CN115094238A - Device and method for recovering rare earth elements from zinc sulfide-based fluorescent powder - Google Patents
Device and method for recovering rare earth elements from zinc sulfide-based fluorescent powder Download PDFInfo
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- CN115094238A CN115094238A CN202210501672.5A CN202210501672A CN115094238A CN 115094238 A CN115094238 A CN 115094238A CN 202210501672 A CN202210501672 A CN 202210501672A CN 115094238 A CN115094238 A CN 115094238A
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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
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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
- 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
- C22B3/06—Extraction 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
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical 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
- C22B59/00—Obtaining rare earth metals
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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
Abstract
A device for recovering rare earth elements from zinc sulfide-based fluorescent powder comprises a leaching unit, a regulating 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 comprises the following steps: adding zinc sulfide-based fluorescent powder, water and concentrated sulfuric acid into a leaching unit for reaction to obtain H-containing 2 S gas and leachate; introducing the leachate into an adjusting unit, and adjusting the end point pH of the solution to 1-2.5; then the slurry is introduced into a purification treatment unit, and simultaneously H is introduced 2 Gas of S to obtain diluteAnd (4) enriching the soil element. The invention effectively utilizes H generated in the leaching stage 2 S gas can reduce the cost for treating harmful gas in the leaching process, reduce the difficulty of subsequent rare earth separation and extraction, improve the purity of rare earth products and ensure that the whole process is more environment-friendly.
Description
Technical Field
The invention belongs to the field of waste resource treatment, and particularly relates to a device and a method for recovering rare earth elements from zinc sulfide-based fluorescent powder.
Background
Rare earth elements are 17 transition elements including lanthanides and yttrium and scandium, and are called as 'industrial monosodium glutamate' due to their unique properties. China is a large resource country of rare earth, accounts for 38 percent of the world, and the rare earth mined in China almost accounts for 80-90 percent of the world output in nearly 20 years, thus becoming a large export country of rare earth raw ore. Rare earth is used as non-renewable resource, the country strictly controls mineral exploitation, stabilizes the market, reasonably prices, encourages resource circulation, and vigorously develops secondary resources to recover rare earth, such as waste rare earth-containing products, associated minerals, production waste residues and the like.
The zinc sulfide-based fluorescent powder is waste CRT (cathode ray tube) fluorescent powder, and 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 fire-wet method. For example, Luciene and the like adopt sulfuric acid as a 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 exists in the leaching process 2 S gas is generated, requiring further treatment of the exhaust. Patent application publication No. CN108517426A discloses a method for efficiently separating and recovering rare earth from waste CRT fluorescent powder under mild conditions, which comprises the steps of performing ball-milling mechanical activation on the waste CRT fluorescent powder, mixing the activated waste CRT fluorescent powder with dilute sulfuric acid and hydrogen peroxide, and performing pressure catalytic oxidation liquid-phase leaching reaction in a polymerization reaction kettle to obtain leaching solution containing yttrium and europium, wherein the leaching rates of the yttrium and the europium can reach more than 99%. Publication number CN105039698A discloses a method for efficiently recovering rare earth from waste CRT fluorescent powder, which comprises the steps of pretreating the waste fluorescent powder with dilute hydrochloric acid to reduce non-rare earth impurities in the leaching stage and reduce the acid consumption in the leaching stage, dissolving and leaching with high-concentration hydrochloric acid, and recovering rare earth by combining hydroxide precipitation and oxalic acid precipitation, wherein the recovery rate of the rare earth can reach more than 90%. The patent application with publication number CN110512099A discloses a method for recycling rare earth in waste CRT fluorescent powder, which comprises the steps of uniformly mixing the fluorescent powder after impurity removal with strong base and an oxidant, carrying out heating reaction, adding water for washing until the pH value of the system is 7-8, adding hydrochloric acid for dissolving, adding glacial acetic acid, maintaining the pH value of the system to be 3.5-4, and then filtering to obtain a leaching solution containing rare earth. Mehmet Ali et al mixed waste CRT phosphor with zinc sulfate, calcined at 750 deg.C for 30min to form water insoluble zinc oxide from zinc sulfide in the phosphor, and water leaching the calcined slag to obtain leaching solution containing yttrium and europium, with yttrium leaching rate of about 93.4% and europium leaching rate of about 94.9%.
In summary, the current methods for recovering rare earth from zinc sulfide-based phosphor powder mainly include wet acid leaching, high pressure leaching and leaching after pyrogenic calcination treatment. Although the existing method for recovering rare earth from zinc sulfide-based fluorescent powder can achieve better rare earth leaching effect, some unsolved problems still exist, mainly comprising the following steps:
(1) the acid leaching method uses sulfuric acid as a leaching agent, and can cause zinc sulfide in raw materials to react with the 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 required to be alternately used, so that the overall process cost is increased, and the hydrochloric acid has high corrosion to equipment.
(2) Although the high-pressure leaching process can obtain better rare earth recovery efficiency, special equipment is needed in the process, certain potential safety hazards exist, the reaction temperature is high, the energy consumption is high, and meanwhile, the behavior of other impurities in the raw materials is not considered under special conditions.
(3) Leaching after pyrogenic calcination treatmentAlthough better solving H 2 S gas has a problem, but the whole process is long, the equipment investment cost is high, the process treatment conditions are harsh, and the energy consumption is high.
(4) The existing process does not consider the problems of impurity behaviors and open circuit, the content of zinc sulfide in the zinc sulfide-based fluorescent powder exceeds 40 percent, the zinc sulfide can inevitably enter a solution in the leaching process, and the product purity can be greatly influenced in the extraction and selective precipitation processes.
Therefore, a more efficient waste zinc sulfide-based phosphor powder recovery process with more accessible conditions is urgently needed to complete the recycling of rare earth at normal temperature and normal pressure, and meanwhile, the influence of zinc impurities on the subsequent process can be effectively avoided, and rare earth products with higher purity can be obtained.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a device and a method for recovering 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, a regulating unit and a purifying unit;
leach the leakage fluid dram of unit and the inlet intercommunication of regulating unit, leach the gas vent of unit and purify the air inlet intercommunication of unit, the leakage fluid dram of regulating unit and the inlet intercommunication of purifying the unit. The leaching unit is used for acid leaching of the zinc sulfide-based fluorescent powder and simultaneously generating subsequent required H 2 S gas; the adjusting unit is used for solid-liquid separation and pH adjustment of the leachate; 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 the air inlet of the leaching container, and the air outlet of the leaching container is communicated with the air inlet of the purifying unit. The air pump is used for blowing air into the leaching container to drive H generated by the reaction 2 The S gas enters a purification unit.
Preferably, the adjusting unit comprises a plate-and-frame filter press and a liquid storage container which are connected in sequence, 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 conveying pump. The pH adjusting system can realize automatic adjustment of the pH of the liquid in the liquid storage container, and after a preset value is input on an operation interface, the system performs acid-base adjustment according to the measured value until the integral 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 purification unit after the pH adjustment of the solution is completed.
In the above device, preferably, the exhaust port of the leaching container is communicated with the air inlet of the purification unit through a vent pipe, the vent pipe comprises a main vent pipe and a plurality of branch vent pipes connected to the tail end of the main vent pipe, the branch vent pipes are communicated with the bottom of the purification unit, the outlet at the tail end of the branch vent pipe is blocked, and a plurality of exhaust holes are formed in the side surface (upper part) of each branch vent pipe, so that introduced gas is uniformly dispersed and contacts with a solution, and the reaction contact area is increased.
In the above apparatus, preferably, the purification unit includes a purification reaction vessel and a tail gas absorption tower, and the purification reaction vessel is communicated with the tail gas absorption 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-alkalinity 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 provided in the purification reaction vessel. The grid plate further divides bubbles entering the solution to form small bubbles, so that the contact between the small bubbles and the liquid is increased, and the reaction is enhanced.
Furthermore, the number of the grid plates is 2, and the grid plates are respectively arranged at one quarter and one half of the height of the purification reaction container; supporting buckles are installed at one fourth and one half of the purification reaction container, gaps corresponding to the supporting buckles are formed in the grid plate, and the purification reaction container can be installed through rotating the grid to stagger the gaps; the central opening of the grid plate can be penetrated by the main ventilation pipe.
The specific process of the invention is as follows: the leaching unit leaches to obtain slurry containing rare earth, the slurry enters the regulating unit, and H is generated at the same time 2 S gas enters a purification unit; filtering the slurry entering the adjusting unit to obtain a leaching solution containing rare earth, adjusting the pH of the leaching solution, then entering the purifying unit, and introducing H 2 And (3) removing zinc by the reaction of S gas, and obtaining a zinc-removed liquid which is the enriched liquid containing yttrium and europium, wherein the enriched liquid containing yttrium and europium can be precipitated and calcined to obtain a rare earth oxide product.
As a general inventive concept, the present invention also provides a method for recovering rare earth elements from zinc sulfide-based phosphors 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 H-containing fluorescent powder 2 S gas and leachate;
(2) introducing the leachate into an adjusting unit, adjusting the pH value to 1-2.5, and stirring;
(3) introducing the slurry treated in the step (2) into a purification treatment unit, and simultaneously introducing the H-containing material obtained in the next batch in the step (1) 2 And S to obtain the rare earth element enrichment liquid.
The zinc sulfide-based fluorescent powder reacts with sulfuric acid in the leaching process, and the following reactions mainly occur in a reaction container:
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 mentioning that the gas generated from the Nth batch of material processed in the leaching unit is introduced into the purification unit to process the leachate generated from the Nth-1 st batch of material.
The following reactions mainly occur in the reaction vessel during the purification process:
Zn 2+ +H 2 S＝ZnS↓+2H + 。
in the method, preferably, in the step (1), the weight ratio of the water to the zinc sulfide-based fluorescent powder is 5-10: 1; the adding amount of concentrated sulfuric acid is controlled to be 1-2.5 mol/L by controlling the concentration of sulfuric acid in the leaching unit.
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 gas flow rate of the air pump is controlled to be 100-400 mL/min.
Preferably, in the step (2), the rotating 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 the rare earth elements from the zinc sulfide-based fluorescent powder, from the aspects of device design and strengthened reaction, a leaching unit, a regulating unit and a purifying unit are designed and are mutually connected, leachate generated in the leaching unit enters the regulating unit, and waste gas enters the purifying unit; leachate is pumped into the purification unit after passing through the regulating unit and then reacts with waste entering the purification unit, so that the effects of purification and impurity removal are 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 beneficial to changing into harmful gas, so that the treatment cost of the harmful gas in the leaching process can be reduced, the subsequent rare earth separation and extraction difficulty can be reduced, the purity of a rare earth product is improved, and the whole process is more green and environment-friendly.
(3) The invention adopts a full wet process, realizes the high-efficiency and selective recovery of rare earth in the zinc sulfide-based fluorescent powder at low temperature and normal pressure, can greatly reduce the requirements of equipment and operation under the condition, simultaneously can reasonably utilize sulfur in the raw material, and realizes the circulation of sulfur in the whole process.
(4) According to the method for recovering the rare earth elements from the zinc sulfide-based fluorescent powder, 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 a pure rare earth solution, and a rare earth oxide product can be obtained by precipitation and calcination processes, so that the method has low overall process condition difficulty and production cost, and has great industrial significance.
Drawings
FIG. 1 is a schematic view of a recovery apparatus for recovering rare earth from zinc sulfide-based phosphor according to the present invention.
Figure 2 is a schematic view of a vent manifold of the present invention.
FIG. 3 is a plan view of a purification reactor vessel according to the present invention
Fig. 4 is a schematic structural view of the mesh plate of the present invention.
Illustration of the drawings:
1. an air pump; 2. a leaching vessel; 3. a stirrer; 4. a plate-and-frame filter press; 5. a pH regulator; 6. a liquid delivery pump; 7. a breather pipe; 8. a grid plate; 9. a tail gas absorption tower; 10. purifying the reaction vessel; 11. a reservoir; 12. a main ventilation pipe; 13. a vent branch; 14. an air outlet; 15. a support buckle; 16. and (5) grid plate notches.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art 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 limit the scope of the present invention.
Unless otherwise specified, the reagents and materials used in the present invention are commercially available products or products obtained by a known method.
Example (b):
a device for recovering rare earth elements from zinc sulfide-based fluorescent powder is shown in figure 1 and comprises a leaching unit, a regulating unit and a purifying unit; the leaching unit comprises a leaching container 2 and an air pump 1, 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 a leaching reaction process; the purification unit comprises a purification reaction container 10 and a tail gas absorption tower 9, the purification reaction container 10 is communicated with the tail gas absorption tower 9 through an air pipe, and a low-alkali solution is filled in the tail gas absorption tower 9; the air outlet of the leaching container 2 is communicated with the air inlet of a purification reaction container 10 in a purification unit through an air pipe 7, the air pipe 7 comprises a main air pipe 12 and a plurality of branch air pipes 13 connected to the tail ends of the main air pipe, the branch air pipes 13 are arranged at the bottom of the purification unit, the tail end outlets of the pipe bodies of the branch air pipes 13 are blocked, and a plurality of air outlet holes 14 are formed in the branch air pipes 13, as shown in fig. 2, so that introduced gas is uniformly dispersed and contacted with a solution, and the reaction contact area is increased. The purification reaction vessel 10 is provided with a grid plate 8 therein to divide bubbles entering the solution to form small bubbles, thereby increasing contact with the liquid and enhancing the reaction. The number of the grid plates 8 is 2, the grid plates are respectively positioned at the quarter and the half of the height of the purification reaction container 10, the support buckles 15 are arranged at the quarter and the half of the height of the purification reaction container 10, as shown in fig. 3, grid plate gaps 16 corresponding to the support buckles 15 are arranged on the grid plates 8, and as shown in fig. 4, the grid plates can be placed at the quarter of the height by rotating the staggered gaps of the grids to penetrate through the half of the height; the central opening of the mesh plate 8 is penetrated by the main aeration pipe 12. The adjusting unit comprises a pH adjusting instrument 5 and a plate-and-frame filter press 4 and a liquid storage container 11 which are sequentially connected, wherein the pH adjusting instrument 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 purification reaction container 10 through a liquid delivery pump 6 and a pipeline.
The method for recovering rare earth from zinc sulfide-based phosphor (main components: Y: 18.12%, Zn: 29.25%, Eu: 1.34%, and A: 2.13%) by using the apparatus for recovering rare earth from zinc sulfide-based phosphor of this embodiment includes the following steps:
(1) screening the waste CRT fluorescence by using an 80-target quasi-Taylor screen to remove other impurities such as glass slag, large aluminum foils and the like, placing undersize materials into a leaching container 2 of a leaching unit, adding water according to the mass ratio of the materials to the water of 1:8, and adding a certain amount of concentrated sulfuric acid to ensure that the concentration of sulfuric acid in the leaching container 2 is kept at 1.5mol/L as a whole. Controlling the stirrer in the leaching container 2 to stir at a speed of 150r/min, adjusting the air flow rate of air introduced into the leaching container 2 to 200mL/min through an air pump 1, and reacting for 1.5 h.
(2) Filter-pressing the leaching slurry obtained in the step (1) by a plate-and-frame filter press 4 into a liquid storage container 11, adjusting the end point pH of the reaction solution to 2 under the condition of a stirring speed of 250r/min, pumping the adjusted slurry into a purification reaction container 10 by a liquid delivery pump 6, and leaching H generated by leaching the materials in the next leaching container 2 2 And simultaneously introducing the S gas into the purification reaction container 10 to remove the impurity zinc in the solution, wherein the concentration of the impurity zinc in the obtained rare earth element enrichment solution is only 0.002 g/L. The result shows that the leaching rate of yttrium in the zinc sulfide-based fluorescent powder is 99.34%, the leaching rate of europium is 99.12%, and the removal rate of zinc in a purification system is 99.87%.
Claims (10)
1. A device for recovering rare earth elements from zinc sulfide-based fluorescent powder is characterized by comprising a leaching unit, a regulating 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.
2. The apparatus of claim 1, wherein the extraction unit comprises an extraction vessel and an air pump, the air pump being in communication with an air inlet of the extraction vessel, an air outlet of the extraction vessel being in communication with an air inlet of the decontamination unit.
3. The device according to claim 2, wherein the adjusting unit comprises a plate-and-frame filter press and a liquid storage container which are connected in sequence, 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 a liquid outlet of the liquid storage container is communicated with a liquid inlet of the purifying unit.
4. The apparatus according to claim 2, wherein the exhaust port of the leaching container is communicated with the air inlet of the purification unit through a vent pipe, the vent pipe comprises a main vent pipe and a plurality of branch vent pipes connected to the tail end of the main vent pipe, the branch vent pipes are arranged at the bottom of the purification unit, the tail end outlets of the pipe bodies of the branch vent pipes are blocked, and the side surfaces of the branch vent pipes are provided with a plurality of air outlet holes.
5. 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 is communicated with the tail gas absorption tower through a vent pipe.
6. The apparatus of claim 5, wherein a grid plate is disposed within the purification reactor vessel.
7. A method for recovering rare earth elements from zinc sulfide-based phosphors using the apparatus of any one of claims 1 to 6, 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 H-containing phosphor powder 2 S gas and leachate;
(2) introducing the leachate into an adjusting unit, filtering, and adjusting the pH value of the reaction end point of the solution to 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 And S to obtain the rare earth element enrichment liquid.
8. The method according to claim 7, wherein in the step (1), the weight ratio of the water to the zinc sulfide-based phosphor is 5-10: 1; the adding amount of concentrated sulfuric acid is controlled to be 1-2.5 mol/L by controlling the concentration of sulfuric acid in the leaching unit.
9. The method according to claim 7, 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 controlled to be 100-400 mL/min.
10. The method according to claim 7, wherein in the step (2), the rotation speed of the stirring in the regulating unit is controlled to be 150-300 r/min.
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