CN114261985A - High-valued treatment method for zinc-iron-containing solid waste - Google Patents

High-valued treatment method for zinc-iron-containing solid waste Download PDF

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CN114261985A
CN114261985A CN202111549909.9A CN202111549909A CN114261985A CN 114261985 A CN114261985 A CN 114261985A CN 202111549909 A CN202111549909 A CN 202111549909A CN 114261985 A CN114261985 A CN 114261985A
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iron
zinc
solid waste
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roasting
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姚海威
毛瑞
王飞
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Jiangsu Shagang Group Co Ltd
Zhangjiagang Hongchang Steel Plate Co Ltd
Jiangsu Shagang Iron and Steel Research Institute Co Ltd
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Jiangsu Shagang Group Co Ltd
Zhangjiagang Hongchang Steel Plate Co Ltd
Jiangsu Shagang Iron and Steel Research Institute Co Ltd
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Priority to PCT/CN2022/119340 priority patent/WO2023109224A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/06—Ferric oxide [Fe2O3]
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/34—Obtaining zinc oxide
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/02—Working-up flue dust
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • General Physics & Mathematics (AREA)
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  • Composite Materials (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a high-valued treatment method for zinc-iron-containing solid waste, belonging to the technical field of metal recycling. The method comprises the following steps: washing, filtering, drying and grinding the zinc-iron-containing solid waste to obtain a water washing sample; adding the water washed sample into a choline chloride-oxalic acid dihydrate eutectic solvent, heating and stirring until the solution is clear, and standing the solution; adding supernatant of the solution after standing into deionized water, hydrolyzing, filtering to obtain filtrate and filter residue, drying the filter residue, and roasting to obtain nano zinc oxide; standing the filtrate, filtering, drying and roasting to obtain the nano iron oxide. The method can efficiently separate the zinc oxide and the iron oxide from the zinc-containing iron solid waste, and prepare the nano zinc oxide and the nano iron oxide under the condition of not adding a surfactant.

Description

High-valued treatment method for zinc-iron-containing solid waste
Technical Field
The invention belongs to the technical field of metal recycling, and particularly relates to a high-valued treatment method for zinc-iron-containing solid waste.
Background
The iron and steel enterprises are energy and resource consuming households and also pollutant discharging households. Solid waste is inevitably generated in the steel production process. Billions of tons of solid wastes are generated every year in China, and the zinc content in most of the solid wastes is increased due to the increase of the proportion of the electric furnace steelmaking process and the increase of the proportion of galvanized steel scraps. Therefore, the high-value treatment of solid wastes containing zinc and iron becomes a hot problem nowadays. At present, the recycling of the zinc-containing iron solid waste is realized to a certain extent, but the utilization rate and the added value are not high.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides a high-valued treatment method of zinc-containing iron solid waste, which can efficiently separate zinc oxide and iron oxide from the zinc-containing iron solid waste and prepare nano zinc oxide and nano iron oxide without adding a surfactant.
The technical scheme is as follows: a high-value treatment method for solid waste containing zinc and iron comprises the following steps:
(1) washing, filtering, drying and grinding the zinc-iron-containing solid waste to obtain a water washing sample;
(2) adding the water washed sample into a choline chloride-oxalic acid dihydrate eutectic solvent, heating and stirring until the solution is clear, and standing the solution;
(3) adding supernatant of the solution after standing into deionized water, hydrolyzing, filtering to obtain filtrate and filter residue, drying the filter residue, and roasting to obtain nano zinc oxide; standing the filtrate, filtering, drying and roasting to obtain the nano iron oxide.
Preferably, the mol ratio of the choline chloride to the oxalic acid dihydrate in the choline chloride-oxalic acid dihydrate eutectic solvent in the step (2) is 1: 1-1.5.
Preferably, the heating and stirring temperature in the step (2) is 60-80 ℃, and the heating and stirring time is 20-40 min.
Preferably, the standing temperature in the step (2) is 60-80 ℃, and the standing time is 60-120 min.
Preferably, the hydrolysis temperature in the step (3) is 60-80 ℃, and the hydrolysis time is 20-40 min.
Preferably, the roasting temperature of the filter residue in the step (3) is 450-500 ℃, and the roasting time is 90-120 min.
Preferably, the standing temperature of the filtrate in the step (3) is 60-80 ℃, and the standing time is 48-64 h.
Preferably, after standing, filtering and drying the filtrate obtained in the step (3), the roasting temperature is 400-450 ℃, and the roasting time is 90-120 min.
Has the advantages that: (1) the choline chloride-oxalic acid dihydrate (CC-OA) eutectic solvent has high solubility only to zinc oxide and ferric oxide, is basically insoluble to other oxides, and can efficiently extract zinc and iron in the zinc-iron-containing solid waste.
(2) In the hydrolysis process, a zinc precursor is directly separated out, an iron precursor can be separated out after a period of time, and the separation of zinc and iron can be realized.
(3) The nano material can be prepared without adding a surfactant, and the raw material has low price, is easy to biodegrade and is environment-friendly.
The principle of the invention is as follows:
choline chloride and oxalic acid dihydrate are mixed and heated and stirred at the temperature of 80 ℃ to form a clear and transparent choline chloride-oxalic acid dihydrate (CC-OA) eutectic solvent, wherein CC-OA can selectively dissolve metal oxides, and has high solubility only for zinc oxide and ferric oxide, but has basically no solubility for aluminum oxide, calcium oxide, silicon oxide, lead oxide and the like. Based on the selective solubility of CC-OA to metal oxides, CC-OA is used for treating zinc-iron-containing solid waste and can prepare a nano material without adding a surfactant, the CC-OA is an ideal extracting agent for the zinc-iron-containing solid waste, and zinc oxide and iron oxide react in the CC-OA as follows:
Figure 926235DEST_PATH_IMAGE001
and (3) carrying out hydrolysis reaction on the supernatant in deionized water:
Figure 991844DEST_PATH_IMAGE002
the zinc-iron precursor is roasted to react as follows:
Figure 37160DEST_PATH_IMAGE003
drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a microscopic topography of the zinc end product of example 1, with the scales of panels a and b being 500nm and 200nm, respectively;
FIG. 3 is a microscopic topography of the iron end product of example 1, with the scales of panels a and b being 500nm and 200nm, respectively.
Detailed Description
The invention is further described below with reference to the accompanying drawings and specific embodiments.
Example 1
The zinc and iron containing dust to be treated has the following components:
50.6%Fe2O3-29.2%ZnO-4.21%SiO2-5.64%CaSO4-4.48%C-1.6%KCl-0.64NaCl-0.645%
MgO-0.564%PbO-0.864%Al2O3-0.456%P2O5。
as shown in fig. 1, the solid waste containing zinc and iron is treated according to the following steps:
(1) and (3) washing the zinc-iron-containing solid waste with water at the washing temperature of 50 ℃ for 5min, filtering, drying at 105 ℃, and grinding to obtain a water washing sample.
(2) Adding the washed zinc-containing iron solid waste into a choline chloride-oxalic acid dihydrate (molar ratio is 1:1) eutectic solvent, heating and stirring at 80 ℃ for 30min until the solution is clear, and standing at 80 ℃ for 60 min.
(3) Adding the supernatant into 80 deg.C deionized water, hydrolyzing for 30min, filtering to obtain filtrate and residue, and roasting the residue at 450 deg.C for 120min to obtain nanometer zinc oxide; standing the filtrate for 48h, filtering, drying, and roasting at 400 ℃ for 120min to obtain the nano-iron oxide.
After the zinc-iron-containing solid waste is treated, the ZnO content in the obtained nano zinc oxide is 99.768%, and the Fe content in the nano iron oxide is obtained2O3The content of (B) was 99.67%. The micro-morphology of the nano zinc oxide is shown in figure 2 and is relatively uniform and spherical, the average grain diameter is 28nm, and the micro-morphology of the nano iron oxide is shown in figure 3 and is irregular cubic crystal structure, and the average grain diameter is 37.1 nm.
Example 2
The zinc and iron containing dust to be treated has the following components:
50.6%Fe2O3-29.2%ZnO-4.21%SiO2-5.64%CaSO4-4.48%C-1.6%KCl-0.64NaCl-0.645%
MgO-0.564%PbO-0.864%Al2O3-0.456%P2O5。
as shown in fig. 1, the solid waste containing zinc and iron is treated according to the following steps:
(1) and (3) washing the zinc-iron-containing solid waste with water at the washing temperature of 50 ℃ for 5min, filtering, drying at 105 ℃, and grinding to obtain a water washing sample.
(2) Adding the zinc-containing iron solid waste after washing into a choline chloride-oxalic acid dihydrate (molar ratio is 1:1) eutectic solvent, heating and stirring at 70 ℃ for 40min until the solution is clear, and standing at 70 ℃ for 90 min.
(3) Adding the supernatant into deionized water at 70 deg.C, hydrolyzing for 40min, filtering to obtain filtrate and residue, and roasting the residue at 450 deg.C for 120min to obtain nanometer zinc oxide; standing the filtrate for 48h, filtering, drying, and roasting at 400 ℃ for 120min to obtain the nano-iron oxide.
After the zinc-iron-containing solid waste is treated, the ZnO content in the obtained nano zinc oxide is 99.689%, and the Fe content in the nano iron oxide is obtained2O3The content of (A) is 99.702%. The average grain diameter of the nano zinc oxide is 27.9nm, and the average grain diameter of the nano iron oxide is 37.4 nm.
Example 3
The zinc and iron containing dust to be treated has the following components:
50.6%Fe2O3-29.2%ZnO-4.21%SiO2-5.64%CaSO4-4.48%C-1.6%KCl-0.64NaCl-0.645%
MgO-0.564%PbO-0.864%Al2O3-0.456%P2O5。
as shown in fig. 1, the solid waste containing zinc and iron is treated according to the following steps:
(1) and (3) washing the zinc-iron-containing solid waste with water at the washing temperature of 50 ℃ for 5min, filtering, drying at 105 ℃, and grinding to obtain a water washing sample.
(2) Adding the washed zinc-containing iron solid waste into a choline chloride-oxalic acid dihydrate (molar ratio is 1:1) eutectic solvent, heating and stirring at 80 ℃ for 30min until the solution is clear, and standing at 80 ℃ for 60 min.
(3) Adding the supernatant into 80 deg.C deionized water, hydrolyzing for 30min, filtering to obtain filtrate and residue, and roasting the residue at 500 deg.C for 90min to obtain nanometer zinc oxide; standing the filtrate for 48h, filtering, drying, and roasting at 450 ℃ for 90min to obtain the nano-iron oxide.
After the zinc-iron-containing solid waste is treated, the ZnO content in the obtained nano zinc oxide is 99.695%, and the Fe content in the nano iron oxide is obtained2O3The content of (A) is 99.685%. The average grain diameter of the nano zinc oxide is 34.5nm, and the average grain diameter of the nano iron oxide is 41.3 nm.
Example 4
The zinc and iron containing dust to be treated has the following components:
50.6%Fe2O3-29.2%ZnO-4.21%SiO2-5.64%CaSO4-4.48%C-1.6%KCl-0.64NaCl-0.645%
MgO-0.564%PbO-0.864%Al2O3-0.456%P2O5。
as shown in fig. 1, the solid waste containing zinc and iron is treated according to the following steps:
(1) and (3) washing the zinc-iron-containing solid waste with water at the washing temperature of 50 ℃ for 5min, filtering, drying at 105 ℃, and grinding to obtain a water washing sample.
(2) Adding the washed zinc-containing iron solid waste into a choline chloride-oxalic acid dihydrate (molar ratio is 1:1.3) eutectic solvent, heating and stirring at 80 ℃ for 30min until the solution is clear, and standing at 80 ℃ for 60 min.
(3) Adding the supernatant into 80 deg.C deionized water, hydrolyzing for 30min, filtering to obtain filtrate and residue, and roasting the residue at 450 deg.C for 120min to obtain nanometer zinc oxide; standing the filtrate for 48h, filtering, drying, and roasting at 400 ℃ for 120min to obtain the nano-iron oxide.
After the zinc-iron-containing solid waste is treated, the ZnO content in the obtained nano zinc oxide is 99.738%, and the Fe content in the nano iron oxide is obtained2O3The content of (A) is 99.665%. The average grain diameter of the nano zinc oxide is 27.8nm, and the average grain diameter of the nano iron oxide is 38.4 nm.

Claims (8)

1. A high-value treatment method for solid waste containing zinc and iron is characterized by comprising the following steps:
(1) washing, filtering, drying and grinding the zinc-iron-containing solid waste to obtain a water washing sample;
(2) adding the water washed sample into a choline chloride-oxalic acid dihydrate eutectic solvent, heating and stirring until the solution is clear, and standing the solution;
(3) adding supernatant of the solution after standing into deionized water, hydrolyzing, filtering to obtain filtrate and filter residue, drying the filter residue, and roasting to obtain nano zinc oxide; standing the filtrate, filtering, drying and roasting to obtain the nano iron oxide.
2. The method for high-valued treatment of solid waste containing zinc and iron according to claim 1, wherein the molar ratio of choline chloride to oxalic acid dihydrate in the choline chloride-oxalic acid dihydrate eutectic solvent in step (2) is 1: 1-1.5.
3. The high-valued treatment method for the solid waste containing zinc and iron according to claim 1, wherein the heating and stirring temperature in the step (2) is 60-80 ℃, and the heating and stirring time is 20-40 min.
4. The high-valued treatment method for the solid waste containing zinc and iron according to claim 1, wherein the standing temperature in the step (2) is 60-80 ℃, and the standing time is 60-120 min.
5. The high-valued treatment method for the solid waste containing zinc and iron according to claim 1, wherein the hydrolysis temperature in the step (3) is 60-80 ℃, and the hydrolysis time is 20-40 min.
6. The high-valued treatment method for the solid waste containing zinc and iron according to claim 1, wherein the roasting temperature of the filter residue in the step (3) is 450-500 ℃, and the roasting time is 90-120 min.
7. The high-valued treatment method for the solid waste containing zinc and iron according to claim 1, wherein the standing temperature of the filtrate in the step (3) is 60-80 ℃, and the standing time is 48-64 h.
8. The high-valued treatment method for the solid waste containing zinc and iron according to claim 1, wherein the roasting temperature is 400-450 ℃ and the roasting time is 90-120 min after the filtrate in the step (3) is allowed to stand, filtered and dried.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023109224A1 (en) * 2021-12-17 2023-06-22 江苏沙钢集团有限公司 High-value processing method for solid waste containing zinc and iron

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CN110357145A (en) * 2019-08-15 2019-10-22 昆明理工大学 A method of zinc oxalate is prepared using zinc oxide fumes and prepares nano zine oxide
CN110358923A (en) * 2019-08-15 2019-10-22 昆明理工大学 A method of indium is extracted using zinc oxide fumes and recycles zinc oxide fumes

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