CN107674984A - The recovery method of valuable metal in a kind of metallurgical slag - Google Patents
The recovery method of valuable metal in a kind of metallurgical slag Download PDFInfo
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- CN107674984A CN107674984A CN201710893154.1A CN201710893154A CN107674984A CN 107674984 A CN107674984 A CN 107674984A CN 201710893154 A CN201710893154 A CN 201710893154A CN 107674984 A CN107674984 A CN 107674984A
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- 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
- C22B7/04—Working-up slag
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- 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
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- 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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- 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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Abstract
The present invention relates to the recovery method of valuable metal in metallurgical slag, using reduction roasting, again water logging, reoxidize acidleach, be finally segmented the mode of cyclone electrolytic cell, auxiliary agent be specifically added in roasting, make the reaction of metallurgical slag fully, good fluidity, beneficial to sedimentation separation.First water logging reoxidizes acidleach, and cyclone electrolytic cell is carried out again after mixing water lixivium and oxidation acid leaching leachate, has certain help to the rate of recovery for improving valuable metal cupro-nickel.The present invention is lower than traditional nickel fibers slag recovery process production cost, and compares conventional cyclone electrolytic cell mode, and the rate of recovery of the invention is higher.
Description
Technical field
The present invention relates to metallurgical slag recycling field, is a kind of recovery side for being related to valuable metal in metallurgical slag specifically
Method.
Background technology
The comprehensive reutilization of solid waste secondary resource is a big theme of world today's environmental protection, especially coloured
Metal and its compound field, either still economically all it is necessary in environmental protection.Solid waste goods and materials simultaneously
Source comprehensive utilization is that shortage of resources problem is alleviated in country, walks sustainable development path, creates the only way of conservation-minded society.Closely
Year, in the case where a series of encouragement of country help the policy of secondary resource comprehensive reutilization project to guide, China's solid waste
Comprehensive reutilization achieves remarkable effect.Synthetical recovery has from enormous amount, miscellaneous various more metal wastes
Valency metals resources, accomplish to turn waste into wealth, realize solid waste resource recovery, minimizing and innoxious, be economic, society, environment
The inevitable choice of sustainable development.Therefore, as the stable development of economy, the increasingly shortage of metals resources, people give birth to environment
The continuous improvement that state protection requires, China's solid waste resource utilization project will have huge development prospect, particularly from having
The various valuable metal compositions of separation and Extraction synthetical recovery in non-ferrous metal melting waste slag.Traditional resource regeneration and resource reclaim row
Industry, limited by factors such as technology, production capacity and secondary pollutions to environment, rest on manual individual workship or small-sized extensive always
The type process segment, in recent years the deep processing and utilization of renewable resource just gradually paid attention to by national governments, China is also " 12
In five " development outlines, the policy support to regenerated resources comprehensive reutilization project is increased again.Utilization are new to return
Technological means is received, realizes to the multi-level comprehensive reutilization of resource in solid waste, accomplishes to integrate back from a kind of waste material
A variety of valuable metal compositions are received, the circulating repetition utilization from raw material, product and recovery process flow is realized, realizes that resource maximizes
Comprehensive reutilization.
Nickel is mainly used in the industries such as stainless steel, high temperature alloy, plating and chemical industry.Therefore, nickel has in the national economic development
There is extremely important status.Sum up, the purposes of nickel mainly includes:Manufacture stainless steel and other metal materials;For electroplating industry;
Make petrochemical catalyst;Manufacture electrochmical power source;As pigment and dyestuff;Manufacture high temperature alloy.According to not counting not exclusively, entirely
The nickel of ball about 2/3 is used to produce stainless steel.
Cyclone electrolytic cell technology is a kind of difference using each metal ion species deposition potential, hard by efficient " turbocharging "
Part system, the method that valuable metal is selectively purified from solution.The technology just can be from solution by simple single step process
The middle various valuable metals of recovery, reduce or cancel the intermediate link such as chemical cleaning method or solvent extraction, save to amplitude peak production
Cost.
The content of the invention
In order to solve the rate of recovery and Cost Problems of nickel fibers slag recovery process, the invention provides in a kind of nickel fibers slag
The recovery method of valuable metal, it includes the steps such as roasting, water logging, acidleach, cyclone electrolytic cell, so that copper in nickel fibers slag,
Nickel recovery is up to more than 99% and eliminates the processes such as extraction.
The recovery method of valuable metal in nickel fibers slag, including:
(1) nickel fibers slag, auxiliary agent and quick lime are mixed, obtains mixed material;
(2) mixed material is calcined, the solid mixture after being calcined;
(3) by the solid mixture carry out crushing grinding, hot water pulp, after stirring reheat water to liquid-solid ratio be 3~
5:1, it is stirred for, is filtrated to get filtrate and filter residue;
(4) after filter residue being added into sulfuric acid, the logical oxygen progress Oxidation Leaching in autoclave, leaching 2~4 hours, afterwards
Separating treatment is carried out, obtains leachate and leached mud;
(5) filtrate and the leachate are mixed 1~2 hour, adjusts pH value afterwards to 4~5, carry out two sections
Cyclone electrolytic cell;Current density is 50~80A/m when first stage is electrolysed2, electrolyte circular flow is 30L/h, temperature is 40~
50 DEG C, it is 200mg/L to control terminal copper ion concentration, and negative electrode copper products are obtained using cyclone electrolytic cell;Electrolyte after decopper(ing) after
Continuous to carry out second stage cyclone electrolytic cell, current density is 30~50A/m2, electrolyte circular flow is 20L/h, temperature is 40~
50 DEG C, when terminal copper ion concentration is in 300mg/L, nickeliferous more than 98% cathode nickel product is obtained using eddy flow electrodeposition.
The auxiliary agent is made up of following components in percentage by weight:Lime stone 12~15%, iron ore 10~13%, silicic acid
Aluminium 8~10%, carborundum 5~8%, flyash 3~5%, surplus are coke.
In the step (1), nickel fibers slag, auxiliary agent and quick lime are 1 according to mass ratio:(2~2.5):(5~6.5)
Mixed.
In the step (2), the temperature of the calcination process is 1000~1200 DEG C;Carried out by the mixed material
Before calcination process, forming processes are carried out to the mixed material in advance, obtain mixing pelletizing.
In the step (3), powder of the particle diameter less than 0.056mm accounts for total amount in the powder after the crushing grinding
More than 75wt%.
In the step (3), with 80~95 DEG C of hot water pulps, the volume of hot water and the mass ratio 1 of solid mixture:1,
After stirring 0.5~1.0 hour, then 80~95 DEG C of hot water to liquid-solid ratio is added to be 3~5:1, it is stirred for 0.5~1.0 hour, filters
To filtrate and filter residue.
The present invention using reduction roasting, again water logging, reoxidize acidleach, finally be segmented cyclone electrolytic cell mode, roasting when
Be specifically added auxiliary agent, make metallurgical slag reaction fully, good fluidity, beneficial to sedimentation separation.First water logging reoxidizes acidleach, mixing
Cyclone electrolytic cell is carried out again after water logging filtrate and oxidation acid leaching leachate, has certain side to the rate of recovery for improving valuable metal cupro-nickel
Help.The present invention is lower than traditional nickel fibers slag recovery process production cost, and compares conventional cyclone electrolytic cell mode, and of the invention returns
Yield is higher.
Embodiment
With reference to embodiment and comparative example, the present invention is described in more detail.
Embodiment 1:
The recovery method of valuable metal in nickel fibers slag, including:(1) nickel fibers slag, auxiliary agent and quick lime are mixed,
Obtain mixed material.Nickel fibers slag, auxiliary agent and quick lime are 1 according to mass ratio:2:5 are mixed.The auxiliary agent is by following heavy
The component of amount percentage is made:Lime stone 12%, iron ore 10%, alumina silicate 8%, carborundum 5%, flyash 3%, surplus are
Coke.(2) mixed material is calcined, the solid mixture after being calcined, the temperature of the calcination process is
1000℃;Before the mixed material is carried out into calcination process, forming processes are carried out to the mixed material in advance, mixed
Close pelletizing.(3) solid mixture is subjected to crushing grinding, particle diameter is less than 0.056mm in the powder after the crushing grinding
Powder account for more than the 75wt% of total amount, with 80 DEG C of hot water pulps, the volume of hot water and the mass ratio 1 of solid mixture:1, stir
After mixing 0.5 hour, then 80 DEG C of hot water to liquid-solid ratio is added to be 3:1, it is stirred for 0.5 hour, is filtrated to get filtrate and filter residue.(4) will
After filter residue adds sulfuric acid, oxygen progress Oxidation Leaching is led in autoclave, leaching 2 hours, separating treatment is carried out afterwards, is soaked
Go out liquid and leached mud;(5) filtrate and the leachate are mixed 1 hour, adjusts pH value afterwards to 4, carry out two sections
Cyclone electrolytic cell;Current density is 50A/m when first stage is electrolysed2, electrolyte circular flow is 30L/h, and temperature is 40 DEG C, control
Terminal copper ion concentration is 200mg/L, and negative electrode copper products are obtained using cyclone electrolytic cell;Electrolyte after decopper(ing) continues second
Stage cyclone electrolytic cell, current density 30A/m2, electrolyte circular flow is 20L/h, and temperature is 40 DEG C, dense in terminal copper ion
Degree obtains nickeliferous more than 98% cathode nickel product in 300mg/L using eddy flow electrodeposition.Wherein, copper recovery is
99.15%th, nickel recovery is up to 99.05%.
Embodiment 2:
The recovery method of valuable metal in nickel fibers slag, including:(1) nickel fibers slag, auxiliary agent and quick lime are mixed,
Obtain mixed material.Nickel fibers slag, auxiliary agent and quick lime are 1 according to mass ratio:2.5:6.5 are mixed.The auxiliary agent by with
The component of lower percentage by weight is made:Lime stone 15%, iron ore 13%, alumina silicate 10%, carborundum 8%, flyash 5%,
Surplus is coke.(2) mixed material is calcined, the solid mixture after being calcined, the temperature of the calcination process
Spend for 1200 DEG C;Before the mixed material is carried out into calcination process, forming processes are carried out to the mixed material in advance, obtained
To mixing pelletizing.(3) solid mixture is subjected to crushing grinding, particle diameter is less than in the powder after the crushing grinding
0.056mm powder accounts for more than the 75wt% of total amount, with 95 DEG C of hot water pulps, the volume of hot water and the mass ratio of solid mixture
1:1, after stirring 1.0 hours, then add 95 DEG C of hot water to liquid-solid ratio to be 5:1, it is stirred for 1.0 hours, is filtrated to get filtrate and filter residue.
(4) after filter residue being added into sulfuric acid, oxygen progress Oxidation Leaching is led in autoclave, leaching 4 hours, carries out separating treatment afterwards,
Obtain leachate and leached mud;(5) filtrate and the leachate are mixed 2 hours, adjusts pH value afterwards to 5, enter
Two sections of cyclone electrolytic cells of row;Current density is 80A/m when first stage is electrolysed2, electrolyte circular flow is 30L/h, temperature 50
DEG C, it is 200mg/L to control terminal copper ion concentration, and negative electrode copper products are obtained using cyclone electrolytic cell;Electrolyte after decopper(ing) continues
Carry out second stage cyclone electrolytic cell, current density 50A/m2, electrolyte circular flow is 20L/h, and temperature is 50 DEG C, in terminal
Copper ion concentration obtains nickeliferous more than 98% cathode nickel product in 300mg/L, using eddy flow electrodeposition.Wherein, copper recovery
It is 99.04%, nickel recovery up to 99.11%.
Embodiment 3:
The recovery method of valuable metal in nickel fibers slag, including:(1) nickel fibers slag, auxiliary agent and quick lime are mixed,
Obtain mixed material.Nickel fibers slag, auxiliary agent and quick lime are 1 according to mass ratio:2:5.5 are mixed.The auxiliary agent is by following
The component of percentage by weight is made:Lime stone 14%, iron ore 12%, alumina silicate 9%, carborundum 6%, flyash 4%, surplus
For coke.(2) mixed material is calcined, the solid mixture after being calcined, the temperature of the calcination process is
1100℃;Before the mixed material is carried out into calcination process, forming processes are carried out to the mixed material in advance, mixed
Close pelletizing.(3) solid mixture is subjected to crushing grinding, particle diameter is less than 0.056mm in the powder after the crushing grinding
Powder account for more than the 75wt% of total amount, with 90 DEG C of hot water pulps, the volume of hot water and the mass ratio 1 of solid mixture:1, stir
After mixing 1.0 hours, then 90 DEG C of hot water to liquid-solid ratio is added to be 4:1, it is stirred for 1.0 hours, is filtrated to get filtrate and filter residue.(4) will
After filter residue adds sulfuric acid, oxygen progress Oxidation Leaching is led in autoclave, leaching 3 hours, separating treatment is carried out afterwards, is soaked
Go out liquid and leached mud;(5) filtrate and the leachate are mixed 1.5 hours, adjusts pH value afterwards to 4, carry out two
Section cyclone electrolytic cell;Current density is 60A/m when first stage is electrolysed2, electrolyte circular flow is 30L/h, and temperature is 45 DEG C, control
Terminal copper ion concentration processed is 200mg/L, and negative electrode copper products are obtained using cyclone electrolytic cell;Electrolyte after decopper(ing) continues
Two-stage cyclone electrolytic cell, current density 40A/m2, electrolyte circular flow is 20L/h, and temperature is 45 DEG C, in terminal copper ion
Concentration obtains nickeliferous more than 98% cathode nickel product in 300mg/L, using eddy flow electrodeposition.Wherein, copper recovery is
99.10%th, nickel recovery is up to 99.20%.
Comparative example 1:
Will be with nickel fibers slag of the present invention without water logging or acidleach, and only carry out cyclone electrolytic cell after a wherein step leaches, then
For resulting negative electrode copper products for nickel fibers slag, copper, the rate of recovery of nickel are below 90%.
Comparative example 2:
Using other ways of recycling such as the extractions different from cyclone electrolytic cell mode of the present invention, copper, nickel in its nickel fibers slag
The rate of recovery be only 83% or so, and extract, the cost of stripping process it is higher.
Comparative example 3:
If the auxiliary agent for being added without the present invention is mixed, two step leaching effects will be reduced substantially, final so as to cause
For cyclone electrolytic cell negative electrode copper products for nickel fibers slag, copper, the rate of recovery of nickel are 88% or so.
It can be seen from embodiment 1-3 and comparative example 1-3 reduction roasting of the present invention, again water logging, reoxidize acid
Leaching, the mode of cyclone electrolytic cell is finally segmented, its step and technological parameter are that applicant verifies by repeated tests.
Auxiliary agent has been specifically added during roasting, make metallurgical slag reaction fully, good fluidity, beneficial to sedimentation separation.First water logging reoxidizes acid
Soak, segmentation cyclone electrolytic cell is carried out again after mixing water lixivium and oxidation acid leaching leachate, have to the rate of recovery for improving metal cupro-nickel
It is certain to help.The present invention is lower than traditional nickel fibers slag recovery process production cost, and compares conventional cyclone electrolytic cell mode, this hair
The bright rate of recovery is higher.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that:Not
In the case of departing from the principle and objective of the present invention a variety of change, modification, replacement and modification can be carried out to these embodiments, this
The scope of invention is limited by claim and its equivalent.
Claims (6)
1. the recovery method of valuable metal in nickel fibers slag, it is characterised in that including:
(1) nickel fibers slag, auxiliary agent and quick lime are mixed, obtains mixed material;
(2) mixed material is calcined, the solid mixture after being calcined;
(3) solid mixture is subjected to crushing grinding, hot water pulp, it is 3~5 that water to liquid-solid ratio is reheated after stirring:1,
It is stirred for, is filtrated to get filtrate and filter residue;
(4) after filter residue being added into sulfuric acid, oxygen progress Oxidation Leaching is led in autoclave, leaching 2~4 hours, is carried out afterwards
Separating treatment, obtain leachate and leached mud;
(5) filtrate and the leachate are mixed 1~2 hour, adjusts pH value afterwards to 4~5, carry out two sections of eddy flows
Electrolysis;Current density is 50~80A/m when first stage is electrolysed2, electrolyte circular flow is 30L/h, and temperature is 40~50 DEG C,
It is 200mg/L to control terminal copper ion concentration, and negative electrode copper products are obtained using cyclone electrolytic cell;Electrolyte after decopper(ing) continues
Second stage cyclone electrolytic cell, current density are 30~50A/m2, electrolyte circular flow is 20L/h, and temperature is 40~50 DEG C,
Terminal copper ion concentration obtains nickeliferous more than 98% cathode nickel product in 300mg/L, using eddy flow electrodeposition.
2. the recovery method of valuable metal in nickel fibers slag according to claim 1, it is characterised in that:The auxiliary agent by with
The component of lower percentage by weight is made:Lime stone 12~15%, iron ore 10~13%, alumina silicate 8~10%, carborundum 5~
8%th, flyash 3~5%, surplus are coke.
3. according to the method for claim 1, it is characterised in that:In the step (1), nickel fibers slag, auxiliary agent and raw stone
Ash is 1 according to mass ratio:(2~2.5):(5~6.5) are mixed.
4. according to the method for claim 4, it is characterised in that:In the step (2), the temperature of the calcination process is
1000~1200 DEG C;Before the mixed material is carried out into calcination process, forming processes are carried out to the mixed material in advance,
Obtain mixing pelletizing.
5. the described method according to Claims 1-4, it is characterised in that:In the step (3), the crushing grinding
Powder of the particle diameter less than 0.056mm accounts for more than the 75wt% of total amount in powder afterwards.
6. the method according to claim 1 to 5, it is characterised in that:In the step (3), starched with 80~95 DEG C of hot water
Change, the volume of hot water and the mass ratio 1 of solid mixture:1, after stirring 0.5~1.0 hour, then add 80~95 DEG C of hot water to liquid
Gu than being 3~5:1, it is stirred for 0.5~1.0 hour, is filtrated to get filtrate and filter residue.
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Cited By (6)
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CN110863216A (en) * | 2019-10-28 | 2020-03-06 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
CN112458293A (en) * | 2020-11-17 | 2021-03-09 | 湖南仁发材料科技有限公司 | Method for recovering valuable metals in chlorine leaching displacement tail liquid |
CN113528826A (en) * | 2021-06-25 | 2021-10-22 | 广东邦普循环科技有限公司 | Method for recovering metal in laterite-nickel ore slag |
CN114150157A (en) * | 2021-12-01 | 2022-03-08 | 中冶建筑研究总院有限公司 | Method for diluting copper slag |
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109022824A (en) * | 2018-07-13 | 2018-12-18 | 金川集团股份有限公司 | A method of nickel fibers clinker is handled using silicon carbide |
CN110863216A (en) * | 2019-10-28 | 2020-03-06 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
CN110863216B (en) * | 2019-10-28 | 2020-12-11 | 中南大学 | Method for preparing high-purity indium through step cyclone electrodeposition |
CN112458293A (en) * | 2020-11-17 | 2021-03-09 | 湖南仁发材料科技有限公司 | Method for recovering valuable metals in chlorine leaching displacement tail liquid |
CN113528826A (en) * | 2021-06-25 | 2021-10-22 | 广东邦普循环科技有限公司 | Method for recovering metal in laterite-nickel ore slag |
WO2022267426A1 (en) * | 2021-06-25 | 2022-12-29 | 广东邦普循环科技有限公司 | Method for recovering metal from laterite-nickel ore slag |
WO2023000845A1 (en) * | 2021-07-21 | 2023-01-26 | 广东邦普循环科技有限公司 | Method for extracting valuable metal from low-matte nickel converter slag |
GB2619853A (en) * | 2021-07-21 | 2023-12-20 | Guangdong Brunp Recycling Technology Co Ltd | Method for extracting valuable metal from low-matte nickel converter slag |
US12018346B2 (en) | 2021-07-21 | 2024-06-25 | Guangdong Brunp Recycling Technology Co., Ltd. | Method for extracting valuable metal from low-matte nickel converter slag |
CN114150157A (en) * | 2021-12-01 | 2022-03-08 | 中冶建筑研究总院有限公司 | Method for diluting copper slag |
CN114150157B (en) * | 2021-12-01 | 2023-10-27 | 中冶建筑研究总院有限公司 | Copper slag depletion method |
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