CN107299359A - A kind of method for reclaiming selenium in liquid after point copper - Google Patents
A kind of method for reclaiming selenium in liquid after point copper Download PDFInfo
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Abstract
The present invention relates to a kind of method for reclaiming selenium in liquid after point copper, it is electrolysed by regarding liquid after point copper as electrolyte, and then selenium simple substance is obtained in negative electrode.The present invention is realized using the method for electrolysis and can complete to reclaim in the high efficiente callback from liquid after point copper to selenium, the rate of recovery >=90% of selenium, and organic efficiency height, 10~90min.Realize the cleaning to selenium from liquid after point copper simultaneously to reclaim, the concentration of sulfuric acid is low in electrolyte, and unharmful substance is generated in removal process, and environmental pollution is small.The method technique that the present invention is provided is simple, it is easy to operate, and can carry out industrialized production, have a good application prospect.
Description
Technical field
Metal field is reclaimed the present invention relates to electro-deposition, is related to a kind of method for reclaiming selenium in liquid after point copper.
Background technology
Selenium (Se) is a kind of tellurian rare element, and the content in the earth's crust is only 0.05 × 10-6, its abundance is by weight
Amount estimation is only the 10 of the earth's crust-7%, therefore be general very difficult to form industrial concentration in nature.Natural selenium seldom, and often with naturally
Sulphur symbiosis, mainly exists with the selenides of heavy metal.Selenium is a kind of typical light-sensitive semiconductor material, its chemical property between
Metal and it is nonmetallic between, be typical semimetal.Selenium has metallic luster, can conductive, heat conduction, electrical conductivity with illumination power
And drastically change.Chemical property is similar to sulphur, but its metallicity is stronger than sulphur, and its most significant is photoelectric effect, therefore it can
For photocell, the fields such as metallurgy, glass, rubber industry are also used for.From Sweden chemist Bel Cai Liwusi in 1817 first
Since being found in the mine tailing of production sulfuric acid, selenium is widely used in the daily life of industry, agricultural and the mankind.
At present, the industrial main earth of positive pole using electrolytical refined copper, the flue dust of lead blast furnace, the residual mud of sulfuric acid plant, refining
Steel flue dust, lead and zinc concentrate calcination fume, pyrite roasting slag and mercury, the waste material of gold production etc. are used as the main original for extracting selenium
Material.And wherein topmost raw material is the copper anode mud formed in cupric electrolysis production process, the 90% of total amount is accounted for.
It is industrial generally using handling copper anode mud by the way of sulfating roasting-substep leaching, with reclaim it is therein it is golden,
The valuable metals such as silver, platinum, palladium, selenium, tellurium, copper.Because selenium is amphoteric metal, therefore there is during point copper part selenium to enter point
It is lost in after copper in liquid, accounts for 6% or so of selenium total amount.The directly discharge of liquid after point copper the waste to raw material was both caused into, again
Severe contamination is caused to environment.Therefore, it is from the aspect of environmental protection, in liquid after point copper either to be further contemplated from economic benefit
Selenium, which is reclaimed, to be all very important.
A kind of method for reclaiming selenium is disclosed in CN1923674A, refining selenium waste liquid is warming up to 50~90 DEG C, is passed through containing two
Sulfur oxide gas, stirring reaction was precipitated, filtered, being dried, obtained impure selenium raw material, return and carried in dispensing after 3~12 hours
Selenium.Sulfur dioxide gas is passed through in this method method complex operation, removal process, secondary pollution easily is caused to environment.
A kind of method that selenium is reclaimed during waste water from platinum group metal containing selenium is disclosed in CN106282575A, including following step
Suddenly：Metal 1~the 2mol/L of feed acidity of platinum group containing selenium is controlled, solution 75~85 DEG C are warming up to, by selenium material in solution
Cooled down after 2.5~3 times of addition sodium hydrogensulfites of amount, 2~4h of reaction, filtering, filter residue is washed till after neutrality and to selenium recovery system；
Filtrate reclaims noble metal using methods such as metal replacement, chemical precipitation, ion exchange, absorption and electrolysis.This method step is various,
Separation process is complicated, and needs to be operated under highly acid, is unfavorable for being promoted.
Accordingly, it would be desirable to develop, a kind of new, flow is simple, the efficient method for reclaiming selenium in liquid after point copper of separation.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of method for reclaiming selenium in liquid after point copper, utilizing electrolysis
Method realize from liquid after point copper to selenium cleaning, it is efficient reclaim, the rate of recovery >=90% of selenium.
The invention provides a kind of method for reclaiming selenium in liquid after point copper, methods described is：Electricity is used as using liquid after point copper
Solution liquid is electrolysed, and selenium simple substance is obtained in negative electrode.
According to the present invention, after liquid is electrolytical refined copper after described point of copper, at the mode using sulfating roasting-substep leaching
The solution obtained after reason copper anode mud.
According to the present invention, the concentration of sulfuric acid is 25~100g/L in the electrolyte, for example can be 25g/L, 30g/L,
Specific point value, is limited to a piece between 40g/L, 50g/L, 60g/L, 70g/L, 80g/L, 90g/L or 100g/L, and above-mentioned numerical value
Width and the consideration for simplicity, the present invention no longer exclusive list.
According to the present invention, the concentration of selenium is 0.1~0.5g/L in the electrolyte, for example, can be 0.1g/L, 0.15g/
It is specific between L, 0.2g/L, 0.25g/L, 0.3g/L, 0.35g/L, 0.4g/L, 0.45g/L or 0.5g/L, and above-mentioned numerical value
Point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
The present invention adds thiocarbamide into the electrolyte, and the concentration of the thiocarbamide is 0.5~12mmol/L, for example, can be
0.5mmol/L、1mmol/L、2mmol/L、3mmol/L、4mmol/L、5mmol/L、6mmol/L、7mmol/L、8mmol/L、
Specific point value between 9mmol/L, 10mmol/L, 11mmol/L or 12mmol/L, and above-mentioned numerical value, as space is limited and for
Concise consideration, the present invention no longer exclusive list.
The concentration of thiocarbamide is preferably 1~10mmol/L in electrolyte of the present invention.
Present invention selection is electrolysed in three-electrode system, and the reference electrode that the three-electrode system is used is Ag/
AgCl electrodes or Hg/Hg2Cl2Electrode, working electrode is stainless steel, is coated titanium DSA to electrode.
According to the present invention, the voltage of the electrolysis is -0.1~-1.2V, for example can be -0.1V, -0.2V, -0.3V, -
It is specific between 0.4V, -0.5V, -0.6V, -0.7V, -0.8V, -0.9V, -1.0V, -1.1V or -1.2V, and above-mentioned numerical value
Point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
The voltage of electrolysis of the present invention is preferably -0.3~-1.0V.Voltage is excessive or too small, can all reduce the recovery of selenium
Rate, when decomposition voltage persistently increases, has gas and generates and separate out.
According to the present invention, the temperature of the electrolysis is 20~50 DEG C, for example can be 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40
DEG C, specific point value between 45 DEG C or 50 DEG C, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is no longer
Exclusive list.
According to the present invention, the time of the electrolysis is 10~90min, for example can be 10min, 20min, 30min,
Specific point value between 40min, 50min, 60min, 70min, 80min or 90min, and above-mentioned numerical value, as space is limited and goes out
In concise consideration, the present invention no longer exclusive list.
The time of electrolysis of the present invention is preferably 30~80min.
According to the present invention, it is stirred in the electrolytic process with 0~2100r/min speed, for example, can is 0r/
min、50r/min、100r/min、200r/min、400r/min、600r/min、800r/min、1000r/min、1200r/min、
Specific point between 1400r/min, 1600r/min, 1800r/min, 2000r/min or 2100r/min, and above-mentioned numerical value
Value, as space is limited and for concise consideration, the present invention no longer exclusive list.
Electrolytic process, which is stirred, can increase Ion transfer speed, help to shorten electrolysis time.When the speed of stirring
During for 0r/min, i.e., without stirring.
As preferred technical scheme, the method for the present invention for reclaiming selenium in liquid after point copper comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 25~100g/L in liquid after described point of copper, and the concentration of selenium is 0.1~0.5g/L；
(2) thiocarbamide is added in liquid after point copper obtained to step (1), is carried out in this, as electrolyte in three-electrode system
Electrolysis, selenium simple substance is obtained in negative electrode；The concentration of thiocarbamide is 0.5~12mmol/L in the electrolyte, and the electrolysis temperature is 20
~50 DEG C, decomposition voltage is -0.1~-1.2V, and electrolysis time is 10~90min, with 0~2100r/min speed in electrolytic process
Degree is stirred.
As further preferred technical scheme, the method for the present invention for reclaiming selenium in liquid after point copper includes following step
Suddenly：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 25~100g/L in liquid after described point of copper, and the concentration of selenium is 0.1~0.5g/L；
(2) thiocarbamide is added in liquid after point copper obtained to step (1), is carried out in this, as electrolyte in three-electrode system
Electrolysis, selenium simple substance is obtained in negative electrode；In the electrolyte concentration of thiocarbamide be 1~10mmol/L, the electrolysis temperature be 20~
50 DEG C, decomposition voltage is -0.3~-1.0V, and electrolysis time is 30~80min, with 0~2100r/min speed in electrolytic process
It is stirred.
Compared with prior art, the present invention at least has the advantages that：
(1) present invention realizes the high efficiente callback from liquid after point copper to selenium using the method for electrolysis, and the rate of recovery of selenium >=
90%, and organic efficiency is high, can complete to reclaim in 10~90min.
(2) cleaning that the present invention is realized to selenium from liquid after point copper is reclaimed, and the concentration of sulfuric acid is low in electrolyte, and is reclaimed
During unharmful substance generate, environmental pollution is small.
(3) the method technique that the present invention is provided is simple, it is easy to operates, can carry out industrialized production.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in understanding the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 25g/L in liquid after described point of copper, and the concentration of selenium is 0.32g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, and Ag/AgCl electrodes are used as ginseng
Than electrode, three electrolysis devices are collectively constituted；Thiocarbamide is added as electrolyte, sulphur in liquid after point copper obtained to step (1)
The concentration of urea is 2mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -0.5V, electrolysis 80min is carried out at 25 DEG C,
Electrolytic process stirs electrolyte with 2100r/min speed, and selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 95%.
Embodiment 2
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 30g/L in liquid after described point of copper, and the concentration of selenium is 0.32g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, and Ag/AgCl electrodes are used as ginseng
Than electrode, three electrolysis devices are collectively constituted；Thiocarbamide is added as electrolyte, sulphur in liquid after point copper obtained to step (1)
The concentration of urea is 2mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -0.6V, electrolysis 90min is carried out at 25 DEG C,
Electrolytic process stirs electrolyte with 1400r/min speed, and selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 93%.
Embodiment 3
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 45g/L in liquid after described point of copper, and the concentration of selenium is 0.25g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, Hg/Hg2Cl2Electrode conduct
Reference electrode, collectively constitutes three electrolysis devices；Thiocarbamide is added as electrolyte in liquid after point copper obtained to step (1),
The concentration of thiocarbamide is 4mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -0.4V, electrolysis 90min is carried out at 20 DEG C,
Electrolytic process stirs electrolyte with 2100r/min speed, and selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 92%.
Embodiment 4
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 60g/L in liquid after described point of copper, and the concentration of selenium is 0.5g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, and Ag/AgCl electrodes are used as ginseng
Than electrode, three electrolysis devices are collectively constituted；Thiocarbamide is added as electrolyte, sulphur in liquid after point copper obtained to step (1)
The concentration of urea is 10mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -1.2V, electrolysis 70min is carried out at 50 DEG C,
Electrolytic process stirs electrolyte with 2100r/min speed, and selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 90%.
Embodiment 5
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 30g/L in liquid after described point of copper, and the concentration of selenium is 0.1g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, Hg/Hg2Cl2Electrode conduct
Reference electrode, collectively constitutes three electrolysis devices；Thiocarbamide is added as electrolyte in liquid after point copper obtained to step (1),
The concentration of thiocarbamide is 0.8mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -0.7V, electrolysis 90min is carried out at 40 DEG C,
Electrolytic process stirs electrolyte with 300r/min speed, and selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 91%.
Embodiment 6
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 73g/L in liquid after described point of copper, and the concentration of selenium is 0.2g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, and Ag/AgCl electrodes are used as ginseng
Than electrode, three electrolysis devices are collectively constituted；Thiocarbamide is added as electrolyte, sulphur in liquid after point copper obtained to step (1)
The concentration of urea is 5.5mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -0.5V, electrolysis 70min is carried out at 35 DEG C,
Electrolytic process stirs electrolyte with 450r/min speed, and selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 92%.
Embodiment 7
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 35g/L in liquid after described point of copper, and the concentration of selenium is 0.25g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, Hg/Hg2Cl2Electrode conduct
Reference electrode, collectively constitutes three electrolysis devices；Thiocarbamide is added as electrolyte in liquid after point copper obtained to step (1),
The concentration of thiocarbamide is 2mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -0.6V, electrolysis 60min is carried out at 30 DEG C,
Electrolytic process stirs electrolyte with 700r/min speed, and selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 92%.
Embodiment 8
A kind of method for reclaiming selenium in liquid after point copper, the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains after point copper
Liquid；The concentration of sulfuric acid is 30g/L in liquid after described point of copper, and the concentration of selenium is 0.32g/L；
(2) using stainless steel electrode as working electrode, coated titanium DSA electrodes are as to electrode, and Ag/AgCl electrodes are used as ginseng
Than electrode, three electrolysis devices are collectively constituted；Thiocarbamide is added as electrolyte, sulphur in liquid after point copper obtained to step (1)
The concentration of urea is 2.7mmol/L；
(3) electrolysis unit that step (2) is constituted is powered, control voltage is -0.1V, electrolysis 90min is carried out at 30 DEG C,
Selenium simple substance is obtained in negative electrode.
By detection, the rate of recovery of selenium is 90%.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, do not mean that the present invention has to rely on above-mentioned detailed
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (10)
1. a kind of method that selenium is reclaimed from liquid after point copper, it is characterised in that methods described is：Electrolyte is used as using liquid after point copper
It is electrolysed, selenium simple substance is obtained in negative electrode.
2. the method as described in claim 1, it is characterised in that after liquid is electrolytical refined copper after described point of copper, use sulphation
The mode that roasting-substep is leached handles the solution obtained after copper anode mud.
3. method as claimed in claim 1 or 2, it is characterised in that the concentration of sulfuric acid is 25~100g/L in the electrolyte.
4. the method as described in any one of claims 1 to 3, it is characterised in that in the electrolyte concentration of selenium be 0.1~
0.5g/L。
5. the method as described in any one of Claims 1 to 4, it is characterised in that contain thiocarbamide in the electrolyte；
Preferably, the concentration of the thiocarbamide is 0.5~12mmol/L, preferably 1~10mmol/L.
6. the method as described in any one of Claims 1 to 5, it is characterised in that the electrolysis is carried out in three-electrode system.
7. method as claimed in claim 6, it is characterised in that the reference electrode that the three-electrode system is used is Ag/AgCl
Electrode or Hg/Hg2Cl2Electrode；
Preferably, the working electrode that the three-electrode system is used is stainless steel；
Preferably, what the three-electrode system was used is coated titanium DSA to electrode.
8. the method as described in any one of claim 1~7, it is characterised in that the voltage of the electrolysis is -0.1~-1.2V,
Preferably -0.3~-1.0V；
Preferably, the temperature of the electrolysis is 20~50 DEG C；
Preferably, the time of the electrolysis is 10~90min, preferably 30~80min.
9. the method as described in any one of claim 1~8, it is characterised in that with 0~2100r/min in the electrolytic process
Speed be stirred.
10. the method as described in any one of claim 1~9, it is characterised in that the described method comprises the following steps：
(1) after electrolytical refined copper, the mode leached using sulfating roasting-substep handles copper anode mud, obtains liquid after point copper；Institute
The concentration for stating sulfuric acid in liquid after point copper is 25~100g/L, and the concentration of selenium is 0.1~0.5g/L；
(2) thiocarbamide is added in liquid after point copper obtained to step (1), carries out electricity in three-electrode system in this, as electrolyte
Solution, selenium simple substance is obtained in negative electrode；In the electrolyte concentration of thiocarbamide be 0.5~12mmol/L, the electrolysis temperature be 20~
50 DEG C, decomposition voltage is -0.1~-1.2V, and electrolysis time is 10~90min, with 0~2100r/min speed in electrolytic process
It is stirred.
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