CN115094238B - Device and method for recycling rare earth elements from zinc sulfide-based fluorescent powder - Google Patents

Device and method for recycling rare earth elements from zinc sulfide-based fluorescent powder Download PDF

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CN115094238B
CN115094238B CN202210501672.5A CN202210501672A CN115094238B CN 115094238 B CN115094238 B CN 115094238B CN 202210501672 A CN202210501672 A CN 202210501672A CN 115094238 B CN115094238 B CN 115094238B
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leaching
unit
liquid
rare earth
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CN115094238A (en
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李栋
李雅彬
乔晋玺
郭学益
田庆华
许志鹏
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Central South University
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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
    • 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
    • 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
    • C22B3/08Sulfuric acid, other sulfurated 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00Obtaining rare earth metals
    • 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

Abstract

A device for recovering rare earth elements from zinc sulfide-based fluorescent powder comprises a leaching unit, an adjusting unit and a purifying unit; the liquid outlet of the leaching unit is communicated with the liquid inlet of the adjusting unit, the air outlet of the leaching unit is communicated with the air inlet of the purifying unit, and the liquid outlet of the adjusting unit is communicated with the liquid inlet of the purifying unit. A method for recovering rare earth elements from zinc sulfide-based fluorescent powder: adding zinc sulfide-based fluorescent powder and water and concentrated sulfuric acid into a leaching unit for reaction to obtain a product containing H 2 S, gas and leaching liquid; the leaching solution is introduced into an adjusting unit, and the pH value of the end point of the solution is adjusted to be 1-2.5; then the slurry is led into a purifying treatment unit and is led into an H-containing unit at the same time 2 S, obtaining rare earth element enrichment liquid. The invention effectively utilizes H generated in the leaching stage 2 S gas not only can reduce the treatment cost of harmful gas in the leaching process, but also can reduce the subsequent separation and extraction difficulty of rare earth, and improve the purity of rare earth products, so that the whole process is more environment-friendly.

Description

Device and method for recycling rare earth elements from zinc sulfide-based fluorescent powder
Technical Field
The invention belongs to the field of waste resource treatment, and particularly relates to a device and a method for recycling rare earth elements from zinc sulfide-based fluorescent powder.
Background
Rare earth elements are 17 transition elements including lanthanoid elements, yttrium and scandium, and are called "industrial monosodium glutamate" due to their unique properties. The rare earth is a large country of rare earth resources, accounting for 38% of the world, the rare earth mined in China almost accounts for 80-90% of the world yield in the last 20 years, and the rare earth is an export large country of rare earth raw ores, and a series of policies are issued along with the increasing recognition of important roles of rare earth elements by the countries, so that the rare earth is classified as strategic metal, the rare earth industry is standardized, and illegal mining and buying and selling of rare earth mineral products are hit. Rare earth is taken as non-renewable resource, mineral exploitation is strictly controlled by the country, the market is stabilized, reasonable pricing is realized, meanwhile, resource circulation is encouraged, and secondary resource recovery rare earth such as waste rare earth-containing products, associated ores, production waste residues and the like is greatly developed.
The zinc sulfide-based phosphor is a waste CRT (cathode ray tube) phosphor, which is a rare earth secondary resource containing yttrium and europium. The method for recovering rare earth from waste CRT fluorescent powder is mainly divided into wet method and pyrogenic-wet method. For example, the Luciene and the like adopt sulfuric acid as leaching agent, and are directly mixed with CRT fluorescent powder, the leaching rate of yttrium and europium can reach 98 percent and 96 percent, but a large amount of H can be generated in the leaching process 2 S gas generation requires further treatment of the exhaust gas. The patent application with publication number of CN108517426A discloses a method for efficiently separating and recycling rare earth in waste CRT fluorescent powder under mild conditions, wherein the waste CRT fluorescent powder is mechanically activated by ball milling, then mixed with dilute sulfuric acid and hydrogen peroxide, and subjected to pressurized catalytic oxidation liquid phase leaching reaction in a polymerization reaction kettle to obtain leaching solution containing yttrium and europium, wherein the leaching rates of yttrium and europium can reach more than 99 percent. The patent application with publication number of CN105039698A discloses a method for efficiently recycling rare earth in waste CRT fluorescent powder, which comprises the steps of pre-treating the waste fluorescent powder by adopting dilute hydrochloric acid, reducing non-rare earth impurities in a leaching stage, reducing the acid consumption in the leaching stage, dissolving and leaching by adopting high-concentration hydrochloric acid, recycling rare earth by combining hydroxide precipitation and oxalic acid precipitation, and finally recycling the rare earth to more than 90%. The patent application with publication number of CN110512099A discloses a method for recycling rare earth in waste CRT fluorescent powder, which comprises mixing the fluorescent powder after impurity removal with strong alkali and oxidant uniformly, heating for reaction, adding water for washing until the pH value of the system is 7-8 after the reaction is finished, adding hydrochloric acid for dissolution, adding glacial acetic acid, maintaining the pH value of the system at 3.5-4,and then filtering to obtain the leaching solution containing rare earth. The waste CRT fluorescent powder and zinc sulfate are mixed by Mehmet Ali et al, and calcined for 30min at 750 ℃, zinc sulfide in the fluorescent powder generates zinc oxide which is insoluble in water, and leaching residues are leached by water to obtain leaching liquid containing yttrium and europium, wherein the leaching rate of yttrium is about 93.4%, and the leaching rate of europium is about 94.9%.
In summary, the current method for recovering rare earth from zinc sulfide-based fluorescent powder mainly comprises wet acid leaching, high-pressure leaching and leaching after fire calcination treatment. The existing method for recovering rare earth from zinc sulfide-based fluorescent powder can achieve better rare earth leaching effect, but still has some unresolved problems, mainly comprising the following steps:
(1) The acid leaching method uses sulfuric acid as a leaching agent, which can lead to the reaction of zinc sulfide in the raw materials with sulfuric acid to generate a large amount of H 2 S harmful gas not only has huge poisoning risk, but also belongs to inflammable gas, and has great potential safety hazard. Hydrochloric acid is used as a leaching agent, high and low concentrations are needed to be used alternately, so that the overall process cost is increased, and the hydrochloric acid is relatively high in corrosion to equipment.
(2) Although the high-pressure leaching process can obtain a better rare earth recovery efficiency, special equipment is needed in the process, a certain potential safety hazard exists, the reaction temperature is high, the energy consumption is high, and the behavior of other impurities in the raw materials is not considered under special conditions.
(3) Leaching after the fire calcination treatment, although better solving the problem of H 2 S gas is generated, but the whole process flow of the process is longer, the equipment investment cost is high, the process treatment condition is more severe, and the energy consumption is higher.
(4) The existing technology does not consider the problems of impurity behavior and open circuit, the content of zinc sulfide in the zinc sulfide-based fluorescent powder exceeds 40%, the zinc sulfide can not enter the solution in the leaching process, and the purity of the product can be greatly influenced in the extraction and selective precipitation processes.
Therefore, a process for recycling waste zinc sulfide-based fluorescent powder is needed to be easier to reach and more efficient, so that recycling of rare earth can be completed at normal temperature and normal pressure, and meanwhile, influence of mixed zinc on a subsequent process can be effectively avoided, and a rare earth product with higher purity is obtained.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing a device and a method for recycling rare earth elements from zinc sulfide-based fluorescent powder.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a device for recovering rare earth elements from zinc sulfide-based fluorescent powder comprises a leaching unit, an adjusting unit and a purifying unit;
the liquid outlet of the leaching unit is communicated with the liquid inlet of the adjusting unit, the air outlet of the leaching unit is communicated with the air inlet of the purifying unit, and the liquid outlet of the adjusting unit is communicated with the liquid inlet of the purifying unit. The leaching unit is used for acid leaching of the zinc sulfide-based fluorescent powder and simultaneously generates H required subsequently 2 S gas; the adjusting unit is used for solid-liquid separation and pH adjustment of the leaching liquid; the purification unit is used for removing impurity zinc in the solution.
In the above apparatus, preferably, the leaching unit includes a leaching container and an air pump, the air pump is communicated with an air inlet of the leaching container, and an air outlet of the leaching container is communicated with an air inlet of the purifying unit. The air pump is used for pumping air into the leaching container to drive H generated by the reaction 2 S gas enters the purifying unit.
The device is preferable, the adjusting unit comprises a plate-and-frame filter press and a liquid storage container which are sequentially connected, a pH adjusting system is arranged in the liquid storage container, the pH adjusting system is inserted into the liquid storage container, a pH probe is positioned below the liquid level of the liquid storage container, a liquid inlet of the plate-and-frame filter press is communicated with a liquid outlet of the leaching container, and the liquid outlet of the liquid storage container is communicated with a liquid inlet of the purifying unit through a liquid material conveying pump. The pH adjusting system can realize automatic adjustment of the pH value of the liquid in the liquid storage container, and after the operation interface inputs a preset value, the system adjusts the pH value according to the measured value until the whole pH value of the solution reaches a preset value. And the liquid material conveying pump conveys the solution in the liquid storage container to the purifying unit after the pH value of the solution is regulated.
The above device, preferably, the air outlet of the leaching container is communicated with the air inlet of the purifying unit through an air pipe, the air pipe comprises an air main pipe and a plurality of air branch pipes connected at the tail end of the air main pipe, the air branch pipes are led into the bottom of the purifying unit, the tail end outlets of the air branch pipe bodies are blocked, a plurality of air outlet holes are formed in the side surfaces (upper parts) of the air branch pipes, so that the led air is uniformly dispersed to be in contact with the solution, and the reaction contact area is increased.
In the above apparatus, preferably, the purifying unit includes a purifying reaction container and a tail gas absorbing tower, and the purifying reaction container is communicated with the tail gas absorbing tower through a vent pipe. And a stirring device is arranged in the leaching reaction container and used for reinforcing the leaching reaction process, and a low-alkaline solution is stored in the absorption tower. The redundant gas can be discharged after being treated by a subsequent tail gas absorption tower.
In the above apparatus, preferably, a grid plate is disposed in the purifying reaction container. The mesh plate further divides bubbles entering the solution to form small bubbles, and increases contact with the liquid to strengthen the reaction.
Further, the number of the grid plates is 2, and the grid plates are respectively arranged at one fourth and one half of the height of the purifying reaction container; support buckles are arranged at one fourth and one half of the purification reaction container, notches corresponding to the support buckles are arranged on the grid plates, and the purification reaction container can be installed through rotating grid staggered notches; the central opening of the grid plate can be used for the ventilation main pipe to pass through.
The specific flow of the invention is as follows: leaching by a leaching unit to obtain slurry containing rare earth, feeding the slurry into an adjusting unit, and generating H simultaneously 2 S gas enters a purification unit; filtering the slurry entering the regulating unit to obtain a leaching solution containing rare earth, regulating pH of the leaching solution, entering the purifying unit, and introducing H 2 S gas reacts to remove zinc, and finally the obtained zinc-removed liquid is the enriched liquid containing yttrium and europium, and the enriched liquid containing yttrium and europium can be precipitated and calcined to obtain rare earth oxide products.
As a general inventive concept, the present invention also provides a method for recovering rare earth elements from zinc sulfide-based phosphor using the above-described apparatus, comprising the steps of:
(1) Adding zinc sulfide-based fluorescent powder and water into a leaching unit for mixing, and then adding concentrated sulfuric acid into the leaching unit to obtain a product containing H 2 S, gas and leaching liquid;
(2) Introducing the leaching solution into a regulating unit, regulating the pH value to 1-2.5, and stirring;
(3) Introducing the slurry processed in the step (2) into a purification treatment unit, and simultaneously introducing the H-containing material obtained in the next batch of material step (1) 2 S, obtaining rare earth element enrichment liquid.
In the leaching process, zinc sulfide-based fluorescent powder reacts with sulfuric acid, and the following reaction mainly occurs in a reaction vessel:
ZnS+H 2 SO 4 =ZnSO 4 +H 2 S↑ (1);
Y 2 O 2 S+3H 2 SO 4 =Y 2 (SO 4 ) 3 +H 2 S↑+2H 2 O (2)。
it is worth to say that the gas generated by the Nth batch processed in the leaching unit is led into the purifying unit to post-treat the leaching liquid generated by the N-1 th batch.
The following reactions mainly occur in the reaction vessel during the purification process:
Zn 2+ +H 2 S=ZnS↓+2H +
in the above method, preferably, in the step (1), the weight ratio of water to zinc sulfide-based fluorescent powder is 5-10:1; the adding amount of the concentrated sulfuric acid is controlled to be 1-2.5 mol/L by controlling the concentration of the sulfuric acid in the leaching unit.
In the above method, preferably, in the step (1), the rotation speed of the stirring paddle in the leaching unit is controlled to be 100-200 r/min, and the air flow rate of the air pump is controlled to be 100-400 mL/min.
In the above method, preferably, in the step (2), the rotation speed of the stirring paddle in the adjusting unit is adjusted to be 200-300 r/min.
Compared with the prior art, the invention has the advantages that:
(1) According to the device for recovering rare earth elements from zinc sulfide-based fluorescent powder, from the aspects of device design and enhanced reaction, a leaching unit, an adjusting unit and a purifying unit are designed and are connected with each other, leaching liquid generated in the leaching unit enters the adjusting unit, and waste gas enters the purifying unit; the leachate is pumped into the purification unit after passing through the regulation unit and then is subjected to waste reaction with the wastewater entering the purification unit, so that the effect of purifying and removing impurities is achieved, and harmless utilization of harmful gas in the treatment process is realized.
(2) The device of the invention can effectively utilize H generated in the leaching stage 2 S harmful gas is used for removing a large amount of zinc ions in the leaching solution, and is changed into beneficial effect, so that the treatment cost of the harmful gas in the leaching process can be reduced, the subsequent separation and extraction difficulty of rare earth can be reduced, the purity of the rare earth product is improved, and the whole process is more environment-friendly.
(3) The invention adopts the full wet process, realizes the efficient and selective recovery of rare earth in zinc sulfide-based fluorescent powder at low temperature and normal pressure, can greatly reduce the requirements of equipment and operation under the condition, can reasonably utilize sulfur in raw materials, and realizes the circulation of sulfur in the whole process.
(4) The method for recovering rare earth elements from zinc sulfide-based fluorescent powder has the advantages that the leaching rates of yttrium and europium can reach more than 99%, the zinc removal rate is close to 100%, yttrium and europium can be easily separated by an extraction separation method in the later stage to obtain pure rare earth solution, and the rare earth oxide product can be obtained through precipitation and calcination processes, so that the whole process condition is low in difficulty and production cost, and great industrialization significance is realized.
Drawings
FIG. 1 is a schematic diagram of a recovery apparatus for recovering rare earth from zinc sulfide-based phosphor according to the present invention.
Fig. 2 is a schematic view of a vent manifold of the present invention.
FIG. 3 is a plan view of the purification reaction vessel of the present invention
Fig. 4 is a schematic view of the structure of the mesh plate of the present invention.
Legend description:
1. an air pump; 2. a leaching container; 3. a stirrer; 4. a plate and frame filter press; 5. a pH regulator; 6. a liquid transfer pump; 7. a vent pipe; 8. a grid plate; 9. a tail gas absorption tower; 10. purifying the reaction vessel; 11. a liquid storage container; 12. a ventilation main pipe; 13. a ventilation manifold; 14. an air outlet hole; 15. a support buckle; 16. and a grid plate notch.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
The various reagents and materials used in the present invention are commercially available or may be prepared by known methods unless otherwise specified.
Examples:
an apparatus for recovering rare earth elements from zinc sulfide-based phosphor, as shown in fig. 1, comprises a leaching unit, a regulating unit and a purifying unit; the leaching unit comprises a leaching container 2 and an air pump 1, wherein the air pump 1 is communicated with an air inlet of the leaching container 2, and a stirrer 3 is arranged in the leaching container 2 and used for reinforcing the leaching reaction process; the purification unit comprises a purification reaction container 10 and a tail gas absorption tower 9, wherein the purification reaction container 10 is communicated with the tail gas absorption tower 9 through a gas pipe, and the tail gas absorption tower 9 is internally provided with low alkali solution; the gas outlet of the leaching container 2 is communicated with the gas inlet of the purifying reaction container 10 in the purifying unit through a breather pipe 7, the breather pipe 7 comprises a breather main pipe 12 and a plurality of breather branch pipes 13 connected at the tail end of the breather main pipe, the breather branch pipes 13 are arranged at the bottom of the purifying unit, the tail end outlets of the pipe bodies of the breather branch pipes 13 are blocked, a plurality of gas outlet holes 14 are arranged on the breather branch pipes 13, as shown in fig. 2, the introduced gas is uniformly dispersed to be contacted with the solution, and the reaction contact area is increased. The inside of the purification reaction vessel 10 is provided with a mesh plate 8 to divide bubbles entering the solution into small bubbles, thereby increasing contact with the liquid and strengthening the reaction. The number of the grid plates 8 is 2, the grid plates are respectively positioned at one quarter and one half of the height of the purification reaction container 10, the purification reaction container 10 is provided with supporting buckles 15 at one quarter and one half, as shown in fig. 3, grid plate notches 16 corresponding to the supporting buckles 15 are arranged on the grid plates 8, and as shown in fig. 4, the grid plates can be placed at one quarter through the positions of one half of the rotating grid staggered notches; the central opening of the grid plate 8 is provided for the ventilation main pipe 12 to pass through. The regulating unit comprises a pH regulator 5 and a plate-and-frame filter press 4 and a liquid storage container 11 which are sequentially connected, wherein the pH regulator 5 is inserted into the liquid storage container 11, a stirring device is arranged in the liquid storage container 11, a liquid inlet of the plate-and-frame filter press 4 is communicated with a liquid outlet of the leaching container 2, and the liquid outlet of the liquid storage container 11 is communicated with a liquid inlet of the purifying reaction container 10 through a liquid conveying pump 6 and a pipeline.
The device for recycling rare earth elements from zinc sulfide-based fluorescent powder in the embodiment is used for recycling rare earth elements from zinc sulfide-based fluorescent powder (the main components are that Y is 18.12%, zn is 29.25%, eu is 1.34%, A is 2.13%), and the specific method comprises the following steps:
(1) Screening waste CRT fluorescence by using an 80-target Taylor sieve to remove glass slag, large aluminum foils and other impurities, placing the screened material into a leaching container 2 of a leaching unit, adding water according to the mass ratio of the material to water of 1:8, and adding a certain amount of concentrated sulfuric acid to ensure that the concentration of the sulfuric acid in the leaching container 2 is integrally maintained at 1.5mol/L. The stirrer in the leaching container 2 is controlled to stir at 150r/min, and the air flow rate of the air flowing into the leaching container 2 is regulated to be 200mL/min by the air pump 1, so that the reaction lasts for 1.5h.
(2) The leached slurry obtained in the step (1) is pressed and filtered by a plate-and-frame filter press 4 and enters a liquid storage container 11, the end pH value of the reaction solution is regulated to be 2 under the condition of the stirring speed of 250r/min, the regulated slurry is pumped into a purification reaction container 10 by a liquid delivery pump 6, and H generated by leaching the materials in the next leaching container 2 is leached 2 S gas is simultaneously introduced into the purification reaction vessel 10 to remove impurity zinc in the solution, and the concentration of the impurity zinc in the obtained rare earth element enrichment solution is only 0.002g/L. The results show thatThe leaching rate of yttrium in the zinc sulfide-based fluorescent powder is 99.34 percent, the leaching rate of europium is 99.12 percent, and the removal rate of zinc in a purification system is 99.87 percent.

Claims (8)

1. The device for recovering the rare earth elements from the zinc sulfide-based fluorescent powder is characterized by comprising a leaching unit, an adjusting unit and a purifying unit;
the liquid outlet of the leaching unit is communicated with the liquid inlet of the adjusting unit, the gas outlet of the leaching unit is communicated with the gas inlet of the purifying unit, and the liquid outlet of the adjusting unit is communicated with the liquid inlet of the purifying unit;
the leaching unit comprises a leaching container and an air pump, wherein the air pump is communicated with an air inlet of the leaching container, and an air outlet of the leaching container is communicated with an air inlet of the purifying unit;
the adjusting unit comprises a plate-and-frame filter press and a liquid storage container which are sequentially connected, a pH adjusting system is arranged in the liquid storage container, a liquid inlet of the plate-and-frame filter press is communicated with a liquid outlet of the leaching container, and the liquid outlet of the liquid storage container is communicated with a liquid inlet of the purifying unit; and (3) introducing gas generated by the N batch of materials treated in the leaching unit into a purifying unit to post-treat leaching liquid generated by the N-1 batch of materials.
2. The apparatus of claim 1, wherein the leaching vessel exhaust port is in communication with the purification unit air inlet through a vent pipe, the vent pipe comprises a vent main pipe and a plurality of vent branches connected at the tail end of the vent main pipe, the vent branches are arranged at the bottom of the purification unit, the tail end outlet of the vent branch pipe body is blocked, and a plurality of air outlet holes are arranged at the side surface of the vent branch pipe.
3. The apparatus of claim 1, wherein the purification unit comprises a purification reaction vessel and a tail gas absorption tower, and the purification reaction vessel and the tail gas absorption tower are communicated through a vent pipe.
4. A device according to claim 3, wherein a mesh plate is provided in the purification reaction vessel.
5. A method for recovering rare earth elements from zinc sulfide-based phosphor using the apparatus of any one of claims 1 to 4, comprising the steps of:
(1) Adding zinc sulfide-based fluorescent powder and water into a leaching unit for mixing, and then adding concentrated sulfuric acid into the leaching unit for reaction to obtain the product containing H 2 S, gas and leaching liquid;
(2) Introducing the leaching solution into a regulating unit, filtering, and regulating the pH value of the solution at the reaction end point to be 1-2.5 under the stirring condition;
(3) Introducing the slurry treated in the step (2) into a purification treatment unit, and simultaneously introducing the H-containing slurry obtained in the step (1) 2 S, obtaining rare earth element enrichment liquid.
6. The method of claim 5, wherein in step (1), the weight ratio of water to zinc sulfide-based phosphor is 5-10:1; the adding amount of the concentrated sulfuric acid is controlled to be 1-2.5 mol/L by controlling the concentration of the sulfuric acid in the leaching unit.
7. The method according to claim 5, wherein in the step (1), the stirring speed in the leaching unit is controlled to be 100-200 r/min, the reaction time is 0.5-2 h, and the air pump gas flow rate is 100-400 mL/min.
8. The method according to claim 5, wherein in the step (2), the rotation speed of stirring in the adjusting unit is controlled to 150 to 300r/min.
CN202210501672.5A 2022-05-09 2022-05-09 Device and method for recycling rare earth elements from zinc sulfide-based fluorescent powder Active CN115094238B (en)

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