CN104674300B - Method for recycling zinc from low-concentration zinc-ammonia solution through all-ammonia system - Google Patents
Method for recycling zinc from low-concentration zinc-ammonia solution through all-ammonia system Download PDFInfo
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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Abstract
The invention discloses a method for recycling zinc from a low-concentration zinc-ammonia solution through an all-ammonia system. The method specifically comprises the following steps: 1) extracting low-concentration zinc ions from an ammonia solution containing low-concentration zinc ions by using an extracting agent, thereby obtaining an organic phase with zinc and extraction raffinate, wherein the extraction raffinate can be fed back to be used in an ammonia leaching process; 2) performing reverse extraction on the organic phase with zinc by using an ammonia solution, thereby achieving enrichment of zinc ions and obtaining an ammonia reverse extraction enriched liquid and a regenerated organic phase, wherein the regenerated organic phase can be fed back for extraction; 3) directly electrolyzing the enriched liquid obtained through reverse extraction of ammonia, thereby obtaining metal zinc, and feeding back ammonia electrolysis barren liquor for zinc reverse extraction, thereby achieving the purpose of recycling low-concentration zinc from the all-ammonia system. As the reaction parameters are controlled, the processes are all implemented in the ammonia system, the grade requirement for processing zinc-containing resources by using an ammonia method is degraded, the process procedures are reduced, the wastewater discharge is effectively reduced, the production cost is lowered, and the utilization rate of a low-grade resource is increased.
Description
Technical field
The invention belongs to low grade zinc recovery technology field is and in particular to a kind of pass through full ammonia gonosome system from low concentration zinc ammonia
The method reclaiming zinc in solution.
Background technology
China's zinc resource difficult smelting oxide ore of difficult choosing or composite ore mostly, has that basic gangue content is high, mineral composition is multiple
Miscellaneous, many metals symbiosis and be difficult the features such as sort, middle-low grade mineral deposit accounts for the 77.32% of gross reserves, be mainly distributed on southwest and
In the Northwest, such as the zinc reserves in Yunnan Province, 76.4% is oxide ore and COMPLEX MIXED ore deposit, and zinc average grade is 5.74%.Using
Traditional sulfuric acid leaching processes low-grade zinc oxide resource to be had that leaching process acid consumption is big, leachate impurity content is high, purifies and remove
Miscellaneous difficult the problems such as, it is only capable of using the Ore containing zinc more than 15% at present, resource utilization is less than 50%.Ammonia leaching can be from low product
Zinc is optionally extracted containing in zinc resource in position, can effectively improve the leaching rate of zinc；Meanwhile, in mineral, the basic gangue of high-load is not
It is dissolved in ammonia solution, consumption acid problem during sulfuric acid leaching can be prevented effectively from, become domestic and international leaching at present and aoxidized zinc resource
Main method, but the ammonia leachate for low-grade zinc oxide ore still lacks effective post-processing approach.
(the nh such as Yang Shenghai3-nh4cl-h2O system leaches low-grade zinc oxide ore and produces electric zinc. process engineering journal,
2008, s1,219-222.) technique is purified to zinc ammonia leaching solution remove impurity using multistage, then directly it is electrolysed back in ammonia solution
Receive zinc, but the method that above-mentioned flow process shortage is effectively enriched with to low concentration zinc solution, can only process containing zinc is higher than in 15%
High-grade zinc oxide ore and zinc secondary resource, could obtain can directly ammonia electrolysis Treatment with High Concentration Zinc electrolyte, the utilization of resources
Rate is low, and purification and impurity removal process is complicated.In this regard, (the synergistic extraction of zinc from such as Chen Qiyuan
ammoniacal ammonia sulfate solution by a mixture of a sterically hinderedβ-
diketone and tri-n-octylphosphine oxide(topo),hydrometallurgy,2010,105(3-4):
201-206) using solvent extraction, low concentration zinc in ammonia leachate is effectively enriched with, in order to traditional sulfuric acid system zinc
Electrolysis Connection between Processes, they adopt sulphuric acid back extraction organic faciess, so that zinc is enriched in sulfuric acid solution and be electrolysed；Although can obtain
Electrolytic zinc, but this technique exist simultaneously the alkali circulation of " leach-extraction " process with the acid circulation of " back extraction-electrolysis " process so as to
Flow process is more complicated, and soda acid difficult to reach balances, and increases ammonia consumption and acid consumption, can produce a large amount of waste liquids simultaneously, bring very big
Ambient pressure.If being directly enriched with low concentration zinc ammonia solution for Treatment with High Concentration Zinc ammonia solution, then carrying out ammonia electrolysis, not only may be used
Reclaim low concentration zinc ammonia solution and obtain metallic zinc to realize full ammono-system short route, and ammonia solution can in full-range circulation
Wastewater discharge is made to greatly reduce.However, being succeeded not yet so far based on the low concentration zinc recovering method of full ammonia gonosome system, its
In major reason be to lack can simultaneously ammonia gonosome system carry out extracting and back extraction method, be directed to ammonia in existing method
Property solution in the extraction system of zinc substantially all back extraction is carried out using the sulfuric acid solution containing 100-180g/l, the present invention passes through to extraction
Take-the reasonable adjusting of stripping process solution composition and parameter, can effectively realize the short stream that full ammono-system reclaims low concentration zinc ion
Cheng Fangfa.
Content of the invention
It is an object of the invention to provide a kind of simple to operate, cost reduces, environmental protection, and the solution in system all can circulate
Use, wastewater discharge greatly reduce by full ammonia gonosome system, from low concentration zinc ammonia solution reclaim Zn content be less than 2.5g/
The method of the low grade zinc of l.
The purpose of the present invention is realized by the following method:
A kind of method being reclaimed zinc by full ammonia gonosome system from low concentration zinc ammonia solution, is comprised the following steps:
(1) extract: extract low concentration zinc ion from the ammonia solution containing low concentration zinc ion using extractant, obtain negative
Carry organic faciess and the raffinate of zinc, raffinate returns and leaches for ammonia；
(2) back extraction: using the organic faciess of ammonia stripping workshop back extraction zinc supported, realize the enrichment of zinc ion, obtain ammonia anti-
Extraction pregnant solution and regeneration organic faciess, are used for extracting in regeneration organic faciess return to step (1)；
(3) it is electrolysed: use in Direct Electrolysis ammonia back extraction pregnant solution, prepared metallic zinc, remaining lean electrolyte return to step (2)
In back extraction；
Wherein, contain zinc ion concentration in the ammonia solution of low concentration zinc ion in step (1) and be less than 2.5g/l, total ammonia density
For 10-50g/l；
In step (1), extractant is 1- phenyl -4- ethyl -1,3- acetyl caproyl, and the starting ph of extraction system is 10.5-
12；
Ammonia stripping workshop in step (2) is one or more of ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate ammonium
Salt and the mixed liquor of ammonia；The ph scope of ammonia stripping workshop is 8.5-9.5；Total ammonia density of ammonia stripping workshop is 50-
80g/l；
It is used ammonia back extraction pregnant solution as electrolyte in step (3), is 2.5-3.5v in voltage, electric current density is 150-
250a/m2Under conditions of be electrolysed.
In the stripping process of step (2), the organic faciess of zinc supported and the volume ratio of ammonia stripping workshop are preferably 4-5.
Ammonia solution containing low concentration zinc ion pass through by containing zinc be less than 9% low-grade zinc oxide ore, mine tailing, waste residue or
Multi-metal complex ore deposit adds one or more of ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate ammonium salt and the ammonia of ammonia composition
In solution, dipping obtains.
In the extraction process of step (1) in addition to using extractant, additive can also be added in organic faciess, wherein add
Agent is one or more of tributyl phosphate, tributyl phosphorus, trioctylphosphine or Long carbon chain alcohol.
The diluent such as sulfonated kerosene or toluene can be added in organic faciess in the extraction process of step (1).
Above-mentioned steps (1) (2) (3) achieve the solution circulation of full ammonia gonosome system, have reclaimed low in ammonia solution simultaneously
Concentration zinc.The raffinate of step (1) extraction process returns the dipped journey of ammonia, and zinc load organic phases enter the ammonia back extraction of step (2)
Journey；The back extraction pregnant solution of step (2) is used for ammonia electrolytic process, and regeneration organic faciess come back for extracting；Step (3) electrolysis is obtained
After metallic zinc, ammonia lean electrolyte is used for the stripping process of step (2).
The present invention achieves first and reclaims zinc from the ammonia solution containing low concentration zinc ion by full ammonia gonosome system.First
First, inventor passes through the selection to extractant, stripping workshop in extraction, stripping process, and total parameter such as ammonia density, solution ph
The coordinated controlling, makes each course of reaction of the present invention all carry out in ammonia gonosome system, realizes full ammono-system circular treatment
Low concentration ammonia solution containing zinc, the solution of each step all can be recycled, so that wastewater discharge is greatly reduced so that this
The cost of invention hinge structure substantially reduces, and using this flow process first from containing zinc be less than 2.5g/l ammonia solution return
Receipts have obtained fine and close zinc metal sheet, and this is that prior art cannot be realized at all.Reclaimed by the full ammonia gonosome system of the present invention it is also possible to
Process, from largely reducing ammonia process, the grade requirement containing zinc resource, improve the utilization rate of Low grade resource.The present invention's is each
Individual process is all carried out in ammonia gonosome system, reduces ammonia process and processes the grade requirement containing zinc resource, shortens technological process, can have
Effect reduces discharge of wastewater, reduces production cost, improves the utilization rate of Low grade resource.The present invention's is simple to operate, it is easy to accomplish,
Suitable large-scale industrialization application, environmental protection, thus there is very major and immediate significance.
Brief description
Fig. 1 is the recovery process flow chart of the present invention.
The metal zinc metal sheet that Fig. 2 prepares for embodiment 1, the metallic zinc chip architecture as can be seen from the figure obtaining is fine and close,
Purity is high.
The metal zinc metal sheet that Fig. 3 prepares for embodiment 2, the metallic zinc chip architecture as can be seen from the figure obtaining is fine and close,
Purity is high.
Specific embodiment
With reference to embodiment, the invention will be further described, and it is right that following examples are intended to illustrate rather than
The restriction further of the present invention.
Embodiment 1
The first step: extraction
Using low concentration zinc ammonia solution (1g/l containing zinc) containing different total ammonia density as aqueous phase, in organic faciess, extractant is 1-
Phenyl -4- ethyl -1,3- acetyl caproyl, diluent is kerosene, and extractant and diluent volume ratio is for 3:7, additive-free, extraction water
Volume ratio with organic faciess is 4, and zinc extraction yield and organic faciess zinc concentration are as shown in table 1 below:
| Experiment sequence number | Solution ph | Total ammonia density | Zinc extraction yield % | Organic faciess zinc concentration |
| 1 | 6.5 | 20g/l | 42.5 | 1.57g/l |
| 2 | 7.5 | 20g/l | 77.4 | 3.10g/l |
| 3 | 8.5 | 20g/l | 51.5 | 2.06g/l |
| 4 | 9.5 | 20g/l | 35.1 | 1.4g/l |
| 5 | 10 | 20g/l | 51.7 | 2.07g/l |
| 6 | 10.5 | 20g/l | 82.8 | 3.31g/l |
| 7 | 11.5 | 20g/l | 92.5 | 3.70g/l |
| 8 | 12 | 20g/l | 96.9 | 3.88g/l |
| 9 | 6.5 | 40g/l | 19.6 | 0.78g/l |
| 10 | 7.5 | 40g/l | 39.1 | 1.56g/l |
| 11 | 8.5 | 40g/l | 22.5 | 0.9g/l |
| 12 | 9.5 | 40g/l | 9.8 | 0.39g/l |
| 13 | 10 | 40g/l | 41.2 | 1.65g/l |
| 14 | 10.5 | 40g/l | 75.7 | 3.03g/l |
| 15 | 11.5 | 40g/l | 80.5 | 3.22g/l |
| 16 | 12 | 40g/l | 88.2 | 3.53g/l |
Table 1
Result shows, under the conditions of total ammonia density of 20g/l, when solution ph is adjusted to 10.5-12 scope, in organic faciess
In the case of not needing other additives, zinc extraction yield can bring up to more than 82%；Meanwhile, the extraction yield in the range of high ph is more steady
Fixed, organic faciess zinc concentration highest can be enriched to 3.88g/l, has preferable zinc concentration ratio.When the total ammonia density of solution increases to
During 40g/l, in the range of solution ph=6.5-10, zinc extraction yield all significantly reduces, but ph zinc extraction yield in the range of 10.5-12
More than 75% still can be maintained.
Second step: ammonia back extraction
Prepare the ammonia stripping workshop of different total ammonia density and ph, then back extraction table 1- tests the zinc supported that sequence number 7 obtains
Content is the organic phase solution of 3.7g/l, controls organic faciess to be 4 with the volume ratio of aqueous phase, zinc in zinc back extraction ratio and back extraction pregnant solution
Concentration is as shown in table 2 below:
| Experiment sequence number | Solution ph | Total ammonia density | Zinc stripping rate % | Strip aqueous zinc concentration |
| 1 | 8 | 50g/l | 47.6 | 7.04g/l |
| 2 | 8.5 | 50g/l | 74.2 | 10.98g/l |
| 3 | 9 | 50g/l | 78.6 | 11.63g/l |
| 4 | 9.5 | 50g/l | 60.2 | 8.91g/l |
| 5 | 10 | 50g/l | 54.8 | 8.11g/l |
| 6 | 10.5 | 50g/l | 26.5 | 3.92g/l |
| 7 | 8 | 80g/l | 56.5 | 8.36g/l |
| 8 | 8.5 | 80g/l | 91.4 | 13.53g/l |
| 9 | 9 | 80g/l | 96.3 | 14.25g/l |
| 10 | 9.5 | 80g/l | 86.8 | 12.85g/l |
| 11 | 10 | 80g/l | 65.6 | 9.71g/l |
| 12 | 10.5 | 80g/l | 37.2 | 5.51g/l |
Table 2
Result shows, by adjusting total ammonia density and the solution ph of strip liquor, can enter the zinc back extraction of extraction organic faciess
Ammonia solution, obtains zinc ammonia pregnant solution；There is in the range of ph=8.5-9.5 higher zinc stripping efficiency, increase strip liquor
Total ammonia density can be obviously promoted the back extraction of zinc, in strip liquor under the total ammonia density of 80g/l zinc enriched concentration reach as high as 14g/l with
On.
3rd step: ammonia electrolysis
Table 2- is tested the zinc pregnant solution that in sequence number 3, ammonia back extraction obtains and is used as zinc electrolyte, Zn content 11.6g/l, groove electricity
Pressure 3v, electric current density 200a/m2, electrolysis time 2h, fine and close zinc metal sheet, outward appearance such as Fig. 2 institute of the zinc metal sheet of acquisition can be obtained in negative electrode
Show, current efficiency is up to 90.6%.
Embodiment 2
The first step: extraction
Using low concentration zinc ammonia solution (1g/l containing zinc) containing different total ammonia density as aqueous phase, organic extractant phase agent is 1- benzene
Base -4- ethyl -1,3- acetyl caproyl, additive is tributyl phosphate, and diluent is kerosene, extractant, additive and diluent
Volume ratio is 30:15:55, and the volume ratio of aqueous phase extracted and organic faciess is 5, zinc extraction yield and organic faciess zinc concentration such as table 3 below institute
Show:
| Experiment sequence number | Solution ph | Total ammonia density | Zinc extraction yield % | Organic faciess zinc concentration |
| 1 | 6.5 | 20g/l | 53.0 | 2.65g/l |
| 2 | 7.5 | 20g/l | 80.2 | 4.01g/l |
| 3 | 8.5 | 20g/l | 63.5 | 3.18g/l |
| 4 | 9.5 | 20g/l | 41.6 | 2.08g/l |
| 5 | 10 | 20g/l | 53.6 | 2.68g/l |
| 6 | 10.5 | 20g/l | 86.4 | 4.32g/l |
| 7 | 11.5 | 20g/l | 95.1 | 4.76g/l |
| 8 | 12 | 20g/l | 99.2 | 4.96g/l |
| 9 | 6.5 | 40g/l | 28.7 | 1.44g/l |
| 10 | 7.5 | 40g/l | 53.5 | 2.68g/l |
| 11 | 8.5 | 40g/l | 34.2 | 1.71g/l |
| 12 | 9.5 | 40g/l | 18.5 | 0.93g/l |
| 13 | 10 | 40g/l | 40.8 | 2.04g/l |
| 14 | 10.5 | 40g/l | 78.4 | 3.92g/l |
| 15 | 11.5 | 40g/l | 87.3 | 4.37g/l |
| 16 | 12 | 40g/l | 90.2 | 4.51g/l |
Table 3
Result shows, under the conditions of total ammonia density of 20g/l, when solution ph is adjusted to 10.5-12 scope, in organic faciess
In the case that addition tributyl phosphate is as additive, zinc extraction yield can bring up to 99%, and in the range of high ph, zinc extraction yield is more steady
Fixed；Compared with Example 1, add additive to be more beneficial for raising to compare, promote the enrichment of zinc in organic faciess, zinc enriched concentration is
Height is up to 4.96g/l.When the total ammonia density of solution increases to 40g/l, the zinc extraction yield in the range of solution ph=6.5-10 is all aobvious
Write and reduce, but zinc extraction yield still can maintain more than 78% in ph=10.5-12 scope.
Second step: ammonia back extraction
Prepare the ammonia stripping workshop of different total ammonia density and ph, then back extraction table 3- tests the zinc supported that sequence number 7 obtains
Content is the organic phase solution of 4.8g/l, controls organic faciess to be 5 with the volume ratio of aqueous phase, zinc in zinc back extraction ratio and back extraction pregnant solution
Concentration is as shown in table 4 below:
| Experiment sequence number | Solution ph | Total ammonia density | Zinc stripping rate % | Strip aqueous zinc concentration |
| 1 | 8 | 50g/l | 43.3 | 10.39g/l |
| 2 | 8.5 | 50g/l | 77.6 | 18.62g/l |
| 3 | 9 | 50g/l | 84.4 | 20.26g/l |
| 4 | 9.5 | 50g/l | 68.5 | 16.44g/l |
| 5 | 10 | 50g/l | 59.2 | 14.21g/l |
| 6 | 10.5 | 50g/l | 28.8 | 6.91g/l |
| 7 | 8 | 80g/l | 47.7 | 11.45g/l |
| 8 | 8.5 | 80g/l | 82.1 | 19.7g/l |
| 9 | 9 | 80g/l | 90.3 | 21.67g/l |
| 10 | 9.5 | 80g/l | 80.8 | 19.39g/l |
| 11 | 10 | 80g/l | 65.2 | 15.65g/l |
| 12 | 10.5 | 80g/l | 35.1 | 8.42g/l |
Table 4
Result shows, organic be added to tributyl phosphate as additive in the case of, by adjust strip liquor total
The zinc back extraction of extraction organic faciess still can be entered ammonia solution, obtain zinc ammonia pregnant solution by ammonia density and solution ph；In ph=8.5-
There is in the range of 9.5 higher zinc stripping efficiency；And, the total ammonia density increasing strip liquor can be obviously promoted the back extraction of zinc,
In strip liquor under the conditions of the total ammonia density of 80g/l, zinc concentration highest can be enriched to 21.7g/l.
3rd step: ammonia electrolysis
Table 4- is tested the solution that in sequence number 3, ammonia back extraction obtains as zinc electrolyte, Zn content 20.3g/l, tank voltage 3v,
Electric current density 200a/m2, electrolysis time 2h, fine and close zinc metal sheet can be obtained in negative electrode, outward appearance is as shown in figure 3, current efficiency 93.5%.
Claims (6)
1. a kind of method reclaiming zinc by full ammonia gonosome system from low concentration zinc ammonia solution is it is characterised in that walk below including
Rapid:
(1) extract: extract low concentration zinc ion from the ammonia solution containing low concentration zinc ion using extractant, obtain zinc supported
Organic faciess and raffinate, raffinate return for ammonia leach；
(2) back extraction: using the organic faciess of ammonia stripping workshop back extraction zinc supported, realize the enrichment of zinc ion, obtain ammonia back extraction rich
Liquid collecting and regeneration organic faciess, are used for extracting in regeneration organic faciess return to step (1)；
(3) it is electrolysed: Direct Electrolysis ammonia back extraction pregnant solution, prepared metallic zinc, it is used for anti-in remaining lean electrolyte return to step (2)
Extraction；
Wherein, contain zinc ion concentration in the ammonia solution of low concentration zinc ion in step (1) and be less than 2.5g/l, total ammonia density is
10-50g/l；
In step (1), extractant is 1- phenyl -4- ethyl -1,3- acetyl caproyl, and the starting ph of extraction system is 10.5-12；
Ammonia stripping workshop in step (2) be one or more of ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate ammonium salt with
The mixed liquor of ammonia；The ph scope of ammonia stripping workshop is 8.5-9.5；Total ammonia density of ammonia stripping workshop is 50-80g/l；
It is used ammonia back extraction pregnant solution as electrolyte in step (3), is 2.5-3.5v in voltage, electric current density is 150-250a/m2
Under conditions of be electrolysed.
2. method according to claim 1 is it is characterised in that contain low concentration zinc ion in the extraction process of step (1)
Ammonia solution is 4-5 with the volume ratio of organic faciess.
3. method according to claim 1 it is characterised in that in the extraction process of step (1) organic faciess be additionally added interpolation
Agent, wherein additive are one or more of tributyl phosphate, tributylphosphine, trioctylphosphine or Long carbon chain alcohol.
4. the method according to any one of claim 1-3 it is characterised in that in the extraction process of step (1) organic faciess add
Plus diluent, diluent is sulfonated kerosene or toluene.
5. method according to claim 1 it is characterised in that in the stripping process of step (2) organic faciess of zinc supported with
The volume ratio of ammonia stripping workshop is 4-5.
6. method according to claim 1 is it is characterised in that the ammonia solution containing low concentration zinc ion is low by containing zinc
Low-grade zinc oxide ore in 9%, mine tailing, waste residue or multi-metal complex ore deposit add ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate
One or more of impregnate in the ammonia solution that forms with ammonia of ammonium salt and obtain.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4015980A (en) * | 1975-08-04 | 1977-04-05 | General Mills Chemicals, Inc. | Use of fluorinated β-diketones in the solvent extraction of zinc |
| CN1148029A (en) * | 1995-10-16 | 1997-04-23 | 李寅高 | Method for treating waste water contg. ammonia and zinc from dry cell factory |
-
2015
- 2015-03-16 CN CN201510114821.2A patent/CN104674300B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4015980A (en) * | 1975-08-04 | 1977-04-05 | General Mills Chemicals, Inc. | Use of fluorinated β-diketones in the solvent extraction of zinc |
| CN1148029A (en) * | 1995-10-16 | 1997-04-23 | 李寅高 | Method for treating waste water contg. ammonia and zinc from dry cell factory |
Non-Patent Citations (2)
| Title |
|---|
| A Contributive Study on the Stripping of Zinc(II) from Loaded TBP Using an Ammonia/Ammonium Chloride Solution;Ivo V. Mishonov et al;《solvent extraction and ion exchange》;20041231;第22卷(第2期);第219-241页 * |
| 氨性溶液中铜_镍_锌金属离子的萃取行为及微观机理研究;胡久刚;《中国博士学位论文全文数据库工程科技Ⅰ辑》;20140315;第B021-26页 * |
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