CN103352122A - Method for efficiently removing iron in solution - Google Patents
Method for efficiently removing iron in solution Download PDFInfo
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- CN103352122A CN103352122A CN2013102463893A CN201310246389A CN103352122A CN 103352122 A CN103352122 A CN 103352122A CN 2013102463893 A CN2013102463893 A CN 2013102463893A CN 201310246389 A CN201310246389 A CN 201310246389A CN 103352122 A CN103352122 A CN 103352122A
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Abstract
The invention discloses a method for efficiently removing iron in a solution. The method comprises the following steps of: adding an iron-to-be-removed solution into a specially-designed reaction tank, and controlling the temperature of the reaction tank between 45 DEG C and 98 DEG C; adding an oxidant, a reductant and a regulator according to the property of the iron-to-be-removed solution to establish a self-balance catalytic reaction system, wherein the oxidant, the reductant and the regulator meet the condition for the self-balance catalytic reaction system; and meanwhile, introducing air or oxygen-enriched air or oxygen to enable iron in the iron-to-be-removed solution to rapidly generate needle ironstone under the condition of mechanical stirring until the iron in the iron-to-be-removed solution is completely removed. The method is simple, stable and reliable in technological process, low in cost and high in reaction speed and efficiency; the iron concentration of the iron-removed solution is low; and the particle size of the separated needle ironstone is easy to control.
Description
Technical field
The present invention relates to a kind of method that efficiently removes iron in the solution, particularly a kind of self-equilibrating redox catalysis goethite process.
Background technology
The problem that removes iron from iron-containing liquor is prevalent in the industries such as metallurgy, chemical industry, material, to reach the purpose of cleansing soln.Remove iron in the so-called solution, even the iron (Fe in the solution
2+, Fe
3+) generate difficulty soluble salt or oxide compound, then by solid-liquid separation iron is separated, and then the process that solution is purified.Be extracted as example with non-ferrous metal, nonferrous metals ore usually and the compound association of iron, in leaching or leaching process, iron enters leach liquor or extracting solution inevitably, and in order to obtain high-quality metal product and good technico-economical comparison, must at first the iron in leach liquor or the extracting solution be removed, degree of eliminating is more high better.
At present, from iron-containing liquor, remove the method for iron, in industrial production, use the most yellow potassium (or sodium, ammonium) siderotil method.Secondly also have goethite process and iron oxide process.Yellow potassium (or sodium, ammonium) siderotil method maturation is applied to industrial production reality, technology maturation.Its shortcoming is that cost is higher, and the iron vitriol slag iron content is lower, and the quantity of slag is large, and isolated iron vitriol slag is Industrial Solid Waste substantially, can not fully utilize.And traditional goethite process, even the iron in the solution generates nature iron ore---pyrrhosiderite (FeOOH or Fe
2O
3.H
2O) precipitation, and then remove iron in the solution, although the method scum iron content is higher, scum can be realized comprehensive utilization, and the condition that generates is relatively harsher, and production operation is restive, although theoretical investigation is a lot, uses wideless.Especially in sulfate system, separate out with the state of pyrrhosiderite for making iron, necessary strict red-tape operati condition especially must be controlled the ferric iron (Fe in the solution
3+) concentration is not more than 1g/L.Avoid generating carphosiderite, the ironic hydroxide of colloid, make to remove the iron process and can't proceed.To avoid simultaneously the generation of yellow potassium (or sodium, ammonium) siderotil.Temperature of reaction should be greater than 90 ℃.Traditional goethite process removes the iron in the solution, and iron removal is longer, and efficient is low, and energy consumption and comprehensive cost are all higher.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned prior art, provide a kind of technological process simple, reliable and stable, cost is low, and speed of response is fast, and efficient is high, and it is low that the solution after the deironing contains concentration of iron, the method for removing iron that the pyrrhosiderite granularity of separating out is easy to control.It is self-equilibrating redox catalysis goethite process.
The present invention for the technical scheme that solves its technical problem employing is:
A kind of method that efficiently removes iron in the solution, comprise and to treat to add custom-designed reactive tank except ferrous solution, control reactive tank temperature is between 45 ℃ to 98 ℃, according to treating that the character except ferrous solution adds oxygenant, reductive agent and the conditioning agent that satisfies self-equilibrating catalystic converter system condition, set up the self-equilibrating catalystic converter system, blast simultaneously air or oxygen-rich air or oxygen, under the mechanical stirring condition, impel the iron for the treatment of except in the ferrous solution to generate rapidly pyrrhosiderite, until will treat to remove complete except the iron in the ferrous solution.
Further, in described self-equilibrating catalystic converter system, chemical reaction between the reactant that adds reaches dynamic molecular balance with the reactant and the chemical reaction between the reaction product that add, and then the chemical reaction process in the reaction system is constantly carried out towards the reaction product direction, until reaction end.
Preferably, the actual add-on of described oxygenant will be for treating except the ferrous iron (Fe in the ferrous solution
2+) all be oxidized to ferric iron (Fe
3+) 0～2.5 times of required oxygenant calculated value, the actual add-on of described reductive agent will be for treating except the ferric iron (Fe in the ferrous solution
3+) Restore All is ferrous iron (Fe
2+) 0～2.5 times of required reductive agent calculated value, the add-on of described conditioning agent is 0.2～2.5 times that treats except iron content total amount in the ferrous solution.
Preferably, described oxygenant, reductive agent and conditioning agent can be solid, liquid or gas, and the adding mode can be disposable adding, also can be that discontinuous adds or adds continuously.
Preferably, describedly treat that pH value except ferrous solution is between 0.5 to 6.5.
Preferably, the selection condition of described oxygenant is that its oxidizing potential is enough to and will treats except the ferrous iron (Fe in the ferrous solution under the specified conditions of reaction system
2+) be oxidized to ferric iron (Fe
3+), the adding of described oxygenant can be a kind of, two or more.
Preferably, the selection condition of described reductive agent is that its reduction potential is enough to and will treats except the ferric iron (Fe in the ferrous solution under the specified conditions of reaction system
3+) be reduced to ferrous iron (Fe
2+), the adding of described reductive agent can be a kind of, two or more.
Preferably, the selection condition of described conditioning agent be can the conditioned reaction system under the specified conditions of reaction system in the balance of each chemical reaction, make it to satisfy the formation condition of pyrrhosiderite, the adding of described conditioning agent can be a kind of, two or more.
Preferably, described oxygenant can be air, oxygen, sodium chlorate or hydrogen peroxide, and described reductive agent can be copper powder, iron powder, manganese powder or cuprous chloride.
Preferably, described conditioning agent has the reactive behavior with acid or alkali, can be in metallic copper, metallic zinc, manganese metal, cobalt metal, metallic iron, cupric oxide, zinc oxide, ferric oxide, ferric oxide, yellow soda ash, Vanadium Pentoxide in FLAKES, the sulfurous gas any one, also can be any two or the mixture more than two kinds in these materials.
The invention has the beneficial effects as follows: 1. the deferrization process process stabilization is reliable, and is simple to operate, is easy to control.2. deironing speed of response is fast, by control self-equilibrating condition, can control the degree of deironing time, deironing and the granularity of the pyrrhosiderite of separating out.3. the deironing cost is low.4. be that chlorate system, sulfate system or the two mixed system are all applicable equally, be particularly useful for sulfate system.5. to the full concentration of iron in the iron-containing liquor or ferrous iron concentration or the unrestricted condition of ferric iron concentration, no matter its concentration is high or low does not affect normally carrying out of iron removal.What be worth special proposition is for sulfate system, and the concentration of sulfate radical does not affect normally carrying out of iron removal.6. by condition control, can remove simultaneously the silicon in the solution.
Embodiment
According to a kind of method that efficiently removes iron in the solution provided by the invention, comprise and to treat to add custom-designed reactive tank except ferrous solution, control reactive tank temperature is between 45 ℃ to 98 ℃, according to treating that the character except ferrous solution adds oxygenant, reductive agent and the conditioning agent that satisfies self-equilibrating catalystic converter system condition, set up the self-equilibrating catalystic converter system, blast simultaneously air or oxygen-rich air or oxygen, under the mechanical stirring condition, impel the iron for the treatment of except in the ferrous solution to generate rapidly pyrrhosiderite, until will treat to remove complete except the iron in the ferrous solution.So-called self-equilibrating catalystic converter system, treat exactly to reach a metastable running balance except the reaction system that the chemical reaction processes such as the redox reaction in the ferrous solution, the reaction that generates pyrrhosiderite and other chemical reaction form, and this balance not only is conducive to the continuous generation of pyrrhosiderite, and the formation reaction process of pyrrhosiderite there is certain katalysis, make iron in the solution constantly generate goethite precipitation and be removed, until reaction end.Reactant (ABC) in the system: the chemical reaction between oxygenant, reductive agent, conditioning agent, the aqueous solution, oxygen, ferrous iron and the ferric iron can generate pyrrhosiderite (FeOOH or Fe
2O
3.H
2O) and other reaction product, other reaction product except pyrrhosiderite can be further with above-mentioned reactant (ABC) in one or more chemical reactions occur, and reach a dynamic molecular balance, make simultaneously the reaction process that generates pyrrhosiderite obtain catalysis.
The actual add-on of oxygenant will be for treating except the ferrous iron (Fe in the ferrous solution
2+) all be oxidized to ferric iron (Fe
3+) 0～2.5 times of required oxygenant calculated value, the actual add-on of reductive agent will be for treating except the ferric iron (Fe in the ferrous solution
3+) Restore All is ferrous iron (Fe
2+) 0～2.5 times of required reductive agent calculated value, the add-on of conditioning agent is 0.2～2.5 times that treats except iron content total amount in the ferrous solution.
Oxygenant, reductive agent and conditioning agent can be solid, liquid or gas, and the adding mode can be disposable adding, also can be that discontinuous adds or adds continuously.Wait to remove the pH value of ferrous solution between 0.5 to 6.5.
The selection condition of oxygenant is that its oxidizing potential is enough to and will treats except the ferrous iron (Fe in the ferrous solution under the specified conditions of reaction system
2+) be oxidized to ferric iron (Fe
3+), for example: select air, oxygen, sodium chlorate or hydrogen peroxide as oxygenant, the adding of oxygenant can be a kind of, two or more.The selection condition of reductive agent is that its reduction potential is enough to and will treats except the ferric iron (Fe in the ferrous solution under the specified conditions of reaction system
3+) be reduced to ferrous iron (Fe
2+), for example: select copper powder, iron powder, manganese powder or cuprous chloride as reductive agent, the adding of reductive agent can be a kind of, two or more.The selection condition of conditioning agent be can the conditioned reaction system under the specified conditions of reaction system in the balance of each chemical reaction, make it to satisfy the formation condition of pyrrhosiderite, the adding of conditioning agent can be a kind of, two or more.
Conditioning agent has the reactive behavior with acid or alkali, can be in metallic copper, metallic zinc, manganese metal, cobalt metal, metallic iron, cupric oxide, zinc oxide, ferric oxide, ferric oxide, yellow soda ash, Vanadium Pentoxide in FLAKES, the sulfurous gas any one, also can be any two or the mixture more than two kinds in these materials.
Churned mechanically purpose is in order to keep each reactant and the reaction product relative degree of uniformity in reaction system.The air that blasts simultaneously or oxygen-rich air or oxygen are to add as reactant, are the prerequisites that guarantees the self-equilibrating catalystic converter system on the one hand, can reduce on the other hand the power consumption of stirring.
By control reaction system self-equilibrating condition, can control the time of whole iron removal between 15Min to 300Min.By control reaction system self-equilibrating condition, can control separate out the solid pyrrhosiderite granularity between 0.05 μ m to 1000 μ m.By control reaction system self-equilibrating condition, can control the solution iron content that removes behind the iron between 0.01g/L to 0.001mg/L.
In addition, can design a reaction system automatic control system, the impact by automatic control system elimination human factor makes each control condition or the parameter of reaction system relatively stable.For example, automatic temperature control system; Material adds and the discharge automatic control system; Operating parameters automatic control system etc.
Specify below by three examples and in ferrous solution to be removed, to add the effect that oxygenant, reductive agent and conditioning agent carry out deironing.Oxygenant, reductive agent and conditioning agent all add in the example one, and namely the add-on of three kinds of reactants only adds reductive agent and conditioning agent all greater than 0 in the example two, the oxygenant add-on is 0, only add conditioning agent in the example three, oxygenant, reductive agent add-on are 0, and be specific as follows:
Example one ferrous solution to be removed (L01) 800mL, solution contains full iron 80g/L, ferrous iron 57g/L wherein, ferric iron 23g/L adds in the high pin beaker of 1000mL, 80 ℃ of control temperature, pass into air (flow is 1.2L/min), then add reductive agent and conditioning agent: copper powder 50g, cupric oxide powder 55.3g, iron powder 20g.The adding of reductive agent and conditioning agent should begin to add in rear 120 minutes complete in reaction.Reaction is 180 minutes under agitation condition.The pH value self-equilibrating of solution is about 3.5 ± 0.5 in the reaction process.Filter, get the solution sample and analyze, solution iron content 0.05mg/L, ie in solution iron content 0.05PPm, the iron in the solution removes; Get the filter residue analysis, filter residue iron content 56.9%.
Example two ferrous solution to be removed (L01) 800mL, solution contains full iron 80g/L, ferrous iron 57g/L wherein, ferric iron 23g/L adds in the high pin beaker of 1000mL (SB01).80 ℃ of control temperature pass into oxygen (flow is 0.5L/min), then add reductive agent and conditioning agent: copper powder 30g, zinc oxide (ZnO) powder 50g, cupric oxide (CuO) powder 57.2g.The adding of reductive agent and conditioning agent should begin to add in rear 60 minutes complete in reaction.Continue oxidizer (airborne oxygen) in the whole process of reaction: take out solution in the beaker (SB01) with pump to air atomization nozzle, and then be back in the beaker (SB01), reaction is 90 minutes under agitation condition.The pH value self-equilibrating of solution is about 4.0 ± 1.0 in the reaction process.Filter, get the solution sample and analyze, solution iron content 0.03mg/L, ie in solution iron content 0.03PPm, the iron in the solution removes; Get the filter residue analysis, filter residue iron content 57.7%.
Example three ferrous solution to be removed (L03) 800mL, solution contains full iron 20g/L, ferrous iron 12g/L wherein, ferric iron 8g/L, add in the high pin beaker of 1000mL, 80 ℃ of control temperature pass into air (flow is 1.5L/min), then add conditioning agent: iron powder 5g, ferric oxide (FeO) powder 20g, zinc oxide (ZnO) powder 29.2g, the adding of conditioning agent should add in the reaction beginning complete in rear 30 minutes, and reaction is 45 minutes under agitation condition.The pH value self-equilibrating of solution is about 4.0 ± 1.0 in the reaction process.Filter, get the solution sample and analyze, solution iron content 0.02mg/L, ie in solution iron content 0.02PPm, the iron in the solution removes; Get the filter residue analysis, filter residue iron content 58.7%.
Above-described embodiment is only for explanation the present invention's; and be not that the present invention is limited; the those of ordinary skill in relevant technologies field; in the situation that does not break away from the spirit and scope of the present invention; can also make a variety of changes and modification; therefore all technical schemes that are equal to also belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (10)
1. method that efficiently removes iron in the solution, it is characterized in that: comprise adding custom-designed reactive tank with treating except ferrous solution, control reactive tank temperature is between 45 ℃ to 98 ℃, according to treating that the character except ferrous solution adds oxygenant, reductive agent and the conditioning agent that satisfies self-equilibrating catalystic converter system condition, set up the self-equilibrating catalystic converter system, blast simultaneously air or oxygen-rich air or oxygen, under the mechanical stirring condition, impel the iron for the treatment of except in the ferrous solution to generate rapidly pyrrhosiderite, until will treat to remove complete except the iron in the ferrous solution.
2. described a kind of method that efficiently removes iron in the solution according to claim 1, it is characterized in that: in described self-equilibrating catalystic converter system, chemical reaction between the reactant that adds reaches dynamic molecular balance with the reactant and the chemical reaction between the reaction product that add, and then the chemical reaction process in the reaction system is constantly carried out towards the reaction product direction, until reaction end.
3. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2, it is characterized in that: the actual add-on of described oxygenant will be for treating except the ferrous iron (Fe in the ferrous solution
2+) all be oxidized to ferric iron (Fe
3+) 0～2.5 times of required oxygenant calculated value, the actual add-on of described reductive agent will be for treating except the ferric iron (Fe in the ferrous solution
3+) Restore All is ferrous iron (Fe
2+) 0～2.5 times of required reductive agent calculated value, the add-on of described conditioning agent is 0.2～2.5 times that treats except iron content total amount in the ferrous solution.
4. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2, it is characterized in that: described oxygenant, reductive agent and conditioning agent can be solid, liquid or gas, the adding mode can be disposable adding, also can be that discontinuous adds or adds continuously.
5. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2 is characterized in that: describedly treat that pH value except ferrous solution is between 0.5 to 6.5.
6. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2 is characterized in that: the selection condition of described oxygenant is that its oxidizing potential is enough to treat ferrous iron (Fe except in the ferrous solution under the specified conditions of reaction system
2+) be oxidized to ferric iron (Fe
3+), the adding of described oxygenant can be a kind of, two or more.
7. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2 is characterized in that: the selection condition of described reductive agent is that its reduction potential is enough to treat ferric iron (Fe except in the ferrous solution under the specified conditions of reaction system
3+) be reduced to ferrous iron (Fe
2+), the adding of described reductive agent can be a kind of, two or more.
8. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2, it is characterized in that: the selection condition of described conditioning agent be can the conditioned reaction system under the specified conditions of reaction system in the balance of each chemical reaction, make it to satisfy the formation condition of pyrrhosiderite, the adding of described conditioning agent can be a kind of, two or more.
9. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2, it is characterized in that: described oxygenant can be air, oxygen, sodium chlorate or hydrogen peroxide, described reductive agent can be copper powder, iron powder, manganese powder or cuprous chloride.
10. described a kind of method that efficiently removes iron in the solution according to claim 1 and 2, it is characterized in that: described conditioning agent has the reactive behavior with acid or alkali, can be in metallic copper, metallic zinc, manganese metal, cobalt metal, metallic iron, cupric oxide, zinc oxide, ferric oxide, ferric oxide, yellow soda ash, Vanadium Pentoxide in FLAKES, the sulfurous gas any one, also can be any two or the mixture more than two kinds in these materials.
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Cited By (8)
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|---|---|---|---|---|
| CN103911511A (en) * | 2014-04-28 | 2014-07-09 | 北京矿冶研究总院 | Method for removing iron from zinc solution |
| CN103924083A (en) * | 2014-04-28 | 2014-07-16 | 北京矿冶研究总院 | Method for reducing ferric iron by zinc leachate |
| CN106011468A (en) * | 2016-06-13 | 2016-10-12 | 云南祥云飞龙再生科技股份有限公司 | Method for removing ferrous ions from iron-containing zinc sulfate solution by using industrial enriched oxygen |
| CN106566926A (en) * | 2016-11-22 | 2017-04-19 | 江苏凯力克钴业股份有限公司 | Deironing device, and low-temperature continuous deironing method |
| CN106868304A (en) * | 2016-12-27 | 2017-06-20 | 河南豫光锌业有限公司 | A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum |
| CN109942032A (en) * | 2017-12-20 | 2019-06-28 | 深圳泛科环保产业发展有限公司 | A kind of production technology of nickelous carbonate |
| CN111304693A (en) * | 2018-12-12 | 2020-06-19 | 格林美（江苏）钴业股份有限公司 | Iron removal method for reducing accumulated iron ions in electrodeposition solution |
| WO2023124935A1 (en) * | 2021-12-31 | 2023-07-06 | 比亚迪股份有限公司 | Method for separating iron element from brine and use thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911511A (en) * | 2014-04-28 | 2014-07-09 | 北京矿冶研究总院 | Method for removing iron from zinc solution |
| CN103924083A (en) * | 2014-04-28 | 2014-07-16 | 北京矿冶研究总院 | Method for reducing ferric iron by zinc leachate |
| CN103924083B (en) * | 2014-04-28 | 2016-08-24 | 北京矿冶研究总院 | Method for reducing ferric iron by zinc leachate |
| CN106011468A (en) * | 2016-06-13 | 2016-10-12 | 云南祥云飞龙再生科技股份有限公司 | Method for removing ferrous ions from iron-containing zinc sulfate solution by using industrial enriched oxygen |
| CN106566926A (en) * | 2016-11-22 | 2017-04-19 | 江苏凯力克钴业股份有限公司 | Deironing device, and low-temperature continuous deironing method |
| CN106566926B (en) * | 2016-11-22 | 2019-03-15 | 格林美（江苏）钴业股份有限公司 | A kind of deironing apparatus and low temperature continuous deferrization technique |
| CN106868304A (en) * | 2016-12-27 | 2017-06-20 | 河南豫光锌业有限公司 | A kind of method for reducing impurity content in zinc hydrometallurgy oxidation scum |
| CN109942032A (en) * | 2017-12-20 | 2019-06-28 | 深圳泛科环保产业发展有限公司 | A kind of production technology of nickelous carbonate |
| CN111304693A (en) * | 2018-12-12 | 2020-06-19 | 格林美（江苏）钴业股份有限公司 | Iron removal method for reducing accumulated iron ions in electrodeposition solution |
| WO2023124935A1 (en) * | 2021-12-31 | 2023-07-06 | 比亚迪股份有限公司 | Method for separating iron element from brine and use thereof |
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