CN103993172A - Iron-containing solution treatment method - Google Patents
Iron-containing solution treatment method Download PDFInfo
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- CN103993172A CN103993172A CN201410221863.1A CN201410221863A CN103993172A CN 103993172 A CN103993172 A CN 103993172A CN 201410221863 A CN201410221863 A CN 201410221863A CN 103993172 A CN103993172 A CN 103993172A
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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 invention provides an iron-containing solution treatment method, comprising the following steps: regulating the pH value of an iron-containing solution to 0.5-1.5; precipitating alkaline ferric sulfate in the iron-containing solution at high temperature of 180-220 DEG C and under high pressure of 1.0MPa to 2.4MPa; filtering the solution which contains the alkaline ferric sulfate precipitate to obtain a filter cake and filtrate; and washing the filter cake so as to obtain an alkaline ferric sulfate product. By adopting the method, the iron removal rate of the iron-containing solution can be increased effectively, and the iron in the iron-containing solution can be transformed into recyclable alkaline ferric sulfate.
Description
Technical field
The present invention relates to field of metallurgy, particularly, the present invention relates to the treatment process of iron-containing liquor.
Background technology
At present when wet production zinc, nickel, cobalt or other valuable metal, conventionally adopt acid leaching process, when valuable metal is leached, the iron in ore is also leached.In follow-up cleaning section, comprise this step of deironing, in industry, conventionally adopt yellow (sodium, ammonium) siderotil or separation of iron in goethite form, control and leach rear liquid temp under higher level, in leach liquor, introduce sodium/potassium/ammonium ion, be combined to siderotil with iron ion wherein, or ferric iron in leach liquor is reduced to divalence, under oxidizing condition, iron is to pyrrhosiderite and removes.Scum after deironing is sent into tailing dam after washing after filtration and is stored up.After the method deironing, the quantity of slag is large, and this slag cannot be used as resources circulation at present, not only take that a large amount of soils are stored up and wherein the slow stripping of unwanted component caused environmental pollution.
Summary of the invention
The present invention is intended to solve at least to a certain extent one of technical problem in correlation technique.For this reason, one object of the present invention is to propose a kind for the treatment of process of iron-containing liquor.Utilize the method the iron in iron-containing liquor can be separated out and removed with the form of ferric subsulfate.
The treatment process of iron-containing liquor according to an embodiment of the invention, comprising:
Regulate pH value to 0.5～1.5 of described iron-containing liquor;
Under high temperature and high pressure condition, make to be settled out ferric subsulfate in described iron-containing liquor;
The solution that contains ferric subsulfate precipitation is carried out to filtration treatment, to obtain filter cake and filtrate; And
Described filter cake is carried out to carrying out washing treatment, 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 reaction process processing condition, can directly generate ferric subsulfate.Through aforesaid method, iron-containing liquor is processed, in the filtrate after precipitation, not only the deposition rate of iron ion can reach more than 90%, and it is few in ferric subsulfate, to be entrained with valence metal ion.Therefore product is single ferric subsulfate, can be applied to other operations or field.
In addition, the treatment process of iron-containing liquor according to the above embodiment of the present invention can also have following additional technical characterictic:
In some embodiments of the invention, described iron-containing liquor is liquid after the sulfuric acid leaching of wet production valuable metal.
In some embodiments of the invention, in described iron-containing liquor, ferric concentration is not less than 30g/L.Can further improve deironing rate thus.
In some embodiments of the invention, utilize at least one in potassium hydroxide, sodium hydroxide, ironic hydroxide, sulfuric acid to regulate pH value to 0.5～1.5 of described iron-containing liquor.
In some embodiments of the invention, the time of described precipitation is 0.5～2.5h.Can further improve deironing aluminium thus.
In some embodiments of the invention, a part for described ferric subsulfate precipitation is returned for described precipitation.Can further improve the deposition efficiency of ferric subsulfate thus.
In some embodiments of the invention, described carrying out washing treatment is that 3～5:1 carries out according to liquid-solid mass ratio.Can further improve the quality of ferric subsulfate thus.
Accompanying drawing explanation
Fig. 1 is the schema of processing according to an embodiment of the invention the method for iron-containing liquor.
Fig. 2 is the schema of processing in accordance with another embodiment of the present invention the method for iron-containing liquor.
Fig. 3 utilizes the method for the processing iron-containing liquor of one embodiment of the invention to process the XRD figure spectrum of the ferric subsulfate obtain.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Below by the embodiment being described with reference to the drawings, be exemplary, be intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
In metallurgy industry, conventionally adopt wet process acid to leach and extract valuable metal, yet a large amount of iron in ore are also leached simultaneously, and then formed a large amount of iron content leach liquors, yet more there is the quantity of slag greatly in existing method of removing in iron content leach liquor and slag cannot recycle and can only store up, and take the defect in a large amount of soils.The present inventor is surprised to find that, without extra other reagent that add, only by suitably controlling and regulate the condition of iron content leach liquor, can so that the iron ion in iron-containing liquor with the form of ferric subsulfate, separate out, and in the ferric subsulfate of separating out by the method, valuable metal foreign matter content is few, can recycle for other field, when having avoided storing up in a large number, improve the by product kind of metallurgy industry.
Below with reference to Fig. 1, describe the treatment process of the iron-containing liquor of the embodiment of the present invention in detail.The treatment process of the iron-containing liquor of the embodiment of the present invention comprises:
S100: regulate pH value
The treatment process of iron-containing liquor goes for any iron-containing liquor according to an embodiment of the invention, and for example iron-containing liquor can be pure iron-containing liquor, can be also liquid after the sulfuric acid leaching of wet production valuable metal.Such as the leach liquor that can be nickel, cobalt, copper, zinc etc., utilize thus aforesaid method effectively to a large amount of iron content leach liquor producing in Metallurgy Industry, to process, other valuable metal ions foreign matter contents of produced simultaneously ferric subsulfate are few, therefore can be recycled in other field.
According to a particular embodiment of the invention, in above-mentioned iron-containing liquor, ferric concentration is not less than 30g/L.The iron ion that can further improve thus wherein changes into the productive rate of ferric subsulfate, to improve deironing rate.According to concrete example of the present invention, if ferric concentration, lower than 30g/L, easily generates hydration siderotil.And then affect purity and the productive rate of ferric subsulfate.
According to a particular embodiment of the invention, process pH value to 0.5～1.5 that first above-mentioned iron-containing liquor needs to regulate iron-containing liquor.If pH value is lower than easily causing ferric subsulfate deposition rate low below 0.5, deironing rate obviously declines, if pH value is too high to surpassing 1.5, the material that has similar rhombohedral iron ore one class generates.Therefore, the pH value of iron-containing liquor is adjusted to 0.5～1.5 and can significantly improves ferric subsulfate deposition rate and purity.According to a particular embodiment of the invention, can by adding acid or alkali to regulate pH, for example, can utilize pH value to 0.5～1.5 of at least one the adjusting iron-containing liquor in potassium hydroxide, sodium hydroxide, ironic hydroxide, sulfuric acid.
S200: precipitation
According to a particular embodiment of the invention, the iron-containing liquor that is 0.5～1.5 by the above-mentioned pH of being adjusted to further makes its inside react under high temperature and high pressure condition, and then makes to be settled out in iron-containing liquor ferric subsulfate.According to a particular embodiment of the invention, the condition optimization of above-mentioned precipitation carries out under the pressure of 180～220 degrees Celsius and 1.0～2.4MPa.Can without additionally adding other reagent, and then not only can save cost and can also avoid introducing other impurity so that the iron ion in iron-containing liquor is precipitated out with the form of ferric subsulfate thus, the method is simple, and separation of iron ion effect is remarkable.
According to a particular embodiment of the invention, controlling the time of precipitating can be 0.5～2.5h.Thus can be so that the iron ion in iron-containing liquor be precipitated out fully, and then improve deironing rate.
According to a particular embodiment of the invention, the treatment process of above-mentioned iron-containing liquor can also comprise: a part for ferric subsulfate precipitation is returned for precipitation as crystal seed.According to a particular embodiment of the invention, the amount of returning can be to return to 1～8 times of crystal seed amount to carry out according to generating ferric subsulfate precipitation capacity, can further improve thus the precipitation capacity of ferric subsulfate, improves the deironing rate of iron-containing liquor.
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 to filtration treatment, to obtain filter cake and filtrate; And the filter cake that filtration is obtained carries out carrying out washing treatment, to obtain ferric subsulfate product.According to a particular embodiment of the invention, above-mentioned carrying out washing treatment can be that 3～5:1 carries out according to liquid-solid mass ratio.Can further improve detersive efficiency thus, improve the quality of ferric subsulfate.According to concrete example of the present invention, the ferric subsulfate product obtaining can other operations or field, for example, can be used as water purification agent recycling.Can further improve the by-product value of iron-containing liquor thus.
Embodiment 1
With reference to figure 2, get liquid 1L after nickel laterite acidleach, wherein iron level is 42g/L (ferric iron content is 98%), containing acid, is 50g/L, adds sodium hydroxide adjusting pH to 1.2.Add in autoclave, temperature is 200 degrees Celsius, and 6 times of circulations of crystal seed are filtered after reaction, with the water of 3 times of weight, wash, and finally dry, and are precipitated thing.By analysis, the iron deposition rate after acidleach in liquid is 90.6%, and as shown in Figure 3, as shown in Figure 3, sedimentary thing is single ferric subsulfate to sedimentary XRD figure spectrum mutually.
Embodiment 2
With reference to figure 2, get zinc lixiviating solution 1L, wherein iron level is 30g/L (ferric iron content is 98%).Add NaOH to regulate pH to 1.0, add in autoclave, temperature is 180 degrees Celsius, and 4 times of circulations of crystal seed are filtered after reaction, with the water of 3 times of weight, wash, and finally dry, and are precipitated thing.By analysis, the iron deposition rate after acidleach in liquid is 95.0%, and sedimentary thing is single ferric subsulfate mutually.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, to the schematic statement of above-mentioned term needn't for be identical embodiment or example.And, the specific features of description, structure, material or feature can one or more embodiment in office or example in suitable mode combination.In addition,, not conflicting in the situation that, those skilled in the art can carry out combination and combination by the feature of the different embodiment that describe in this specification sheets or example and different embodiment or example.
Although illustrated and described embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, and those of ordinary skill in the art can change above-described embodiment within the scope of the invention, modification, replacement and modification.
Claims (7)
1. a treatment process for iron-containing liquor, is characterized in that, comprising:
Regulate pH value to 0.5～1.5 of described iron-containing liquor;
Under high temperature and high pressure condition, make to be settled out ferric subsulfate in described iron-containing liquor;
The solution that contains ferric subsulfate precipitation is carried out to filtration treatment, to obtain filter cake and filtrate; And
Described filter cake is carried out to carrying out washing treatment, to obtain ferric subsulfate product,
Wherein,
Described high temperature is 180～220 degrees Celsius, and described high pressure is 1.0～2.4MPa.
2. treatment process according to claim 1, is characterized in that, described iron-containing liquor is liquid after the sulfuric acid leaching of wet production valuable metal.
3. treatment process according to claim 1, is characterized in that, in described iron-containing liquor, ferric concentration is not less than 30g/L.
4. treatment process according to claim 1, is characterized in that, utilizes at least one in potassium hydroxide, sodium hydroxide, ironic hydroxide, sulfuric acid to regulate pH value to 05～1.5 of described iron-containing liquor.
5. treatment process according to claim 1, is characterized in that, the time of described precipitation is 0.5～2.5h.
6. treatment process according to claim 1, is characterized in that, a part for described ferric subsulfate precipitation is returned for described precipitation.
7. treatment process according to claim 1, is characterized in that, described carrying out washing treatment is that 3～5:1 carries out according to liquid-solid mass ratio.
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| CN103993172B CN103993172B (en) | 2016-11-02 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498442A (en) * | 2016-11-02 | 2017-03-15 | 中南大学 | A kind of antimony electrolyte selectivity removes ferrum the method for preparing Ferrox. |
| CN106521555A (en) * | 2016-11-02 | 2017-03-22 | 中南大学 | Selective iron removal method for antimony electrolyte |
| 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 |
| 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 |
| CN111036642A (en) * | 2018-10-12 | 2020-04-21 | 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 |
| 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 |
| CN116770069A (en) * | 2023-06-25 | 2023-09-19 | 四川顺应动力电池材料有限公司 | Method for removing iron ions and recycling acid from high-concentration iron-containing waste liquid |
| CN117613262A (en) * | 2024-01-10 | 2024-02-27 | 武汉理工大学 | Application of iron-based sulfate positive electrode material in sodium ion battery |
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Patent Citations (5)
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| US3730860A (en) * | 1972-02-18 | 1973-05-01 | Inspiration Cons Copper | Electrolytic recovery of copper from oxidizable cupriferous material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498442A (en) * | 2016-11-02 | 2017-03-15 | 中南大学 | A kind of antimony electrolyte selectivity removes ferrum the method for preparing Ferrox. |
| CN106521555A (en) * | 2016-11-02 | 2017-03-22 | 中南大学 | Selective iron removal method for antimony electrolyte |
| 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 |
| CN111036642A (en) * | 2018-10-12 | 2020-04-21 | 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 |
| 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 |
| CN116770069A (en) * | 2023-06-25 | 2023-09-19 | 四川顺应动力电池材料有限公司 | Method for removing iron ions and recycling acid from high-concentration iron-containing waste liquid |
| CN117613262A (en) * | 2024-01-10 | 2024-02-27 | 武汉理工大学 | Application of iron-based sulfate positive electrode material in sodium ion battery |
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| CN103993172B (en) | 2016-11-02 |
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