CN103572051A - Dechlorination method of zinc sulfate solution - Google Patents
Dechlorination method of zinc sulfate solution Download PDFInfo
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Abstract
The invention discloses a dechlorination method of a zinc sulfate solution, which comprises the steps that sulfuric acid is added to a zinc sulfate solution containing 100-150g/L zinc and 0.5-5.0g/L chlorine; an acid solution with the sulfuric acid concentration of 20-75g/L is obtained; the acid solution is subjected to selective electrodialysis in four diaphragm electrolytic cells at a room temperature and at the current density of 50-200A/m<2>; a low-chlorine solution containing 0.1-0.3g/L chlorine and a high-chlorine solution containing 5-20g/L chlorine are obtained; the low-chlorine solution is used for producing electric zinc; the high-chlorine solution is subjected to chlorine precipitation by a cuprous chloride method; a chlorine precipitation solution containing 0.4-1.0g/L chlorine is obtained; zinc powder is added to the chlorine precipitation solution for replacing and removing copper; a copper removal solution containing 0.4-1.0g/L chlorine is produced; the copper removal solution is returned for acid addition, and subjected to the selective electrodialysis. With the adoption of the method, chloride ions in the zinc sulfate solution can be removed at low cost and high efficiency.
Description
Technical field
The present invention relates to the dechlorination method in non-ferrous metal hydrometallurgy field, particularly a kind of solution of zinc sulfate.
Background technology
In the production hard and fast rule of metallic zinc, account for more than 75% metallic zinc of total amount by wet production.The generalized flowsheet of wet production metallic zinc is: zinc ore concentrate carries out desulphurizing roasting output calcining, and-------negative electrode zinc metal sheet fusion-cast obtains zinc ingot metal product to Purification of zinc sulfate solution removal of impurities output zinc sulfate scavenging solution---zinc sulfate scavenging solution electrolysis output negative electrode zinc metal sheet---to sulfuric acid leaching output solution of zinc sulfate for calcining.
In the technique of wet production metallic zinc, the purification and impurity removal of solution of zinc sulfate is a very important process, and in this process, the impurity element that need to remove has copper, cadmium, arsenic, antimony, cobalt, nickel, tin, gallium, germanium, selenium, calcium, magnesium, fluorine, chlorine etc.Remove the elements such as copper, cadmium, arsenic, antimony, cobalt, nickel, tin, gallium, germanium, selenium, mainly by adding zinc powder to replace, make the impurity element in solution change simple substance solid or solid chemical compound into by ion, from solution, separate out, to reach, remove object; Remove calcium, magnesium, main by reduction method, the solution that temperature is higher carries out fast cooling, to reduce the solubleness of calcium sulfate and sal epsom, calcium, magnesium are precipitated out respectively from solution, to reach the object that reduces calcium, magnesium with calcium sulphate crystal and magnesium sulfate crystals form; Remove the fluorine in solution, mainly by fluorion and some metal sublayers, generate the salt that solubleness is less, as Calcium Fluoride (Fluorspan), magnesium fluoride etc.; Remove the chlorion in solution, main method has following five kinds:
(1), silver nitride precipitation method: the method is to utilize silver ions to react with chlorion, generate the very little and good silver chloride sediment of stability of solubleness, the method has advantages of that speed of response is fast, dechlorination degree is high, its shortcoming is that production cost is very high, cannot in industrial production, apply at all.
(2), the cuprous chloride precipitator method: the method is to utilize cupric ion, copper simple substance and chlorion acting in conjunction, generation solubleness is less, the cuprous chloride throw out of less stable, the method has advantages of that production cost is lower, be applicable to the chloride higher solution for the treatment of soln, its shortcoming is that dechlorination degree is poor, dechlorination unstable products, and dechlorination solution also needs to carry out copper removal, should not process chloride lower solution.
(3), pyrrhosiderite coprecipitation method: the method is to utilize in the heavy iron process of solution, while generating goethite precipitation thing, part chloride ions displace also substitutes the hydroxide ion in pyrrhosiderite molecule, and together with pyrrhosiderite, forming co-precipitation, the method has advantages of that production cost is lower, product is stable very, be applicable to process the very high and chloride lower solution of iron content, its shortcoming is that handled solution needs higher iron level, and dechlorination efficiency is not high, should not process low iron-holder solution.
(4), ion-exchange resin: the method is to utilize the specific function unity structure on basic resin or modification basic resin chlorion to be had to the characteristic of preferential absorption, when solution stream is during through resin, chlorion in solution is adsorbed onto on resin, reaches the object of removing chloride ion.The method have advantages of production cost compared with low, processing power is large, its shortcoming is that dechlorination efficiency is low, zinc metal loss is large, leacheate difficult treatment, and waste discharge.
(5), organic solvent extractionprocess: the method is to utilize the specific function unity structure on neutral organic extractant muriate to be had to the characteristic of preferential extraction (complexing), in extraction equipment, organic extractant and containing chlorine solution under the effect of stirring facility, mutual high dispersing, muriate in solution is extracted (complexing) in organic extraction agent molecule, reaches the object of removing chloride ion.The method have advantages of production cost compared with low, processing power is large, metal loss is little, its shortcoming is that dechlorination efficiency is low, anti-stripping agent difficult treatment, and waste discharge.
Summary of the invention
The dechlorination method that the object of this invention is to provide a kind of solution of zinc sulfate; can be low-cost, high-level efficiency sloughs the chlorion in solution of zinc sulfate; make chloride ion content in solution reach the specification of quality of producing electrolytic zinc, and technological process not output waste liquid, effectively protection of the environment.
The present invention is achieved through the following technical solutions above-mentioned purpose: a kind of dechlorination method of solution of zinc sulfate, comprises the steps:
(1), complex acid: containing the solution of zinc sulfate of zinc 100～150 grams per liters, chloride 0.5～5.0 grams per liter, allocate sulfuric acid into, obtain the acidic solution of sulfuric acid concentration 20～75 grams per liters;
(2), selectivity electrodialysis: acidic solution is 50～200A/m in normal temperature, current density
2condition under, in four diaphragm sells, carry out electrolysis; Obtain the low chlorine solution of chloride 0.1～0.3 grams per liter and the high chlorine solution of chloride 5～20 grams per liters, low chlorine solution is for the production of electric zinc;
(3) the heavy chlorine of high chlorine liquid: high chlorine solution, 20～80 ℃ of temperature, adds copper sulfate and copper powder, adopts conventional cuprous chloride method to sink chlorine, obtains the heavy chlorine solution of chloride 0.4～1.0 grams per liter;
(4) heavy chlorine liquid copper removal: heavy chlorine solution, 20～80 ℃ of temperature, adds zinc dust precipitation copper removal, the copper removal liquid of chloride 0.4～1.0 grams per liter of output; Copper removal liquid returns to step (1) complex acid again.
Four diaphragm sells of the present invention are that 15～20 diaphram tanks are installed in a main electrolyzer, and four resin moldings have been installed in each diaphram tank altogether, and one is cationic exchange membrane, and one is anion-exchange membrane, and other two is nanofiltration membrane.
Outstanding advantages of the present invention is:
Adopt the present invention can be low-cost, high validity sloughs the chlorion in solution of zinc sulfate, the standard-required ，Wei enterprise that makes the chloride ion content of solution reach electrolytic solution widens raw material sources, strengthens the market competitiveness.
In complex acid process, due to chemical reaction not occurring, just ion spreads in solution, and equipment is succinct, simple to operate.
Four diaphragm sells in electrolytic process, have been used, when chloride 0.5～5.0 grams per liter, zinc sulfate acidic solution containing acid 20～75 grams per liters enters after electrolyzer, under the effect of DC electric field, sulfate ion in solution, chlorion, zine ion and hydrogen ion are made directional migration, in electrolyzer, cationic exchange membrane has and only allows positively charged ion to pass through, the feature that does not allow negatively charged ion to pass through, anion-exchange membrane is contrary, only allow negatively charged ion to pass through, do not allow positively charged ion to pass through, and nanofiltration membrane only allows minor radius ion and the water molecules of monovalence to pass through, divalence and above ion and other molecule will be trapped.As a result, in the effect of electric field, after the displacement of ion and the qualitative interception of film, in diaphram tank, chamber obtains chloride higher solution, and the solution flowing out from electrolyzer is chloride lower solution.
While carrying out electrolysis in four diaphragm sells, except cathode-anode plate generation chemical reaction, the various leading ions in diaphram tank and between diaphram tank are just made directional migration, there is not electrochemical reaction, therefore, when four diaphragm sell electrolysis, the electric weight consuming is few, and the cost of electric energy is low.
The low chlorine solution flowing out from electrolyzer, its chloride ion content reaches the specification of quality of producing electrolytic zinc, carries out electrolysis production electricity zinc.
The high chlorine solution of collecting from chamber in diaphragm sell, is applicable to adopting the heavy chlorine method dechlorination of cuprous chloride method, adopts after the heavy chlorine of conventional cuprous chloride method, and heavy chlorine solution adopts zinc dust precipitation copper removal again, and copper removal liquid returns to complex acid again and carries out diaphragm electrolysis again.
In whole dechlorination process of the present invention, all solution is realized closed circulation, there is no waste liquid output, therefore, has higher zinc metal recovery rate.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the dechlorination method of solution of zinc sulfate of the present invention.
Fig. 2 is four special diaphragm sell structure iron of the present invention,
In figure, be labeled as:
Embodiment
By the following examples technical scheme of the present invention is described further.
The present embodiment is dechlorination method first example of a kind of solution of zinc sulfate of the present invention, comprises the steps:
(1), complex acid: containing 90 cubic metres of the solution of zinc sulfate of zinc 100 grams per liters, chloride 0.5 grams per liter, allocate 1 ton, sulfuric acid into, obtain 90.5 cubic metres of the acidic solutions of sulfuric acid concentration 20 grams per liters;
(2), electrolysis: in four diaphragm sells of 15 diaphram tanks are installed, acidic solution is 50A/m in 25 ℃ of temperature, current density
2, total bath voltage 12V, every barrier film useful area be 680mm*670mm=0.6m
2, feed liquor speed 0.4m
3under the condition of/h, carry out electrolysis, output 0.37m
3the chloride 0.1 grams per liter solution of/h and obtain 0.03m
3the chloride 5.4 grams per liter solution of/h, the solution of chloride 0.1 grams per liter is for the production of electric zinc;
(3) the heavy chlorine of high chlorine liquid: 6.8 cubic metres of high chlorine solution, 20 ℃ of temperature, add 40 kilograms of 210 kilograms of cupric sulfate pentahydrates and copper powders, stir after 30 minutes, filter, obtain 139 kilograms of 6.8 cubic metres of the heavy chlorine solution of chloride 0.4 grams per liter, cupric 3.0 grams per liters and cupric 51%, chloride 25% protochloride copper ashes;
(4) heavy chlorine liquid copper removal: 6.8 cubic metres of heavy chlorine solution, 20 ℃ of temperature, add 30 kilograms of zinc powders, stir after 60 minutes and filter, 6.8 cubic metres of the copper removal liquid of chloride 0.4 grams per liter of output, cupric 0.2 mg/litre; 6.8 cubic metres of copper removal liquid return to step (1) complex acid again.
The present embodiment is the second example of the dechlorination method of a kind of solution of zinc sulfate of the present invention, comprises the steps:
(1), complex acid: containing 120 cubic metres of the solution of zinc sulfate of zinc 130 grams per liters, chloride 3 grams per liters, allocate 3 tons, sulfuric acid into, obtain 121 cubic metres of the acidic solutions of sulfuric acid concentration 45 grams per liters;
(2), electrolysis: in four diaphragm sells of 20 diaphram tanks have been installed, acidic solution is 120A/m in 30 ℃ of temperature, current density
2, total bath voltage 25V, every barrier film useful area be 980mm*970mm=0.95m
2, feed liquor speed 0.4m
3electrolysis under the condition of/h, output 0.32m
3the low chlorine solution of chloride 0.25 grams per liter and the 0.08m of/h
3the high chlorine solution of chloride 15 grams per liter of/h, the solution of chloride 0.25 grams per liter is for the production of electric zinc;
(3) the heavy chlorine of high chlorine liquid: 24 cubic metres of high chlorine solution, at temperature 50 C, add 350 kilograms of 1500 kilograms of cupric sulfate pentahydrates and copper powders, stir after 30 minutes, filter, obtain 1355 kilograms of 24 cubic metres of the heavy chlorine solution of chloride 0.5 grams per liter, cupric 2.5 grams per liters and cupric 49.1%, chloride 25.7% protochloride copper ashes;
(4) heavy chlorine liquid copper removal: 24 cubic metres of heavy chlorine solution, at temperature 50 C, add 90 kilograms of zinc powders, stir after 60 minutes and filter, 24 cubic metres of the copper removal liquid of chloride 0.5 grams per liter of output, cupric 0.2 mg/litre; 24 cubic metres of copper removal liquid return to step (1) complex acid again.
The present embodiment is the 3rd example of the dechlorination method of a kind of solution of zinc sulfate of the present invention, comprises the steps:
(1), complex acid: containing 100 cubic metres of the solution of zinc sulfate of zinc 150 grams per liters, chloride 5 grams per liters, allocate 7.7 tons, sulfuric acid into, obtain containing 103 cubic metres of the acidic solutions of zinc 146 grams per liters, sulfur acid 75 grams per liters, chloride 4.85 grams per liters;
(2), electrolysis: in four diaphragm sells of 20 diaphram tanks have been installed, acidic solution is 200A/m in 35 ℃ of temperature, current density
2, total bath voltage 24V, every barrier film useful area be 980mm*970mm=0.95m
2, feed liquor speed 0.35m
3under the condition of/h, carry out electrolysis, output 0.27m
3chloride 0.3 grams per liter solution and the 0.08m of/h
3the chloride 20 grams per liter solution of/h, the solution of chloride 0.3 grams per liter is for the production of electric zinc;
(3) the heavy chlorine of high chlorine liquid: 23.5 cubic metres of the high chlorine solution of chloride 20 grams per liters, 80 ℃ of temperature, add 440 kilograms of 1750 kilograms of cupric sulfate pentahydrates and copper powders, stir after 30 minutes, filter, obtain 1665 kilograms of 22.8 cubic metres of the heavy chlorine solution of chloride 1.0 grams per liters, cupric 2.0 grams per liters and cupric 49.2%, chloride 26.0% protochloride copper ashes;
(4) heavy chlorine liquid copper removal: heavy chlorine solution 23.5 side's rice, 80 ℃ of temperature, add 70 kilograms of zinc powders, stir after 60 minutes and filter, 23.5 cubic metres of the copper removal liquid of chloride 1.0 grams per liters of output, cupric 0.15 mg/litre; 23.5 cubic metres of copper removal liquid return to step (1) complex acid again.
Embodiment 4
As shown in Figure 2, four diaphragm sells of the present invention, comprise main electrolyzer 1, negative plate 2, diaphram tank 3, and in Fig. 2, signal has four diaphram tanks, wherein, anion-exchange membrane 3-1, nanofiltration membrane 3-2, cationic exchange membrane 3-3, acid solution of zinc sulfate 4, positive plate 5.Its structure and mode of connection are:
15～20 diaphram tanks are installed in a main electrolyzer, four resin moldings have been installed in each diaphram tank altogether, one is cationic exchange membrane, and one is anion-exchange membrane, and other two is nanofiltration membrane.
Claims (2)
1. a dechlorination method for solution of zinc sulfate, is characterized in that, the method comprises the steps:
(1), complex acid: containing the solution of zinc sulfate of zinc 100～150 grams per liters, chloride 0.5～5.0 grams per liter, allocate sulfuric acid into, obtain the acidic solution of sulfur acid 20～75 grams per liters;
(2), selectivity electrodialysis: acidic solution is 50～200A/m in normal temperature, current density
2condition under, in four diaphragm sells, carry out selectivity electrodialysis; Obtain the low chlorine solution of chloride 0.1～0.3 grams per liter and the high chlorine solution of chloride 5～20 grams per liters, low chlorine solution is for the production of electric zinc;
(3) the heavy chlorine of high chlorine liquid: high chlorine solution, 20～80 ℃ of temperature, adds copper sulfate and copper powder, adopts conventional cuprous chloride method to sink chlorine, obtains the heavy chlorine solution of chloride 0.4～1.0 grams per liter;
(4) heavy chlorine liquid copper removal: heavy chlorine solution, 20～80 ℃ of temperature, adds zinc dust precipitation copper removal, the copper removal liquid of chloride 0.4～1.0 grams per liter of output; Copper removal liquid returns to step (1) complex acid again.
2. the dechlorination method of solution of zinc sulfate according to claim 1, it is characterized in that, four described diaphragm sells are that 15～20 diaphram tanks are installed in a main electrolyzer, four resin barrier films are installed in each diaphram tank altogether, one is cationic exchange membrane, one is anion-exchange membrane, and other two is nanofiltration membrane.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046793A (en) * | 2014-06-27 | 2014-09-17 | 湖南水口山有色金属集团有限公司 | Method of removing chlorine in zinc sulfate solution |
| CN104404254A (en) * | 2014-12-22 | 2015-03-11 | 湖南水口山有色金属集团有限公司 | Dechlorinating method |
| CN105132684A (en) * | 2015-08-18 | 2015-12-09 | 云南驰宏锌锗股份有限公司 | Method for extracting selenium and tellurium in zinc sulfate solution through high aluminum alloy zinc powder |
| CN105274355A (en) * | 2015-11-18 | 2016-01-27 | 来宾华锡冶炼有限公司 | Method and device for removing copper and cadmium in zinc sulfate solution in replacement manner |
| CN106673144A (en) * | 2017-01-24 | 2017-05-17 | 天津碧水源膜材料有限公司 | Electric nanofiltration device with low salt removing rate and high organic matter reject rate |
| CN106868544A (en) * | 2017-03-06 | 2017-06-20 | 温州大学 | A kind of method of selective removal univalent anion impurity in electrolyte from sulfuric acid system |
| CN112941329A (en) * | 2021-01-27 | 2021-06-11 | 赵坤 | Method for recovering zinc in fuming material containing chlorine zinc oxide by wet process |
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| CN101780998A (en) * | 2010-03-20 | 2010-07-21 | 杭州天创净水设备有限公司 | Recycle treatment method for wafer rinse waste liquor |
| CN101857315A (en) * | 2010-06-22 | 2010-10-13 | 赵胜利 | Noble metal waste liquor recovering and regenerating process by film integration-dialysis separation and concentration |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046793A (en) * | 2014-06-27 | 2014-09-17 | 湖南水口山有色金属集团有限公司 | Method of removing chlorine in zinc sulfate solution |
| CN104046793B (en) * | 2014-06-27 | 2015-11-25 | 湖南水口山有色金属集团有限公司 | A kind of method removing chlorine in solution of zinc sulfate |
| CN104404254A (en) * | 2014-12-22 | 2015-03-11 | 湖南水口山有色金属集团有限公司 | Dechlorinating method |
| CN105132684A (en) * | 2015-08-18 | 2015-12-09 | 云南驰宏锌锗股份有限公司 | Method for extracting selenium and tellurium in zinc sulfate solution through high aluminum alloy zinc powder |
| CN105132684B (en) * | 2015-08-18 | 2017-06-23 | 云南驰宏锌锗股份有限公司 | A kind of method of selenium and tellurium in use high-aluminium alloy zinc powder abjection solution of zinc sulfate |
| CN105274355A (en) * | 2015-11-18 | 2016-01-27 | 来宾华锡冶炼有限公司 | Method and device for removing copper and cadmium in zinc sulfate solution in replacement manner |
| CN105274355B (en) * | 2015-11-18 | 2017-04-12 | 来宾华锡冶炼有限公司 | Method and device for removing copper and cadmium in zinc sulfate solution in replacement manner |
| CN106673144A (en) * | 2017-01-24 | 2017-05-17 | 天津碧水源膜材料有限公司 | Electric nanofiltration device with low salt removing rate and high organic matter reject rate |
| CN106673144B (en) * | 2017-01-24 | 2019-09-03 | 天津碧水源膜材料有限公司 | A kind of electric nanofiltration device with low salt rejection rate and high rejection to organics rate |
| CN106868544A (en) * | 2017-03-06 | 2017-06-20 | 温州大学 | A kind of method of selective removal univalent anion impurity in electrolyte from sulfuric acid system |
| CN106868544B (en) * | 2017-03-06 | 2019-07-19 | 温州大学 | A method of the selective removal univalent anion impurity from sulfuric acid system electrolyte |
| CN112941329A (en) * | 2021-01-27 | 2021-06-11 | 赵坤 | Method for recovering zinc in fuming material containing chlorine zinc oxide by wet process |
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Application publication date: 20140212 |