CN107096384B - The method for extracting lithium isotope 6Li using centrifugal extractor - Google Patents
The method for extracting lithium isotope 6Li using centrifugal extractor Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/22—Separation by extracting
- B01D59/24—Separation by extracting by solvent extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/20—Separation by centrifuging
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Abstract
The invention discloses a kind of application centrifugal extractors to extract lithium isotope6The method of Li, including extraction section, alkali wash section and back extraction section.Lithium isotope extract equipment provided by the invention is a kind of new and effective centrifugal extraction equipment, after the technology of solvent extraction extraction lithium isotope is in conjunction with equipment of the present invention, greatly improve stage efficiency and separating effect, reduce extraction series, increase treating capacity, improve the rate of recovery of extractant simultaneously, solve the problems, such as it is existing in the prior art it is at high cost, treating capacity is small and separation is difficult, there is good market application prospect.
Description
Technical field
The present invention relates to a kind of lithium isotopes6The extracting method of Li is extracted more particularly, to a kind of application centrifugal extractor
Lithium isotope6The method of Li.
Background technique
Lithium is the most light metal of nature, and there are two kinds of stable isotopes to be6Li and7Li, relative abundance are respectively6Li is 7.53%,7Li is 92.47%.In nuclear power industry,6Li and7Li has different nuclear reactivity energy, in nuclear material
It occupies an important position.It therefore, is always the research topic paid attention to their separation.
The separation method of lithium isotope has much at present, is broadly divided into chemical method and physical method.Chemical method packet
Method containing lithium amalgam, solvent extraction, ion-exchange chromatography, fractional precipitation and fractional crystallization etc..Physical method includes electromagnetic method, fused salt
Electrolysis method, electron transfer, molecular distillation and separation by laser etc..Wherein, lithium amalgam method is current separation highest and really throws
Enter the method for actual production, but the disadvantage of this method is that a large amount of mercury used in separation process will bring environment and peace
Full problem;The shortcomings that ion exchange mechansim lithium isotope is to struggle that coefficient is small, equilibration time is long, operation is discontinuous and exchange
Agent stability difference etc.;Although laser method improves separation, but this method requires height to technology and material installation, point
It is low from yield.
And commonly have for the solvent extraction of mercury-free separation lithium isotope since lithium ion has very big hydratability
The complexing of solvent is very weak, little to the separating effect of lithium isotope, and it is very tired to be applied to separation lithium isotope in industry
It is difficult.Furthermore this method the disadvantages of there is also solvent selections to be more troublesome, higher cost, separation are smaller, treating capacity is few.In the presence of
On the one hand the reason of above problem is that system separation is small, traditional extraction equipment cannot two phases were separated well opens, into
And need to increase extraction series, cause equipment investment and energy consumption to increase, substantially increases processing cost;On the other hand, segregative line
The biggish excellent extractant of number is mostly crown ether, the cave ethers organic matter of more difficult synthesis, and which increases being extracted into for lithium isotope
This.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of extractions of application centrifugal extractor
Lithium isotope6The method of Li solves the problems such as higher cost, separation are smaller, treating capacity is few while having reached higher
Recovery rate.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A kind of application centrifugal extractor extraction lithium isotope6The method of Li, including the following steps:
(1) lithium hydroxide aqueous solution and extractant extraction section: are mixed to join centrifugal extractor with volume ratio for 1: 1-6
It is extracted;Room temperature, the extraction of 5-6 stage countercurrent;
(2) alkali wash section: extracting organic be added in centrifugal extractor of gained for step 1) and carry out alkali cleaning, room temperature, and 2-3 grades
Counter-current extraction;The organic phase and the volume ratio of lye are 1-3: 1;
(3) it is stripped section: organic phase obtained by step 2) being stripped in the centrifugal extractor, room temperature, 4-5 grades
Countercurrent reextraction takes;The organic phase and the volume ratio of strippant are 3-6: 1;Strippant is the sulfuric acid that mass concentration is 25%
Sodium water solution.
Further, the step 1) extractant is tributyl phosphate and kerosene, and volume ratio is tributyl phosphate/coal
Oil=1: 2-4.
Further, the step 2) lye is the sodium hydroxide solution that mass concentration is 20%-30%.
Further, the centrifugal extractor, including rack, motor, shell, heavy phase weir plate and horizontal cover, the level
Lid and shell are individually fixed in rack, and the side wall of outer shell is equipped with heavy out and light phase export, under the horizontal cover
Portion is symmetrically arranged with damping block;The motor is fixed on above horizontal cover;It further include the rotary drum being hung on by axle suspension in horizontal cover,
The rotary drum is fixed on axis by locknut, and the outer wall of the shell is equipped with the feed inlet tangent with shell, the feed inlet
Including heavy phase feed inlet and light phase feed inlet, upper inside wall is equipped with heavy phase liquid collecting cavity, light phase liquid collecting cavity, and inner wall lower is equipped with water conservancy diversion
Leaf, housing bottom inner surface are equipped with spinning disk, are equipped with baiting valve among spinning disk;The axis is customization motor shaft, is motor
Axis integrally lengthens.
Further, the rotary drum is inside and outside double-layer structure or four-layer structure.
Further, the rotary drum is hung in horizontal cover, its underpart bearing-free, without mechanical seal, and rotary drum is composite wood
Expect it is molded, material be polypropylene or perfluoroalkoxy resin.
Further, the shell is the Unitarily molded molding of composite material, and material is polypropylene or perfluoro alkoxy tree
Rouge.
Further, the heavy phase weir plate is to be divided into multiple segmental arcs, and heavy phase weir plate is spliced by multiple segmental arc.
Further, the feed inlet, heavy out, light phase export are all made of the wave of flanged (FLGD) elbow and telescopic tube
The connection of line pipe, pipeline connection are the Unitarily molded molding of composite material, and material is polypropylene or perfluoroalkoxy resin.
The centrifugal extractor heavy out, light phase export are provided with sampling valve, temperature detection mouth.
In order to improve extraction efficiency, centrifugal extractor and extraction process of the invention are effectively combined, We conducted
A large amount of experimental exploring, it is especially desirable to, it is noted that the selection of extractant, the selection of multi-stage counter current extraction test solvent and parameter
Setting, multistage back extraction experiment rank selection and being set in entire effect of extracting for test parameters be particularly important.
Our screenings to extractant below, the setting of multi-stage counter current extraction experiment parameter, the setting of multistage back extraction experiment parameter are real
It tests etc. and briefly to enumerate and carry out brief analysis.
Experiment 1: the choice experiment of extractant
Ingredient of cave ether [2,2, the 1]-chloroform, TBP-N503- kerosene, TBP- kerosene as extractant is selected, extraction is changed
Agent type and proportion carry out pilot plant test.The extractant of fermentation liquid and variety classes and proportion is separately heated to 30 DEG C, is being divided
Shake flat experiment is carried out in liquid funnel, after two-phase is layered completely, sample detection.Experimental result is as follows.
Shaking flask extraction experiments result under 1. variety classes extractant of table
According to the experimental result in upper table: it selects cave ether [2,2,1]: when chloroform=1:1 is as extractant, extraction yield
Highest, but cave ether extration agent producing process is complicated, cost is high, and is not easily recycled, and cannot achieve industrial applications, comprehensive
Consider, select TBP: sulfonated kerosene=1:4 extractant system is best.
Experiment 2: multi-stage counter current extraction experiment
It is 180ml/min in flux, volume ratio 5: 1, feeding temperature is room temperature, under the operating condition of counter-current extraction, is adopted
It uses CWL50-M Novel series efficient centrifugal extracter as extraction equipment, changes extraction series, observation experiment effect.LiOH water
Solution enters equipment from the heavy phase feed inlet of extractor with the inlet amount of 30ml/min, and extractant is with the inlet amount of 150ml/min
Enter equipment from the light phase feed inlet of extractor, after two-phase discharges and stablizes, sample detection, while observing two-phase situation.Extraction
Taking series to set gradually is 1,2,3,4,5,6,7, repeats aforesaid operations, experimental result such as table 2:
2. multi-stage counter current extraction experimental result of table
Serial number | Extract series | Extraction yield/% | Separating effect |
1 | 1 | 14.23 | Water phase is organic to compare muddiness without muddiness |
2 | 2 | 26.44 | Water phase is organic to compare muddiness without muddiness |
3 | 3 | 36.90 | Water phase is without muddiness, organic phase slight turbid |
4 | 4 | 45.88 | Water phase is without muddiness, organic phase slight turbid |
5 | 5 | 53.58 | Water phase and organic phase are without muddiness |
6 | 6 | 60.16 | Water phase and organic phase are without muddiness |
7 | 7 | 61.05 | Water phase and organic phase are without muddiness |
According to the experimental result in upper table: after extraction,6Li is entered in organic phase in the form of complex compound,7Li
Then enter water phase, with the increase of extraction series, extraction yield is gradually risen, and separating effect gradually improves, but is extracted after 7 grades of extractions
Rate has no compared to 6 grades and obviously increases, therefore selects the extraction of 6 stage countercurrents best.
Experiment 3: multi-stage countercurrent back extraction experiment
It is 180ml/min in flux, volume ratio 5: 1, feeding temperature is 35 DEG C, under the operating condition that countercurrent reextraction takes,
Using CWL50-M Novel series efficient centrifugal extracter as back extraction equipment, change back extraction series, observation experiment effect.
Strippant enters equipment from the heavy phase feed inlet of extractor with the inlet amount of 30ml/min, and load organic phases are with 150ml/min
Inlet amount enter equipment from the light phase feed inlet of extractor, after two-phase discharges and stablizes, sample detection, while observing separation
Effect.It is 1,2,3,4,5,6 that extraction series, which is set gradually, repeats aforesaid operations, experimental result such as table 3:
3. multi-stage countercurrent of table is stripped experimental result
Serial number | It is stripped series | Stripping rate/% | Separating effect |
1 | 1 | 21.72 | Water phase and organic phase are without muddiness |
2 | 2 | 38.70 | Water phase and organic phase are without muddiness |
3 | 3 | 52.03 | Water phase and organic phase are without muddiness |
4 | 4 | 62.45 | Water phase and organic phase are without muddiness |
5 | 5 | 70.62 | Water phase and organic phase are without muddiness |
6 | 6 | 70.88 | Water phase and organic phase are without muddiness |
According to the experimental result in upper table: by being stripped,6Li is with Li2The form of SO4 enters water phase, and extractant obtains
Regeneration.With the increase of back extraction series, stripping rate is gradually risen, and good separating effect, is stripped by 5 stage countercurrents
Afterwards, stripping rate can reach 70.62%, and 6 grades of back extraction ratios do not occur obviously increasing trend compared to 5 grades, therefore, select 5 grades
Countercurrent reextraction takes most preferably.
Lithium isotope is extracted using CWL-M Series Centrifugal extracter, LiOH aqueous solution is extracted by 6 stage countercurrents, 3 grades of alkali
It washes, after the back extraction of 5 stage countercurrents,6The extraction yield of Li has reached 60.16%, final products Li2SO4, purity reach 80%.
The beneficial effects of the present invention are:
Beneficial effects of the present invention
1. centrifugal extractor provided by the invention is a kind of extract equipment of new and effective lithium isotope, have corrosion-resistant
Strong, the delicate structure of property, the significant advantages such as extraction yield height.Centrifugal extractor shell, rotary drum and pipeline are composite material entirety mould
It is moulded into type, material is polypropylene, and perfluoroalkoxy resin effectively raises the corrosion resistance of equipment.Centrifugal extractor is logical
Crossing motor drives extraction reactor to carry out extraction reaction, realizes the semi-automation and integration of extraction, back extraction and pickling, together
When, the rotary drum of the centrifugal extractor as used in the present invention is inside and outside double-layer structure or four-layer structure, and multilayer separation is conducive to improve
Separative efficiency.
2. the extracting method of lithium isotope provided by the invention obtains higher degree by extraction, alkali cleaning and back extraction6Li isotope, preferred tributyl phosphate/kerosene=1 of extraction stages: 2 are used as extractant, both ensure that higher recovery rate, together
When obtain6Li isotopic purity is up to 80%,6Li isotopic purity obtains marked improvement in extracting.Both reduced production at
This, and easy to promote and utilize and industrialized production.
3. lithium isotope extract equipment of the present invention is a kind of new and effective centrifugal extraction equipment, solvent extraction
After the technology of extraction lithium isotope is in conjunction with equipment of the present invention, stage efficiency and separating effect are greatly improved, is reduced
Extraction series, increases treating capacity, while improving the rate of recovery of extractant, solves cost existing in the prior art
Problem high, treating capacity is small and separation is difficult, has good market application prospect.
Detailed description of the invention
Fig. 1 is work flow diagram of the invention;
Fig. 2 is the structural schematic diagram of centrifugal extractor of the invention.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
A kind of application centrifugal extractor extraction lithium isotope6The method of Li, including the following steps:
(1) extraction section: by lithium hydroxide aqueous solution and extractant with volume ratio be 1: 1 be mixed to join centrifugal extractor into
Row extraction;Room temperature, the extraction of 5 stage countercurrents;The extractant is tributyl phosphate and kerosene, and volume ratio is tributyl phosphate/coal
Oil=1: 2;
(2) alkali wash section: extracting organic be added in centrifugal extractor of gained for step 1) and carry out alkali cleaning, room temperature, and 2-3 grades
Counter-current extraction;The organic phase and the volume of lye are 1: 1;The lye is the sodium hydroxide solution that mass concentration is 20%;
(3) it is stripped section: organic phase obtained by step 2) being stripped in the centrifugal extractor, room temperature, 4-5 grades
Countercurrent reextraction takes;The organic phase and the volume of strippant are 3: 1;Strippant is the sodium sulphate water that mass concentration is 25%
Solution.
Including rack 14, motor 1, shell 13, heavy phase weir plate 4 and horizontal cover 2, horizontal cover 2 and shell 13 are individually fixed in
In rack 14,13 side wall of shell is equipped with heavy out 5 and light phase export 16, and the lower part of horizontal cover 2 is symmetrically arranged with damping block
3;Motor 1 is fixed on 2 top of horizontal cover;Centrifugal extractor of the invention further includes the rotary drum hung in horizontal cover 2 by axis 6
12, rotary drum 12 is fixed on axis 6 by locknut 7, and the outer wall of shell 13 is equipped with the feed inlet 11 tangent with 13 shell of shell, into
Material mouth 11 includes heavy phase feed inlet and light phase feed inlet, and upper inside wall is equipped with heavy phase liquid collecting cavity 15, light phase liquid collecting cavity 17, under inner wall
Portion is equipped with water conservancy diversion leaf 8, and 13 bottom interior surface of shell is equipped with spinning disk 9, is equipped with baiting valve 10 among spinning disk 9;Its axis 6 is fixed
Motor shaft processed integrally lengthens for motor shaft.Rotary drum 12 is inside and outside double-layer structure or four-layer structure.Rotary drum 12 hangs on horizontal cover 2
On, its underpart bearing-free, without mechanical seal, rotary drum 12 is that composite material is molded, and material is polypropylene or perfluoro alkoxy
Resin.Shell 13 be the Unitarily molded molding of composite material, material be polypropylene or perfluoroalkoxy resin.Heavy phase weir plate 4 is
Multiple segmental arcs are divided into, heavy phase weir plate 4 is spliced by multiple segmental arc.It is Centrifugical extraction machine inlet 11, heavy out 5, light
Mutually outlet 16 is all made of flanged (FLGD) elbow and connects with the bellows of telescopic tube, and pipeline connection is that composite material is Unitarily molded
Molding, material are polypropylene or perfluoroalkoxy resin;Heavy out 5, light phase export 16 are provided with sampling valve, temperature detection
Mouthful.
As shown in Figure 1, giving work flow diagram of the invention.(a) it is lithium hydroxide aqueous solution, provides it to extraction
In reactor (b), it is contacted with extractant (c) herein.Raffinate (e) discharge that will be flowed out from novel extraction reactor (b).
The load organic liquid (d) that will be flowed out from the extraction reactor (b) is provided into alkali cleaning extraction reactor (f), make herein it and
The lye (g) of offer contacts.Alkali cleaning extraction raffinate (h) discharge that will be flowed out from the alkali cleaning extraction reactor (f), by pipeline by alkali cleaning
Load organic liquid (i) afterwards is supplied to novel reversed extractor (j), contacts it with the strippant (k) provided.It is logical
The regeneration organic liquid (l) that piping will be flowed out from the back extraction device (j) is provided in organic phase storage tank (n), then again
It is recycled in extraction reactor (b), is product from the aqueous solution (m) flowed out in back extraction device (j).The extraction reactor
(b), alkali cleaning extraction reactor (f) and back extraction device (j) are the structure of extraction reactor of the present invention.
Embodiment 2
A kind of application centrifugal extractor extraction lithium isotope6The method of Li, including the following steps:
(1) extraction section: by lithium hydroxide aqueous solution and extractant with volume ratio be 1: 6 be mixed to join centrifugal extractor into
Row extraction;Room temperature, the extraction of 6 stage countercurrents;The extractant is tributyl phosphate and kerosene, and volume ratio is tributyl phosphate/coal
Oil=1: 4;
(2) alkali wash section: step 1) is extracted into organic be added in centrifugal extractor of gained and carries out alkali cleaning, room temperature, 3 grades inverse
Stream extraction;The organic phase and the volume ratio of lye are 3: 1;The lye is the sodium hydroxide solution that mass concentration is 30%;
(3) it is stripped section: organic phase obtained by step 2) being stripped in the centrifugal extractor, room temperature, 4-5 grades
Countercurrent reextraction takes;The organic phase and the volume of strippant are than 6: 1;Strippant is the sodium sulphate that mass concentration is 25%
Aqueous solution.
The structure of the centrifugal extractor is shown in embodiment 1.
Embodiment 3
A kind of application centrifugal extractor extraction lithium isotope6The method of Li, including the following steps:
(1) extraction section: by lithium hydroxide aqueous solution and extractant with volume ratio be 1: 5 be mixed to join centrifugal extractor into
Row extraction;Room temperature, the extraction of 5 stage countercurrents;The extractant is tributyl phosphate and kerosene, and volume ratio is tributyl phosphate/coal
Oil=1: 3;
(2) alkali wash section: step 1) is extracted into organic be added in centrifugal extractor of gained and carries out alkali cleaning, room temperature, 3 grades inverse
Stream extraction;The organic phase and the volume ratio of lye are 2: 1;The lye is the sodium hydroxide solution that mass concentration is 25%;
(3) it is stripped section: organic phase obtained by step 2) being stripped in the centrifugal extractor, room temperature, 4 grades inverse
Stream back extraction;The organic phase and the volume ratio of strippant are 5: 1;Strippant is the sodium sulphate water that mass concentration is 25%
Solution.
The structure of the centrifugal extractor is shown in embodiment 1.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, this field is common
Other modifications or equivalent replacement that technical staff makes technical solution of the present invention, without departing from technical solution of the present invention
Spirit and scope, be intended to be within the scope of the claims of the invention.
Claims (1)
1. a kind of application centrifugal extractor extracts lithium isotope6The method of Li, which is characterized in that including the following steps:
1) extraction section: lithium hydroxide aqueous solution and extractant are mixed to join centrifugal extractor with volume ratio for 1: 1-6 and carried out
Extraction;Room temperature, the extraction of 5-6 stage countercurrent;The extractant is tributyl phosphate and kerosene, and volume ratio is tributyl phosphate/coal
Oil=1: 2-4;
2) alkali wash section: step 1) is extracted into organic be added in centrifugal extractor of gained and carries out alkali cleaning, room temperature, 2-3 with lye
Stage countercurrent extraction;The lye is the sodium hydroxide solution that mass concentration is 20%-30%;The volume ratio of the organic phase and lye
It is 1-3: 1;
3) it is stripped section: organic phase obtained by step 2 being stripped in the centrifugal extractor, room temperature, 4-5 stage countercurrent
Back extraction;The organic phase and the volume ratio of strippant are 3-6: 1;Strippant is the sodium sulphate water that mass concentration is 25%
Solution;
The centrifugal extractor, including rack (14), motor (1), shell (13), heavy phase weir plate (4) and horizontal cover (2), it is described
Horizontal cover (2) and shell (13) are individually fixed on rack (14), and shell (13) side wall is equipped with heavy out (5) and light
Mutually outlet (16), the lower part of the horizontal cover (2) is symmetrically arranged with damping block (3);The motor (1) is fixed on horizontal cover (2)
Top;It further include the rotary drum (12) hung on by axis (6) on horizontal cover (2), the rotary drum (12) is fixed on by locknut (7)
On axis (6), the outer wall of the shell (13) is equipped with the feed inlet (11) tangent with shell, and the feed inlet (11) includes heavy phase
Feed inlet and light phase feed inlet, upper inside wall are equipped with heavy phase liquid collecting cavity (15), light phase liquid collecting cavity (17), and inner wall lower is equipped with water conservancy diversion
Leaf (8), shell (13) bottom interior surface are equipped with spinning disk (9), are equipped with baiting valve (10) among spinning disk (9);The axis (6)
To customize motor shaft, integrally lengthened for motor shaft;The rotary drum (12) is inside and outside double-layer structure or four-layer structure;The rotary drum
(12) it hangs on horizontal cover (2), its underpart bearing-free, without mechanical seal, rotary drum (12) is that composite material is molded, material
For polypropylene or perfluoroalkoxy resin;The shell (13) be the Unitarily molded molding of composite material, material be polypropylene or
Perfluoroalkoxy resin;The heavy phase weir plate (4) is to be divided into multiple segmental arcs, heavy phase weir plate (4) spliced by multiple segmental arc and
At;The feed inlet (11), heavy out (5), light phase export (16) are all made of the ripple of flanged (FLGD) elbow and telescopic tube
Pipe connection, pipeline connection are the Unitarily molded molding of composite material, and material is polypropylene or perfluoroalkoxy resin;The heavy phase
Outlet (5), light phase export (16) are provided with sampling valve, temperature detection mouth.
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CN112058088B (en) * | 2020-09-10 | 2024-07-05 | 中国科学院青海盐湖研究所 | Multistage oscillation-based extraction and separation method of lithium isotopes |
CN115105857B (en) * | 2021-03-23 | 2024-07-19 | 郑州天一萃取科技有限公司 | Purification treatment agent and purification method for tributyl phosphate waste organic phase |
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CN203816271U (en) * | 2014-04-14 | 2014-09-10 | 郑州天一萃取科技有限公司 | High-flux centrifugal extractor |
CN106075952A (en) * | 2016-07-25 | 2016-11-09 | 郑州天萃取科技有限公司 | Centrifugal extractor rotary drum and the manufacture method of this rotary drum |
CN106337138A (en) * | 2016-11-03 | 2017-01-18 | 深圳市捷鑫资产管理有限公司 | Technology for preparing high-purity anhydrous lithium chloride through centrifugal extraction of salt lake brine |
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CN87103431A (en) * | 1987-05-07 | 1987-11-04 | 中国科学院青海盐湖研究所 | A kind of method of from contain lithium bittern, extracting Lithium chloride (anhydrous) |
CN203816271U (en) * | 2014-04-14 | 2014-09-10 | 郑州天一萃取科技有限公司 | High-flux centrifugal extractor |
CN106075952A (en) * | 2016-07-25 | 2016-11-09 | 郑州天萃取科技有限公司 | Centrifugal extractor rotary drum and the manufacture method of this rotary drum |
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Inventor after: Wang Lijun Inventor after: Yang Pengfei Inventor before: Wang Lijun |
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