |
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2018
- 2018-05-16 CN CN201810469745.0A patent/CN108570559A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439355A (en) * | 2015-12-28 | 2016-03-30 | 中南大学 | Polluted acid resource recovery and advanced treatment method and device |
| CN105603190A (en) * | 2015-12-28 | 2016-05-25 | 中南大学 | Method for purifying and recovering valuable metal by copper electrolyte |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110283999A (en) * | 2019-07-02 | 2019-09-27 | 株洲三特环保节能股份有限公司 | A kind of processing method of waste solution of copper electrolysis |
| CN110669932A (en) * | 2019-09-25 | 2020-01-10 | 中南大学 | Method for comprehensively utilizing copper electrolyte purification resources |
| CN110669932B (en) * | 2019-09-25 | 2021-04-20 | 中南大学 | Method for comprehensively utilizing copper electrolyte purification resources |
| CN113667828A (en) * | 2021-09-06 | 2021-11-19 | 长沙有色冶金设计研究院有限公司 | Method for comprehensively recovering valuable metals and arsenic trioxide from copper ash and arsenic sulfide slag |
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