CN103993172B - The processing method of iron-containing liquor - Google Patents
The processing method of iron-containing liquor Download PDFInfo
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- CN103993172B CN103993172B CN201410221863.1A CN201410221863A CN103993172B CN 103993172 B CN103993172 B CN 103993172B CN 201410221863 A CN201410221863 A CN 201410221863A CN 103993172 B CN103993172 B CN 103993172B
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- iron
- containing liquor
- processing method
- ferric subsulfate
- ferric
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The present invention proposes the processing method of iron-containing liquor, including: the pH value of regulation iron-containing liquor is to 0.5~1.5;Make iron-containing liquor is settled out ferric subsulfate under elevated temperature and pressure conditions;The solution precipitated containing ferric subsulfate is carried out filtration treatment, in order to obtain filter cake and filtrate;And filter cake is carried out carrying out washing treatment, in order to obtaining ferric subsulfate product, wherein, high temperature is 180~220 degrees Celsius, and high pressure is 1.0~2.4MPa.Utilize said method can be effectively improved iron-containing liquor except ferrum rate, and ferrum therein is converted into recycling ferric subsulfate.
Description
Technical field
The present invention relates to field of metallurgy, specifically, the present invention relates to the processing method of iron-containing liquor.
Background technology
At present when wet production zinc, nickel, cobalt or other valuable metal, generally use acid leaching process, be leached at valuable metal
Time, the ferrum in Ore is also leached.The step for that subsequent purification operation comprising except ferrum, industry generally uses Huang (sodium,
Ammonium) siderotil or separation of iron in goethite form, after i.e. controlling to leach, liquid temp is under higher level, introduce in leachate sodium/potassium/ammonium from
Son, is combined to siderotil with wherein iron ion, or is bivalence by ferric iron back in leachate, is pin by ferrum under oxidative conditions
Iron mine removes.After filtration washing, send into tailing dam except the scum after ferrum to store up.After the method removes ferrum, the quantity of slag is big, this slag at present
Cannot use as resources circulation, do not only take up a large amount of soil store up and wherein the slow dissolution of harmful constituent to cause environment dirty
Dye.
Summary of the invention
It is contemplated that one of technical problem solved the most to a certain extent in correlation technique.To this end, the one of the present invention
Purpose is to propose the processing method of a kind of iron-containing liquor.Utilize the method can be by the ferrum in iron-containing liquor with ferric subsulfate
Form separate out and remove.
The processing method of iron-containing liquor according to an embodiment of the invention, including:
Regulate the pH value of described iron-containing liquor to 0.5~1.5;
Make under elevated temperature and pressure conditions described iron-containing liquor is settled out ferric subsulfate;
The solution precipitated containing ferric subsulfate is carried out filtration treatment, in order to obtain filter cake and filtrate;And
Described filter cake is carried out carrying out washing treatment, in order to obtain ferric subsulfate product,
Wherein, described high temperature is 180~220 degrees Celsius, and described high pressure is 1.0~2.4MPa.
Thus, by regulating the pH value of iron-containing liquor and controlling course of reaction process conditions, then alkali formula sulfur can be directly generated
Acid ferrum.Through said method, iron-containing liquor is processed, in the filtrate after precipitation not only the rate of deposition of iron ion up to 90% with
On, and it is few to be entrained with valence metal ion in ferric subsulfate.Therefore product is single ferric subsulfate, can apply to
Other operations or field.
It addition, the processing method of iron-containing liquor according to the above embodiment of the present invention can also have a following additional technical characteristic:
In some embodiments of the invention, described iron-containing liquor be wet production valuable metal sulfuric acid leaching after liquid.
In some embodiments of the invention, in described iron-containing liquor, ferric concentration is not less than 30g/L.Thus can enter one
Step improves except ferrum rate.
In some embodiments of the invention, at least one in potassium hydroxide, sodium hydroxide, hydrated ferric oxide., sulphuric acid is utilized
Regulate the pH value of described iron-containing liquor to 0.5~1.5.
In some embodiments of the invention, the time of described precipitation is 0.5~2.5h.Thus can improve further except ferrum aluminum.
In some embodiments of the invention, the part precipitated by described ferric subsulfate returns and is used for described precipitation.Thus
The deposition efficiency of ferric subsulfate can be improved further.
In some embodiments of the invention, described carrying out washing treatment is 3~5:1 to carry out according to liquid-solid mass ratio.Thus may be used
To improve the quality of ferric subsulfate further.
Accompanying drawing explanation
Fig. 1 is the flow chart of the method processing iron-containing liquor according to an embodiment of the invention.
Fig. 2 is the flow chart of the method processing iron-containing liquor in accordance with another embodiment of the present invention.
Fig. 3 is the XRD figure utilizing the method processing iron-containing liquor of one embodiment of the invention to process the ferric subsulfate obtained
Spectrum.
Detailed description of the invention
Embodiments of the invention are described below in detail, and the example of described embodiment is shown in the drawings, the most identical
Or similar label represents same or similar element or has the element of same or like function.Retouch below with reference to accompanying drawing
The embodiment stated is exemplary, it is intended to is used for explaining the present invention, and is not considered as limiting the invention.
In metallurgy industry, generally use wet process acid to leach and extract valuable metal, but a large amount of ferrum in Ore are the most immersed simultaneously
Go out, and then define substantial amounts of iron content leachate, however the method in existing removing iron content leachate exist more the quantity of slag big and
Slag cannot recycle can only be stored up, and takies the defect in a large amount of soil.Present inventors discovered unexpectedly that, it is not necessary to extra
Add other reagent, only by suitably controlling and regulate the condition of iron content leachate so that the ferrum in iron-containing liquor from
Son separates out with the form of ferric subsulfate, and in the ferric subsulfate separated out by the method, valuable metal impurity content is few,
May be used for other field to recycle, it is to avoid while storing up in a large number, improve the by-product kind of metallurgy industry.
The processing method of the iron-containing liquor of the embodiment of the present invention is described in detail below with reference to Fig. 1.The iron content of the embodiment of the present invention is molten
The processing method of liquid includes:
S100: regulation pH value
The processing method of iron-containing liquor goes for any iron-containing liquor, such as iron-containing liquor according to an embodiment of the invention
Can be pure iron-containing liquor, it is also possible to be liquid after the sulfuric acid leaching of wet production valuable metal.Can be such as nickel, cobalt,
The leachate of copper, zinc etc., thus utilizes said method effectively can enter the substantial amounts of iron content leachate produced in Metallurgy Industry
Row processes, and other valuable metal ions impurity contents of the ferric subsulfate simultaneously produced are few, therefore can be reused in it
His field.
According to a particular embodiment of the invention, in above-mentioned iron-containing liquor, ferric concentration is not less than 30g/L.Thus can enter one
Step improves iron ion therein and changes into the productivity of ferric subsulfate, in order to improve except ferrum rate.According to the concrete example of the present invention,
If ferric concentration is less than 30g/L, then easily generate hydration siderotil.And then affect purity and the productivity of ferric subsulfate.
According to a particular embodiment of the invention, above-mentioned iron-containing liquor is processed firstly the need of regulating the pH value of iron-containing liquor extremely
0.5~1.5.If it is low that pH value is easily caused ferric subsulfate rate of deposition less than less than 0.5, except ferrum rate is decreased obviously, if
PH value crosses the material generation up to having similar bloodstone one class more than 1.5.Therefore, the pH value of iron-containing liquor is regulated
Ferric subsulfate rate of deposition and purity can be significantly improved to 0.5~1.5.According to a particular embodiment of the invention, can be by adding
Enter acid or alkali regulation pH, such as, at least one in potassium hydroxide, sodium hydroxide, hydrated ferric oxide., sulphuric acid can be utilized to adjust
The pH value of joint iron-containing liquor is to 0.5~1.5.
S200: precipitation
According to a particular embodiment of the invention, further by iron-containing liquor that above-mentioned regulation to pH is 0.5~1.5 at high temperature and
Make under condition of high voltage to react inside it, and then make iron-containing liquor is settled out ferric subsulfate.Concrete according to the present invention
Embodiment, the condition of above-mentioned precipitation preferably 180~220 degrees Celsius and 1.0~2.4MPa pressure under carry out.Thus may be used
So that the iron ion in iron-containing liquor is precipitated out with the form of ferric subsulfate, it is not necessary to extra other reagent that adds, and then
Being possible not only to cost-effective can also avoiding and introduce other impurity, the method is simple, and it is notable to separate iron ion effect.
According to a particular embodiment of the invention, the time controlling precipitation can be 0.5~2.5h.Thus so that in iron-containing liquor
Iron ion be precipitated out fully, and then improve except ferrum rate.
According to a particular embodiment of the invention, the processing method of above-mentioned iron-containing liquor can also include: is precipitated by ferric subsulfate
A part as crystal seed return be used for precipitating.According to a particular embodiment of the invention, the amount of return can be according to generating alkali formula
Ferric sulphate precipitate amount is 1~8 times of return crystal seed amount and carries out, and thus can improve the precipitation capacity of ferric subsulfate further, carry
High iron-containing liquor except ferrum rate.
S300: filtration washing
According to a particular embodiment of the invention, further the solution of the above-mentioned ferric subsulfate being settled out is carried out filtration treatment,
To obtain filter cake and filtrate;And the filter cake being filtrated to get is carried out carrying out washing treatment, in order to obtain ferric subsulfate product.
According to a particular embodiment of the invention, above-mentioned carrying out washing treatment can be 3~5:1 to carry out according to liquid-solid mass ratio.Thus can enter
One step improves detersive efficiency, improves the quality of ferric subsulfate.According to the concrete example of the present invention, the ferric subsulfate obtained
Product can be with other operations or field, for example, it is possible to recycle as water purification agent.Thus can improve iron content further molten
The by-product value of liquid.
Embodiment 1
With reference to Fig. 2, taking liquid 1L after nickel laterite acidleach, wherein iron content is 42g/L (ferric iron content is 98%), containing acid
For 50g/L, add sodium hydroxide regulation pH to 1.2.Adding in autoclave, temperature is 200 degrees Celsius, and crystal seed 6 follows again
Ring, filters after reaction, washs with the water of 3 times of weight, finally dry, be precipitated thing.Through analyzing, liquid after acidleach
In ferrum rate of deposition be 90.6%, sedimentary XRD figure is composed as shown in Figure 3, from the figure 3, it may be seen that sedimentary thing be singly mutually
The ferric subsulfate of one.
Embodiment 2
With reference to Fig. 2, taking zinc lixiviating solution 1L, wherein iron content is 30g/L (ferric iron content is 98%).Add NaOH to adjust
Joint pH to 1.0, adds in autoclave, and temperature is 180 degrees Celsius, crystal seed 4 times circulation, filters, with 3 times of weights after reaction
The water of amount washs, and finally dries, is precipitated thing.Through analyzing, after acidleach, the ferrum rate of deposition in liquid is 95.0%, heavy
The thing of shallow lake thing is single ferric subsulfate mutually.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " concrete example ",
Or specific features, structure, material or the feature bag that the description of " some examples " etc. means to combine this embodiment or example describes
It is contained at least one embodiment or the example of the present invention.In this manual, need not pin to the schematic representation of above-mentioned term
To be identical embodiment or example.And, the specific features of description, structure, material or feature can be at any one
Or multiple embodiment or example combine in an appropriate manner.Additionally, in the case of the most conflicting, the technology of this area
Personnel the feature of the different embodiments described in this specification or example and different embodiment or example can be combined and
Combination.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is exemplary,
Being not considered as limiting the invention, those of ordinary skill in the art within the scope of the invention can be to above-described embodiment
It is changed, revises, replaces and modification.
Claims (6)
1. the processing method of an iron-containing liquor, it is characterised in that including:
Regulate the pH value of described iron-containing liquor to 0.5~1.5;
Make under elevated temperature and pressure conditions described iron-containing liquor is settled out ferric subsulfate;
The solution precipitated containing ferric subsulfate is carried out filtration treatment, in order to obtain filter cake and filtrate;And
Described filter cake is carried out carrying out washing treatment, in order to obtain ferric subsulfate product,
Wherein,
Described high temperature is 180~220 degrees Celsius, and described high pressure is 1.0~2.4MPa,
In described iron-containing liquor, ferric concentration is not less than 30g/L.
Processing method the most according to claim 1, it is characterised in that described iron-containing liquor is wet production valuable metal
Sulfuric acid leaching after liquid.
Processing method the most according to claim 1, it is characterised in that utilize potassium hydroxide, sodium hydroxide, hydroxide
At least one in ferrum, sulphuric acid regulates the pH value of described iron-containing liquor to 0.5~1.5.
Processing method the most according to claim 1, it is characterised in that the time of described precipitation is 0.5~2.5h.
Processing method the most according to claim 1, it is characterised in that the part that described ferric subsulfate precipitates is returned
It is back to be settled out ferric subsulfate.
Processing method the most according to claim 1, it is characterised in that described carrying out washing treatment is to be according to liquid-solid mass ratio
3~5:1 are carried out.
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CN106498442B (en) * | 2016-11-02 | 2018-04-10 | 中南大学 | A kind of antimony electrolyte selectivity iron removaling and the method for preparing ferrous oxalate |
CN106521555B (en) * | 2016-11-02 | 2018-04-20 | 中南大学 | A kind of method of antimony electrolyte selectivity iron removaling |
CN107010673A (en) * | 2017-04-18 | 2017-08-04 | 中国恩菲工程技术有限公司 | The method for preparing the mixture of hydration siderotil and ferric subsulfate |
CN111036642B (en) * | 2018-10-12 | 2021-10-29 | 天津海成能源工程技术有限公司 | Method for removing Fe in dichloroethane industrial waste3+Process for preparing (A) a |
CN109319843A (en) * | 2018-12-07 | 2019-02-12 | 贵州大龙汇成新材料有限公司 | A method of high purity manganese sulfate is prepared from poor manganese spar |
CN114405979A (en) * | 2021-12-20 | 2022-04-29 | 荆门市格林美新材料有限公司 | Cobalt-nickel tailing treatment method |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US3529957A (en) * | 1967-08-25 | 1970-09-22 | Sherritt Gordon Mines Ltd | Production of elemental sulphur and iron from iron sulphides |
US3730860A (en) * | 1972-02-18 | 1973-05-01 | Inspiration Cons Copper | Electrolytic recovery of copper from oxidizable cupriferous material |
US3923617A (en) * | 1974-08-15 | 1975-12-02 | Inspiration Cons Copper | Electrolytic recovery of zinc |
CN1875120A (en) * | 2003-11-03 | 2006-12-06 | 奥克斯安娜有限公司 | Leach extraction method |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS53123368A (en) * | 1977-04-02 | 1978-10-27 | Dowa Mining Co | Removal of arsenic |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3529957A (en) * | 1967-08-25 | 1970-09-22 | Sherritt Gordon Mines Ltd | Production of elemental sulphur and iron from iron sulphides |
US3730860A (en) * | 1972-02-18 | 1973-05-01 | Inspiration Cons Copper | Electrolytic recovery of copper from oxidizable cupriferous material |
US3923617A (en) * | 1974-08-15 | 1975-12-02 | Inspiration Cons Copper | Electrolytic recovery of zinc |
CN1875120A (en) * | 2003-11-03 | 2006-12-06 | 奥克斯安娜有限公司 | Leach extraction method |
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