CN105000537B - A kind of method for separating selenium in alkaline leaching liquid - Google Patents
A kind of method for separating selenium in alkaline leaching liquid Download PDFInfo
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- CN105000537B CN105000537B CN201510366835.3A CN201510366835A CN105000537B CN 105000537 B CN105000537 B CN 105000537B CN 201510366835 A CN201510366835 A CN 201510366835A CN 105000537 B CN105000537 B CN 105000537B
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- leaching liquid
- alkaline leaching
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Abstract
The invention discloses a kind of method for separating selenium in alkaline leaching liquid, comprise the following steps：1) by Ca (OH)2And 3CaOAl2O3It is slowly added into containing SeO3 2‑And/or SeO4 2‑Alkaline leaching liquid in, stirring, controlling reaction temperature be 40~80 DEG C, generation precipitation；2) by step 1) after mixed liquor filtering, obtain filter residue containing selenium and filtrate；3) selenium filter residue will be contained to be washed with deionized for several times and dry, will then mix the filter residue containing selenium after drying with chloride solution, stirred, and carried out solid-liquor separation after the completion of question response, obtain washing lotion containing selenium and Ca Al Cl type adsorbents；The Ca Al Cl type adsorbents are mainly 3CaOAl2O3·CaCl2·10H2O；4) from step 3) selenium is reclaimed in obtained washing lotion containing selenium.The present invention technique realize adsorbent recycle and leachate in alkali reuse, technique clean environment firendly.
Description
Technical field
The invention belongs to technical field of wet metallurgy, more particularly to a kind of method for separating selenium in alkaline leaching liquid.
Background technology
Copper anode mud is a class of electrolytic refining course of copper output containing valuable elemental copper, lead, antimony, selenium, tellurium and noble metal etc.
Intermediate product.The alkaline process metallurgical technologies such as copper anode mud is leached through soda Roasting And Leaching, caustic fusion, pressurization alkaline leaching are handled
Afterwards, Se accumulation is in alkaline leaching liquid.
At present, the main sorting method of selenium has acidifying reducing process, evaporative crystallization method and absorption method in alkaline leaching liquid.
Acidifying reducing process is by after alkaline leaching liquid sulfuric acid or hydrochloric acid acidifying, then using sulfur dioxide, sodium sulfite etc.
Selenium is reduced to reclaim after elemental selenium by reducing agent, and subject matter is that acid consumption and wastewater flow rate are big；Meanwhile, acidifying reduction selenium is not accounted for
The recycling of alkali, it is impossible to adapt to the processing of copper anode mud alkaline leaching liquid.
Evaporative crystallization method is that, by the concentration of alkaline leaching liquid heating evaporation, selenium is analysed with sodium selenite or the crystallization of selenic acid na form
Go out, the serial process such as reduction with carbon and oxydrolysis is subsequently adopted again selenium is reclaimed with simple substance form.Evaporative crystallization method subject matter is
High energy consumption, and high selenium concentration alkaline leaching liquid can only be handled, while solution alkali concn is unsuitable too high.
Absorption method is to separate the selenium in solution to the adsorption capacity of selenite radical or selenate radical using solid reagent：For example
CN201310518720 discloses a kind of processing method of selenium-containing wastewater, and its adsorbent used is only suitable for for chitosan
Handle low concentration acid waste water (solution ph 3-5, selenium maximum concentration 30mg/L).
The content of the invention
The technical problem to be solved in the present invention be overcome the deficiencies in the prior art to have there is provided one kind raw material is cheap, flow
The method of selenium in the separation alkaline leaching liquid of the advantages of short, selenium separation rate height, alkali recycling, clean environment firendly, this method can be real
Show recycling for adsorbent.
In order to solve the above technical problems, technical scheme proposed by the present invention is：
A kind of method for separating selenium in alkaline leaching liquid, comprises the following steps：
1) by Ca (OH)2And 3CaOAl2O3It is slowly added into containing SeO3 2-And/or SeO4 2-Alkaline leaching liquid in, stir
Mix, controlling reaction temperature is 40~80 DEG C, generation precipitation；
2) by step 1) after mixed liquor filtering, obtain filter residue containing selenium and filtrate；
3) by step 2) after filter residue containing selenium be washed with deionized for several times and dry, then by the filter residue containing selenium after drying
Mix, stir with chloride solution, carry out solid-liquor separation after the completion of question response, obtain washing lotion containing selenium and Ca-Al-Cl type adsorbents；
The Ca-Al-Cl types adsorbent is mainly 3CaOAl2O3·CaCl2·10H2O；
4) from step 3) selenium is reclaimed in obtained washing lotion containing selenium.
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 3) in Ca-Al-Cl type adsorbents
Return to step 1) middle replacement Ca (OH)2And 3CaOAl2O3。
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 1) in, alkaline leaching liquid is copper anode
Selenium is dense in the strong alkaline aqueous solution containing selenium that mud caustic fusion leaching process or alkaline pressure leaching process are produced, alkaline leaching liquid
Spend for 2gL-1~25gL-1, alkali concn is 0.5molL-1~3molL-1。
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 2) in filtrate return to copper anode mud
Caustic fusion leaching process or alkaline pressure leaching process.
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 2) in filtrate directly pass through evaporation
Alkali is reclaimed in crystallization.
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 1) in, Ca (OH)2And 3CaO
Al2O3Mol ratio be 1~2:1；3CaO·Al2O3Mol ratio with selenium element in alkaline leaching liquid is 1~3:1.
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 1) in, 3CaOAl2O3It is general mole
Than for 3:1 CaCO3And Al2O3After uniform mixing, it is placed in Muffle furnace at a temperature of 1300~1400 DEG C and calcines 4h preparations
's.
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 1) in, time of stirring for 6~
18h, 200~500r/min of mixing speed.
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 3) in, villaumite be NaCl, KCl or
CaCl2；Cl in chloride solution-Concentration be 0.01~1.0mol/L, the matter of the filter residue containing selenium after the volume of chloride solution and drying
Amount is than being 3~50mL/g；The time of stirring is 1~3h, 200~500r/min of mixing speed.It is further preferred that villaumite is
NaCl。
The method of selenium in above-mentioned separation alkaline leaching liquid, it is preferred that the step 3) in, the temperature of the drying of filter residue containing selenium
For 80 DEG C.
The process of the present invention is based primarily upon following know-why：First, Ca is added in the alkaline leaching liquid containing selenium
(OH)2And 3CaOAl2O3, with the SeO in alkaline leaching liquid3 2-Or/and SeO4 2-With reference to tool of the generation insoluble in alkaline solution
There is bimetal composite oxide (such as 3CaOAl of layer structure2O3·CaSeO3·10H2O or/and 3CaOAl2O3·
CaSeO4·10H2O)；After being separated by filtration, the alkali containing high concentration in filtrate directly can carry out alkali collection or directly return to upstream
In alkaline leaching (copper anode mud caustic fusion leaching process or alkaline pressure leaching process)；Filter residue containing selenium uses chloride solution
(being preferably NaCl solution) elution, Cl-With the SeO in filter residue3 2-Or SeO4 2-Generation ion-exchange reactions simultaneously forms Ca-Al-Cl
Type adsorbent (such as 3CaOAl2O3·CaCl2·10H2O), it can return to instead of Ca (OH)2And 3CaOAl2O3For separating alkali
SeO in Cl- and solution in selenium in property leachate, Ca-Al-Cl type adsorbents3 2-Or SeO4 2-Generation ion-exchange reactions,
Cl- enters alkaline solution, and forms Ca-Al-Se solid products (main component is bimetal composite oxide, i.e. 3CaO
Al2O3·CaSeO3·10H2O or/and 3CaOAl2O3·CaSeO4·10H2O), then salt is carried out by chloride solution to wash, it is again raw
Into Ca-Al-Cl type adsorbents, the adsorbent, which is returned, to be re-used；The main component of the washing lotion containing selenium is villaumite and Na2SeO3Or
Na2SeO4, can be using existing SO2Reduction technique reclaims selenium.
Compared with prior art, the advantage of the invention is that：
1) start to use Ca (OH) in technical process of the invention2And 3CaOAl2O3It is used as adsorbent, alkaline leaching liquid
Formed after the absorption of original position containing the solid sample of selenium, filter residue containing selenium washed through salt after output Ca-Al-Cl type adsorbents, the adsorbent is to SeO3 2-
Or SeO4 2-With stronger adsorption capacity, it can return to instead of Ca (OH)2And 3CaOAl2O3For adsorbing separation alkaline leaching liquid
In selenium, and by absorption-desorption realize recycle.
2) technique of the invention realizes the reuse of alkali in leachate, technique clean environment firendly.The biography of the liquid of alkaline leaching containing selenium
System handling process is general to be first neutralized to the alkali in solution progress acidification, therefore solution, and alkali can not be recycled, and be produced
A large amount of brine wastes.And the present invention uses the PROCESS FOR TREATMENT alkaline leaching liquid of adsorbing separation in situ, while selenium is efficiently separated,
Base in leachate is not originally lost, and is reclaimed by evaporative crystallization or solution is directly returned into leaching process, realize alkali
Reuse；Separation process neutral and alkali solution is all of no waste water is produced.
3) technological process of the invention is short, simple to operate, realizes efficiently separating for selenium in alkaline leaching liquid.Alkaline solution
In the traditional separation method of selenium be usually to be reoxidized after solution is acidified, then separated using sulfur dioxide reduction method,
Technological process is long, and reagent consumption is big, and required equipment is more, complex operation.And the technological process that the present invention is used is short, equipment is few, behaviour
Make simple, and good separating effect, selenium original position adsorption rate is higher than 98%, and salt washes desorption efficiency more than 90%.
4) technique of the invention is adapted to the higher alkaline leaching liquid of processing selenium concentration, and separation selenium efficiency high.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
For the ease of understanding the present invention, more complete is made to the present invention below in conjunction with Figure of description and preferred embodiment
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical terms used hereinafter are generally understood that with those skilled in the art
It is identical.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to the limitation present invention
Protection domain.
Except there is a special instruction, the various reagents used in the present invention, raw material be can be commercially commodity or
Person can pass through product made from known method.
Embodiment 1：
A kind of method for separating selenium in alkaline leaching liquid, its technical process is as shown in figure 1, comprise the following steps：
1) by 1L alkaline leaching liquid (Se：2g/L, OH-：40 DEG C 0.5mol/L) are heated to, is then 1 by mol ratio:1
Ca(OH)2And 3CaOAl2O3(be by mol ratio be 3:1 CaCO3And Al2O3After uniform mixing, it is placed in Muffle furnace 1300
Calcine prepared by 4h at a temperature of DEG C) (3CaOAl in alkaline leaching liquid is slowly added to as adsorbent after mixing2O3With selenium member
The ratio between plain molal quantity 1:1) 6h, is persistently stirred, mixing speed is 200r/min.
2) by step 1) after solution filtering, obtain filter residue containing selenium and filtrate.After testing, selenium concentration is 38mg/ in filtrate
L, by calculating, selenium adsorption rate is 98.10% in filter residue containing selenium；Alkali is reclaimed from filtrate.
3) by step 2) after filter residue containing selenium be washed with deionized and in 80 DEG C dry, then will after drying contain selenium
Filter residue is added in 0.1mol/L NaCl solution that (mass ratio of the filter residue containing selenium after the volume of NaCl solution and drying is
50mL/g), solid-liquor separation is carried out after the completion of stirring 1h, question response with 500r/min mixing speed, washing lotion containing selenium and Ca- is obtained
Al-Cl type adsorbents (3CaOAl2O3·CaCl2·10H2O)；After testing, 1.78g/L containing selenium in washing lotion containing selenium, desorption efficiency reaches
91.13%.
4) existing SO is used2Reduction technique is from step 3) selenium is reclaimed in obtained washing lotion containing selenium.
Embodiment 2：
A kind of method for separating selenium in alkaline leaching liquid, its technical process is as shown in figure 1, comprise the following steps：
1) by 1L alkaline leaching liquid (Se：10g/L, OH-：60 DEG C 1.5mol/L) are heated to, is then 1.5 by mol ratio:1
Ca (OH)2And 3CaOAl2O3(be by mol ratio be 3:1 CaCO3And Al2O3After uniform mixing, it is placed in Muffle furnace
Calcine prepared by 4h at a temperature of 1350 DEG C) (3CaOAl in alkaline leaching liquid is slowly added to as adsorbent after mixing2O3With
The ratio between selenium element molal quantity 2:1) 12h, is persistently stirred, mixing speed is 300r/min.
2) by step 1) after solution filtering, obtain filter residue containing selenium and filtrate.After testing, selenium concentration is 87mg/ in filtrate
L, by calculating, selenium adsorption rate is 99.13% in filter residue containing selenium；Alkali is reclaimed from filtrate.
3) by step 2) after filter residue containing selenium be washed with deionized and in 80 DEG C dry, then will after drying contain selenium
Filter residue is added in 0.1mol/L NaCl solution that (mass ratio of the filter residue containing selenium after the volume of NaCl solution and drying is
20mL/g), solid-liquor separation is carried out after the completion of stirring 2h, question response with 300r/min mixing speed, washing lotion containing selenium and Ca- is obtained
Al-Cl type adsorbents (3CaOAl2O3·CaCl2·10H2O)；After testing, 4.44g/L containing selenium in washing lotion containing selenium, desorption efficiency reaches
93.58%.
4) existing SO is used2Reduction technique is from step 3) selenium is reclaimed in obtained washing lotion containing selenium.
Embodiment 3：
A kind of method for separating selenium in alkaline leaching liquid, its technical process is as shown in figure 1, comprise the following steps：
1) by 1L alkaline leaching liquid (Se：25g/L, OH-：80 DEG C 3mol/L) are heated to, is then 2 by mol ratio:1 Ca
(OH)2And 3CaOAl2O3(be by mol ratio be 3:1 CaCO3And Al2O3After uniform mixing, it is placed in Muffle furnace at 1400 DEG C
At a temperature of calcine prepared by 4h) be slowly added to (3CaOAl in alkaline leaching liquid as adsorbent after mixing2O3With selenium element
The ratio between molal quantity 3:1) 18h, is persistently stirred, mixing speed is 500r/min.
2) by step 1) after solution filtering, obtain filter residue containing selenium and filtrate.After testing, selenium concentration is 135mg/ in filtrate
L, by calculating, selenium adsorption rate is 99.46% in filter residue containing selenium；Alkali is reclaimed from filtrate.
3) by step 2) after filter residue containing selenium be washed with deionized and in 80 DEG C dry, then will after drying contain selenium
Filter residue be added in 1mol/L NaCl solution (mass ratio of the filter residue containing selenium after the volume of NaCl solution and drying be 3mL/
G), solid-liquor separation is carried out after the completion of stirring 3h, question response with 200r/min mixing speed, washing lotion containing selenium and Ca-Al-Cl is obtained
Type adsorbent (3CaOAl2O3·CaCl2·10H2O)；After testing, 17.18g/L containing selenium in washing lotion, desorption efficiency is up to 90.76%.
4) existing SO is used2Reduction technique is from step 3) selenium is reclaimed in obtained washing lotion containing selenium.
Claims (7)
1. a kind of method for separating selenium in alkaline leaching liquid, it is characterised in that comprise the following steps：
1) by Ca (OH)2And 3CaOAl2O3It is slowly added into containing SeO3 2-And/or SeO4 2-Alkaline leaching liquid in, stir, control
Reaction temperature processed is 40~80 DEG C, generation precipitation；The alkaline leaching liquid is copper anode mud caustic fusion leaching process or alkalescence
Selenium concentration is 2gL in the strong alkaline aqueous solution containing selenium that pressure leaching process is produced, alkaline leaching liquid-1~25gL-1, alkali
Concentration is 0.5molL-1~3molL-1；Ca(OH)2And 3CaOAl2O3Mol ratio be 1~2:1；3CaO·Al2O3With
The mol ratio of selenium element is 1~3 in alkaline leaching liquid:1；The time of stirring is 6~18h, 200~500r/min of mixing speed；
2) by step 1) after mixed liquor filtering, obtain filter residue containing selenium and filtrate；
3) by step 2) after filter residue containing selenium be washed with deionized for several times and dry, then by the filter residue containing selenium and chlorine after drying
Salting liquid is mixed, stirring, is carried out solid-liquor separation after the completion of question response, is obtained washing lotion containing selenium and Ca-Al-Cl type adsorbents；It is described
Ca-Al-Cl type adsorbents are mainly 3CaOAl2O3·CaCl2·10H2O；
4) from step 3) selenium is reclaimed in obtained washing lotion containing selenium.
2. as claimed in claim 1 separation alkaline leaching liquid in selenium method, it is characterised in that the step 3) in Ca-
Al-Cl type adsorbents return to step 1) middle replacement Ca (OH)2And 3CaOAl2O3。
3. as claimed in claim 1 separation alkaline leaching liquid in selenium method, it is characterised in that the step 2) in filtrate
Return to copper anode mud caustic fusion leaching process or alkaline pressure leaching process.
4. as claimed in claim 1 separation alkaline leaching liquid in selenium method, it is characterised in that the step 2) in filtrate
Alkali is directly reclaimed by evaporative crystallization.
5. the method for selenium in alkaline leaching liquid is separated as claimed in claim 1, it is characterised in that the step 1) in,
3CaO·Al2O3Be by mol ratio be 3:1 CaCO3And Al2O3After uniform mixing, it is placed in Muffle furnace at 1300~1400 DEG C
Prepared by temperature lower calcination 4h.
6. the method for selenium in alkaline leaching liquid is separated as claimed in claim 1, it is characterised in that the step 3) in, villaumite
For NaCl, KCl or CaCl2；Cl in chloride solution-Concentration be 0.01~1.0mol/L, after the volume of chloride solution and drying
The mass ratio of the filter residue containing selenium is 3~50mL/g；The time of stirring is 1~3h, 200~500r/min of mixing speed.
7. the method for selenium in alkaline leaching liquid is separated as claimed in claim 1, it is characterised in that the step 3) in, containing selenium
The temperature of filter residue drying is 80 DEG C.
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| CN107101905B (en) * | 2017-04-24 | 2020-03-24 | 阳谷祥光铜业有限公司 | Method for measuring selenium content in crude selenium |
| CN109097568B (en) * | 2018-09-21 | 2020-06-26 | 中南大学 | Method for separating selenium and arsenic from alkaline leaching solution containing selenium and arsenic |
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| CN102363522A (en) * | 2011-11-21 | 2012-02-29 | 郴州雄风稀贵金属材料股份有限公司 | Technology for extracting selenium from low-grade selenium-containing material |
| CN102491287A (en) * | 2011-12-11 | 2012-06-13 | 郴州市金贵银业股份有限公司 | Process for separating and recovering selenium from selenium-containing material |
| CN103922511A (en) * | 2014-05-05 | 2014-07-16 | 哈尔滨工业大学 | Method for removing trace selenium in water |
| CN103951120A (en) * | 2014-04-22 | 2014-07-30 | 北京赛科康仑环保科技有限公司 | Method for treating selenium (Se) and/or tellurium (Te) containing wastewater |
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| CN102363522A (en) * | 2011-11-21 | 2012-02-29 | 郴州雄风稀贵金属材料股份有限公司 | Technology for extracting selenium from low-grade selenium-containing material |
| CN102491287A (en) * | 2011-12-11 | 2012-06-13 | 郴州市金贵银业股份有限公司 | Process for separating and recovering selenium from selenium-containing material |
| CN103951120A (en) * | 2014-04-22 | 2014-07-30 | 北京赛科康仑环保科技有限公司 | Method for treating selenium (Se) and/or tellurium (Te) containing wastewater |
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