CN105000537A - Method for separating selenium in alkaline leachate - Google Patents

Method for separating selenium in alkaline leachate Download PDF

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CN105000537A
CN105000537A CN201510366835.3A CN201510366835A CN105000537A CN 105000537 A CN105000537 A CN 105000537A CN 201510366835 A CN201510366835 A CN 201510366835A CN 105000537 A CN105000537 A CN 105000537A
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selenium
leaching liquid
alkaline leaching
alkaline
filter residue
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CN105000537B (en
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李栋
郭学益
田庆华
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Central South University
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Central South University
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Abstract

The invention discloses a method for separating selenium in alkaline leachate. The method comprises 1, slowly adding Ca(OH)2 and 3CaO.Al2O3 into an alkaline leaching liquid containing SeO3<2-> and/or SeO4<2->, and carrying out stirring for a reaction at a temperature of 40-80 DEG C to produce precipitates, 2, filtering the mixed solution obtained by the step 1 to obtain selenium-containing filter residue and filtrate, 3, washing the selenium-containing filter residue by deionized water many times, carrying out drying, mixing the dried selenium-containing filter residue and a chlorine salt solution, carrying out stirring, and carrying out liquid-solid separation after the reaction to obtain a selenium-containing washing lotion and a Ca-Al-Cl adsorbent which mainly comprises 3CaO. Al2O3. CaCl2. 10H2O, and 4, recovering selenium from the selenium-containing washing lotion obtained by the step 3. The method realizes adsorbent cyclic utilization and recovery of alkali in the leachate and has environmentally friendly processes.

Description

A kind of method being separated selenium in alkaline leaching liquid
Technical field
The invention belongs to technical field of wet metallurgy, particularly relate to a kind of method being separated selenium in alkaline leaching liquid.
Background technology
Copper anode mud is the intermediate product that a class of electrolytic refining course of copper output contains valency elemental copper, lead, antimony, selenium, tellurium and precious metal etc.Copper anode mud is after the alkaline process metallurgical technology process such as soda Roasting And Leaching, caustic fusion leaching, pressurization alkaline leaching, and Se accumulation is in alkaline leaching liquid.
At present, in alkaline leaching liquid, the main sorting method of selenium has acidifying reduction method, evaporative crystallization method and absorption method.
Acidifying reduction method is by after alkaline leaching liquid sulfuric acid or hcl acidifying, then reclaims after adopting the reductive agent such as sulfurous gas, S-WAT that selenium is reduced to elemental selenium, and subject matter is that acid consumption and wastewater flow rate are large; Meanwhile, acidifying reduction selenium does not consider recycling of alkali, cannot adapt to the process of copper anode mud alkaline leaching liquid.
Evaporative crystallization method is concentrated by alkaline leaching liquid heating evaporation, and selenium is with Sodium Selenite or sodium selenate form crystallization, and the follow-up serial operation such as reduction with carbon and oxydrolysis of adopting again reclaims selenium with simple substance form.Evaporative crystallization method subject matter is that energy consumption is high, and can only process high selenium concentration alkaline leaching liquid, and solution alkali concn is unsuitable too high simultaneously.
Absorption method is the selenium utilizing the adsorptive power of solid reagent to selenite radical or selenate radical to come in separation solution: such as CN201310518720 discloses a kind for the treatment of process containing selenium waste water, its sorbent material adopted is chitosan, but be only suitable for process lower concentration acid waste water (solution ph 3-5, selenium maximum concentration 30mg/L).
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, there is provided a kind of there is cheaper starting materials, the method for selenium in the separation alkaline leaching liquid of the advantage such as flow process is short, selenium separation rate is high, alkali recycles, clean environment firendly, the method can realize the recycle of sorbent material.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is:
Be separated a method for selenium in alkaline leaching liquid, comprise the following steps:
1) by Ca (OH) 2and 3CaOAl 2o 3slowly join containing SeO 3 2-and/or SeO 4 2-alkaline leaching liquid in, stir, control temperature of reaction be 40 ~ 80 DEG C, generate precipitation;
2) by step 1) after mixed solution filter, obtain containing selenium filter residue and filtrate;
3) by step 2) after containing selenium filter residue deionized water wash for several times and dry, then by mix with chloride solution containing selenium filter residue after drying, stirring, carries out solid-liquor separation after question response completes, and obtains containing selenium washing lotion and Ca-Al-Cl type sorbent material; Described Ca-Al-Cl type sorbent material is mainly 3CaOAl 2o 3caCl 210H 2o;
4) from step 3) obtain containing reclaiming selenium selenium washing lotion.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 3) in Ca-Al-Cl type sorbent material return step 1) in replace Ca (OH) 2and 3CaOAl 2o 3.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 1) in, alkaline leaching liquid is the strong alkaline aqueous solution containing selenium that copper anode mud caustic fusion leaching process or alkaline pressure leaching process produce, and in alkaline leaching liquid, selenium concentration is 2gL -1~ 25gL -1, alkali concn is 0.5molL -1~ 3molL -1.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 2) in filtrate return copper anode mud caustic fusion leaching process or alkaline pressure leaching process.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 2) in filtrate directly reclaim alkali by evaporative crystallization.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 1) in, Ca (OH) 2and 3CaOAl 2o 3mol ratio be 1 ~ 2:1; 3CaOAl 2o 3be 1 ~ 3:1 with the mol ratio of selenium element in alkaline leaching liquid.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 1) in, 3CaOAl 2o 3be the CaCO of 3:1 by mol ratio 3and Al 2o 3after Homogeneous phase mixing, be placed in that retort furnace prepared at the temperature lower calcination 4h of 1300 ~ 1400 DEG C.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 1) in, the time of stirring is 6 ~ 18h, stirring velocity 200 ~ 500r/min.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 3) in, villaumite is NaCl, KCl or CaCl 2; Cl in chloride solution -concentration be 0.01 ~ 1.0mol/L, the volume of chloride solution with dry after the mass ratio containing selenium filter residue be 3 ~ 50mL/g; The time of stirring is 1 ~ 3h, stirring velocity 200 ~ 500r/min.Preferred further, villaumite is NaCl.
The method of selenium in above-mentioned separation alkaline leaching liquid, preferably, described step 3) in, the temperature of drying containing selenium filter residue is 80 DEG C.
Processing method of the present invention is mainly based on following know-why: first, in containing the alkaline leaching liquid of selenium, add Ca (OH) 2and 3CaOAl 2o 3, with the SeO in alkaline leaching liquid 3 2-or/and SeO 4 2-in conjunction with, generation is insoluble to the bimetal composite oxide with laminate structure of basic solution (as 3CaOAl 2o 3caSeO 310H 2o is or/and 3CaOAl 2o 3caSeO 410H 2o); After filtering separation, the alkali containing high density in filtrate, can directly carry out alkali collection or directly return in upstream alkaline leaching (copper anode mud caustic fusion leaching process or alkaline pressure leaching process); Chloride solution (being preferably NaCl solution) wash-out is adopted, Cl containing selenium filter residue -with the SeO in filter residue 3 2-or SeO 4 2-there is ion exchange reaction and form Ca-Al-Cl type sorbent material (as 3CaOAl 2o 3caCl 210H 2o), replacement Ca (OH) can be returned 2and 3CaOAl 2o 3for separating of the selenium in alkaline leaching liquid, SeO in the Cl-in Ca-Al-Cl type sorbent material and solution 3 2-or SeO 4 2-ion exchange reaction occurs, and Cl-enters basic solution, and (main component is bimetal composite oxide, i.e. 3CaOAl to form Ca-Al-Se solid product 2o 3caSeO 310H 2o is or/and 3CaOAl 2o 3caSeO 410H 2o), then carry out salt through chloride solution and wash, generate again Ca-Al-Cl type sorbent material, this sorbent material returns re-using; Main component containing selenium washing lotion is villaumite and Na 2seO 3or Na 2seO 4, existing SO can be adopted 2reduction technique reclaims selenium.
Compared with prior art, the invention has the advantages that:
1) start in technological process of the present invention to adopt Ca (OH) 2and 3CaOAl 2o 3as sorbent material, alkaline leaching liquid is formed containing the solid sample of selenium after original position absorption, and containing selenium filter residue output Ca-Al-Cl type sorbent material after salt is washed, this sorbent material is to SeO 3 2-or SeO 4 2-there is stronger adsorptive power, can return and replace Ca (OH) 2and 3CaOAl 2o 3for the selenium in fractionation by adsorption alkaline leaching liquid, and realize recycle by absorption-desorption.
2) technique of the present invention achieves the reuse of alkali in leach liquor, technique clean environment firendly.Conventional processes containing selenium alkaline leaching liquid generally first carries out acidification to solution, and the alkali therefore in solution is neutralized, and alkali cannot recycle, and produces a large amount of brine waste.And the present invention adopts the art breading alkaline leaching liquid of original position fractionation by adsorption, while high efficiency separation selenium, the base in leach liquor is not originally lost, and is reclaimed or solution is directly returned leaching process by evaporative crystallization, achieves the reuse of alkali; Sepn process neutral and alkali solution all utilizes, and produces without waste water.
3) technical process of the present invention is short, simple to operate, achieves the high efficiency separation of selenium in alkaline leaching liquid.The traditional separation method of the selenium in basic solution is generally reoxidize after acidify solution, and then adopt using sulfur dioxide reduction method to be separated, technical process is long, and reagent consumption is large, and required equipment is many, complicated operation.And the technical process that the present invention adopts is short, equipment is few, simple to operate, and good separating effect, selenium original position adsorption rate is higher than 98%, and salt is washed desorption efficiency and is greater than 90%.
4) technique of the present invention is applicable to processing the higher alkaline leaching liquid of selenium concentration, and it is high to be separated selenium efficiency.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with Figure of description and preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
Unless otherwise defined, hereinafter used all technical terms are identical with the implication that those skilled in the art understand usually.The object of technical term used herein just in order to describe specific embodiment is not be intended to limit the scope of the invention.
Apart from special instruction, all ingredients used in the present invention, raw material are can commodity commercially or can by the obtained product of known method.
Embodiment 1:
Be separated a method for selenium in alkaline leaching liquid, its technological process as shown in Figure 1, comprises the following steps:
1) by 1L alkaline leaching liquid (Se:2g/L, OH -: 0.5mol/L) be heated to 40 DEG C, be then the Ca (OH) of 1:1 by mol ratio 2and 3CaOAl 2o 3(be the CaCO of 3:1 by mol ratio 3and Al 2o 3after Homogeneous phase mixing, be placed in that retort furnace prepared at the temperature lower calcination 4h of 1300 DEG C) slowly add alkaline leaching liquid (3CaOAl as sorbent material after mixing 2o 3with the ratio 1:1 of selenium element mole number), Keep agitation 6h, stirring velocity is 200r/min.
2) by step 1) after solution filter, obtain containing selenium filter residue and filtrate.After testing, in filtrate, selenium concentration is 38mg/L, by calculating, is 98.10% containing selenium adsorption rate in selenium filter residue; Alkali is reclaimed from filtrate.
3) by step 2) after containing selenium filter residue deionized water wash and in 80 DEG C dry, then the selenium filter residue that contains after oven dry is joined (volume of NaCl solution and the mass ratio containing selenium filter residue after drying are 50mL/g) in the NaCl solution of 0.1mol/L, 1h is stirred with the stirring velocity of 500r/min, carry out solid-liquor separation after question response completes, obtain containing selenium washing lotion and Ca-Al-Cl type sorbent material (3CaOAl 2o 3caCl 210H 2o); After testing, contain selenium 1.78g/L containing in selenium washing lotion, desorption efficiency reaches 91.13%.
4) existing SO is adopted 2reduction technique is from step 3) obtain containing reclaiming selenium selenium washing lotion.
Embodiment 2:
Be separated a method for selenium in alkaline leaching liquid, its technological process as shown in Figure 1, comprises the following steps:
1) by 1L alkaline leaching liquid (Se:10g/L, OH -: 1.5mol/L) be heated to 60 DEG C, be then the Ca (OH) of 1.5:1 by mol ratio 2and 3CaOAl 2o 3(be the CaCO of 3:1 by mol ratio 3and Al 2o 3after Homogeneous phase mixing, be placed in that retort furnace prepared at the temperature lower calcination 4h of 1350 DEG C) slowly add alkaline leaching liquid (3CaOAl as sorbent material after mixing 2o 3with the ratio 2:1 of selenium element mole number), Keep agitation 12h, stirring velocity is 300r/min.
2) by step 1) after solution filter, obtain containing selenium filter residue and filtrate.After testing, in filtrate, selenium concentration is 87mg/L, by calculating, is 99.13% containing selenium adsorption rate in selenium filter residue; Alkali is reclaimed from filtrate.
3) by step 2) after containing selenium filter residue deionized water wash and in 80 DEG C dry, then the selenium filter residue that contains after oven dry is joined (volume of NaCl solution and the mass ratio containing selenium filter residue after drying are 20mL/g) in the NaCl solution of 0.1mol/L, 2h is stirred with the stirring velocity of 300r/min, carry out solid-liquor separation after question response completes, obtain containing selenium washing lotion and Ca-Al-Cl type sorbent material (3CaOAl 2o 3caCl 210H 2o); After testing, contain selenium 4.44g/L containing in selenium washing lotion, desorption efficiency reaches 93.58%.
4) existing SO is adopted 2reduction technique is from step 3) obtain containing reclaiming selenium selenium washing lotion.
Embodiment 3:
Be separated a method for selenium in alkaline leaching liquid, its technological process as shown in Figure 1, comprises the following steps:
1) by 1L alkaline leaching liquid (Se:25g/L, OH -: 3mol/L) be heated to 80 DEG C, be then the Ca (OH) of 2:1 by mol ratio 2and 3CaOAl 2o 3(be the CaCO of 3:1 by mol ratio 3and Al 2o 3after Homogeneous phase mixing, be placed in that retort furnace prepared at the temperature lower calcination 4h of 1400 DEG C) slowly add alkaline leaching liquid (3CaOAl as sorbent material after mixing 2o 3with the ratio 3:1 of selenium element mole number), Keep agitation 18h, stirring velocity is 500r/min.
2) by step 1) after solution filter, obtain containing selenium filter residue and filtrate.After testing, in filtrate, selenium concentration is 135mg/L, by calculating, is 99.46% containing selenium adsorption rate in selenium filter residue; Alkali is reclaimed from filtrate.
3) by step 2) after containing selenium filter residue deionized water wash and in 80 DEG C dry, then the selenium filter residue that contains after oven dry is joined (volume of NaCl solution and the mass ratio containing selenium filter residue after drying are 3mL/g) in the NaCl solution of 1mol/L, 3h is stirred with the stirring velocity of 200r/min, carry out solid-liquor separation after question response completes, obtain containing selenium washing lotion and Ca-Al-Cl type sorbent material (3CaOAl 2o 3caCl 210H 2o); After testing, containing selenium 17.18g/L in washing lotion, desorption efficiency reaches 90.76%.
4) existing SO is adopted 2reduction technique is from step 3) obtain containing reclaiming selenium selenium washing lotion.

Claims (10)

1. be separated a method for selenium in alkaline leaching liquid, it is characterized in that, comprise the following steps:
1) by Ca (OH) 2and 3CaOAl 2o 3slowly join containing SeO 3 2-and/or SeO 4 2-alkaline leaching liquid in, stir, control temperature of reaction be 40 ~ 80 DEG C, generate precipitation;
2) by step 1) after mixed solution filter, obtain containing selenium filter residue and filtrate;
3) by step 2) after containing selenium filter residue deionized water wash for several times and dry, then by mix with chloride solution containing selenium filter residue after drying, stirring, carries out solid-liquor separation after question response completes, and obtains containing selenium washing lotion and Ca-Al-Cl type sorbent material; Described Ca-Al-Cl type sorbent material is mainly 3CaOAl 2o 3caCl 210H 2o;
4) from step 3) obtain containing reclaiming selenium selenium washing lotion.
2. the as claimed in claim 1 method being separated selenium in alkaline leaching liquid, is characterized in that, described step 3) in Ca-Al-Cl type sorbent material return step 1) in replace Ca (OH) 2and 3CaOAl 2o 3.
3. the method being separated selenium in alkaline leaching liquid as claimed in claim 1 or 2, it is characterized in that, described step 1) in, alkaline leaching liquid is the strong alkaline aqueous solution containing selenium that copper anode mud caustic fusion leaching process or alkaline pressure leaching process produce, and in alkaline leaching liquid, selenium concentration is 2gL -1~ 25gL -1, alkali concn is 0.5molL -1~ 3molL -1.
4. the as claimed in claim 3 method being separated selenium in alkaline leaching liquid, is characterized in that, described step 2) in filtrate return copper anode mud caustic fusion leaching process or alkaline pressure leaching process.
5. the as claimed in claim 3 method being separated selenium in alkaline leaching liquid, is characterized in that, described step 2) in filtrate directly reclaim alkali by evaporative crystallization.
6. the method for selenium in separation alkaline leaching liquid according to claim 1, is characterized in that, described step 1) in, Ca (OH) 2and 3CaOAl 2o 3mol ratio be 1 ~ 2:1; 3CaOAl 2o 3be 1 ~ 3:1 with the mol ratio of selenium element in alkaline leaching liquid.
7. in the separation alkaline leaching liquid as described in claim 1 or 6, the method for selenium, is characterized in that, described step 1) in, 3CaOAl 2o 3be the CaCO of 3:1 by mol ratio 3and Al 2o 3after Homogeneous phase mixing, be placed in that retort furnace prepared at the temperature lower calcination 4h of 1300 ~ 1400 DEG C.
8. in the separation alkaline leaching liquid described in claim 1 or 2, the method for selenium, is characterized in that, described step 1) in, the time of stirring is 6 ~ 18h, stirring velocity 200 ~ 500r/min.
9. the method being separated selenium in alkaline leaching liquid as claimed in claim 1 or 2, is characterized in that, described step 3) in, villaumite is NaCl, KCl or CaCl 2; Cl in chloride solution -concentration be 0.01 ~ 1.0mol/L, the volume of chloride solution with dry after the mass ratio containing selenium filter residue be 3 ~ 50mL/g; The time of stirring is 1 ~ 3h, stirring velocity 200 ~ 500r/min.
10. the method being separated selenium in alkaline leaching liquid as claimed in claim 1 or 2, is characterized in that, described step 3) in, the temperature of drying containing selenium filter residue is 80 DEG C.
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CN109097568A (en) * 2018-09-21 2018-12-28 中南大学 A method of separating selenium and arsenic from the alkaline leaching liquid of arsenic containing selenium

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CN109097568A (en) * 2018-09-21 2018-12-28 中南大学 A method of separating selenium and arsenic from the alkaline leaching liquid of arsenic containing selenium
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