CN108754548A - A kind of method to dechlorinate in ammonia process electrolysis zinc technology - Google Patents
A kind of method to dechlorinate in ammonia process electrolysis zinc technology Download PDFInfo
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- CN108754548A CN108754548A CN201810671200.8A CN201810671200A CN108754548A CN 108754548 A CN108754548 A CN 108754548A CN 201810671200 A CN201810671200 A CN 201810671200A CN 108754548 A CN108754548 A CN 108754548A
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- electrolysis
- dechlorinate
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
- C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
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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
- 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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- 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
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Abstract
The invention belongs to chemical industry processing technology field, a kind of be related to dechlorinating in ammonia process electrolysis zinc technology method.This method includes：1. leaching：Alkaline leaching is carried out to high chlorine material containing zinc with liquefied ammonia；2. being separated by solid-liquid separation：Obtain leachate；3. purification：Leachate is subjected to oxidation deferrization and zinc dust precipitation, obtains electrolysis net liquid；4. electrolysis：Obtain residual electrolyte；5. dechlorination：When the concentration of chlorion in residual electrolyte is in 180g/L~280g/L, use it for leaching process；When concentration is more than 280g/L, partial electrolyte raffinate is stood into cooling for leaching process, another part in cooling bay, clear liquid is back to electrowinning process and uses.Using the present invention, the concentration of chlorion in electrolyte effectively being reduced, the current efficiency of electrolytic process is improved, it is ensured that production is carried out continuously, meanwhile, the speed of separating out of ammonium chloride, energy-saving safe, easy to operate, small, the environmentally friendly no discharge of investment are improved by cooling bay.
Description
Technical field
The invention belongs to chemical industry processing technology field, a kind of be related to dechlorinating in ammonia process electrolysis zinc technology method.
Background technology
Since the chlorinity of acidic electrolysis bath in electrolysis zinc technology need to be less than 0.2g/L so that chlorine element becomes traditional acid system
The harmful element being electrolysed in zinc technology, causes high chlorine material containing zinc that can not be preferred and use；Meanwhile high chlorine material containing zinc
Dechlorination cost it is also very high, mainly due to：Burner hearth or rotary kiln heating roasting chlorine removal rate are low；Alkali wash technique is tediously long, zinc
It is difficult that loss is big, processing cost is high, blowdown is administered；Ion-exchange hardware input is big, consumables cost is high；Thus has clear superiority
Ammonia process electrolytic zinc electrolytic zinc enterprise extensive concern and fallen over each other to research and develop, specifically, ammonia process is electrolysed zinc technology, and there are hardware throwings
Enter less, raw material is applied widely, removal of impurities flow is short, environmental protection pressure is small, the advantages such as cheap.
Although ammonia process electrolytic zinc has above-mentioned advantage, really input industrialization, the producer of mass production are very few,
The enterprise gone into operation cannot achieve serialization there is also problems such as the control of such as temperature, additive selection, chlorine pipe plugging by crystallization
Production.Wherein, it is the main bugbear for influencing production with chlorine pipe plugging by crystallization, mainly due in the long-term use, chlorion
Concentration can gradually rise and reach saturation, and will be precipitated with the crystallization of chlorination ammonium form after supersaturation, so as to cause hydraulic pressure is leached
Filter the harm such as difficulty, the reduction of electrolyte pipeline blockage, Faradaic current efficiency；Meanwhile only referred in many ammonia process technique documents can
It limit value using high chlorine material containing zinc, but to chlorine ion concentration in electrolyte and is not described in detail beyond how to dechlorinate after limit value, sternly
The serialization for affecting ammonia process electrolysis zinc technology again carries out.
Invention content
The purpose of the present invention is to provide a kind of ammonia process to be electrolysed the method to dechlorinate in zinc technology, effectively controls the dense of chlorion
Degree, avoids electrolyte pipeline blockage, easy to operate, efficient.
The present invention solve above-mentioned technical problem technical solution be：
The method to dechlorinate in a kind of ammonia process electrolysis zinc technology, including following process：
(1) it leaches：Alkaline leaching is carried out to high chlorine material containing zinc with liquefied ammonia, and control reaction end pH be 8.0~
8.5；Preferably, reaction temperature is 45 DEG C~50 DEG C；
(2) it is separated by solid-liquid separation：Product after the completion of leaching is separated by solid-liquid separation, leachate and leached mud are obtained；
(3) it purifies：Leachate is delivered in purification pot, and oxidant is added and carries out oxidation deferrization, add zinc powder into
Line replacement cleans, and the temperature for controlling reaction end is 40 DEG C~45 DEG C, the electrolysis net liquid after being purified；Preferably, it aoxidizes
Agent is hydrogen peroxide；
(4) it is electrolysed：The outlet temperature that electrolysis net liquid is delivered to electrolytic cell to be electrolysed, and controls cell reaction is 50 DEG C
~55 DEG C, obtain electrolysis rolled tin and residual electrolyte；
(5) it dechlorinates：
When the concentration of chlorion in residual electrolyte is between 180g/L~280g/L, it is stored in waste liquid pool, and
For the leaching process of step (1), recycle；
When the concentration of chlorion in residual electrolyte is more than 280g/L, partial electrolyte raffinate is used for the leaching of step (1)
Process continues cycling through production；Meanwhile another part residual electrolyte being delivered in cooling bay and carries out standing cooling, after cooling
Chlorion crystallizes precipitation in the form of ammonium chloride, and clear liquid is then back in the electrolytic cell of step (4) electrowinning process and uses.
In addition, the set-up mode of cooling bay is underground type, and the positions Chi Kou of the upper end are located at earth's surface, and the depth of bottom of pond is
The bottom of pond of 40cm~60cm, cooling bay are arranged in parallel at least 2 diversion trenches, and the centre position of bottom of pond is provided with catch pit, interior
Wall is coated with epoxy resin, and overlay film tarpaulin is covered at Chi Kou.
It is electrolysed having the beneficial effect that for the method that dechlorinates in zinc technology using ammonia process of the present invention：Pass through cooling dechlorination and cycle electricity
The mode for solving raffinate, the chlorion crystallization being dissolved in leachate is precipitated, and then reduces the concentration of chlorion in electrolyte, has
Effect solves the problems, such as electrolyte pipeline blockage caused by ammonium chloride crystals, improves the current efficiency of electrolytic process, it is ensured that production
Be carried out continuously；By setting cooling bay, and the structure of cooling bay is improved, keeps its heat dissipation effect more preferable, prevented simultaneously
Rotten antiseepage, energy-saving safe, and the speed of separating out of ammonium chloride can be effectively improved；This method is in actual production through Reusability, behaviour
Make that process is stable, chlorine removal rate is high, indices are up to standard, easy to operate, investment is small, zinc loss is small, and environmental protection is conducive to electricity without discharge
The promotion and application of Xie Xin enterprises.
Description of the drawings
Fig. 1 is that ammonia process of the present invention is electrolysed the method to dechlorinate in zinc technology.
Specific implementation mode
As shown in Figure 1, a kind of method to dechlorinate in ammonia process electrolysis zinc technology, including following process：
(1) it leaches：Alkaline leaching is carried out to high chlorine material containing zinc with liquefied ammonia, reaction temperature is 45 DEG C~50 DEG C, and is controlled
The pH of reaction end is 8.0~8.5；
(2) it is separated by solid-liquid separation：Product after the completion of leaching is separated by solid-liquid separation, leachate and leached mud, leached mud are obtained
Recyclable recycling；
(3) it purifies：Leachate is delivered in purification pot, and hydrogen peroxide is added and carries out oxidation deferrization, add zinc powder into
Line replacement cleans, and the temperature for controlling reaction end is 40 DEG C~45 DEG C, the electrolysis net liquid after being purified and purification slag, purification
The recyclable recycling of slag；
(4) it is electrolysed：Electrolysis net liquid is electrolysed by pipeline to electrolytic cell, and controls the terminal temperature of cell reaction
Degree is 50 DEG C~55 DEG C, obtains electrolysis rolled tin and residual electrolyte, and electrolytic zinc micromicro founding is zinc ingot metal；
(5) it dechlorinates：Its whereabouts is determined according to the concentration of chlorion in residual electrolyte, it is specific as follows：
When the concentration of chlorion in residual electrolyte is between 180g/L~280g/L, it is stored in waste liquid pool, and
For the leaching process of step (1), recycle；
When the concentration of chlorion in residual electrolyte is more than 280g/L, 10%~40% residual electrolyte is used for step (1)
Leaching process, continue cycling through production；Meanwhile it is 20%~50% residual electrolyte is quiet by being carried out in pipeline to cooling bay
Cooling is set, heat exchange is carried out using the temperature difference of natural environment and scavenging solution, the temperature difference is bigger, and heat exchanger effectiveness is higher, specific to stand
The speed that time is precipitated by crystallization determines；Chlorion after cooling crystallizes precipitation, the ammonium chloride after crystallization in the form of ammonium chloride
Side wall and the bottom of cooling bay are depended on, are deposited in, clear liquid, which is then back to by pipeline in the electrolytic cell of step (4) electrowinning process, to be made
With；After clear liquid discharges, by manually or mechanically rooting out ammonium chloride.In addition, the day and night temperature of environment is bigger, dechlorination is crystallized
Effect is better, and e.g., cold region in winter, day and night temperature is larger, when the nighttime temperature in winter is -20 DEG C reachable, after purification
Electrolysis net liquid the temperature difference up to as many as 70 DEG C, amount of precipitation is big for crystallization, the time is short, and dechlorinate significant effect, if residing region is round the clock
The temperature difference is smaller or the lowest temperature is higher, is unfavorable for the precipitation of crystallization, then can be by installing the electricity in cooling device assistance cooling bay additional
Solution raffinate cools down.
It selects to carry out part cooling treatment when chlorine ion concentration is more than 280g/L in residual electrolyte, is due to by for many years
Large-scale production is worked out and is at 20 DEG C~50 DEG C by recording the variation and influence of chlorine ion concentration in electrolyte in detail
Under running temperature of uniting, saturation is up in electrolyte when the concentration of chlorion up to 320g/L, it will be with ammonium chloride after supersaturation
The crystallization of form is precipitated, and then leads to the harm such as leachate press filtration difficulty, the reduction of electrolyte pipeline blockage, Faradaic current efficiency；
Thus, by reference to ammonium chloride solubility in water and between chlorine ion concentration reaches saturation, residual electrolyte is cooled down
Cooling reduces chlorine ion concentration, it is ensured that continuous production to make the chlorion being dissolved in leachate crystallization be precipitated with this.
In addition, for the ease of heat dissipation, it sets cooling bay to underground type, and the positions Chi Kou of the upper end are located at earth's surface, pond
The depth at bottom is 50cm；The surface area of cooling bay is big, and specific volume then depends on production scale；The bottom of pond of cooling bay is flat
Row is provided at least 2 diversion trenches, the centre position of cooling bay bottom of pond and is provided with catch pit, be conducive to residual electrolyte flowing and
The crystallization of ammonium chloride；The inner wall of cooling bay is coated with epoxy resin, for anti-corrosion, antiseepage；It is covered at the Chi Kou of cooling bay
Film tarpaulin avoids solarization and ammonia loss.
After testing, the content of ammonium chloride is about 80% to ammonium chloride after crystallization precipitation, and the content of water is about 18%, zinc
Content is about 0.2%, remaining is calcium, magnesium, silicon, manganese etc., and dechlorinate excellent effect；Meanwhile the ammonium chloride is recycled by chemical plant,
No solid waste generates.
Claims (8)
1. a kind of method to dechlorinate in ammonia process electrolysis zinc technology, which is characterized in that including following process：
(1) it leaches：Alkaline leaching is carried out to high chlorine material containing zinc with liquefied ammonia, the pH for controlling reaction end is 8.0~8.5；
(2) it is separated by solid-liquid separation：Product after the completion of leaching is separated by solid-liquid separation, leachate and leached mud are obtained；
(3) it purifies：Leachate is delivered in purification pot, and oxidant is added and carries out oxidation deferrization, zinc powder is added and is set
The temperature changed removal of impurities, and control reaction end is 40 DEG C~45 DEG C, the electrolysis net liquid after being purified；
(4) it is electrolysed：The outlet temperature that electrolysis net liquid is delivered to electrolytic cell to be electrolysed, and controls cell reaction is 50 DEG C~55
DEG C, obtain electrolysis rolled tin and residual electrolyte；
(5) it dechlorinates：
When the concentration of chlorion in residual electrolyte is between 180g/L~280g/L, it is stored in waste liquid pool, and recycle
Leaching process for step (1)；
When the concentration of chlorion in residual electrolyte is more than 280g/L, the leaching by partial electrolyte raffinate cycle for step (1)
Process；Meanwhile another part residual electrolyte being delivered in cooling bay and carries out standing cooling, the chlorion after cooling is with ammonium chloride
Form crystallization be precipitated, clear liquid is then back in the electrolytic cell of step (4) electrowinning process.
2. the method to dechlorinate in a kind of ammonia process electrolysis zinc technology as described in claim 1, which is characterized in that the step (1)
It leaches in process, the reaction temperature of leaching process is 45 DEG C~50 DEG C.
3. the method to dechlorinate in a kind of ammonia process electrolysis zinc technology as described in claim 1, which is characterized in that the step (3)
In cleaning procedure, oxidant is hydrogen peroxide.
4. a kind of method to dechlorinate in ammonia process electrolysis zinc technology as described in claim 1, which is characterized in that the cooling bay
Set-up mode be underground type, and the positions Chi Kou of the upper end are located at earth's surface, and the depth of bottom of pond is 40cm~60cm.
5. the method to dechlorinate in a kind of ammonia process electrolysis zinc technology as claimed in claim 4, which is characterized in that the cooling bay pond
The centre position at bottom is provided with catch pit.
6. a kind of method to dechlorinate in ammonia process electrolysis zinc technology as described in claim 4 or 5, which is characterized in that the cooling
The bottom of pond in pond is arranged in parallel at least 2 diversion trenches.
7. a kind of method to dechlorinate in ammonia process electrolysis zinc technology as described in claim 4 or 5, which is characterized in that the cooling
The inner wall in pond is coated with epoxy resin.
8. a kind of method to dechlorinate in ammonia process electrolysis zinc technology as described in claim 4 or 5, which is characterized in that the cooling
Overlay film tarpaulin is covered at the Chi Kou in pond.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1069297A (en) * | 1991-08-02 | 1993-02-24 | 北京矿冶研究总院 | Method for producing zinc powder from zinc-containing material by leaching electrolysis method |
| CN102286759A (en) * | 2011-07-31 | 2011-12-21 | 红河锌联科技发展有限公司 | Method for preparing electrodeposited zinc from high-fluorine high-chlorine secondary zinc oxide powder |
| CN106399715A (en) * | 2016-09-27 | 2017-02-15 | 吉首市金湘资源科技开发有限公司 | Method for producing electrolytic zinc through high-chloride zinc ash material ammonia leaching ion exchange combined process |
| CN107099665A (en) * | 2017-06-20 | 2017-08-29 | 青铜峡市鼎辉工贸有限公司 | A kind of production technology of electrolytic zinc |
| CN107475526A (en) * | 2017-08-26 | 2017-12-15 | 麻江县金泰工业废渣综合利用回收有限责任公司 | A kind of method for preparing zinc metal sheet and ammonium chloride using high chlorine smelting ash |
-
2018
- 2018-06-26 CN CN201810671200.8A patent/CN108754548A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1069297A (en) * | 1991-08-02 | 1993-02-24 | 北京矿冶研究总院 | Method for producing zinc powder from zinc-containing material by leaching electrolysis method |
| CN102286759A (en) * | 2011-07-31 | 2011-12-21 | 红河锌联科技发展有限公司 | Method for preparing electrodeposited zinc from high-fluorine high-chlorine secondary zinc oxide powder |
| CN106399715A (en) * | 2016-09-27 | 2017-02-15 | 吉首市金湘资源科技开发有限公司 | Method for producing electrolytic zinc through high-chloride zinc ash material ammonia leaching ion exchange combined process |
| CN107099665A (en) * | 2017-06-20 | 2017-08-29 | 青铜峡市鼎辉工贸有限公司 | A kind of production technology of electrolytic zinc |
| CN107475526A (en) * | 2017-08-26 | 2017-12-15 | 麻江县金泰工业废渣综合利用回收有限责任公司 | A kind of method for preparing zinc metal sheet and ammonium chloride using high chlorine smelting ash |
Non-Patent Citations (2)
| Title |
|---|
| 张元福等: "铵盐法处理氧化锌矿的研究", 《贵州工业大学学报(自然科学版)》 * |
| 童晓忠等: "高氯锌灰生产电锌脱氯新技术", 《中国金属通报》 * |
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Application publication date: 20181106 |