CN103160689A - Method of iron extraction and removal with solvent extraction agent - Google Patents
Method of iron extraction and removal with solvent extraction agent Download PDFInfo
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- CN103160689A CN103160689A CN2013100600909A CN201310060090A CN103160689A CN 103160689 A CN103160689 A CN 103160689A CN 2013100600909 A CN2013100600909 A CN 2013100600909A CN 201310060090 A CN201310060090 A CN 201310060090A CN 103160689 A CN103160689 A CN 103160689A
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Abstract
The invention relates to a method of iron extraction and removal with solvent extraction agent and belongs to the technical field of wet metallurgy. The method includes processes of extraction, reverse extraction and iron precipitation conversion. The detailed operation is that an organic phase is used for extracting iron in an aqueous phase, then an iron-rich organic phase is obtained, iron reverse extraction agent is directly used for reversely extracting iron, or firstly, non-ferrous metals are reversely extracted with mineral acid, and then the iron reverse extraction agent is again used for reversely extracting the iron. The iron reverse extraction agent is hydrochloric acid-chloride solution, wherein the concentration of C1- is 4-18 mol/L, and the concentration of H+ is 0.2-3 mol/L. At the time of reverse extraction, contact reverse extraction is carried out on the iron-rich organic phase and the reverse extraction iron agent according to the volume rate of 0.3-3:1. After phase splitting, an iron content water phase and a blank organic phase are obtained. The blank organic phase is washed with acid water and then returned to the extraction process for recycling. Alkaline substance is added into the iron content water phase and the value of potential of hydrogen (pH) is adjusted to 2.5-8.5, iron precipitation is filtered, and iron containing filter residues and chloride solution are obtained. The hydrochloric acid is added into the chloride solution, the concentration of H+ is adjusted to 0.2-3mol/L, then the chloride solution is returned to the iron reverse extraction process for recycling, and iron is comprehensively recovered from the iron content filter residues. The method of the iron extraction and removal with the solvent extraction agent has the advantages of being simple in the technology, good in iron reverse extraction, low in production cost, environment-friendly and the like and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of method of solvent extraction agent extraction deironing, belong to technical field of wet metallurgy.
Background technology
Iron is one of occurring in nature high yield element.Almost all contain iron in all Non-ferrous Metallurgy materials, and the content of iron is often taller than the content of valuable metal.In the acidleach process, iron and valuable metal together enter solution, and the iron in leach liquor must be removed as detrimental impurity.Iron purification is the important procedure in hydrometallurgy.Current due to the dilution of nonferrous metal ore resource in world wide and the raising of environmental standard, the exploitation utilization of many metal composite ore deposit and mineral intergrowth makes impurities removal more complicated, and the control of iron is particularly important.
Operation is miscellaneous owing to existing, the valuable metal loss is large except iron processes for traditional precipitation, and throw out stacks shortcomings such as causing secondary pollution, is replaced by new deferrization process gradually, and wherein solvent extraction is the most noticeable method.Extraction process comprises the large master operation of extraction and back-extraction two.Acid phosphoric acid ester is a widely used industrial extractant of class.The acid phosphatase esters extractant is extremely effective to the extraction of Fe under strong acidic condition (III).This kind of extractants extraction iron process is studied more fully, but the problem of iron back extraction difficulty never is well solved.
The acid phosphatase esters extractant extracts Fe (III) from acidic medium, its back extraction difficulty is well-known, and particularly under the peracid condition, iron rule is with the polymerizable molecular of acid and molysite, as nH
2SO
4MFe
2(SO
4)
3, form be extracted, rich iron organic phase is generally with hydrochloric acid or oxalic acid back extraction.With hydrochloric acid back extraction iron, the concentration 8 ~ 10mol/L of hydrochloric acid, not only the solution acid high ferro that obtains of back extraction is high, and acid wherein is difficult to reclaim, and the purifying treatment cost is high, and technological process produces acid mist, etching apparatus, contaminate environment.With oxalic acid back extraction iron, in strip liquor, the recovery process of the separation of iron and oxalic acid is complicated.Therefore, have the human Neutral ammonium fluoride to make reverse-extraction agent back extraction iron, but the use of Neutral ammonium fluoride can produce fluoride waste and waste residue.In addition, also someone adds consisting of phase-transferring agent, make the mineral acid reverse-extraction agent directly change organic phase over to, perhaps the extraction in organic phase is closed molecular moiety and go to water, thereby make the back extraction of iron be converted into the phase internal reaction by surface reaction, with the back extraction ratio of raising iron, or add reductive agent, make Fe (III) change into Fe (II), to change the back extraction course.Yet, although consisting of phase-transferring agent add the back extraction ratio that can improve iron, the extraction to iron that often adds of consisting of phase-transferring agent plays restraining effect, therefore should not adopt.Equally, adding of reductive agent makes the extraction deferrization process complicated, and the activity duration is long, and the deironing cost is high.In a word, acid phosphatase esters extractant extraction deironing, the back extraction difficulty due to iron causes the application of this kind of extractants in industrial production to be placed in an awkward position.
Summary of the invention
The object of the present invention is to provide a kind of efficient high, cost is low, and is easy to use, the method for eco-friendly solvent extraction agent extraction deironing.
The method of a kind of solvent extraction agent extraction of the present invention deironing comprises extraction, back extraction, heavy iron conversion procedure, and is direct with anti-chalybeate back extraction iron with the rich iron organic phase that obtains after organic extractant phase iron, or first with using again anti-chalybeate back extraction iron after mineral acid back extraction non-ferrous metal; Described anti-chalybeate is hydrochloric acid-chloride soln, wherein Cl
-Concentration be 4 ~ 18mol/L, H
+Concentration be 0.2 ~ 3mol/L; During back extraction, rich iron organic phase contacts back extraction by volume with anti-chalybeate at 0.3 ~ 3: 1, obtains iron content water and blank organic phase after phase-splitting; Blank organic phase with acid rinsing after, return to extraction process and recycle; Iron-bearing water is added to alkaline matter and regulates pH value to 2.5 ~ 8.5, and heavy iron filters, and obtains iron content filter residue and chloride soln, and chloride soln adds hydrochloric acid and transfers H+ concentration to 0.2 ~ 3mol/L, returns to iron back extraction operation and recycles, the comprehensive iron that reclaims wherein of iron content filter residue.
The method of a kind of solvent extraction agent extraction of the present invention deironing, described organic phase is comprised of extraction agent and thinner, or is comprised of extraction agent, thinner and conditioning agent; Described extraction agent is the acid phosphatase esters extractant, and thinner is kerosene, and phase modifier is higher alcohols or neutral organophosphorus extractant; In organic phase, the concentration of volume percent of acid phosphatase esters extractant is 5% ~ 50%, and the concentration of volume percent of thinner is 50%-95%, and the concentration of volume percent of phase modifier is 0%-10%.
The method of a kind of solvent extraction agent extraction of the present invention deironing, the general structure of described acid phosphatase esters extractant is:
Or
Wherein R is selected from a kind of in alkyl, alkoxyl group, aryl, aroyl or other substituting group; R
1Be selected from a kind of in alkyl, alkoxyl group, aryl, aroyl or other substituting group; R
2Be selected from a kind of in alkyl, alkoxyl group, aryl, aroyl or other substituting group; R wherein
1And R
2Can be identical, also can be different.
The method of a kind of solvent extraction agent of the present invention extraction deironing, described acid phosphatase esters extractant are selected from a kind of in P204, P507, P538, Cyanex272.
The method of a kind of solvent extraction agent of the present invention extraction deironing, during back extraction, anti-chalybeate and rich iron organic phase are carried out single-stage or MULTI CONTACT back extraction, and back extraction single-stage duration of contact is 5 ~ 50min, and the back extraction temperature is 15 ~ 50 ℃.
The method of a kind of solvent extraction agent extraction of the present invention deironing, described muriate is selected from NH
4Cl, NaCl, KCl, MgCl
2, CaCl
2, BaCl
2In at least a.
The method of a kind of solvent extraction agent extraction of the present invention deironing, described alkaline matter is selected from NH
4OH, NaOH, NaHCO
3, Na
2CO
3, KOH, KHCO
3, K
2CO
3, MgO, Mg (OH)
2, CaO, Ca (OH)
2, Ba (OH)
2, MgCO
3, CaCO
3, ammoniacal liquor, BaCO
3In at least a.
The method of a kind of solvent extraction agent of the present invention extraction deironing, during mineral acid back extraction non-ferrous metal, mineral acid used is selected from a kind of in sulfuric acid, hydrochloric acid, nitric acid.
The method of a kind of solvent extraction agent extraction of the present invention deironing, described acid rinsing refers to the pH value to be 0.1 ~ 2 sulfuric acid or nitric acid or hydrochloric acid soln, ratio by sour water and the volume of blank organic phase is 1:0.5 ~ 2, sour water is mixed stirring at room 10 ~ 30min with blank organic phase.
The present invention compares with existing technology and has the following advantages and effect:
1, the present invention utilizes Fe (III) energy and Cl in muriatic acidic solution dexterously
-Ionic bond forms FeCl
2+, FeCl
2 +, FeCl
3, FeCl
4 -Characteristic Deng complexing ion, with the reverse-extraction agent of hydrochloric acid-chloride soln as acid phosphatase esters extractant extraction deironing, make the positive changes of Fe (III) ion in rich iron organic phase reduce and be easy to by back extraction, effectively reduce the acidity of iron strip liquor, avoid the generation of acid mist.
2, the present invention by add alkaline earth metal chloride in strip liquor, can not only improve the back extraction ability of strip liquor, and can destroy the structure of iron polymerizable molecular in organic phase, as adds CaCl
2Or BaCl
2Can make nH
2SO
4MFe
2(SO
4)
3In iron change into hydrolysis or the Fe (III) of non-hydrolysis, solved the difficult problem that high acid extraction iron is difficult for back extraction.
3, the present invention adopts hydrochloric acid-chloride soln as the reverse-extraction agent of acid phosphatase esters extractant sulfuric acid system extraction deironing, and after back extraction, liquid through the heavy iron that neutralizes, filters and obtains iron content filter residue and chloride soln.Contain scum and can comprehensively reclaim wherein iron, chloride soln adds and can return to iron back extraction operation after the hydrochloric acid acidifying and recycle.In addition, the present invention has also utilized the solubleness of muriate in the aqueous solution to increase the characteristic that reduces with concentration of hydrochloric acid, and after after heavy iron, liquid added the hydrochloric acid acidifying, oversaturated muriate is crystallization from solution automatically, filter and remove chloride solids, so just can keep Cl in anti-chalybeate
-Balance.
In sum: it is simple that the present invention has technique, and sour consumption is few, and the iron back extraction is effective, and production cost is low, extraction agent and the recycle efficiently of anti-chalybeate, and the characteristics such as environmental friendliness, suitability for industrialized is used.
Embodiment
Below in conjunction with embodiment, the invention will be further described, and following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
The Fe-laden acid wastewater that certain enterprise produces wherein contains 34.5g/L Fe
3+With 24.3g/L H
2SO
4, do the organic extractant phase deironing with the P204-kerosene system, in organic phase, the concentration expressed in percentage by volume of P204 is 35%, contains Fe16.2g/L in load organic phases.Load organic phases is made anti-chalybeate with the saturated nacl aqueous solution of 2mol/L HCl hydrochloric acid, by comparing O/A=0.3 contact, 25 ℃ duration of contact 10min, 3 stage countercurrent back extractions, the back extraction ratio of iron is 97.8%.The blank organic phase that back extraction obtains is returned to extraction ironworker order and is recycled by after comparing O/A=1 and adding pH and be 0.5 sulphuric acid soln agitator treating 10min.The iron-bearing water addition NaOH regulator solution pH to 6.5 that back extraction obtains filters to get filter residue and filtrate.The comprehensive iron that reclaims wherein of filter residue; Filtrate adds to filter after the hydrochloric acid acidifying removes the solid sodium chloride of separating out and obtains H
+Concentration is hydrochloric acid-chloride soln of 2mol/L, returns to iron back extraction operation and continues to use.
Embodiment 2
The pH that bone coal oxidizing roasting-acidleach obtains is that 0.8 solution contains Fe
3+11.6gL, V
2O
510.2gL, do the organic extractant phase deironing with the P204-TBP-kerosene system, in organic phase, the concentration expressed in percentage by volume of P204 is 50%, contains Fe5.3gL, V in load organic phases
2O
50.7g/L.1mol/L H
2SO
4Sulphuric acid soln back extraction vanadium after the rich iron organic phase that obtains, use 2mol/L BaCl
2Make anti-chalybeate with hydrochloric acid-chloride soln of 2mol/L NaCl and 0.2mol/L HCl, load organic phases contacts with anti-chalybeate by comparing O/A=3, stirs 50min under 15 ℃, phase-splitting, and the back extraction ratio of iron is 91.7%.The water that back extraction obtains adds barium carbonate, and 30 ℃ are stirred 1h, and regulator solution pH to 2.5 filters to get iron content filter residue and muriate filtrate.Muriate filtrate obtains H after adding the hydrochloric acid acidifying
+Concentration is hydrochloric acid-chloride soln of 0.2mol/L, returns to the anti-chalybeate of preparation; The blank organic phase that back extraction obtains is returned to extraction ironworker order and is recycled by after comparing O/A=2 and adding pH and be 2 sulphuric acid soln agitator treating 15min.
Embodiment 3
Copper electrolyte contains Fe through the sulphuric acid soln that the decopper(ing) removing impurities obtains
3+8.5gL, H
2SO
4404.5g/L, do the organic extractant phase deironing with the P204-TBP-kerosene system, in organic phase, the concentration expressed in percentage by volume of P204 is 25%, contains Fe7.6gL in load organic phases.Use 6mol/L CaCl
2Make anti-chalybeate with hydrochloric acid-calcium chloride solution of 1mol/L HCl, load organic phases contacts with anti-chalybeate by comparing O/A=2.5, stirring at room 45min, and phase-splitting, the back extraction ratio of iron is 92.3%.The water that back extraction obtains adds lime and 2,50 ℃ of stirring 0.5h of Ca (OH), and regulator solution pH to 5.2 filters to get iron content filter residue and calcium chloride filtrate.Calcium chloride filtrate obtains hydrochloric acid-chloride soln that H+ concentration is 1mol/L after adding the hydrochloric acid acidifying, returns to the anti-chalybeate of preparation; The blank organic phase that back extraction obtains is returned to extraction ironworker order and is recycled by after comparing O/A=0.8 and adding pH and be 0.1 sulphuric acid soln agitator treating 20min.Embodiment 4
The pH value is that 0.63 aluminum oxide hydrochloric acid leachate contains Al
3+46.81gL, Fe
3+0.23g/L, do the organic extractant phase deironing with the P507-kerosene system, in organic phase, the concentration expressed in percentage by volume of P507 is 5%, contains Fe1.52gL in rich iron organic phase.Rich iron organic phase is by comparing O/A=1 and containing 6mol/LCaCl
2, 3mol/LNH
4The anti-chalybeate of hydrochloric acid-ammonium chloride solution of Cl and 3mol/L HCl, after 50 ℃ of contact 5min, phase-splitting, the back extraction ratio of iron is 86.6%.The water that back extraction obtains adds ammoniacal liquor regulator solution pH to 8.5, filters to get iron content filter residue and ammonium chloride filtrate.Ammonium chloride filtrate obtains H after adding the hydrochloric acid acidifying
+Concentration is hydrochloric acid-chloride soln of 3mol/L, returns to the anti-chalybeate of preparation; The blank organic phase that back extraction obtains is returned to extraction ironworker order and is recycled by after comparing O/A=0.6 and adding pH and be 1.8 hydrochloric acid soln agitator treating 25min.
Embodiment 5
The pH value is that 0.4 bismuth leaching solution contains Bi
3+52.6g/L, Fe
3+1.2g/L, do the organic extractant phase deironing with Cyanex272-propyl carbinol-kerosene system, in organic phase, the concentration expressed in percentage by volume of Cyanex272 is 15%, contains Fe4.25g/L in rich iron organic phase.Make anti-chalybeate with the solution that contains 1.5mol/L NaCl, 2.2mol/L KCl and 0.3mol/L HCl, load organic phases contacts with reverse-extraction agent by comparing O/A=0.5, after 25 ℃ of contact 25min, and phase-splitting, the back extraction ratio of iron is 78.7%.The water that back extraction obtains adds pure adjusting PH with base to 7.3, makes the iron Precipitation in solution, filters to get iron content filter residue and muriate filtrate.Muriate filtrate obtains H after adding the hydrochloric acid acidifying
+Concentration is hydrochloric acid-chloride soln of 0.3mol/L, returns to the anti-chalybeate of preparation; The blank organic phase that back extraction obtains is returned to extraction ironworker order and is recycled by after comparing O/A=0.5 and adding pH and be 1.3 salpeter solution water agitator treating 30min.
Claims (8)
1. the method for solvent extraction agent extraction deironing, comprise extraction, back extraction, heavy iron conversion procedure, it is characterized in that: direct with anti-chalybeate back extraction iron with the rich iron organic phase that obtains after organic extractant phase iron, or first with using again anti-chalybeate back extraction iron after mineral acid back extraction non-ferrous metal; Described anti-chalybeate is hydrochloric acid-chloride soln, and wherein the concentration of Cl-is 4 ~ 18mol/L, H
+Concentration be 0.2 ~ 3mol/L; During back extraction rich iron organic phase and anti-chalybeate by volume 0.3 ~ 3:1 contact back extraction, obtain iron content water and blank organic phase after phase-splitting; Blank organic phase with acid rinsing after, return to extraction process and recycle; Iron-bearing water is added to alkaline matter and regulates pH value to 2.5 ~ 8.5, and heavy iron filters, and obtains iron content filter residue and chloride soln; Chloride soln adds hydrochloric acid and transfers H
+Concentration to 0.2 ~ 3mol/L returns to iron back extraction operation and recycles, the comprehensive iron that reclaims wherein of iron content filter residue.
2. a kind of solvent extraction agent according to claim 1 extracts the method for deironing, and it is characterized in that: described organic phase is comprised of extraction agent and thinner, or is comprised of extraction agent, thinner and phase modifier; Described extraction agent is the acid phosphatase esters extractant, and thinner is kerosene, and phase modifier is higher alcohols or neutral organophosphorus extractant; In organic phase, the concentration of volume percent of acid phosphatase esters extractant is 5% ~ 50%, and the concentration of volume percent of thinner is 50%-95%, and the concentration of volume percent of phase modifier is 0%-10%.
3. the method for a kind of solvent extraction agent extraction deironing according to claim 2 is characterized in that: described acid phosphatase esters extractant is selected from a kind of in P204, P507, P538, Cyanex272.
4. the method for a kind of solvent extraction agent extraction deironing according to claim 1, it is characterized in that: during back extraction, anti-chalybeate and rich iron organic phase are carried out single-stage or MULTI CONTACT back extraction, and back extraction single-stage duration of contact is 5 ~ 50min, and the back extraction temperature is 15 ~ 50 ℃.
5. a kind of solvent extraction agent according to claim 1 extracts the method for deironing, and it is characterized in that: described muriate is selected from NH
4Cl, NaCl, KCl, MgCl
2, CaCl
2, BaCl
2In at least a.
6. a kind of solvent extraction agent according to claim 1 extracts the method for deironing, and it is characterized in that: described alkaline matter is selected from NH
4OH, NaOH, NaHCO
3, Na
2CO
3, KOH, KHCO
3, K
2CO
3, MgO, Mg (OH)
2, CaO, Ca (OH)
2, Ba (OH)
2, MgCO
3, CaCO
3, ammoniacal liquor, BaCO
3In at least a.
7. the method for a kind of solvent extraction agent extraction deironing according to claim 1 is characterized in that: during mineral acid back extraction non-ferrous metal, mineral acid used is selected from a kind of in sulfuric acid, hydrochloric acid, nitric acid.
8. a kind of solvent extraction agent according to claim 1 extracts the method for deironing, it is characterized in that: described acid rinsing refers to the pH value to be 0.1 ~ 2 sulfuric acid, nitric acid or hydrochloric acid soln, ratio by sour water and the volume of blank organic phase is 1:0.5 ~ 2, sour water is mixed stirring at room 10 ~ 30min with blank organic phase.
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| CN104164562A (en) * | 2014-08-19 | 2014-11-26 | 江西理工大学 | Method for removing iron from extractant by back extraction |
| CN104760938A (en) * | 2015-03-18 | 2015-07-08 | 安庆师范学院 | Method for removing iron ions from concentrated sulfuric acid |
| CN106068336A (en) * | 2014-03-07 | 2016-11-02 | 巴斯夫欧洲公司 | For controlling the method and system of the foreign metal concentration during metallurgical process |
| CN107245582A (en) * | 2017-05-26 | 2017-10-13 | 金川集团股份有限公司 | It is a kind of that iron, the method for zinc are reclaimed from waste hydrochloric acid |
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| CN111348639A (en) * | 2018-12-24 | 2020-06-30 | 四川大学 | Wet phosphoric acid purification process and back extraction method of metal cation extraction liquid thereof |
| CN111348633A (en) * | 2018-12-24 | 2020-06-30 | 四川大学 | Wet phosphoric acid purifying process and its extraction liquid regenerating method |
| CN112062245A (en) * | 2020-09-09 | 2020-12-11 | 昆明理工大学 | Method for preparing polyaluminium chloride water purifying agent by using waste hydrochloric acid containing iron, arsenic and various heavy metals generated by hydrometallurgical germanium |
| CN112481497A (en) * | 2020-10-30 | 2021-03-12 | 神华准能资源综合开发有限公司 | Method for removing heavy metal from aluminum-containing hydrochloric acid wastewater |
| CN115558808A (en) * | 2022-09-27 | 2023-01-03 | 吉安鑫泰科技有限公司 | Separation method of light rare earth elements |
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|---|---|---|---|---|
| CN106068336A (en) * | 2014-03-07 | 2016-11-02 | 巴斯夫欧洲公司 | For controlling the method and system of the foreign metal concentration during metallurgical process |
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| CN107245582A (en) * | 2017-05-26 | 2017-10-13 | 金川集团股份有限公司 | It is a kind of that iron, the method for zinc are reclaimed from waste hydrochloric acid |
| CN107245582B (en) * | 2017-05-26 | 2019-01-22 | 金川集团股份有限公司 | A method of recycling iron, zinc from waste hydrochloric acid |
| CN111348633A (en) * | 2018-12-24 | 2020-06-30 | 四川大学 | Wet phosphoric acid purifying process and its extraction liquid regenerating method |
| CN111348639A (en) * | 2018-12-24 | 2020-06-30 | 四川大学 | Wet phosphoric acid purification process and back extraction method of metal cation extraction liquid thereof |
| CN110029371A (en) * | 2019-04-25 | 2019-07-19 | 江西自立环保科技有限公司 | A kind of method of copper electrolyte open circuit iron ion |
| CN112062245A (en) * | 2020-09-09 | 2020-12-11 | 昆明理工大学 | Method for preparing polyaluminium chloride water purifying agent by using waste hydrochloric acid containing iron, arsenic and various heavy metals generated by hydrometallurgical germanium |
| CN112062245B (en) * | 2020-09-09 | 2021-10-29 | 昆明理工大学 | Method for preparing polyaluminium chloride water purifying agent by using waste hydrochloric acid containing iron, arsenic and various heavy metals generated by hydrometallurgical germanium |
| CN112481497A (en) * | 2020-10-30 | 2021-03-12 | 神华准能资源综合开发有限公司 | Method for removing heavy metal from aluminum-containing hydrochloric acid wastewater |
| CN115558808A (en) * | 2022-09-27 | 2023-01-03 | 吉安鑫泰科技有限公司 | Separation method of light rare earth elements |
| CN115558808B (en) * | 2022-09-27 | 2023-11-28 | 吉安鑫泰科技有限公司 | Separation method of light rare earth element |
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