CN104060093B - A kind for the treatment of process of waste water neutralize gypsum tailings - Google Patents

A kind for the treatment of process of waste water neutralize gypsum tailings Download PDF

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CN104060093B
CN104060093B CN201310533524.2A CN201310533524A CN104060093B CN 104060093 B CN104060093 B CN 104060093B CN 201310533524 A CN201310533524 A CN 201310533524A CN 104060093 B CN104060093 B CN 104060093B
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weight
waste water
impurities
removal
gypsum tailings
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CN104060093A (en
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孟伟巍
彭毅
陶长元
刘作华
钟国梅
何文艺
申彪
卢晓林
叶露
吴封
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention relates to a kind for the treatment of process of waste water neutralize gypsum tailings, described waste water neutralize gypsum tailings contains calcium oxide and manganese, and manganese is with Mn (OH) 2form exist, said method comprising the steps of: (1) leaches operation: mixed with leaching agent by described waste water neutralize gypsum tailings, and by the mixture that obtains and reductive agent contact reacts, the mixture obtained is carried out solid-liquid separation, obtain clear liquid and solid residue after reaction; (2) removal of impurities operation: described clear liquid is carried out removal of impurities to remove vanadium wherein and phosphorus, obtain the liquid after removal of impurities; (3) electrowinning process: the liquid after described removal of impurities is carried out continuous electrolysis.Can effectively be recycled according to the waste water neutralize gypsum tailings after method process of the present invention, therefrom can reclaim gypsum for building and the manganese metal product meeting national YB/T051-2003DJMnD standard, certain economic worth can be produced waste water neutralize gypsum tailings can be avoided again to stack the pressure processing and cause environment.

Description

A kind for the treatment of process of waste water neutralize gypsum tailings
Technical field
The present invention relates to a kind for the treatment of process of waste water neutralize gypsum tailings.
Background technology
The advantages such as at present, metallurgical production enterprise extensively adopts neutralization of lime milk process metallurgical production process waste water, and this kind of method has that processing cost is cheap, waste water treatment process simple, waste water after process 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 process can return vanadium oxide and produce the use of main technological cycle, avoid the outer row of vanadium oxide production wastewater, solve a difficult problem for vanadium metallurgical production process, and process waste water is with low cost, but this method also has inevitable shortcoming, process waste water process in can produce a large amount of in and gypsum tailings, according to the Vanadium Pentoxide in FLAKES meter of annual output 18000 tons, to produce few hundred thousand tonnes of gypsum tailings every year, if gypsum tailings is stacked process can cause great pressure to environment, and any economic benefit can not be produced.
Summary of the invention
The object of the invention is the problems referred to above existed to overcome current waste water neutralize gypsum tailings treatment process, a kind of method utilizing electrolysis tech process waste water neutralize gypsum tailings is provided.
For this reason, the invention provides a kind for the treatment of process of waste water neutralize gypsum tailings, described waste water neutralize gypsum tailings contains calcium oxide and manganese, and manganese is with Mn (OH) 2form exist, said method comprising the steps of:
(1) leach operation: mixed with leaching agent by described waste water neutralize gypsum tailings, and by the mixture that obtains and reductive agent contact reacts, the mixture obtained after reacting is carried out solid-liquid separation, obtains clear liquid and solid residue;
(2) removal of impurities operation: described clear liquid is carried out removal of impurities to remove vanadium wherein and phosphorus, obtain the liquid after removal of impurities;
(3) electrowinning process: the liquid after described removal of impurities is carried out continuous electrolysis.
Can effectively be recycled according to the waste water neutralize gypsum tailings after method process of the present invention, gypsum for building and the manganese metal product meeting national YB/T051-2003DJMnD standard can be reclaimed from the waste water neutralize gypsum tailings after process, certain economic worth can be produced waste water neutralize gypsum tailings can be avoided again to stack the pressure processing and cause environment.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind for the treatment of process of waste water neutralize gypsum tailings, described waste water neutralize gypsum tailings contains calcium oxide and manganese, and manganese is with Mn (OH) 2form exist, said method comprising the steps of:
(1) leach operation: mixed with leaching agent by described waste water neutralize gypsum tailings, and by the mixture that obtains and reductive agent contact reacts, the mixture obtained after reacting is carried out solid-liquid separation, obtains clear liquid and solid residue;
(2) removal of impurities operation: described clear liquid is carried out removal of impurities to remove vanadium wherein and phosphorus, obtain the liquid after removal of impurities;
(3) electrowinning process: the liquid after described removal of impurities is carried out continuous electrolysis.
According to method of the present invention, in step (1), described waste water neutralize gypsum tailings and reductive agent catalytic time do not have strict restriction, can be 10-60 minute.
According to method of the present invention, in step (1), the mass ratio of described leaching agent and described waste water neutralize gypsum tailings consumption does not have strict restriction, can be 5-2:1, is preferably 3-2:1, more preferably 2:1.
According to method of the present invention, in step (1), relative to the described waste water neutralize gypsum tailings of 100 weight parts, the consumption of described reductive agent can be 0.5-2 weight part.
According to method of the present 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 4be 1:1 with the volume ratio of water.
According to method of the present invention, in step (1), the various reductive agents that described reductive agent can be commonly used for this area, can be ferrous sulfate and/or sulfurous acid, be preferably ferrous sulfate.
According to method of the present invention, in step (1), before described contact reacts, described waste water neutralize gypsum tailings expose in atmosphere time≤6h.
According to method of the present invention, in described waste water neutralize gypsum tailings, manganese is at first with Mn (OH) 2form exist, if in atmosphere 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 carry out Leaching reaction to the waste water neutralize gypsum tailings that open-assembly time is in atmosphere longer, manganese can not with Mn 2+form enter into solution, then Leaching reaction must carry out under high temperature, strong reducing leaching condition, and extraction time is longer, thus causes Mn in leach liquor 2+density loss, Fe 2+and SO 4 2-concentration raises, and it is a series of to the disadvantageous factor of subsequent processes that leaching process there will be acid consumption increasing, leaching yield reduction, solution viscosity rising etc.Therefore, the time that the waste water neutralize gypsum tailings carrying out sulfuric acid leaching exposes in atmosphere is unsuitable oversize.
According to method of the present invention, in step (1), washed by described solid residue, can obtain gypsum for building, the washing times of solid residue can be >=6 times, is preferably 6 times.
According to method of the present invention, in step (2), described removal of impurities operation be preferably: the pH value of described clear liquid is adjusted to 4-6 and with CaO contact reacts, pass into pressurized air in the mixture then obtained after contact reacts under the existence of gac.
According to method of the present 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.
According to method of the present invention, in step (2), relative to the described clear liquid of 100 weight parts, the consumption of CaO can be 0.5-2 weight part, and the consumption of gac can be 0.5-2 weight part.
According to method of the present invention, in step (3), described electrowinning process comprises: the liquid pH value after described removal of impurities is adjusted to 6-8, and under tin anhydride solution exists, carry out electrolysis, current density is 400A/m 2, electrolysis temperature is 40-50 DEG C, and bath voltage is 4.5V, after 8-24h is carried out in electrolysis, changes negative plate.
According to method of the present 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.
Method of the present invention waste water neutralize gypsum tailings to be dealt with can be the waste water neutralize gypsum tailings of this area routine, such as can for adopt neutralization of lime milk to the waste water that calcification baking produces vanadium oxide technique process obtained in and gypsum tailings, particularly, the concrete technology flow process of neutralization of lime milk process vanadium oxide calcification manufacture waste water is utilized to comprise: in vanadium wastewater, inject milk of lime slip, under agitation, the pH value of vanadium wastewater is made to rise to 9-11 from about 2, again mixed slurry is filtered by plate-and-frame filter press, the solid residue obtained after filtration is waste water neutralize gypsum tailings.According to method of the present invention, described waste water neutralize gypsum tailings can the titanium dioxide of manganese containing the calcium oxide of 20-30 % by weight, 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, the silicon-dioxide of 1-3 % by weight, the aluminium sesquioxide of 0.1-1 % by weight and 0.1-1 % by weight.Under preferable case, described waste water neutralize gypsum tailings contain 26.48 % by weight calcium oxide, 8.4 % by weight manganese, 0.1 % by weight vanadium, 0.06 % by weight phosphorus, 0.29 % by weight iron, 1.49 % by weight magnesium oxide, 15.66 % by weight sulphur, 0.03 % by weight chromium, the silicon-dioxide of 1.74 % by weight, the aluminium sesquioxide of 0.51 % by weight and 0.76 % by weight titanium dioxide.
Embodiment
Describe the present invention in detail by embodiment below, but scope of the present invention is not limited to these embodiments.
The testing method that the present invention relates to is as follows:
1, leaching yield calculates according to the residual element amount leached in residue and the amount of element in former slag.
2, current efficiency compares according to the actual negative electrode precipitation quality of manganese and the theoretical amount of faraday's formula and draws.
Embodiment 1
Get the waste water neutralize gypsum tailings that 100g exposes 1h in atmosphere and carry out sulfuric acid leaching reaction, described waste water neutralize gypsum tailings contain 26.48 % by weight calcium oxide, 8.4 % by weight manganese, 0.1 % by weight vanadium, 0.06 % by weight phosphorus, 0.29 % by weight iron, 1.49 % by weight magnesium oxide, 15.66 % by weight sulphur, 0.03 % by weight chromium, the silicon-dioxide of 1.74 % by weight, the aluminium sesquioxide of 0.51 % by weight and 0.76 % by weight titanium dioxide.200g leaching agent sulfuric acid and 1g reducing leaching agent FeSO is added under normal temperature condition 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.Use ammoniacal liquor to regulate the pH value of clear liquid to be 5, add 1g calcium oxide, stirring reaction 0.5h, after solid-liquid separation, add 1g gac, under agitation condition, pass into pressurized air, after solid-liquid separation, obtain the liquid after removal of impurities.The pH value using the liquid after ammoniacal liquor adjustment removal of impurities is 7, and add tin anhydride solution stirring evenly, then pass into electrolyzer and carry out continuous electrolysis, current density is 400A/m 2, electrolysis temperature is 45 DEG C, and bath voltage is 4.5V, changes negative plate after electrolysis 8h, and the current efficiency of negative plate after washing, oven dry and lift-off processing completing electrolysis is 60%, can reclaim the manganese metal product that 5g meets national YB/T051-2003DJMnD standard.
Embodiment 2
Get the waste water neutralize gypsum tailings that 100g exposes 3h in atmosphere and carry out sulfuric acid leaching reaction, described waste water neutralize gypsum tailings contain 26.48 % by weight calcium oxide, 8.4 % by weight manganese, 0.1 % by weight vanadium, 0.06 % by weight phosphorus, 0.29 % by weight iron, 1.49 % by weight magnesium oxide, 15.66 % by weight sulphur, 0.03 % by weight chromium, the silicon-dioxide of 1.74 % by weight, the aluminium sesquioxide of 0.51 % by weight and 0.76 % by weight titanium dioxide.200g leaching agent sulfuric acid and 1g reducing leaching agent FeSO is added under normal temperature condition 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.Use ammoniacal liquor to regulate the pH value of clear liquid to be 5, add 1g calcium oxide, stirring reaction 0.5h, after solid-liquid separation, add 1g gac, under agitation condition, pass into pressurized air, after solid-liquid separation, obtain the liquid after removal of impurities.The pH value using the liquid after ammoniacal liquor adjustment removal of impurities is 7, and add tin anhydride solution stirring evenly, then pass into electrolyzer and carry out continuous electrolysis, current density is 400A/m 2electrolysis temperature is 42 DEG C, and bath voltage is 4.5V, changes negative plate after electrolysis 8h, the current efficiency of negative plate after washing, oven dry and lift-off processing completing electrolysis is 54%, can reclaim the manganese metal product that 4.6g meets national YB/T051-2003DJMnD standard.
Embodiment 3
Get the waste water neutralize gypsum tailings that 100g exposes 6h in atmosphere and carry out sulfuric acid leaching reaction, described waste water neutralize gypsum tailings contain 26.48 % by weight calcium oxide, 8.4 % by weight manganese, 0.1 % by weight vanadium, 0.06 % by weight phosphorus, 0.29 % by weight iron, 1.49 % by weight magnesium oxide, 15.66 % by weight sulphur, 0.03 % by weight chromium, the silicon-dioxide of 1.74 % by weight, the aluminium sesquioxide of 0.51 % by weight and 0.76 % by weight titanium dioxide.200g leaching agent sulfuric acid and 1g reducing leaching agent FeSO is added under normal temperature condition 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.Use ammoniacal liquor to regulate the pH value of clear liquid to be 5, add 1g calcium oxide, stirring reaction 0.5h, after solid-liquid separation, add 1g gac, under agitation condition, pass into pressurized air, after solid-liquid separation, obtain the liquid after removal of impurities.The pH value using the liquid after ammoniacal liquor adjustment removal of impurities is 7, and add tin anhydride solution stirring evenly, then pass into electrolyzer and carry out continuous electrolysis, current density is 400A/m 2, electrolysis temperature is 40 DEG C, and bath voltage is 4.5V, changes negative plate after electrolysis 8h, and the current efficiency of negative plate after washing, oven dry and lift-off processing completing electrolysis is 50%, can reclaim the manganese metal product that 4g meets national YB/T051-2003DJMnD standard.
As can be seen here, can realize effectively processing waste water neutralize gypsum tailings according to method of the present invention, and gypsum for building and the manganese metal product meeting national YB/T051-2003DJMnD standard can be reclaimed in the process of process.

Claims (11)

1. a treatment process for waste water neutralize gypsum tailings, described waste water neutralize gypsum tailings contains calcium oxide and manganese, and manganese is with Mn (OH) 2form exist, said method comprising the steps of:
(1) leach operation: mixed with leaching agent by described waste water neutralize gypsum tailings, and by the mixture that obtains and reductive agent contact reacts, the mixture obtained after reacting is carried out solid-liquid separation, obtains clear liquid and solid residue;
(2) removal of impurities operation: described clear liquid is carried out removal of impurities to remove vanadium wherein and phosphorus, obtain the liquid after removal of impurities;
(3) electrowinning process: the liquid after described removal of impurities is carried out continuous electrolysis;
In step (1), relative to the described waste water neutralize gypsum tailings of 100 weight parts, the consumption of described reductive agent is 0.5-2 weight part;
In step (2), described removal of impurities operation comprises: the pH value of described clear liquid is adjusted to 4-6 and with CaO contact reacts, pass into pressurized air in the mixture then obtained after contact reacts under the existence of gac.
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), the mass ratio of described leaching agent and described waste water neutralize gypsum tailings consumption is 2-5:1.
4. method according to claim 3, wherein, in step (1), the mass ratio of described leaching agent and described waste water neutralize gypsum tailings consumption is 2-3:1.
5., according to the method in claim 1,3 and 4 described in any one, wherein, in step (1), described leaching agent is at least one in sulfuric acid, hydrochloric acid, nitric acid, hydrofluoric acid and chloroazotic acid.
6. method according to claim 1, 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, described waste water neutralize gypsum tailings expose in atmosphere time≤6h.
8. method according to claim 1, wherein, in described removal of impurities operation, described contact reacts is under agitation carried out, and the reaction times is 10-60 minute.
9. method according to claim 1, wherein, relative to the described clear liquid of 100 weight parts, the consumption of CaO is 0.5-2 weight part, and the consumption of gac is 0.5-2 weight part.
10. method 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, and under tin anhydride solution exists, carry out electrolysis, current density is 400A/m 2, electrolysis temperature is 40-50 DEG C, and bath voltage is 4.5V, after 8-24h is carried out in electrolysis, changes negative plate.
11. methods according to claim 1, wherein, described waste water neutralize gypsum tailings contains the titanium dioxide of 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, the silicon-dioxide of 1-3 % by weight, the aluminium sesquioxide of 0.1-1 % by weight and 0.1-1 % by weight.
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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
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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