CN107140727A - A kind of method that chlorine-contained wastewater purification is discharged in Zinc Hydrometallurgy Process - Google Patents
A kind of method that chlorine-contained wastewater purification is discharged in Zinc Hydrometallurgy Process Download PDFInfo
- Publication number
- CN107140727A CN107140727A CN201710230663.6A CN201710230663A CN107140727A CN 107140727 A CN107140727 A CN 107140727A CN 201710230663 A CN201710230663 A CN 201710230663A CN 107140727 A CN107140727 A CN 107140727A
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- Prior art keywords
- chlorine
- gas
- contained wastewater
- ozone
- discharged
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/78—Details relating to ozone treatment devices
- C02F2201/782—Ozone generators
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of method that chlorine-contained wastewater purification is discharged in Zinc Hydrometallurgy Process, its technical process is included oxygen or air through quality stream measuring device controlling stream amount, enter ozone generator after metering, ozone generator internal discharge pipe makes partial oxidation be converted into ozone under high pressure, the electric field action of high frequency, and the ozone of generation constitutes mixed gas with unionized gas；Mix after gas is uniformly dispersed through gas distributor with carrying out haptoreaction with certain temperature chlorine-contained wastewater, complete dechlorination；Tail gas is again introduced into ozone generator after alkali liquor absorption chlorine, realizes circulation.This technological reaction mild condition, dechlorination rate is high, and the Mn oxide of regeneration can return to wet zinc-making system, and cost is low.
Description
Technical field
The invention belongs to field of chemical metallurgical technology, relate generally to discharge chlorine-contained wastewater purification in a kind of Zinc Hydrometallurgy Process
Method.
Background technology
At present, the 80% ~ 85% of world's zinc yield is produced by wet processing, i.e. roasting-leaching-purification-electrodeposition,
Because the circulation of waste electrolyte and the tutty of the high chlorinity of a large amount of outsourcings are as raw material in this technique, chlorion is in system
In accumulate rapidly, some chlorine ion concentrations are even as high as thousands of mgL-1.The chlorion of high concentration can not only aggravate equipment and pipe
The corrosiveness in road, and have destruction to anode and negative electrode in electrolytic deposition process.Chloride ion corrosion anode, increases electrolyte
In lead content, make the leaded rise of precipitation zinc and reduce grade, while shortening anode life, chlorion is also possible in anodic oxidation
Into chlorate, aggravate the corrosion of anode.Due to corrosion, anode becomes uneven, anodic current density skewness, increase electricity
Consumption.In addition, the Cl in electrolyte-The dissolving of cathode zinc can also be accelerated, current efficiency is reduced.It is generally believed that when chlorine in electrolyte
Ion concentration is less than 100 mgL-1When, above-mentioned adverse effect will be significantly reduced.
At present the method that is dechlorinated from zinc electrolyte mainly have the silver sulfate precipitation method, the stannous chloride precipitation method, goethite process,
Extraction and ion-exchange.Wherein silver sulfate precipitation method dechlorination effect is best, but silver salt is expensive, silver-colored regeneration efficiency
It is low, it is unsuitable for industrial production.The stannous chloride precipitation method are widely used in industrial production, but in order to which chlorion is down into 100 mg
L-1Need to add large excess of CuSO below4And zinc powder, and the reaction time is longer, such as Chinese patent CN104046793B.
Goethite process is used for removing chloride in the solution of zinc sulfate of iron content, makes the precipitation adsorption chlorine in the form of goethite ore deposit of the iron in solution
Ion, such as Chinese patent CN106381388A, but method dechlorination effect is poor, less than 40% or so.Extraction is to chlorion
Selectivity is stronger, and dechlorination effect is good, such as Chinese patent CN103451449B, CN102732722A, but extraction is in industry
On exist extractant dissolving and volatilization loss, cause the method cost too high, be not suitable for industrialization.Ion-exchange
（CN204529926U、CN101492772A）Flow is short, simple to operate, operation cost is relatively low, and domestic many zinc hydrometallurgy factories adopt
Use the method dechlorination, but resin regeneration process water consumption is big, dechlorination regenerative wastewater need to further handle discharge or circulate makes
With.The resin regeneration waste water produced for ion-exchange, some producers are just neutralized with lime, output calcium sulfate slag, by
Part of sulfuric acid zinc solution is by resin mechanical entrapment when dechlorination, and the zinc sulfate that these are entrained during regeneration largely enters dechlorination liquid
In, therefore, dechlorination waste water contains a small amount of zinc metal simultaneously, and zinc metal generates calcium sulfate and hydroxide cadmia also by lime precipitation,
Substantial amounts of zinc is caused to lose.In general, chlorine ion concentration is up to more than 1000ppm in resin regeneration waste water, contain about 50 g/
L sulfuric acid and a small amount of Zn2+、Mn2+.If the chlorine ion concentration in waste water is less than 0.50 gL-1, the cleaning solution after dechlorination can make
For leacheate reuse and resin regeneration process, emission reduction and the resource circulation utilization of washing dechlorination waste water are realized, dechlorination can be both reduced
Cost, while can also solve gypsum stacks the environmental problem brought.
In summary, the chlorion in zinc electrolyte is removed with ion-exchange at present, there is chlorine-contained wastewater reluctant
Problem, therefore, a kind of useless water purification method of resin dechlorination are urgently developed, and dechlorination waste liquid can just can make as regenerated liquid circulation
With.
The content of the invention
The problem of present invention is existed for the chlorion removed at present using ion-exchange in zinc electrolyte, i.e. resin are again
The purification of raw waste water, it is proposed that a kind of method that chlorine-contained wastewater purification is discharged in Zinc Hydrometallurgy Process, its technical process includes will
Oxygen or air enter ozone generator through quality stream measuring device controlling stream amount after metering, ozone generator internal discharge pipe makes portion
Oxygen is divided to be converted into ozone under high pressure, the electric field action of high frequency, the ozone of generation constitutes mixed gas with unionized gas；
Mix after gas is uniformly dispersed through gas distributor with carrying out haptoreaction with certain temperature chlorine-contained wastewater, complete dechlorination；Tail
Gas is again introduced into ozone generator after alkali liquor absorption chlorine, realizes circulation.
In the above method, the reaction mainly occurred is as follows：
1. ozone is generated：
3O
2
→2O
3
2. dechlorination reaction：
O 3 +2Cl - +2H + →H 2 O+O 2 ↑+Cl 2 ↑
3. side reaction：
O
3
+Mn
2+
+ H
2
O → MnO
2
+ O
2
+2H
+
5O
3
+2Mn
2+
+3H
2
O→2MnO
4
-
+ 5O
2
+6H
+
3O
3
+2MnO
2
+H
2
O→2MnO
4
-
+ 3O
2
+2H
+
2MnO
4
-
+10Cl
-
+16H
+
→5Cl
2
+2Mn
2+
+8H
2
O
The present invention has advantages below compared with prior art：（1）This technological reaction mild condition, during dechlorination without
Walk valuable metal the element such as zinc, manganese in waste liquid, purification of waste water Posterior circle is reclaimed using can be enriched with Zn-ef ficiency；
（2）After waste water is purified in this technique, secondary wastewater or waste gas are not produced, and obtain the high Mn oxide of added value, Ke Yiyong
The purification of iron ion in Zinc Hydrometallurgy Process；（3）This technique ozone can be recycled, and utilization rate is high.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
The present invention is elaborated with reference to embodiment, but protection scope of the present invention is not limited only to following reality
Apply example.
Embodiment one
（1）, oxygen after decompression through flowmeter control flow after import ozone generator in, ozone generator internal discharge pipe makes
Partial oxidation is converted into ozone under high pressure, the electric field action of high frequency, and the ozone of generation constitutes gaseous mixture with unionized gas
Body, wherein it is 55 mg/L to mix ozone concentration in gas.
（2）, by step（1）The mixing gas of gained be uniformly dispersed through gas distributor after with being containing chlorine ion concentration
The waste water that 1000 mg/L, sulfuric acid concentration are 50 g/L, zinc ion concentration is 4 g/L, the concentration of manganese ion is 0.1 g/L is 70°C carries out the min of haptoreaction 60, completes dechlorination and discharges the waste gas containing a small amount of chlorine.
（3）, through step（2）Waste water after processing, chlorine ion concentration is 80 mg/L, and dechlorination rate is 92%.
（4）, by step（2）The waste gas of generation is passed through is 20% NaOH solution to mass fraction, useless after being purified
Gas.
（5）, by step（4）Waste gas after middle gained purification is imported in ozone generator, circulation step（2）Arrive（4）.
Embodiment two
（1）, oxygen after decompression through flowmeter control flow after import ozone generator in, ozone generator internal discharge pipe makes
Partial oxidation is converted into ozone under high pressure, the electric field action of high frequency, and the ozone of generation constitutes gaseous mixture with unionized gas
Body, wherein it is 75 mg/L to mix ozone concentration in gas.
（2）, by step（1）The mixing gas of gained be uniformly dispersed through gas distributor after with being containing chlorine ion concentration
The waste water that 1500 mg/L, sulfuric acid concentration are 25 g/L, zinc ion concentration is 10 g/L, the concentration of manganese ion is 5 g/L is 30°
C carries out the min of haptoreaction 180, completes dechlorination and discharges the waste gas containing a small amount of chlorine.
（3）, through step（2）Waste water after processing, chlorine ion concentration is 250 mg/L, and dechlorination rate is 83.33%.
（4）, by step（2）The waste gas of generation is passed through is 20% NaOH solution to mass fraction, useless after being purified
Gas.
（5）, by step（4）Waste gas after middle gained purification is imported in ozone generator, circulation step（2）Arrive（4）.
Embodiment three（1）, oxygen after decompression through flowmeter control flow after import ozone generator in, inside ozone generator
Discharge tube makes partial oxidation be converted into ozone, the ozone of generation and unionized gas group under high pressure, the electric field action of high frequency
Into mixed gas, wherein it is 150 mg/L to mix ozone concentration in gas.
（2）, by step（1）The mixing gas of gained be uniformly dispersed through gas distributor after with being containing chlorine ion concentration
The waste water that 2000 mg/L, sulfuric acid concentration are 100 g/L, zinc ion concentration is 25 g/L, the concentration of manganese ion is 3 g/L is 50°C carries out the min of haptoreaction 120, completes dechlorination and discharges the waste gas containing a small amount of chlorine.
（3）, through step（2）Waste water after processing, chlorine ion concentration is 150 mg/L, and dechlorination rate is 92.5%.
（4）, by step（2）The waste gas of generation is passed through is 20% NaOH solution to mass fraction, useless after being purified
Gas.
（5）, by step（4）Waste gas after middle gained purification is imported in ozone generator, circulation step（2）Arrive（4）.
Example IV
（1）, oxygen after decompression through flowmeter control flow after import ozone generator in, ozone generator internal discharge pipe makes
Partial oxidation is converted into ozone under high pressure, the electric field action of high frequency, and the ozone of generation constitutes gaseous mixture with unionized gas
Body, wherein it is 125 mg/L to mix ozone concentration in gas.
（2）, by step（1）The mixing gas of gained be uniformly dispersed through gas distributor after with being containing chlorine ion concentration
The waste water that 2000 mg/L, sulfuric acid concentration are 200 g/L, zinc ion concentration is 8 g/L, the concentration of manganese ion is 0 g/L is 45°
C carries out the min of haptoreaction 150, completes dechlorination and discharges the waste gas containing a small amount of chlorine.
（3）, through step（2）Waste water after processing, chlorine ion concentration is 110 mg/L, and dechlorination rate is 94.5%.
（4）, by step（2）The waste gas of generation is passed through is 20% NaOH solution to mass fraction, useless after being purified
Gas.
（5）, by step（4）Waste gas after middle gained purification is imported in ozone generator, circulation step（2）Arrive（4）.
Embodiment five
（1）, with air pump by air through flowmeter control flow after import ozone generator in, ozone generator internal discharge pipe
Partial oxidation is set to be converted into ozone under high pressure, the electric field action of high frequency, the ozone of generation is mixed with unionized gas composition
Gas, wherein it is 30 mg/L to mix ozone concentration in gas.
（2）, by step（1）The mixing gas of gained be uniformly dispersed through gas distributor after with being containing chlorine ion concentration
The waste water that 800 mg/L, sulfuric acid concentration are 150 g/L, zinc ion concentration is 40 g/L, the concentration of manganese ion is 3 g/L is 90°
C carries out the min of haptoreaction 30, completes dechlorination and discharges the waste gas containing a small amount of chlorine.
（3）, through step（2）Waste water after processing, chlorine ion concentration is 70 mg/L, and dechlorination rate is 91.25%.
（4）, by step（2）The waste gas of generation is passed through is 20% NaOH solution to mass fraction, useless after being purified
Gas.
（5）, by step（4）Waste gas after middle gained purification is imported in ozone generator, circulation step（2）Arrive（4）.
Embodiment six
（1）, with air pump by air through flowmeter control flow after import ozone generator in, ozone generator internal discharge pipe
Partial oxidation is set to be converted into ozone under high pressure, the electric field action of high frequency, the ozone of generation is mixed with unionized gas composition
Gas, wherein it is 40 mg/L to mix ozone concentration in gas.
（2）, by step（1）The mixing gas of gained be uniformly dispersed through gas distributor after with being containing chlorine ion concentration
1500 mg/L, sulfuric acid concentration are that 175 g/L, the waste water that zinc ion concentration is 30 g/L, the concentration of manganese ion is 2.5 g/L exist
60 °C carries out the min of haptoreaction 240, completes dechlorination and discharges the waste gas containing a small amount of chlorine.
（3）, through step（2）Waste water after processing, chlorine ion concentration is 120 mg/L, and dechlorination rate is 92%.
（4）, by step（2）The waste gas of generation is passed through is 20% NaOH solution to mass fraction, useless after being purified
Gas.
（5）, by step（4）Waste gas after middle gained purification is imported in ozone generator, circulation step（2）Arrive（4）.
Claims (7)
1. the method for chlorine-contained wastewater purification is discharged in a kind of Zinc Hydrometallurgy Process, it is characterised in that comprise the following steps：
Step 1 through quality stream measuring device controlling stream amount, enters oxygen or air in ozone generator, ozone generator after metering
Portion's discharge tube makes partial oxidation be converted into ozone, the ozone of generation and unionized gas under high pressure, the electric field action of high frequency
Constitute mixed gas；
Step 2 is mixed after gas is uniformly dispersed through gas distributor with carrying out haptoreaction one with certain temperature chlorine-contained wastewater
The section time, complete dechlorination；
Step 3 tail gas is again introduced into ozone generator after alkali liquor absorption chlorine, realizes circulation.
2. according to the method that chlorine-contained wastewater purification is discharged in claim 1 Zinc Hydrometallurgy Process, it is characterised in that described in step 1
It is 30~200 mg/L to mix ozone content in gas.
3. according to the method that chlorine-contained wastewater purification is discharged in claim 1 Zinc Hydrometallurgy Process, it is characterised in that described in step 2
Chlorine ion concentration is 50~3000 mg/L in chlorine-contained wastewater.
4. according to the method that chlorine-contained wastewater purification is discharged in claim 1 Zinc Hydrometallurgy Process, it is characterised in that described in step 2
Sulfuric acid concentration is 20~200 g/L in chlorine-contained wastewater.
5. according to the method that chlorine-contained wastewater purification is discharged in claim 1 Zinc Hydrometallurgy Process, it is characterised in that described in step 2
Zinc ion concentration is 0~50 g/L in chlorine-contained wastewater, and the concentration of manganese ion is 0~5 g/L.
6. according to the method that chlorine-contained wastewater purification is discharged in claim 1 Zinc Hydrometallurgy Process, it is characterised in that described in step 2
The reaction temperature of dechlorination reaction is 25~100°C, the reaction time is 30~240min.
7. according to the method that chlorine-contained wastewater purification is discharged in claim 1 Zinc Hydrometallurgy Process, it is characterised in that described in step 3
Alkali lye is sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710230663.6A CN107140727A (en) | 2017-04-11 | 2017-04-11 | A kind of method that chlorine-contained wastewater purification is discharged in Zinc Hydrometallurgy Process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710230663.6A CN107140727A (en) | 2017-04-11 | 2017-04-11 | A kind of method that chlorine-contained wastewater purification is discharged in Zinc Hydrometallurgy Process |
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|---|---|
| CN107140727A true CN107140727A (en) | 2017-09-08 |
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|---|---|---|---|
| CN201710230663.6A Pending CN107140727A (en) | 2017-04-11 | 2017-04-11 | A kind of method that chlorine-contained wastewater purification is discharged in Zinc Hydrometallurgy Process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110872716A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院过程工程研究所 | Method for removing chloride ions in sulfuric acid solution containing chlorine by adopting photocatalytic fluidized bed |
| CN111675308A (en) * | 2020-06-18 | 2020-09-18 | 山东国舜建设集团有限公司 | Wastewater ozone dechlorination system and process |
| CN112358075A (en) * | 2020-09-24 | 2021-02-12 | 昆明理工大学 | Device for treating chlorine-containing wastewater by using ultrasonic wave and ozone and application method thereof |
| CN113751476A (en) * | 2021-10-18 | 2021-12-07 | 北京科技大学 | Method for cooperative treatment and cyclic utilization of metallurgical solid waste and municipal waste incineration fly ash |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204138406U (en) * | 2014-09-22 | 2015-02-04 | 温州市骐邦环保科技有限公司 | A kind of ozonize waste water purification device |
| CN105617863A (en) * | 2015-12-28 | 2016-06-01 | 安徽理工大学 | Method for desulfurized slurry dechlorination |
-
2017
- 2017-04-11 CN CN201710230663.6A patent/CN107140727A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204138406U (en) * | 2014-09-22 | 2015-02-04 | 温州市骐邦环保科技有限公司 | A kind of ozonize waste water purification device |
| CN105617863A (en) * | 2015-12-28 | 2016-06-01 | 安徽理工大学 | Method for desulfurized slurry dechlorination |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110872716A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院过程工程研究所 | Method for removing chloride ions in sulfuric acid solution containing chlorine by adopting photocatalytic fluidized bed |
| CN110872716B (en) * | 2018-09-04 | 2021-01-08 | 中国科学院过程工程研究所 | Method for removing chloride ions in sulfuric acid solution containing chlorine by adopting photocatalytic fluidized bed |
| CN111675308A (en) * | 2020-06-18 | 2020-09-18 | 山东国舜建设集团有限公司 | Wastewater ozone dechlorination system and process |
| CN111675308B (en) * | 2020-06-18 | 2021-08-24 | 山东国舜建设集团有限公司 | Wastewater ozone dechlorination system and process |
| CN112358075A (en) * | 2020-09-24 | 2021-02-12 | 昆明理工大学 | Device for treating chlorine-containing wastewater by using ultrasonic wave and ozone and application method thereof |
| CN113751476A (en) * | 2021-10-18 | 2021-12-07 | 北京科技大学 | Method for cooperative treatment and cyclic utilization of metallurgical solid waste and municipal waste incineration fly ash |
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