CN116377240A - Method for purifying Ag by washing precipitate obtained by OLED silver target hydrochloric acid - Google Patents

Method for purifying Ag by washing precipitate obtained by OLED silver target hydrochloric acid Download PDF

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CN116377240A
CN116377240A CN202310444455.1A CN202310444455A CN116377240A CN 116377240 A CN116377240 A CN 116377240A CN 202310444455 A CN202310444455 A CN 202310444455A CN 116377240 A CN116377240 A CN 116377240A
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hydrochloric acid
washing
oled
purifying
silver
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李磊
黄勇
武琬越
刘杰
田海洋
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Sichuan University of Science and Engineering
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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
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • C22B11/046Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/005Preliminary treatment of scrap
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/06Chloridising
    • 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
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/10Hydrochloric acid, other halogenated acids or salts thereof
    • 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
    • C22B3/46Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • 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

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Abstract

The invention discloses a method for purifying Ag by using a precipitate obtained by washing an OLED silver target material with hydrochloric acid, and relates to the technical field of hydrometallurgy. The method comprises the following steps: sequentially drying and crushing the precipitate obtained by washing the OLED silver target material with hydrochloric acid to obtain a pretreatment raw material; mixing the pretreated raw material with a low-concentration hydrochloric acid solution, heating and stirring, then adding iron blocks, when the solution is completely changed from white to gray, collecting a solid phase, washing and drying to obtain Ag. The invention uses the precipitate obtained by washing the OLED silver target material with hydrochloric acid as a raw material, prepares Ag with 99.99 purity by a reduction method, and provides a method for purifying Ag, which is environment-friendly, low in energy consumption, simple and controllable in operation. The method solves the problems of high energy consumption, complex technology and low grade of purified Ag in the prior art.

Description

Method for purifying Ag by washing precipitate obtained by OLED silver target hydrochloric acid
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for purifying Ag by using a precipitate obtained by washing an OLED silver target material with hydrochloric acid.
Background
At present, the traditional process for extracting silver from silver chloride is mainly divided into a fire method and a wet method; wherein, the fire method is that silver chloride is added with sodium carbonate to extract silver, and the basic principle of the fire method is that
Figure BDA0004195104020000011
Has the advantages of simple process, basically no impurity generation, high energy consumption and CO generation 2 Does not meet the current carbon emission reduction carbon peak reaching policy; the wet method comprises silver chloride and iron substitution silver, ammonia leaching silver, hydrazine hydrate precipitation silver extraction and silver chloride directly adopting hydrazine hydrate to extract silver, and the principle of silver chloride and iron powder substitution silver is +.>
Figure BDA0004195104020000012
In order to avoid hydroxide precipitation generated by iron salt hydrolysis, mixing the iron powder with silver chloride and silver powder, adding excessive concentrated hydrochloric acid, adding iron powder into the product easily if the reaction is insufficient, and separating the iron powder difficultly, so that the taste of the product is reduced, refining steps are often needed, two parts of treatment are actually needed, a high-grade silver simple substance can be prepared, the crude silver generated in the first step is dissolved by using solvents such as nitric acid and the like, and filtered and then reduced by using copper, the second step has longer process time, complex process, high cost of raw material copper and nitric acid, serious environmental pollution and the like; the principle of ammonia leaching silver and hydrazine hydrate precipitation silver extraction is +.>
Figure BDA0004195104020000013
Figure BDA0004195104020000014
The principle of extracting silver from silver chloride directly by using hydrazine hydrate is 2AgCl+2N 2 H 4 ·H 2 O→2Ag+N 2 +2NH 4 Cl+2H 2 O, both methods need to use hydrazine hydrate, which is an explosive dangerous chemical, and can be adsorbed or inhaled by eyes and skin to cause harm to human bodies, and has extremely high toxicity to aquatic organisms, possibly in aquatic ringsCausing long-term adverse effects in the environment. Therefore, there is an urgent need for a silver extraction method that is environmentally friendly, low in energy consumption, simple to operate, and high in product grade.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for purifying Ag by using a precipitate obtained by washing an OLED silver target material with hydrochloric acid, so as to solve the problems of high energy consumption, complex technology, environmental protection and low grade in the prior art for purifying Ag.
The technical scheme for solving the technical problems is as follows: the method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid comprises the following steps:
(1) Sequentially drying and crushing the precipitate obtained by washing the OLED silver target material with hydrochloric acid to obtain a pretreatment raw material;
(2) Uniformly mixing the pretreated raw material prepared in the step (1) with deionized water, regulating the pH value to be 1.5-2.5, heating and stirring, then adding iron blocks, when the solution is completely changed from white to gray, collecting a solid phase, washing and drying to prepare Ag.
Based on the technical scheme, the invention can also be improved as follows:
further, in the step (1), the drying process is completed by drying at the temperature of 100-110 ℃.
Further, in the step (1), the drying process is completed by drying at 105 ℃.
Further, in the step (1), a vibration ball mill is adopted to grind the materials until the fineness of 280 meshes is more than or equal to 95 percent.
Further, in the step (2), the mass ratio of the pretreated raw material and the deionized water solution prepared in the step (1) is 1:9-11.
Further, in the step (2), the mass ratio of the pretreated raw material and the deionized water solution prepared in the step (1) is 1:10.
further, in the step (2), concentrated hydrochloric acid is adopted to adjust the pH value to be 1.5-2.5.
Further, in the step (2), concentrated hydrochloric acid is used to adjust the pH value to 2.5.
Further, in the step (2), the pH value is adjusted to 1.5 by using concentrated hydrochloric acid.
Further, in the step (2), the mass ratio of the pretreated raw material to the iron nuggets is 5:1-3.
Further, in the step (2), the temperature is heated to 25-45 ℃.
Further, in the step (2), heating to 45 ℃.
Further, in the step (2), after adding the iron block, the gas generated by the reaction is evacuated after washing with water.
The invention also provides Ag prepared by the method for purifying Ag by using the precipitate obtained by washing the OLED silver target material with hydrochloric acid.
The invention has the following beneficial effects:
1. the invention uses the precipitate obtained by washing the OLED silver target material with hydrochloric acid as a raw material, prepares Ag with 99.99 purity by a reduction method, and provides a method for purifying Ag, which is environment-friendly, low in energy consumption, simple and controllable in operation.
2. The invention adopts the iron block as the reducing agent, thereby effectively avoiding the pollution of the unreacted complete iron to the product.
3. The invention adopts deionized water, and then hydrochloric acid is added to adjust the pH, the concentration is lower, the solution only needs to be added with hydrochloric acid to adjust the pH, the solution can be reused, the solvent consumption is low, the external exhaust body has no pollutant, the external exhaust body can be directly exhausted, the reaction temperature is 25-45 ℃, the reaction temperature is basically in the normal temperature condition, the energy consumption is low, and the cost can be effectively controlled.
Drawings
FIG. 1 is a profile of a pretreated feedstock of example 1;
FIG. 2 is a morphology of the product produced in example 1;
FIG. 3 is a morphology of the product produced in example 2;
FIG. 4 is a morphology of the product obtained in example 3;
FIG. 5 is a morphology of the product obtained in example 4;
FIG. 6 is a morphology of the product produced in example 5;
FIG. 7 is a morphology of the product obtained in example 6;
FIG. 8 is a morphology of the product produced in example 7;
FIG. 9 shows the elemental content of the feedstock and the products produced from 1-4;
FIG. 10 shows the elemental content of the products obtained in examples 5-7.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
the method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid comprises the following steps:
(1) Drying the precipitate obtained by washing the OLED silver target material with hydrochloric acid at 105 ℃, and crushing the precipitate by adopting a vibration ball mill until the mass fraction of the fineness of 280 meshes is 95%, thereby obtaining a pretreatment raw material;
(2) The pretreated raw material prepared in the step (1) and deionized water are mixed according to the mass ratio of 1:10, adding concentrated hydrochloric acid to regulate the pH value to 2.5, heating to 40 ℃, adding iron blocks (the mass ratio of the pretreated raw materials to the iron blocks is 5:2), continuously stirring, washing the generated gas with water, evacuating, completely converting the solution into gray when the solution is white, collecting a solid phase, washing and drying to obtain Ag.
Example 2:
the method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid comprises the following steps:
in the step (1), concentrated hydrochloric acid was added to adjust the pH to 2, and the rest was the same as in example 1.
Example 3:
the method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid comprises the following steps:
in the step (1), concentrated hydrochloric acid was added to adjust the pH to 1.5, and the rest was the same as in example 1.
Example 4:
the method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid comprises the following steps:
in the step (1), concentrated hydrochloric acid is added to adjust the pH value to 2, and the mass ratio of the pretreated raw materials to the iron block is 5:1 and the rest are the same as in example 1.
Examples 5 to 7:
the method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid comprises the following steps:
in the step (1), concentrated hydrochloric acid was added to adjust the pH to 2, and the mixture was heated to 30℃at 35℃and 45℃in the step (2), respectively, in the rest of example 1.
Test examples
1. The Ag prepared in examples 1-7 and the pretreated feedstock in example 1 were subjected to electron microscopy and EDS characterization, respectively, and the results are shown in FIGS. 1-10.
2. The Ag prepared in examples 1-7 and the pretreated feedstock components of example 1 were separately tested and the reaction time and yield were counted and the results are shown in Table 1.
TABLE 1 example-Ag component produced
Figure BDA0004195104020000051
Figure BDA0004195104020000061
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (9)

1. The method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid is characterized by comprising the following steps:
(1) Sequentially drying and crushing the precipitate obtained by washing the OLED silver target material with hydrochloric acid to obtain a pretreatment raw material;
(2) Uniformly mixing the pretreated raw material prepared in the step (1) with deionized water, regulating the pH value to be 1.5-2.5, heating and stirring, then adding iron blocks, when the solution is completely changed from white to gray, collecting a solid phase, washing and drying to prepare Ag.
2. The method for purifying Ag by washing the obtained precipitate with hydrochloric acid, according to claim 1, wherein in step (1), the drying process is completed by drying at 100-110 ℃.
3. The method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid according to claim 1, wherein in the step (1), a vibration ball mill is adopted to grind the precipitate to a fineness of 280 meshes, and the mass fraction is more than or equal to 95%.
4. The method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid according to claim 1, wherein in the step (2), the mass ratio of the pretreated raw material prepared in the step (1) to the deionized water solution is 1:9-11.
5. The method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid according to claim 1, wherein in step (2), concentrated hydrochloric acid is used to adjust the pH value to 1.5-2.5.
6. The method for purifying Ag by washing the obtained precipitate with OLED silver target hydrochloric acid according to claim 1, wherein in the step (2), the mass ratio of the pretreatment raw material to the iron block is 5:1-3.
7. The method for purifying Ag by washing the obtained precipitate with hydrochloric acid for silver OLED target according to claim 1, wherein in step (2), the heating is performed to 25 to 45 ℃.
8. The method for purifying Ag by washing the obtained precipitate with hydrochloric acid, which is an OLED silver target material according to claim 1, wherein in the step (2), after adding iron blocks, the gas generated by the reaction is evacuated after washing with water.
9. Ag produced by the method of purifying Ag by washing the obtained precipitate with hydrochloric acid of the silver OLED target according to any one of claims 1 to 8.
CN202310444455.1A 2023-04-23 2023-04-23 Method for purifying Ag by washing precipitate obtained by OLED silver target hydrochloric acid Pending CN116377240A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4874429A (en) * 1986-10-31 1989-10-17 Austria Metall Aktiengesellschaft Hydrometallurgical process for the recovery of silver from copper electrolysis anode sludge
US20070098609A1 (en) * 2005-10-29 2007-05-03 Mcconnell Brian Hydrometallurgical process for the treatment of metal-bearing sulfide mineral concentrates
CN101280430A (en) * 2008-05-15 2008-10-08 金川集团有限公司 Preparation of hyperpure copper
JP2020132957A (en) * 2019-02-20 2020-08-31 三菱マテリアル株式会社 Silver recovery method
EP3802890A1 (en) * 2018-05-29 2021-04-14 Universita' Degli Studi Dell'Aquila Hydrometallurgical method for the recovery of base metals and precious metals from a waste material
JP2021116436A (en) * 2020-01-22 2021-08-10 大口電子株式会社 Recovery method of silver
CN114042469A (en) * 2021-12-02 2022-02-15 四川轻化工大学 Preparation method of bismuth oxycarbonate-based photocatalytic material

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4874429A (en) * 1986-10-31 1989-10-17 Austria Metall Aktiengesellschaft Hydrometallurgical process for the recovery of silver from copper electrolysis anode sludge
US20070098609A1 (en) * 2005-10-29 2007-05-03 Mcconnell Brian Hydrometallurgical process for the treatment of metal-bearing sulfide mineral concentrates
CN101280430A (en) * 2008-05-15 2008-10-08 金川集团有限公司 Preparation of hyperpure copper
EP3802890A1 (en) * 2018-05-29 2021-04-14 Universita' Degli Studi Dell'Aquila Hydrometallurgical method for the recovery of base metals and precious metals from a waste material
JP2020132957A (en) * 2019-02-20 2020-08-31 三菱マテリアル株式会社 Silver recovery method
JP2021116436A (en) * 2020-01-22 2021-08-10 大口電子株式会社 Recovery method of silver
CN114042469A (en) * 2021-12-02 2022-02-15 四川轻化工大学 Preparation method of bismuth oxycarbonate-based photocatalytic material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
无: "镀银后银的置换回收", 材料保护, vol. 44, no. 12, 15 December 2011 (2011-12-15), pages 82 *
杨朝: "铁回收镀银废液中的银", 电镀与环保, no. 4, 31 December 1991 (1991-12-31), pages 37 - 38 *

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