CN111304693A - Iron removal method for reducing accumulated iron ions in electrodeposition solution - Google Patents

Iron removal method for reducing accumulated iron ions in electrodeposition solution Download PDF

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Publication number
CN111304693A
CN111304693A CN201811520810.4A CN201811520810A CN111304693A CN 111304693 A CN111304693 A CN 111304693A CN 201811520810 A CN201811520810 A CN 201811520810A CN 111304693 A CN111304693 A CN 111304693A
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iron
iron removal
removal reaction
temperature
low
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李炳忠
张爱青
王博
伍一根
许东伟
史齐勇
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Gem Jiangsu Cobalt Industry Co Ltd
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Gem Jiangsu Cobalt Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/06Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
    • C25C1/08Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06Operating or servicing

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  • Chemical Kinetics & Catalysis (AREA)
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  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Abstract

The invention discloses an iron removal method for reducing accumulated iron ions in an electrodeposition solution, which comprises the steps of adding the electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, oxidizing bivalent iron ions in the electrodeposition solution into trivalent iron ions by adopting a sodium chlorate solution to obtain a first mixed feed liquid, then continuously carrying out low-temperature iron removal reaction on the first mixed feed liquid, controlling the pH value of the low-temperature iron removal reaction to enable the trivalent iron ions in the first mixed feed liquid to generate goethite, obtaining a second mixed feed liquid, and then carrying out filter pressing treatment to obtain the iron-removed electrodeposition solution; therefore, the invention has low temperature requirement, high iron content of the iron slag and is suitable for continuous production, the entrainment effect on the valuable metal cobalt in the iron removing process is weak, and the iron removing process improves the removal efficiency of ferrous iron, thereby reducing the energy consumption in the iron removing process, reducing the slag yield and further enhancing the operation stability by the continuous process.

Description

Iron removal method for reducing accumulated iron ions in electrodeposition solution
Technical Field
The invention belongs to the technical field of iron removal of an electrodeposition solution, and particularly relates to an iron removal method for reducing accumulated iron ions in the electrodeposition solution.
Background
In the electrodeposition process, iron removal treatment is usually required for the solution after the electrodeposition process, and the iron removal process is not only a key process for cobalt smelting, but also a process with high energy consumption and iron slag solid waste generation.
The prior art usually adopts an iron removal process by an jarosite method, iron ions in the precursor solution exist in the form of jarosite at high temperature, the temperature requirement in the iron removal process by the jarosite method is high, the iron content of iron slag is low, intermittent production is realized, the steam consumption is large, the energy consumption is high, the slag yield is large, and the equipment productivity is low.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an iron removal method for reducing the accumulated iron ions in the electrodeposition solution.
The embodiment of the invention provides an iron removal method for reducing accumulated iron ions in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank, reacting at 55-65 ℃, and oxidizing ferrous ions in the electrodeposition solution into ferric ions to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
and 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
In the above scheme, the step 2 specifically comprises: overflowing the first mixed material liquid obtained in the step 1 into a second iron removal reaction tank, adding liquid caustic soda into the second iron removal reaction tank, and introducing steam to perform a first low-temperature iron removal reaction; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then liquid alkali is added into the third iron removal reaction tank to carry out a second low-temperature iron removal reaction; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, and introducing steam into the fourth iron removal reaction tank to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
In the scheme, the mass fractions of the liquid caustic soda added in the first low-temperature iron removal reaction, the second low-temperature iron removal reaction and the third low-temperature iron removal reaction in the step 2 are all 21%, and the flow rates of the added liquid caustic soda are all 0.5-2 m3/h。
In the scheme, in the step 2, the pH value of the reaction system after the liquid alkali is added in the first low-temperature iron removal reaction, the second low-temperature iron removal reaction and the third low-temperature iron removal reaction is 2.5-3.
In the scheme, the reaction temperature of the first low-temperature iron removal reaction in the step 2 is 70 +/-3 ℃.
In the scheme, the reaction temperature of the second low-temperature iron removal reaction in the step 2 is 60 +/-3 ℃.
In the scheme, the reaction temperature of the third low-temperature iron removal reaction in the step 2 is 60 +/-3 ℃.
In the scheme, the step 1 is specifically that the potential of the feed liquid in the first iron removal reaction tank is controlled to be 550-580 mv by controlling the addition amount of the sodium chlorate solution, and the reaction temperature is 55-65 ℃.
In the scheme, the concentration of the sodium chlorate solution in the step 1 is 450-500 g/L, and the flow rate of adding the sodium chlorate solution is 85-170L/h.
In the scheme, the content of ferrous ions in the first mixed feed liquid in the step 1 is less than or equal to 0.04 g/L.
Compared with the prior art, the method adopts the sodium chlorate solution to oxidize ferrous ions in the electrodeposition solution into ferric ions, then adds liquid alkali into the iron removal reaction tank to carry out continuous low-temperature iron removal reaction, converts the ferric ions in the electrodeposition solution into goethite, and finally removes the goethite through filter pressing. The invention has low temperature requirement, high iron content of the iron slag and is suitable for continuous production, the entrainment effect on the valuable metal cobalt in the iron removing process is weak, and the iron removing process improves the removal efficiency of ferrous iron, thereby reducing the energy consumption in the iron removing process, reducing the slag yield and further enhancing the operation stability by the continuous process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides an iron removal method for reducing accumulated iron ions in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank at a flow rate of 85-170L/h, controlling the potential of feed liquid in the first iron removal reaction tank to be 550-580 mv by controlling the adding amount of the sodium chlorate solution, oxidizing divalent iron ions in the electrodeposition solution into trivalent iron ions at a reaction temperature of 55-65 ℃, sampling and detecting the content of the divalent iron ions, specifically, taking 1mL of filtrate of the first iron removal reaction tank, adding an indicator which is a potassium dichromate standard solution, dropping a drop of potassium dichromate standard solution which is changed into purple, wherein the content of the divalent iron ions is less than or equal to 0.04g/L and qualified, if the content of the divalent iron is higher than 0.04g/L, properly adding the sodium chlorate solution to improve the potential of the feed liquid, and measuring the content of the divalent iron again, when the content of ferrous ions is less than or equal to 0.04g/L, the reaction is complete to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
specifically, the first mixed feed liquid obtained in the step 1 overflows into a second iron removal reaction tank, and then flows into the second iron removal reaction tank by 0.5-2 m3H ofAdding liquid caustic soda with the mass fraction of 21% at a flow rate, introducing steam into the second iron removal reaction tank, and maintaining the temperature of the second iron removal reaction tank at 70 +/-3 ℃ to perform primary low-temperature iron removal; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then flows into the third iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, and maintaining the temperature of the third iron removal reaction tank at 60 +/-3 ℃ to carry out a second low-temperature iron removal reaction; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, and maintaining the temperature of the fourth iron removal reaction tank at 60 +/-3 ℃ to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
Adopt first deironing reaction tank, second deironing reaction tank, third deironing reaction tank, the continuous deironing that carries out of fourth deironing reaction tank, go into the electrodeposition solution in continuous to first deironing reaction tank with certain velocity of flow, use sodium chlorate solution oxidation ferrous iron and concentration 21%'s liquid caustic soda to adjust the pH value of the feed liquid in the second simultaneously, the third, the fourth deironing reaction tank is 2.5 ~ 3, the iron ion that advances to go into the groove like this can form the sediment, produce goethite promptly, the equation that generates goethite is: fe3++2H2O→FeOOH+2H+The actual content of iron ions in the solution is reduced, and when the subsequent iron-containing liquid before iron removal is diluted to be low concentration by the existing solution, the specific condition that the content of the iron ions is less than 1g/l is realized, and the continuous iron removal process is realized by continuously carrying out the process.
And 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
According to the method, a sodium chlorate solution is adopted to oxidize ferrous ions in an electrodeposition solution into ferric ions, then liquid alkali is added into an iron removal reaction tank to carry out continuous low-temperature iron removal reaction, so that the ferric ions in the electrodeposition solution are converted into goethite, and finally the goethite is removed through filter pressing. The invention has low temperature requirement, high iron content of the iron slag and is suitable for continuous production, the entrainment effect on the valuable metal cobalt in the iron removing process is weak, and the iron removing process improves the removal efficiency of ferrous iron, thereby reducing the energy consumption in the iron removing process, reducing the slag yield and further enhancing the operation stability by the continuous process.
Example 1
Embodiment 1 of the present invention provides an iron removal method for reducing iron ions accumulated in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank at a flow rate of 85-170L/h, controlling the potential of feed liquid in the first iron removal reaction tank to be 550-580 mv by controlling the adding amount of the sodium chlorate solution, reacting at 55 ℃, oxidizing ferrous ions in the electrodeposition solution into ferric ions, sampling and detecting the content of the ferrous ions, specifically, taking 1mL of filtrate in the first iron removal reaction tank, adding an indicator, wherein the indicator is a potassium dichromate standard solution, dropping a drop of potassium dichromate standard solution, namely changing into purple, indicates that the content of the ferrous ions is less than or equal to 0.04g/L is qualified, and if the content of the ferrous ions is higher than 0.04g/L, properly adding the solution to increase the potential of the sodium chlorate feed liquid, and measuring the content of the ferrous again, when the content of ferrous ions is less than or equal to 0.04g/L, the reaction is complete to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
specifically, the first mixed feed liquid obtained in the step 1 overflows into a second iron removal reaction tank, and then flows into the second iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, introducing steam into the second iron removal reaction tank, and maintaining the temperature of the second iron removal reaction tank at 70 ℃ to carry out primary low-temperature iron removal; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then flows into the third iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, and maintaining the temperature of the third iron removal reaction tank at 60 ℃ to carry out a second low-temperature iron removal reaction; the solution feed liquid after the second low-temperature iron removal reaction overflows into a fourth iron removal reaction tank, and then steam is introduced into the fourth iron removal reaction tank to maintain the fourth iron removal reactionAnd carrying out a third low-temperature iron removal reaction at the temperature of 60 ℃ to obtain a second mixed feed liquid.
And 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
Example 2
Embodiment 2 of the present invention provides an iron removal method for reducing iron ions accumulated in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank at a flow rate of 85-170L/h, controlling the potential of feed liquid in the first iron removal reaction tank to be 550-580 mv by controlling the adding amount of the sodium chlorate solution, reacting at 60 ℃, oxidizing ferrous ions in the electrodeposition solution into ferric ions, sampling and detecting the content of the ferrous ions, specifically, taking 1mL of filtrate in the first iron removal reaction tank, adding an indicator, wherein the indicator is a potassium dichromate standard solution, dropping a drop of potassium dichromate standard solution, namely changing the color into purple, indicates that the content of the ferrous ions is less than or equal to 0.04g/L is qualified, and if the content of the ferrous ions is higher than 0.04g/L, properly adding the solution to increase the potential of the sodium chlorate feed liquid, and measuring the content of the ferrous again, when the content of ferrous ions is less than or equal to 0.04g/L, the reaction is complete to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
specifically, the first mixed feed liquid obtained in the step 1 overflows into a second iron removal reaction tank, and then flows into the second iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, introducing steam into the second iron removal reaction tank, and maintaining the temperature of the second iron removal reaction tank at 70 ℃ to carry out primary low-temperature iron removal; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then flows into the third iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, and maintaining the third iron removal reaction tankCarrying out a second low-temperature iron removal reaction at the temperature of 60 ℃; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, introducing steam into the fourth iron removal reaction tank, and maintaining the temperature of the fourth iron removal reaction tank at 60 ℃ to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
And 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
Example 3
Embodiment 3 of the present invention provides an iron removal method for reducing iron ions accumulated in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank at a flow rate of 85-170L/h, controlling the potential of feed liquid in the first iron removal reaction tank to be 550-580 mv by controlling the adding amount of the sodium chlorate solution, reacting at 65 ℃, oxidizing ferrous ions in the electrodeposition solution into ferric ions, sampling and detecting the content of the ferrous ions, specifically, taking 1mL of filtrate in the first iron removal reaction tank, adding an indicator, wherein the indicator is a potassium dichromate standard solution, dropping a drop of potassium dichromate standard solution to change the color into purple, wherein the content of the ferrous ions is less than or equal to 0.04g/L is qualified, and if the content of the ferrous ions is higher than 0.04g/L, the indicator can be properly added into the solution to increase the potential of the sodium chlorate feed liquid, and measuring the content of the ferrous again, when the content of ferrous ions is less than or equal to 0.04g/L, the reaction is complete to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
specifically, the first mixed feed liquid obtained in the step 1 overflows into a second iron removal reaction tank, and then flows into the second iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, introducing steam into the second iron removal reaction tank, and maintaining the temperature of the second iron removal reaction tank at 70 ℃ to carry out primary low-temperature iron removal; is low for the first timeThe feed liquid after the warm iron removal reaction overflows into a third iron removal reaction tank, and then flows into the third iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, and maintaining the temperature of the third iron removal reaction tank at 60 ℃ to carry out a second low-temperature iron removal reaction; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, introducing steam into the fourth iron removal reaction tank, and maintaining the temperature of the fourth iron removal reaction tank at 60 ℃ to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
And 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
Example 4
Embodiment 4 of the present invention provides an iron removal method for reducing iron ions accumulated in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank at a flow rate of 85-170L/h, controlling the potential of feed liquid in the first iron removal reaction tank to be 550-580 mv by controlling the adding amount of the sodium chlorate solution, reacting at 60 ℃, oxidizing ferrous ions in the electrodeposition solution into ferric ions, sampling and detecting the content of the ferrous ions, specifically, taking 1mL of filtrate in the first iron removal reaction tank, adding an indicator, wherein the indicator is a potassium dichromate standard solution, dropping a drop of potassium dichromate standard solution, namely changing the color into purple, indicates that the content of the ferrous ions is less than or equal to 0.04g/L is qualified, and if the content of the ferrous ions is higher than 0.04g/L, properly adding the solution to increase the potential of the sodium chlorate feed liquid, and measuring the content of the ferrous again, when the content of ferrous ions is less than or equal to 0.04g/L, the reaction is complete to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
specifically, the first mixed feed liquid obtained in the step 1 overflows into a second iron removal reaction tank, and then 0 is added into the second iron removal reaction tank.5~2m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, introducing steam into the second iron removal reaction tank, and maintaining the temperature of the second iron removal reaction tank at 67 ℃ to carry out primary low-temperature iron removal; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then flows into the third iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, and maintaining the temperature of the third iron removal reaction tank at 60 ℃ to carry out a second low-temperature iron removal reaction; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, introducing steam into the fourth iron removal reaction tank, and maintaining the temperature of the fourth iron removal reaction tank at 57 ℃ to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
And 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
Example 5
Embodiment 5 of the present invention provides an iron removal method for reducing iron ions accumulated in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank at a flow rate of 85-170L/h, controlling the potential of feed liquid in the first iron removal reaction tank to be 550-580 mv by controlling the adding amount of the sodium chlorate solution, reacting at 60 ℃, oxidizing ferrous ions in the electrodeposition solution into ferric ions, sampling and detecting the content of the ferrous ions, specifically, taking 1mL of filtrate in the first iron removal reaction tank, adding an indicator, wherein the indicator is a potassium dichromate standard solution, dropping a drop of potassium dichromate standard solution, namely changing the color into purple, indicates that the content of the ferrous ions is less than or equal to 0.04g/L is qualified, and if the content of the ferrous ions is higher than 0.04g/L, properly adding the solution to increase the potential of the sodium chlorate feed liquid, and measuring the content of the ferrous again, when the content of ferrous ions is less than or equal to 0.04g/L, the reaction is complete to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
specifically, the first mixed feed liquid obtained in the step 1 overflows into a second iron removal reaction tank, and then flows into the second iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, introducing steam into the second iron removal reaction tank, and maintaining the temperature of the second iron removal reaction tank at 70 ℃ to carry out primary low-temperature iron removal; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then flows into the third iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, and maintaining the temperature of the third iron removal reaction tank at 57 ℃ to carry out a second low-temperature iron removal reaction; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, introducing steam into the fourth iron removal reaction tank, and maintaining the temperature of the fourth iron removal reaction tank at 63 ℃ to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
And 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
Example 6
Embodiment 6 of the present invention provides an iron removal method for reducing iron ions accumulated in an electrodeposition solution, which is implemented by the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank at a flow rate of 85-170L/h, controlling the potential of feed liquid in the first iron removal reaction tank to be 550-580 mv by controlling the adding amount of the sodium chlorate solution, reacting at 60 ℃, oxidizing ferrous ions in the electrodeposition solution into ferric ions, sampling and detecting the content of the ferrous ions, specifically, taking 1mL of filtrate in the first iron removal reaction tank, adding an indicator, wherein the indicator is a potassium dichromate standard solution, dropping a drop of potassium dichromate standard solution, namely changing the color into purple, indicates that the content of the ferrous ions is less than or equal to 0.04g/L is qualified, and if the content of the ferrous ions is higher than 0.04g/L, properly adding the solution to increase the potential of the sodium chlorate feed liquid, and measuring the content of the ferrous again, when the content of ferrous ions is less than or equal to 0.04g/L, the reaction is complete to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
specifically, the first mixed feed liquid obtained in the step 1 overflows into a second iron removal reaction tank, and then flows into the second iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, introducing steam into the second iron removal reaction tank, and maintaining the temperature of the second iron removal reaction tank at 73 ℃ to carry out primary low-temperature iron removal; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then flows into the third iron removal reaction tank by 0.5-2 m3Adding 21 mass percent of liquid caustic soda at the flow rate of/h, and maintaining the temperature of the third iron removal reaction tank at 63 ℃ to carry out a second low-temperature iron removal reaction; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, introducing steam into the fourth iron removal reaction tank, and maintaining the temperature of the fourth iron removal reaction tank at 60 ℃ to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
And 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.

Claims (10)

1. An iron removal method for reducing iron ions accumulated in an electrodeposition solution is characterized by comprising the following steps:
step 1, adding an electrodeposition solution obtained by an electrodeposition process into a first iron removal reaction tank, adding a sodium chlorate solution into the first iron removal reaction tank, reacting at 55-65 ℃, and oxidizing ferrous ions in the electrodeposition solution into ferric ions to obtain a first mixed feed liquid;
step 2, continuously carrying out multiple low-temperature iron removal reactions on the first mixed feed liquid obtained in the step 1, and controlling the pH value of the low-temperature iron removal reactions to enable ferric ions in the first mixed feed liquid to generate goethite so as to obtain a second mixed feed liquid;
and 3, performing filter pressing treatment on the second mixed feed liquid to obtain the electrodeposition solution subjected to iron removal.
2. The method for removing iron to reduce the accumulation of iron ions in an electrodeposition solution according to claim 1, wherein the step 2 specifically comprises: overflowing the first mixed material liquid obtained in the step 1 into a second iron removal reaction tank, adding liquid caustic soda into the second iron removal reaction tank, and introducing steam to perform a first low-temperature iron removal reaction; the feed liquid after the first low-temperature iron removal reaction overflows into a third iron removal reaction tank, and then liquid alkali is added into the third iron removal reaction tank to carry out a second low-temperature iron removal reaction; and overflowing the feed liquid after the second low-temperature iron removal reaction into a fourth iron removal reaction tank, and introducing steam into the fourth iron removal reaction tank to perform a third low-temperature iron removal reaction to obtain a second mixed feed liquid.
3. The iron removal method for reducing the iron ions accumulated in the electrodeposition solution as claimed in claim 2, wherein the mass fractions of the liquid caustic soda added in the first low-temperature iron removal reaction, the second low-temperature iron removal reaction and the third low-temperature iron removal reaction in step 2 are all 21%, and the flow rates of the liquid caustic soda added are all 0.5-2 m3/h。
4. The method for removing iron to reduce the accumulated iron ions in the electrodeposition solution as claimed in claim 3, wherein the pH value of the reaction system after the liquid alkali is added in the first low-temperature iron removal reaction, the second low-temperature iron removal reaction and the third low-temperature iron removal reaction in step 2 is 2.5-3.
5. The method for removing iron to reduce the accumulated iron ions in the electrodeposition solution as claimed in claim 4, wherein the reaction temperature of the first low-temperature iron removal reaction in step 2 is 70 ± 3 ℃.
6. The method for removing iron to reduce the accumulated iron ions in the electrodeposition solution as claimed in claim 5, wherein the reaction temperature of the second low-temperature iron removal reaction in step 2 is 60 ± 3 ℃.
7. The method for removing iron to reduce the accumulated iron ions in the electrodeposition solution as claimed in claim 6, wherein the reaction temperature of the third low-temperature iron removal reaction in the step 2 is 60 ± 3 ℃.
8. The method for removing iron to reduce the accumulated iron ions in the electrodeposition solution according to any one of claims 1 to 7, wherein in the step 1, the addition amount of the sodium chlorate solution is controlled to control the potential of the feed liquid in the first iron removal reaction tank to be 550 to 580mv, and the reaction temperature is 55 to 65 ℃.
9. The method for removing iron to reduce the accumulation of iron ions in an electrodeposition solution as claimed in claim 8, wherein the concentration of the sodium chlorate solution in step 1 is 450-500 g/L, and the flow rate of adding the sodium chlorate solution is 85-170L/h.
10. The method for removing iron to reduce iron ions accumulated in an electrodeposition solution according to claim 9, wherein the content of ferrous ions in the first mixed feed liquid in the step 1 is 0.04g/L or less.
CN201811520810.4A 2018-12-12 2018-12-12 Iron removal method for reducing accumulated iron ions in electrodeposition solution Pending CN111304693A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101921914A (en) * 2010-09-17 2010-12-22 浙江华友钴业股份有限公司 Iron removal process for copper cobalt ore leach liquor
CN102031373A (en) * 2009-09-29 2011-04-27 惠州市东江环保技术有限公司 Method for recycling nickel and copper from electroplating sludge
CN103352122A (en) * 2013-06-21 2013-10-16 刘国燕 Method for efficiently removing iron in solution
CN103740931A (en) * 2014-01-21 2014-04-23 江苏仁欣化工股份有限公司 Method for precipitating iron from goethite containing ferro-nickel mixed solution
CN106566926A (en) * 2016-11-22 2017-04-19 江苏凯力克钴业股份有限公司 Deironing device, and low-temperature continuous deironing method
CN108060303A (en) * 2017-11-13 2018-05-22 中国恩菲工程技术有限公司 The method that iron is removed in hydrometallurgy iron-containing liquor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102031373A (en) * 2009-09-29 2011-04-27 惠州市东江环保技术有限公司 Method for recycling nickel and copper from electroplating sludge
CN101921914A (en) * 2010-09-17 2010-12-22 浙江华友钴业股份有限公司 Iron removal process for copper cobalt ore leach liquor
CN103352122A (en) * 2013-06-21 2013-10-16 刘国燕 Method for efficiently removing iron in solution
CN103740931A (en) * 2014-01-21 2014-04-23 江苏仁欣化工股份有限公司 Method for precipitating iron from goethite containing ferro-nickel mixed solution
CN106566926A (en) * 2016-11-22 2017-04-19 江苏凯力克钴业股份有限公司 Deironing device, and low-temperature continuous deironing method
CN108060303A (en) * 2017-11-13 2018-05-22 中国恩菲工程技术有限公司 The method that iron is removed in hydrometallurgy iron-containing liquor

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Application publication date: 20200619