CN113652548A - Anti-iron liquid resin adsorption process - Google Patents

Anti-iron liquid resin adsorption process Download PDF

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Publication number
CN113652548A
CN113652548A CN202110566786.3A CN202110566786A CN113652548A CN 113652548 A CN113652548 A CN 113652548A CN 202110566786 A CN202110566786 A CN 202110566786A CN 113652548 A CN113652548 A CN 113652548A
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iron
liquid
resin
backwash
tank
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周翠平
马步伟
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention belongs to the technical field of ion exchange, and particularly relates to an anti-iron liquid resin adsorption process; the method adopts a resin method exchange process, uses anion exchange resin as an adsorbent, adsorbs iron and zinc ions which have large influence on extraction on the resin by coulomb force, and then uses condensed water or filtered tap water as an eluent to elute the zinc and the iron from the resin to achieve the purpose of separation; the method has the advantages that the anti-iron liquid has a repeated use condition, the consumption of hydrochloric acid is reduced, the extraction system is friendly, and the enrichment of iron and zinc elements in the extractant is avoided; the process has the advantages of mature technology, low engineering investment, high cost performance, small occupied area, reliable system operation, simple operation and maintenance, low operation cost and long service life.

Description

Anti-iron liquid resin adsorption process
Technical Field
The invention belongs to the field of hydrometallurgy assistance, and particularly relates to a resin adsorption process for iron ions in a high-concentration hydrochloric acid system.
Background
The hydrometallurgical extraction section needs to use hydrochloric acid to counter iron, and most of the generated counter iron waste acid is returned to a leaching system to be used as acid.
The problems existing in the prior art mainly comprise the following points: firstly, the hydrochloric acid is higher in price than the sulfuric acid and is monoacid; secondly, the hydrochloric acid can increase the dissolution of calcium ions in the leaching process, so that the calcium ions entering an extraction system exceed more than 0.5g/L, calcium slag is easily formed in an extraction tank, and the continuity and the productivity of production are influenced; thirdly, chloride ions in the hydrochloric acid enter the wastewater treatment, so that the difficulty of the wastewater treatment is increased, and the equipment investment cost is increased; fourthly, the hydrochloric acid is recycled to the leaching procedure, the reaction speed is high, the trough overflow accident is easily caused, and the leaching production is influenced.
And iron, zinc and other ions in the iron-countering liquid of the high-chloride ion system exist in the solution in the form of complex anions, so that the iron, zinc and other ions in the extracting agent are enriched, and the extraction efficiency is influenced.
Therefore, the hydrochloric acid needs to be recycled to the extraction process after iron removal, and the discharge of the hydrochloric acid is reduced.
Disclosure of Invention
In order to make up for the defects of the prior art and solve the problem that iron and zinc ions in the anti-iron liquid exist in the solution in the form of complex anions, so that the iron and zinc ions in the extractant are enriched and the extraction efficiency is influenced in the prior art, the invention provides the anti-iron liquid resin adsorption process.
The technical scheme adopted by the invention for solving the technical problems is as follows: an anti-iron liquid resin adsorption process comprises the following steps:
s1: firstly, treating the solution after iron removal by using an oxidation oil removal system: comprises aerating the iron-reverse solution in an oxidation oil-removing tank and removing Fe in the iron-reverse solution2+Oxidation to Fe3+Collecting floating oil in the anti-iron liquid;
s2: pumping the aerated back iron liquid into a resin tower by using a resin adsorption system: the resin tower is used for preparing one, anion exchange resin is used as an adsorbent in the resin tower, and iron and zinc ions are adsorbed on the resin;
s3: and then backwashing the resin tower which is adsorbed to saturation: backwashing the saturated resin tower by utilizing a water washing adsorption system and a compressed air system in cooperation with a backwashing liquid tank, and discharging final backwashing liquid into a wastewater section through the backwashing liquid tank;
s4: adding new backwash water into the backwash water tank again, and backwashing the resin tower repeatedly: at the moment, the backwashing water after backwashing the resin tower is not discharged to a wastewater working section and is used as primary backwashing water.
Preferably, in S1, before the post-iron-rejection liquid is aerated, the post-iron-rejection liquid pump is used to perform post-iron-rejection in the post-iron-rejection liquid tankQuantitatively pumping the solution into an oxidation oil removal groove, arranging a jet pump in the oxidation oil removal groove for aerating the iron-removed solution, and quantitatively adding hydrogen peroxide by using a dosing pump in the aeration process so as to quantitatively add Fe2+Oxidation to Fe3+Wherein the content of the hydrogen peroxide is generally less than 0.1% of the feeding amount, and the oxidation oil removal tank is recommended to be connected with an acid mist collecting system in a workshop, and an air draft system needs to be communicated before the jet pump is started so as to reduce the volatilization of the hydrochloric acid mist.
Preferably, in S2, two resin towers are connected in series for use, the other resin tower is reserved, the aerated anti-iron liquid is pumped into the resin towers connected in series by using an oxidation transfer pump, the iron and zinc ions in the anti-iron liquid of the high chloride ion system have a large influence on extraction, and are adsorbed on the resin by coulomb force, thereby achieving the purpose of adsorption.
Preferably, in S3, when backwashing the resin tower adsorbed to saturation, the liquid after iron-removing after adsorption in the saturated resin is discharged to an oxidation oil removal tank in cooperation with a compressed air system, and the inside of the resin tower is kept empty; utilize the backwash liquid pump to go into the resin tower with the backwash liquid pump in the backwash liquid jar, until the resin tower is overflow and flow back to the backwash liquid jar, last extrinsic cycle washing a period, rethread compressed air system is whole to be discharged the backwash liquid jar with the inside backwash back liquid of resin tower, finally discharges into the waste water workshop section through the backwash liquid jar.
Preferably, in S4, newly filling a new backwash liquid into the drained backwash liquid tank, pumping the resin tower into the resin tower repeatedly until the resin tower overflows, returning the resin tower to the backwash liquid tank, continuously washing the resin tower for a period of time in an external circulation manner, and then completely draining the backwash liquid in the resin tower to the backwash liquid tank by using compressed air, wherein the backwash liquid in the backwash liquid tank is not drained to a wastewater section and is used as a primary backwash liquid.
Preferably, in S1, Fe in the solution after iron-stripping3+Is less than 100ppm, Zn2+Is less than 400ppm, and the iron-resisting liquid Fe after the treatment of the system outlet3+、Zn2+Are all less than 5ppm and are designed to adsorb Fe3+The efficiency of (1) is more than 95 percent, and Zn is adsorbed by the design2+The efficiency of (a) is greater than 98.5%.
Preferably, in the step S3, the anti-iron liquid adsorbed in the saturated resin tower and filtered by the bag filter does not contain zinc and iron ions, has a reuse condition, reduces the consumption of hydrochloric acid, is friendly to an extraction system, and does not cause enrichment of iron and zinc elements in the extractant.
Preferably, in S3, the backwash water in the backwash liquid tank may be tap water after filtration or evaporated condensate water in principle; the instrument air source in the compressed air system is kept at 0.6Mpa, and the air quantity is more than 40Nm3H; and a DN40 pump interface and a DN50 liquid level meter interface are respectively arranged at the bottom of the liquid tank after iron return.
The invention has the technical effects and advantages that:
the invention provides an anti-iron liquid resin adsorption process, which adopts a resin method exchange process, takes anion exchange resin as an adsorbent, adsorbs iron and zinc ions which have larger influence on extraction on the resin by means of coulomb force, and then uses condensed water or filtered tap water as an eluent to elute the zinc and the iron from the resin so as to achieve the purpose of separation; the method has the advantages that the anti-iron liquid has a repeated use condition, the consumption of hydrochloric acid is reduced, the extraction system is friendly, and the enrichment of iron and zinc elements in the extractant is avoided;
the process has the advantages of mature technology, low engineering investment, high cost performance, small occupied area, reliable system operation, simple operation and maintenance, low operation cost and long service life.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a diagram of the process steps of the present invention;
FIG. 2 is a flow diagram of an adsorption process in the present invention;
FIG. 3 is a schematic view of the structure of a resin tower in the present invention;
1. a back iron liquid pipe; 11. liquid after iron removal; 12. back iron liquid pump; 13. iron liquid reaction; 2. oxidizing the oil removal tank; 21. an oxidation self-circulation pump; 22. an oxidation transfer pump; 3. a hydrogen peroxide tank; 4. a resin tower; 5. a bag filter; 6. a backwash liquid tank; 61. backwashing water; 62. a backwash liquid pump; 63. a wastewater section; 7. the air is compressed.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in fig. 1 to 3, the adsorption process of the anti-iron liquid resin according to the present invention comprises the following steps:
s1: firstly, treating the solution after iron removal by using an oxidation oil removal system: comprises aerating the anti-iron liquid in the oxidation oil-removing tank 2 and removing Fe in the anti-iron liquid2+Oxidation to Fe3+Collecting floating oil in the anti-iron liquid;
s2: pumping the aerated back iron liquid into a resin tower 4 by using a resin adsorption system 12: the resin tower 4 is used for preparing one, anion exchange resin is used as an adsorbent in the resin tower 4, and iron and zinc ions are adsorbed on the resin;
s3: and then backwashing the resin tower 4 which is adsorbed to saturation: a water washing adsorption system and a compressed air system are matched with a backwashing liquid tank 6 to backwash the saturated resin tower 4, and the final backwashing liquid is discharged into a wastewater working section through the backwashing liquid tank 6;
s4: new backwash water is added to the backwash liquid tank 6 again, and the backwash resin tower 4 is repeated: at this time, the backwash water after backwashing the resin tower 4 is not discharged to a wastewater section and is used as primary backwash water.
In the above S1, before the post-iron-rejection liquid is aerated, the post-iron-rejection liquid in the post-iron-rejection liquid tank needs to be quantitatively pumped into the oxidation oil removal tank 2 by using the post-iron-rejection liquid pump 12, and a jet pump is provided in the oxidation oil removal tank 2 for aerating the post-iron-rejection liquid, and during the second aeration, a chemical feeding pump needs to be used to quantitatively feed hydrogen peroxide solution, so as to feed Fe2+Oxidation to Fe3+Wherein the content of the hydrogen peroxide is generally less than 0.1 percent of the feeding amount, and the oxidation oil removal tank 2 is recommended to be connected with an acid mist collecting system in a workshop, and an air draft system needs to be communicated before the jet pump is started so as to reduce the volatilization of the hydrochloric acid mist.
In an embodiment of the present invention, in S2, two resin towers 4 are used in series, the other resin tower 4 is reserved, the aerated anti-iron solution is pumped into the resin towers 4 in series by the oxidation transfer pump 22, the iron and zinc ions in the anti-iron solution of the high chloride ion system have a large influence on the extraction, and are adsorbed on the resin by coulomb force, thereby achieving the purpose of adsorption.
In an embodiment of the present invention, in S3, when backwashing the resin column 4 adsorbed to saturation, the liquid after iron-back adsorption inside the saturated resin is discharged to the oxidation oil removal tank 2 in cooperation with a compressed air system, and the inside of the resin column 4 is kept empty; utilize backwash liquid pump 62 among backwash liquid tank 6 to go into resin tower 4 with backwash liquid pump 62, until resin tower 4 overflow and flow back to backwash liquid tank 6, last extrinsic cycle washing a period, the rethread compressed air system is whole to be discharged the inside backwash back liquid of resin tower 4 to backwash liquid tank 6, finally discharges into the waste water workshop section through backwash liquid tank 6.
In S4, new backwash liquid is refilled into the drained backwash liquid tank 6, and the resin tower 4 is pumped into the resin tower 4 repeatedly until the resin tower 4 overflows and then flows back to the backwash liquid tank 6, the external circulation washing is continued for a period of time, and then all the backwash liquid in the resin tower 4 is drained to the backwash liquid tank 6 by using compressed air, and at this time, the backwash liquid in the backwash liquid tank 6 is not drained to the waste water section and is used as a primary backwash liquid.
In one embodiment of the present invention, in S1, Fe in the anti-iron solution3+Is less than 100ppm, Zn2+Is less than 400ppm, and the iron-resisting liquid Fe after the treatment of the system outlet3+、Zn2+Are all less than 5ppm and are designed to adsorb Fe3+The efficiency of (1) is more than 95 percent, and Zn is adsorbed by the design2+The efficiency of (a) is greater than 98.5%.
In the S3, the anti-iron liquid adsorbed in the saturated resin tower 4 and filtered by the bag filter 5 does not contain zinc and iron ions, so that the method has a reuse condition, reduces the consumption of hydrochloric acid, is friendly to an extraction system, and does not cause enrichment of iron and zinc elements in the extractant.
As the inventionIn S3, the backwash water in the backwash liquid tank 6 may be filtered tap water or evaporated condensate water in principle; the instrument air source in the compressed air system is kept at 0.6Mpa, and the air quantity is more than 40Nm3H; and a DN40 pump interface and a DN50 liquid level meter interface are respectively arranged at the bottom of the liquid tank after iron return.
The process principle is as follows: firstly, before the liquid after the iron-back is aerated, the liquid after the iron-back in the liquid tank after the iron-back needs to be quantitatively pumped into the oxidation oil-removing tank 2 by using the liquid pump 12 after the iron-back, and an injection pump is arranged in the oxidation oil-removing tank 2 and used for aerating the liquid after the iron-back, and secondly, the hydrogen peroxide needs to be quantitatively added by using a dosing pump in the aeration process, so that Fe2+Oxidation to Fe3 +The content of hydrogen peroxide is generally less than 0.1% of the feeding amount, and the oxidation oil removal tank 2 is connected with an acid mist collecting system of a workshop, and an air draft system needs to be communicated before the jet pump is started so as to reduce the volatilization of the hydrochloric acid mist; pumping the aerated anti-iron liquid into resin towers 4 connected in series by using an oxidation transfer pump 22, wherein two resin towers 4 are connected in series for use, the other resin tower 4 is reserved, pumping the anti-iron liquid in the resin tower 4, wherein iron and zinc ions are adsorbed on anion exchange resin by virtue of coulomb force, so that the separation of iron and zinc ions in the anti-iron liquid is realized, backwashing the resin tower 4 adsorbed to saturation, and discharging the adsorbed anti-iron liquid in the saturated resin to an oxidation oil removal tank 2 by matching with a compressed air system, so as to keep the interior of the resin tower 4 empty; a backwash liquid pump 62 in the backwash liquid tank 6 is used for pumping the backwash liquid pump 62 into the resin tower 4 until the resin tower 4 overflows and flows back to the backwash liquid tank 6, the external circulation washing is continued for a period of time, then a compressed air system is used for discharging all backwash liquid in the resin tower 4 to the backwash liquid tank 6, and finally the backwash liquid is discharged into a wastewater working section through the backwash liquid tank 6; finally, new backwash liquid is poured into the drained backwash liquid tank 6 again, the resin tower 4 is pumped into repeatedly until the resin tower 4 overflows and then flows back to the backwash liquid tank 6, the external circulation washing is continued for a period of time, then the backwash liquid in the resin tower 4 is completely drained to the backwash liquid tank 6 by utilizing compressed air, and at the moment, the backwash liquid in the backwash liquid tank 6 is not drained to a wastewater working section and is used as primary backwash liquid; in which the middle school isThe iron-reflecting liquid adsorbed by the resin tower 4 needs to be filtered by a bag filter 5, and Fe in the iron-reflecting liquid is filtered3+、Zn2+The concentration of the iron-removing liquid is less than 5ppm, the repeated use condition of the iron-removing liquid can be realized, the process reduces the consumption of hydrochloric acid, is friendly to an extraction system, and does not cause the enrichment of iron and zinc elements in the extractant.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. An anti-iron liquid resin adsorption process is characterized in that: the adsorption process comprises the following steps:
s1: firstly, treating the solution after iron removal by using an oxidation oil removal system: comprises aerating the iron-reverse solution in an oxidation oil-removing tank and removing Fe in the iron-reverse solution2+Oxidation to Fe3+Collecting floating oil in the anti-iron liquid;
s2: pumping the aerated back iron liquid into a resin tower by using a resin adsorption system: the resin tower is used for preparing one, anion exchange resin is used as an adsorbent in the resin tower, and iron and zinc ions are adsorbed on the resin;
s3: and then backwashing the resin tower which is adsorbed to saturation: backwashing the saturated resin tower by utilizing a water washing adsorption system and a compressed air system in cooperation with a backwashing liquid tank, and discharging final backwashing liquid into a wastewater section through the backwashing liquid tank;
s4: adding new backwash water into the backwash water tank again, and backwashing the resin tower repeatedly: at the moment, the backwashing water after backwashing the resin tower is not discharged to a wastewater working section and is used as primary backwashing water.
2. The anti-iron liquid resin as claimed in claim 1The adsorption process is characterized in that: in S1, before the liquid after the iron-back is aerated, the liquid after the iron-back in the liquid tank after the iron-back needs to be quantitatively pumped into an oxidation oil removing tank by using a liquid pump after the iron-back, a jet pump is arranged in the oxidation oil removing tank and used for aerating the liquid after the iron-back, and hydrogen peroxide needs to be quantitatively added by using a dosing pump in the aeration process, so that Fe is added2+Oxidation to Fe3+Wherein the content of the hydrogen peroxide is generally less than 0.1% of the feeding amount, and the oxidation oil removal tank is recommended to be connected with an acid mist collecting system in a workshop, and an air draft system needs to be communicated before the jet pump is started so as to reduce the volatilization of the hydrochloric acid mist.
3. The anti-iron liquid resin adsorption process according to claim 2, characterized in that: in the S2, two resin towers are connected in series for use, the other resin tower is reserved, the aerated anti-iron liquid is pumped into the resin towers connected in series by using an oxidation transfer pump, iron and zinc ions in the anti-iron liquid of a high chloride ion system have large influence on extraction, and are adsorbed on the resin by means of coulomb force, so that the adsorption purpose is achieved.
4. The anti-iron liquid resin adsorption process according to claim 3, characterized in that: in the step S3, when the resin tower adsorbed to saturation is backwashed, the liquid after iron removal after adsorption in the saturated resin is discharged to an oxidation oil removal tank by matching with a compressed air system, and the interior of the resin tower is kept empty; utilize the backwash liquid pump to go into the resin tower with the backwash liquid pump in the backwash liquid jar, until the resin tower is overflow and flow back to the backwash liquid jar, last extrinsic cycle washing a period, rethread compressed air system is whole to be discharged the backwash liquid jar with the inside backwash back liquid of resin tower, finally discharges into the waste water workshop section through the backwash liquid jar.
5. The anti-iron liquid resin adsorption process according to claim 4, characterized in that: and in S4, newly filling new backwash liquid into the drained backwash liquid tank, repeatedly pumping into the resin tower until the resin tower overflows and then reflowing to the backwash liquid tank, continuously washing for a period of time in an external circulation mode, completely draining the backwash liquid in the resin tower to the backwash liquid tank by utilizing compressed air, and at the moment, not discharging the backwash liquid in the backwash liquid tank to a waste water section, wherein the backwash liquid is used as primary backwash liquid.
6. The anti-iron liquid resin adsorption process according to claim 5, characterized in that: in the S1, Fe in the solution after iron-removing3+Is less than 100ppm, Zn2+Is less than 400ppm, and the iron-resisting liquid Fe after the treatment of the system outlet3+、Zn2+Are all less than 5ppm and are designed to adsorb Fe3+The efficiency of (1) is more than 95 percent, and Zn is adsorbed by the design2+The efficiency of (a) is greater than 98.5%.
7. The anti-iron liquid resin adsorption process according to claim 6, characterized in that: in the S3, the anti-iron liquid absorbed in the saturated resin tower and filtered by the bag filter does not contain zinc and iron ions, so that the method has the advantages of repeated use conditions, reduced hydrochloric acid consumption, friendly extraction system and no enrichment of iron and zinc elements in the extractant.
8. The anti-iron liquid resin adsorption process according to claim 6, characterized in that: in S3, the backwash water in the backwash liquid tank may be, in principle, filtered tap water or evaporated condensate water; the instrument air source in the compressed air system is kept at 0.6Mpa, and the air quantity is more than 40Nm3H; and a DN40 pump interface and a DN50 liquid level meter interface are respectively arranged at the bottom of the liquid tank after iron return.
CN202110566786.3A 2021-05-24 2021-05-24 Anti-iron liquid resin adsorption process Pending CN113652548A (en)

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CN202110566786.3A CN113652548A (en) 2021-05-24 2021-05-24 Anti-iron liquid resin adsorption process

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CN202110566786.3A CN113652548A (en) 2021-05-24 2021-05-24 Anti-iron liquid resin adsorption process

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114853219A (en) * 2022-05-26 2022-08-05 赛恩斯环保股份有限公司 Method for removing COD (chemical oxygen demand) from high ammonia nitrogen manganese raffinate
CN116477814A (en) * 2023-06-19 2023-07-25 深圳永清水务有限责任公司 Resource treatment process and system for waste liquid of hydrometallurgical extraction back iron

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114853219A (en) * 2022-05-26 2022-08-05 赛恩斯环保股份有限公司 Method for removing COD (chemical oxygen demand) from high ammonia nitrogen manganese raffinate
CN116477814A (en) * 2023-06-19 2023-07-25 深圳永清水务有限责任公司 Resource treatment process and system for waste liquid of hydrometallurgical extraction back iron

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Application publication date: 20211116