CN104060093A - Treatment method of wastewater-neutralized gypsum tailing - Google Patents
Treatment method of wastewater-neutralized gypsum tailing Download PDFInfo
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- CN104060093A CN104060093A CN201310533524.2A CN201310533524A CN104060093A CN 104060093 A CN104060093 A CN 104060093A CN 201310533524 A CN201310533524 A CN 201310533524A CN 104060093 A CN104060093 A CN 104060093A
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a treatment method of wastewater-neutralized gypsum tailing, the wastewater-neutralized gypsum tailing comprises calcium oxide and manganese which is in a form of Mn (OH)2, and the method comprises the following steps: (1) a leaching process, to be more specific, mixing gypsum tailing in the wastewater and a leaching agent, contacting the obtained mixture with a reducing agent for reaction, performing solid-liquid separation on the mixture obtained by the reaction to obtain a clear liquid and solid residues; (2) an impurity removing process, to be more specific, removing impurities in the clear liquid for removing vanadium and phosphorus in the clear liquid to obtain a impurity-removed liquid; and (3) an electrolytic process, to be more specific, performing continuous electrolysis on the impurity-removed liquid. The wastewater-neutralized gypsum tailing treated by the method can be effectively recycled, building gypsum and metal manganese products in line with national YB / T0512003DJMnD standards can be recycled, a certain economic value can be produced, and environment pressure caused by stacking treatment of the wastewater-neutralized gypsum tailing can be avoided.
Description
Technical field
The present invention relates in a kind of waste water and the treatment process of gypsum tailings.
Background technology
At present, metallurgical production enterprise extensively adopts neutralization of lime milk to process metallurgical production process waste water, and this kind of method has the advantages such as processing cost is cheap, waste water treatment process is simple, waste water after treatment can recycle.Calcification baking legal system is got Vanadium Pentoxide in FLAKES technique and is also used lime slurry neutralization method processing production process waste water, waste water after treatment can return to vanadium oxide and produce main technological cycle use, avoid the outer row of vanadium oxide production wastewater, solve a difficult problem for vanadium metallurgical production process, and it is with low cost to process waste water, but this method also has inevitable shortcoming, process in the process of waste water, can produce a large amount of in and gypsum tailings, according to the Vanadium Pentoxide in FLAKES meter of producing 18000 tons per year, to produce every year few hundred thousand tonnes of gypsum tailings, if gypsum tailings is stacked to processing meeting, environment is caused to great pressure, and can not produce any economic benefit.
Summary of the invention
The object of the invention is for the problems referred to above that overcome in current waste water and gypsum tailings treatment process exists, provide a kind of electrolysis tech that utilizes to process in waste water and the method for gypsum tailings.
, the invention provides in a kind of waste water and the treatment process of gypsum tailings for this reason, in described waste water and gypsum tailings contain calcium oxide and manganese, manganese is with Mn (OH)
2form exist, said method comprising the steps of:
(1) leach operation: will in described waste water, mix with leaching agent with gypsum tailings, and by the mixture obtaining and reductive agent contact reacts, the mixture obtaining after reaction is carried out to solid-liquid separation, obtain clear liquid and solid residue;
(2) removal of impurities operation: described clear liquid is carried out to removal of impurities to remove vanadium and phosphorus wherein, obtain the liquid after removal of impurities;
(3) electrowinning process: the liquid after described removal of impurities is carried out to continuous electrolysis.
In the method according to this invention waste water after treatment, can effectively be recycled with gypsum tailings, gypsum for building and the manganese metal product that meets national YB/T051-2003DJMnD standard can be from waste water after treatment and in gypsum tailings, reclaimed, the pressure that certain economic worth can be avoided again in waste water and gypsum tailings stacking processing causes environment can be produced.
Other features and advantages of the present invention are described in detail the embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only, for description and interpretation the present invention, is not limited to the present invention.
The invention provides in a kind of waste water and the treatment process of gypsum tailings, in described waste water and gypsum tailings contain calcium oxide and manganese, manganese is with Mn (OH)
2form exist, said method comprising the steps of:
(1) leach operation: will in described waste water, mix with leaching agent with gypsum tailings, and by the mixture obtaining and reductive agent contact reacts, the mixture obtaining after reaction is carried out to solid-liquid separation, obtain clear liquid and solid residue;
(2) removal of impurities operation: described clear liquid is carried out to removal of impurities to remove vanadium and phosphorus wherein, obtain the liquid after removal of impurities;
(3) electrowinning process: the liquid after described removal of impurities is carried out to continuous electrolysis.
The method according to this invention, in step (1), does not have strict restriction with gypsum tailings and catalytic time of reductive agent in described waste water, can be 10-60 minute.
The method according to this invention, in step (1), does not have strict restriction with the mass ratio of gypsum tailings consumption in described leaching agent and described waste water, can be 5-2:1, is preferably 3-2:1, more preferably 2:1.
The method according to this invention, in step (1), with respect in the described waste water of 100 weight parts and gypsum tailings, the consumption of described reductive agent can be 0.5-2 weight part.
The method according to this invention, in step (1), described leaching agent can be at least one in sulfuric acid, hydrochloric acid, nitric acid, hydrofluoric acid and chloroazotic acid.Under preferable case, described leaching agent is sulfuric acid; Further preferably, H in described leaching agent
2sO
4with the volume ratio of water be 1:1.
The method according to this invention, in step (1), described reductive agent can, for the conventional various reductive agents in this area, can be ferrous sulfate and/or sulfurous acid, is preferably ferrous sulfate.
The method according to this invention, in step (1), before described contact reacts, the time≤6h exposing in air with gypsum tailings in described waste water.
The method according to this invention, in described waste water and in gypsum tailings, manganese is at first with Mn (OH)
2form exist, if in air open-assembly time long; generate the oxide compound manganese layer of brown, its main component is MnO, MnO
2and Mn
3o
4in at least one, if in the waste water that open-assembly time is grown in air and gypsum tailings carry out Leaching reaction, manganese can not be with Mn
2+form enter into solution, Leaching reaction must be at high temperature, reduce under leaching condition and carry out by force, and extraction time is longer, thereby causes Mn in leach liquor
2+density loss, Fe
2+and SO
4 2-concentration raises, and leaching process there will be acid consumption increasing, leaching yield reduction, the rising of solution viscosity etc. a series of to the disadvantageous factor of subsequent processes.Therefore, carry out in the waste water of sulfuric acid leaching and time that gypsum tailings exposes in air unsuitable oversize.
The method according to this invention, in step (1), washes described solid residue, can obtain gypsum for building, and the washing times of solid residue can be >=6 times, is preferably 6 times.
The method according to this invention, in step (2), described removal of impurities operation is preferably: by the pH value of described clear liquid be adjusted to 4-6 and with CaO contact reacts, then under the existence of gac, in the mixture obtaining after contact reacts, pass into pressurized air.
The method according to this invention, in step (2), in described removal of impurities operation, described contact reacts is under agitation carried out, and the reaction times can be 10-60 minute.
The method according to this invention, in step (2), with respect to the described clear liquid of 100 weight parts, the consumption of CaO can be 0.5-2 weight part, the consumption of gac can be 0.5-2 weight part.
The method according to this invention, in step (3), described electrowinning process comprises: the liquid pH value after described removal of impurities is adjusted to 6-8, under tin anhydride solution exists, carries out electrolysis, current density is 400A/m
2, electrolysis temperature is 40-50 DEG C, bath voltage is 4.5V, after 8-24h is carried out in electrolysis, changes negative plate.
The method according to this invention, in step (2) and step (3), the pH value of the liquid after described clear liquid and described removal of impurities can adopt the pH adjusting agent of this area routine to regulate, conventional pH adjusting agent can be citric acid, lactic acid, acetic acid, ammoniacal liquor, sodium hydroxide, potassium hydroxide etc., is preferably ammoniacal liquor.
In method of the present invention waste water to be dealt with and gypsum tailings can be in the waste water of this area routine and gypsum tailings, for example can for the waste water that adopts neutralization of lime milk to produce vanadium oxide technique to calcification baking process obtained in and gypsum tailings, particularly, the concrete technology flow process of utilizing neutralization of lime milk to process vanadium oxide calcification manufacture waste water can comprise: in vanadium wastewater, inject milk of lime slip, under agitation condition, make the pH value of vanadium wastewater rise to 9-11 from 2 left and right, again mixed slurry is filtered by plate-and-frame filter press, the solid residue obtaining after filtration is in waste water and gypsum tailings.The method according to this invention, can contain the calcium oxide of 20-30 % by weight, the manganese of 7-9 % by weight, the vanadium of 0.05-0.2 % by weight, the phosphorus of 0.01-0.1 % by weight, the iron of 0.1-0.5 % by weight, the magnesium oxide of 1-2 % by weight, the sulphur of 10-20 % by weight, the chromium of 0.01-0.05 % by weight, silicon-dioxide, the aluminium sesquioxide of 0.1-1 % by weight and the titanium dioxide of 0.1-1 % by weight of 1-3 % by weight with gypsum tailings in described waste water.Under preferable case, the calcium oxide that contains 26.48 % by weight with gypsum tailings in described waste water, the manganese of 8.4 % by weight, the vanadium of 0.1 % by weight, the phosphorus of 0.06 % by weight, the iron of 0.29 % by weight, the magnesium oxide of 1.49 % by weight, the sulphur of 15.66 % by weight, the chromium of 0.03 % by weight, silicon-dioxide, the aluminium sesquioxide of 0.51 % by weight and the titanium dioxide of 0.76 % by weight of 1.74 % by weight.
Embodiment
Describe the present invention in detail by embodiment below, but scope of the present invention is not limited to these embodiment.
The testing method the present invention relates to is as follows:
1, leaching yield is calculated according to the residual element amount in leaching residue and the amount of element in former slag.
2, current efficiency is separated out the quality of manganese according to actual negative electrode and the theoretical amount of faraday's formula compares and draws.
Embodiment 1
Get in the waste water that 100g exposes 1h in air and gypsum tailings carries out sulfuric acid leaching reaction, in described waste water and the gypsum tailings calcium oxide that contains 26.48 % by weight, the manganese of 8.4 % by weight, the vanadium of 0.1 % by weight, the phosphorus of 0.06 % by weight, the iron of 0.29 % by weight, the magnesium oxide of 1.49 % by weight, the sulphur of 15.66 % by weight, the chromium of 0.03 % by weight, silicon-dioxide, the aluminium sesquioxide of 0.51 % by weight and the titanium dioxide of 0.76 % by weight of 1.74 % by weight.Under normal temperature condition, add 200g leaching agent sulfuric acid and 1g reduction leaching agent FeSO
4, extraction time is 0.5h, and leaching yield is 98%, obtains clear liquid and solid residue after solid-liquid separation, and solid residue obtains gypsum for building after 6 washings.Using ammoniacal liquor to regulate the pH value of clear liquid is 5, adds 1g calcium oxide, and stirring reaction 0.5h adds 1g gac after solid-liquid separation, under agitation condition, passes into pressurized air, obtains the liquid after removal of impurities after solid-liquid separation.Using ammoniacal liquor to regulate the pH value of the liquid after removal of impurities is 7, adds tin anhydride solution stirring even, then passes into electrolyzer and carries out continuous electrolysis, and current density is 400A/m
2, electrolysis temperature is 45 DEG C, and bath voltage is 4.5V, after electrolysis 8h, changes negative plate, and the current efficiency of the negative plate that completes electrolysis after washing, oven dry and lift-off processing is 60%, can reclaim the manganese metal product that 5g meets national YB/T051-2003DJMnD standard.
Embodiment 2
Get in the waste water that 100g exposes 3h in air and gypsum tailings carries out sulfuric acid leaching reaction, in described waste water and the gypsum tailings calcium oxide that contains 26.48 % by weight, the manganese of 8.4 % by weight, the vanadium of 0.1 % by weight, the phosphorus of 0.06 % by weight, the iron of 0.29 % by weight, the magnesium oxide of 1.49 % by weight, the sulphur of 15.66 % by weight, the chromium of 0.03 % by weight, silicon-dioxide, the aluminium sesquioxide of 0.51 % by weight and the titanium dioxide of 0.76 % by weight of 1.74 % by weight.Under normal temperature condition, add 200g leaching agent sulfuric acid and 1g reduction leaching agent FeSO
4, extraction time is 0.5h, and leaching yield is 98%, obtains clear liquid and solid residue after solid-liquid separation, and solid residue obtains gypsum for building after 6 washings.Using ammoniacal liquor to regulate the pH value of clear liquid is 5, adds 1g calcium oxide, and stirring reaction 0.5h adds 1g gac after solid-liquid separation, under agitation condition, passes into pressurized air, obtains the liquid after removal of impurities after solid-liquid separation.Using ammoniacal liquor to regulate the pH value of the liquid after removal of impurities is 7, adds tin anhydride solution stirring even, then passes into electrolyzer and carries out continuous electrolysis, and current density is 400A/m
2electrolysis temperature is 42 DEG C, and bath voltage is 4.5V, after electrolysis 8h, changes negative plate, the current efficiency of the negative plate that completes electrolysis after washing, oven dry and lift-off processing is 54%, can reclaim the manganese metal product that 4.6g meets national YB/T051-2003DJMnD standard.
Embodiment 3
Get in the waste water that 100g exposes 6h in air and gypsum tailings carries out sulfuric acid leaching reaction, in described waste water and the gypsum tailings calcium oxide that contains 26.48 % by weight, the manganese of 8.4 % by weight, the vanadium of 0.1 % by weight, the phosphorus of 0.06 % by weight, the iron of 0.29 % by weight, the magnesium oxide of 1.49 % by weight, the sulphur of 15.66 % by weight, the chromium of 0.03 % by weight, silicon-dioxide, the aluminium sesquioxide of 0.51 % by weight and the titanium dioxide of 0.76 % by weight of 1.74 % by weight.Under normal temperature condition, add 200g leaching agent sulfuric acid and 1g reduction leaching agent FeSO
4, extraction time is 0.5h, and leaching yield is 98%, obtains clear liquid and solid residue after solid-liquid separation, and solid residue obtains gypsum for building after 6 washings.Using ammoniacal liquor to regulate the pH value of clear liquid is 5, adds 1g calcium oxide, and stirring reaction 0.5h adds 1g gac after solid-liquid separation, under agitation condition, passes into pressurized air, obtains the liquid after removal of impurities after solid-liquid separation.Using ammoniacal liquor to regulate the pH value of the liquid after removal of impurities is 7, adds tin anhydride solution stirring even, then passes into electrolyzer and carries out continuous electrolysis, and current density is 400A/m
2, electrolysis temperature is 40 DEG C, and bath voltage is 4.5V, after electrolysis 8h, changes negative plate, and the current efficiency of the negative plate that completes electrolysis after washing, oven dry and lift-off processing is 50%, can reclaim the manganese metal product that 4g meets national YB/T051-2003DJMnD standard.
As can be seen here, the method according to this invention can realize effectively processing with gypsum tailings in waste water, and in the process of processing, can reclaim gypsum for building and the manganese metal product that meets national YB/T051-2003DJMnD standard.
Claims (12)
1. in waste water and the treatment process of gypsum tailings, in described waste water and gypsum tailings contain calcium oxide and manganese, manganese is with Mn (OH)
2form exist, said method comprising the steps of:
(1) leach operation: will in described waste water, mix with leaching agent with gypsum tailings, and by the mixture obtaining and reductive agent contact reacts, the mixture obtaining after reaction is carried out to solid-liquid separation, obtain clear liquid and solid residue;
(2) removal of impurities operation: described clear liquid is carried out to removal of impurities to remove vanadium and phosphorus wherein, obtain the liquid after removal of impurities;
(3) electrowinning process: the liquid after described removal of impurities is carried out to continuous electrolysis.
2. method according to claim 1, wherein, in step (1), the described catalytic time is 10-60 minute.
3. method according to claim 1, wherein, in step (1), is 2-5:1 with the mass ratio of gypsum tailings consumption in described leaching agent and described waste water, is preferably 2-3:1.
4. method according to claim 1, wherein, in step (1), with respect in the described waste water of 100 weight parts and gypsum tailings, the consumption of described reductive agent is 0.5-2 weight part.
5. according to the method described in claim 1 or 3, wherein, in step (1), described leaching agent is at least one in sulfuric acid, hydrochloric acid, nitric acid, hydrofluoric acid and chloroazotic acid.
6. according to the method described in claim 1 or 4, wherein, in step (1), described reductive agent is ferrous sulfate and/or sulfurous acid.
7. method according to claim 1, wherein, in step (1), before described contact reacts, the time≤6h exposing in air with gypsum tailings in described waste water.
8. method according to claim 1, wherein, in step (2), described removal of impurities operation comprises: by the pH value of described clear liquid be adjusted to 4-6 and with CaO contact reacts, then under the existence of gac, in the mixture obtaining after contact reacts, pass into pressurized air.
9. method according to claim 8, wherein, in described removal of impurities operation, described contact reacts is under agitation carried out, and the reaction times is 10-60 minute.
10. method according to claim 8, wherein, with respect to the described clear liquid of 100 weight parts, the consumption of CaO is 0.5-2 weight part, the consumption of gac is 0.5-2 weight part.
11. methods according to claim 1, wherein, in step (3), described electrowinning process comprises: the liquid pH value after described removal of impurities is adjusted to 6-8, under tin anhydride solution exists, carries out electrolysis, current density is 400A/m
2, electrolysis temperature is 40-50 DEG C, bath voltage is 4.5V, after 8-24h is carried out in electrolysis, changes negative plate.
12. methods according to claim 1, wherein, the calcium oxide that contains 20-30 % by weight with gypsum tailings in described waste water, the manganese of 7-9 % by weight, the vanadium of 0.05-0.2 % by weight, the phosphorus of 0.01-0.1 % by weight, the iron of 0.1-0.5 % by weight, the magnesium oxide of 1-2 % by weight, the sulphur of 10-20 % by weight, the chromium of 0.01-0.05 % by weight, silicon-dioxide, the aluminium sesquioxide of 0.1-1 % by weight and the titanium dioxide of 0.1-1 % by weight of 1-3 % by weight.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105219969A (en) * | 2015-11-19 | 2016-01-06 | 攀钢集团西昌钢钒有限公司 | Vanadium wastewater and tailings in vanadium extraction is utilized to extract the method for manganese metal |
| CN107640789A (en) * | 2017-10-25 | 2018-01-30 | 成都先进金属材料产业技术研究院有限公司 | A kind of manganese sulfate preparation method for lithium battery |
| CN107815549A (en) * | 2017-11-13 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | The Application way of vanadium wastewater |
| CN112410561A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团研究院有限公司 | Treatment method for neutralizing gypsum slag in vanadium precipitation wastewater |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219969A (en) * | 2015-11-19 | 2016-01-06 | 攀钢集团西昌钢钒有限公司 | Vanadium wastewater and tailings in vanadium extraction is utilized to extract the method for manganese metal |
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| CN107815549A (en) * | 2017-11-13 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | The Application way of vanadium wastewater |
| CN107815549B (en) * | 2017-11-13 | 2019-11-12 | 攀钢集团攀枝花钢铁研究院有限公司 | The utilization method of vanadium wastewater |
| CN112410561A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团研究院有限公司 | Treatment method for neutralizing gypsum slag in vanadium precipitation wastewater |
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