CN104531997A - Method for removing iron from magnesium-containing sulfuric acid leaching liquid - Google Patents
Method for removing iron from magnesium-containing sulfuric acid leaching liquid Download PDFInfo
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- CN104531997A CN104531997A CN201410819256.5A CN201410819256A CN104531997A CN 104531997 A CN104531997 A CN 104531997A CN 201410819256 A CN201410819256 A CN 201410819256A CN 104531997 A CN104531997 A CN 104531997A
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- iron
- magnesium
- leaching liquid
- deironing
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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 relates to a method for removing iron from a magnesium-containing sulfuric acid leaching liquid. The magnesium-containing sulfuric acid leaching liquid comprises 5-30 g/L of magnesium, 5-50 g/L of iron and other metals which mainly comprise copper, nickel and cobalt and have the concentration not higher than 10 g/L, wherein the concentration of H<+1> is 0.1-3.0mol/L. The method is characterized by comprising the following steps: adding an oxidant and oxidizing ferrous iron in the sulfuric acid leaching liquid into ferric iron; heating the leaching liquid to a temperature of 85-100 DEG C, fully stirring, in 2.5-7.0 hours, sequentially dropwise adding a 20-40wt% sodium salt solution and a MgO suspension in which the ratio of liquid to solid is (5:1)-(10:1) until the pH is 2.0-2.5 so as to remove iron, reacting and filtering to obtain iron-removal slag and an iron-removal leaching liquid; extracting copper from the iron-removal leaching liquid, precipitating nickel and cobalt with MgO, and concentrating and crystallizing magnesium salt to respectively recover copper, nickel, cobalt and magnesium. The method is low in cost, simple in process and operation, environmentally friendly and high in iron-removal efficiency.
Description
Technical field
The present invention relates to a kind of from the method containing deironing the sulphuric leachate of magnesium, belong to field of hydrometallurgy.
Background technology
Non-ferrous metal deposit is mostly complex ore, and the sulphuric leachate that its hydrometallurgy obtains often has containing valency metal species many, simultaneously Mg, Fe and H
+the feature that concentration is higher.
For this type of solution valuable metal Separation and Recovery, top priority is removing iron contamination.Common method for removing iron has: yellow modumite method, hematite process, moderate water-cut stage, wherein hematite process equipment requirements high, need High Temperature High Pressure cost intensive; Moderate water-cut stage terminal pH is higher and ferric hydroxide colloid filtration difficulty, valuable metal are mingled with seriously; Yellow modumite method is ripe and industrialized main method for removing iron, and current yellow modumite method deironing is roughly following process: add sodium salt as precipitation agent, slowly add Na in reaction process
2cO
3, NaHCO
3deng the H that neutralizing agent neutralization reaction process generates
2sO
4, making reaction continue to proceed to terminal pH is about 2.0.If above-mentioned iron removal is applied to Mg, Fe and H
+in the sulphuric leachate that concentration is higher, its Na
2cO
3, NaHCO
3consumption is large, deironing cost intensive.The more important thing is, owing to containing Mg in sulphuric leachate, in iron removal, add a large amount of Na
,mix with Mg original in leach liquor and exist, Na, Mg all cannot reclaim, and not only cause the wasting of resources, increase the difficulty of wastewater treatment simultaneously, so existing yellow modumite method has obvious drawback for containing deironing in the sulphuric leachate of magnesium.
The present invention on this background, creatively proposes MgO for the sulphuric leachate containing magnesium and substitutes Na
2cO
3, NaHCO
3deng the yellow modumite method deironing scheme as neutralizing agent, both can ensure that original yellow modumite method deironing was easily filtered, is mingled with the advantages such as little, the drawback such as simultaneously overcome cost intensive, Mg cannot reclaim.Leach liquor after deironing carries copper through extraction, MgO coprecipitated nickel hydroxide cobalt, condensing crystal magnesium salts can reclaim Cu, Ni and Co magnesium respectively.
Summary of the invention
The object of the invention is to, for containing the sulphuric leachate of magnesium, provide a kind of cost low, technique and simple to operate, environmental protection, method for removing iron capable of being industrialized.
Of the present invention from the method containing deironing the sulphuric leachate of magnesium, be made up of following steps: add oxygenant by the ferrous oxidising one-tenth ferric iron in sulphuric leachate; Heating leach liquor to temperature is 85 ~ 100 DEG C, abundant stirring, within 2.5 ~ 7.0h time, successively to drip massfraction be the sodium salt solution of 20 ~ 40%wt and liquid-solid ratio be the MgO suspension liquid of 5:1 ~ 10:1 to pH=2.0 ~ 2.5 deironing, filter the leach liquor after obtaining iron dross removing and deironing after reaction.
The described magnesium sulphuric leachate that contains is containing magnesium 5 ~ 30g/L, iron content 5 ~ 50g/L, and other metals are mainly copper, nickel, cobalt, and concentration is not higher than 10g/L, H
+concentration is 0.1 ~ 3.0mol/L.
Described oxygenant is H
2o
2or/and Sodium Persulfate, its consumption is 1.0 ~ 3.0 times of ferrous oxidising required theoretical amount.
Described sodium salt is NaHCO
3, Na
2cO
3or Na
2sO
4in one or more, consumption is Na:Fe mol ratio 0.3 ~ 2:1.
The chemical reaction that in the present invention, MgO carries out yellow modumite method as neutralizing agent is as follows:
（1）
Principle of the present invention: have cost for traditional yellow modumite method deironing high, a large amount of Na adds makes Na, Mg reclaim.The present invention adopts the MgO of low cost to substitute NaHCO
3, Na
2cO
3as the H generated with sodium jarosite reaction in neutralizing agent
+, make reaction formula (1) continue to carry out reaching the object of deironing to the right, effectively can reduce costs and avoid adding in a large number of Na, meanwhile make Mg concentration in solution improve, be beneficial to magnesium and reclaim with magnesium sulfate heptahydrate crystallized form.
For above-mentioned background, the present invention adopts MgO to substitute Na
2cO
3, NaHCO
3yellow modumite method deironing advantage is carried out as follows as neutralizing agent:
1.MgO is cheap, greatly can reduce running cost and still can obtain yellow modumite method slag and easily filter, and valuable metal loss is few, deironing rate advantages of higher;
2. method only adds MgO and a small amount of Na salt precipitation agent, and wherein most of Na enters in slag with precipitation forms in iron removal, so substantially do not introduce new foreign ion to system; Be conducive to the Mg concentration in former leach liquor is improved adding of MgO simultaneously, be convenient to condensing crystal, the magnesium sulfate quality reclaimed can be ensured.
During 3.MgO reaction, bubble-free and foam produce, and are convenient to actually operating.
Embodiment
Embodiment 1
The sulphuric leachate of certain platinum family concentrate, containing Fe 36.6g/L, Co 3.1g/L, Cu 4.47g/L, Ni 7.41g/L, Mg 18.3g/L, As 0.028g/L, H
+concentration is 0.5mol/L, adds the 30%H of theoretical amount 1.0 times
2o
2after oxidation, be positioned over and hot plate heat and stirs, holding temperature is 95 DEG C, is the Na that 0.3:1 drips massfraction 40% by Na:Fe mol ratio
2sO
4solution, after drip the MgO suspension liquid of liquid-solid ratio 5:1 to pH=2.35, controlling rate of addition makes time for adding be 3.0h, filter after reaction, iron dross removing Contents of Main Components Fe 30.85%, Co 0.04%, Cu 0.27%, Ni 0.020%, Mg 0.084%, As 0.019%, liquid Contents of Main Components Fe 1.32g/L after deironing, Co 3.06g/L, Cu 4.146g/L, Ni 7.33g/L, Mg 51.88g/L, As 0.003g/L, deironing rate is 96.39%, and copper, nickel, cobalt, magnesium rate of loss are respectively 7.25%, 1.08%, 1.29%, 0.19%.
Embodiment 2
The sulphuric leachate of certain platinum family concentrate, Contents of Main Components Fe 28.3g/L, Co 2.7g/L, Cu 4.11g/L, Ni 4.38g/L, Mg 16.7g/L, As 0.026g/L, H
+concentration is 1.5mol/L, adds theoretical amount 2.0 times of 30%H
2o
2after oxidation, be positioned over and hot plate heat and stirs, holding temperature is 86 DEG C, is the NaHCO that 0.3:1 drips massfraction 20% by Na:Fe mol ratio
3solution, after drip the MgO suspension liquid of liquid-solid ratio 10:1 to pH=2.10, controlling rate of addition makes time for adding be 4.5h, filter after reaction, iron dross removing Contents of Main Components Fe 31.85%, Co 0.05%, Cu 0.19%, Ni 0.016%, Mg 0.103%, As 0.024%, liquid Contents of Main Components Fe 0.99g/L after deironing, Co 2.6g/L, Cu 3.82g/L, Ni 4.36g/L, Mg 49.43g/L, As 0.002g/L, deironing rate is 96.50%, and copper, nickel, cobalt, magnesium rate of loss are respectively 7.06%, 0.46%, 3.7%, 0.25%.
Embodiment 3
The sulphuric leachate of certain platinum family concentrate, Contents of Main Components Fe 36.6g/L, Co 3.1g/L, Cu 4.47g/L, Ni 7.41g/L, Mg 18.3g/L, As 0.028g/L, H
+concentration is 0.5mol/L, and after adding the oxidation of theoretical amount 1.0 times of Sodium Persulfates, be positioned over and hot plate heat and stirs, holding temperature is 86 DEG C, is the Na of 0.73:1 dropping massfraction 40% by Na:Fe mol ratio
2cO
3solution, after drip the MgO suspension liquid of liquid-solid ratio 5:1 to pH=2.17, controlling rate of addition makes time for adding be 5h, filter after reaction, iron dross removing Contents of Main Components Fe 31.94%, Co 0.04%, Cu 0.41%, Ni 0.021%, Mg 0.087%, As 0.020%, liquid Contents of Main Components Fe 0.044g/L after deironing, Co 3.0g/L, Cu 4.16g/L, Ni 7.32g/L, Mg 51.86g/L, As 0.003g/L, deironing rate is 99.88%, and copper, nickel, cobalt, magnesium rate of loss are respectively 6.96%, 1.21%, 3.24%, 0.20%.
Embodiment 4
The sulphuric leachate of certain platinum family concentrate, Contents of Main Components Fe 36.6g/L, Co 3.1g/L, Cu 4.47g/L, Ni 7.41g/L, Mg 18.3g/L, As 0.028g/L, H
+concentration is 1.5mol/L, and after adding the oxidation of theoretical amount 3.0 times of Sodium Persulfates, be positioned over and hot plate heat and stirs, holding temperature is 95 DEG C, is 1.0:1 dropping massfraction 20%Na by Na:Fe mol ratio
2sO
4with massfraction 20%NaHCO
3mixing solutions, after drip the MgO suspension liquid of liquid-solid ratio 5:1 to pH=2.35, controlling rate of addition makes time for adding be 7.0h, filter after reaction, iron dross removing Contents of Main Components Fe 31.85%, Co 0.04%, Cu 0.2%, Ni 0.020%, Mg 0.084%, As 0.019%, liquid Contents of Main Components Fe 0.032g/L after deironing, Co 3.06g/L, Cu 4.216g/L, Ni 7.33g/L, Mg 51.88g/L, As 0.003g/L, deironing rate is 99.91%, and copper, nickel, cobalt, magnesium rate of loss are respectively 4.4%, 1.08%, 1.29%, 0.19%.
Claims (3)
1., from the method containing deironing the sulphuric leachate of magnesium, the described magnesium sulphuric leachate that contains is containing magnesium 5 ~ 30g/L, iron content 5 ~ 50g/L, and other metals are mainly copper, nickel, cobalt, and concentration is not higher than 10g/L, H
+concentration is 0.1 ~ 3.0mol/L, it is characterized in that being made up of following steps: add oxygenant by the ferrous oxidising one-tenth ferric iron in sulphuric leachate; Heating leach liquor to temperature is 85 ~ 100 DEG C, abundant stirring, within 2.5 ~ 7.0h time, successively to drip massfraction be the sodium salt solution of 20 ~ 40%wt and liquid-solid ratio be the MgO suspension liquid of 5:1 ~ 10:1 to pH=2.0 ~ 2.5 deironing, filter the leach liquor after obtaining iron dross removing and deironing after reaction.
2. method for removing iron according to claim 1, is characterized in that described oxygenant is H
2o
2or/and Sodium Persulfate, its consumption is 1.0 ~ 3.0 times of ferrous oxidising required theoretical amount.
3. method for removing iron according to claim 1, is characterized in that described sodium salt is NaHCO
3, Na
2cO
3or Na
2sO
4in one or more, consumption is Na:Fe mol ratio 0.3 ~ 2:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410819256.5A CN104531997A (en) | 2014-12-25 | 2014-12-25 | Method for removing iron from magnesium-containing sulfuric acid leaching liquid |
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|---|---|---|---|
| CN201410819256.5A CN104531997A (en) | 2014-12-25 | 2014-12-25 | Method for removing iron from magnesium-containing sulfuric acid leaching liquid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111172392A (en) * | 2020-01-20 | 2020-05-19 | 广西赛可昱新材料科技有限公司 | Environment-friendly iron removal method without impurity in laterite-nickel ore leaching solution |
| CN115679117A (en) * | 2022-11-18 | 2023-02-03 | 金川集团股份有限公司 | Method for reducing cobalt content of iron-removing tailings of cobalt raw material leaching solution |
| 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 |
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| CN102115816A (en) * | 2011-01-07 | 2011-07-06 | 东北大学 | Comprehensive utilization method for laterite-nickel ore |
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| CN103773951A (en) * | 2014-01-21 | 2014-05-07 | 江苏仁欣化工股份有限公司 | Method for recovering nickel and cobalt through leaching laterite-nickel ore by using sulfuric and hydrochloric acid containing mixed waste acid |
| CN104120259A (en) * | 2014-07-30 | 2014-10-29 | 广西师范大学 | Nickel oxide ore acid leaching solution two-step iron removal method |
-
2014
- 2014-12-25 CN CN201410819256.5A patent/CN104531997A/en active Pending
Patent Citations (6)
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| CN101418379A (en) * | 2008-12-11 | 2009-04-29 | 昆明晶石矿冶有限公司 | Method for extracting nickel and cobalt by enclosed leaching nickel oxide mine |
| CN102115816A (en) * | 2011-01-07 | 2011-07-06 | 东北大学 | Comprehensive utilization method for laterite-nickel ore |
| CN102329955A (en) * | 2011-08-25 | 2012-01-25 | 云南锡业集团（控股）有限责任公司 | Comprehensive method for processing laterite nickel ore to produce electrolytic nickel through full wet method |
| CN102321812A (en) * | 2011-09-01 | 2012-01-18 | 东北大学 | Method for comprehensive utilization of laterite nickel ore |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111172392A (en) * | 2020-01-20 | 2020-05-19 | 广西赛可昱新材料科技有限公司 | Environment-friendly iron removal method without impurity in laterite-nickel ore leaching solution |
| CN115679117A (en) * | 2022-11-18 | 2023-02-03 | 金川集团股份有限公司 | Method for reducing cobalt content of iron-removing tailings of cobalt raw material leaching solution |
| 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 |
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Application publication date: 20150422 |