CN106008563A - Method for removing solid impurities in organic metal reagent solution - Google Patents
Method for removing solid impurities in organic metal reagent solution Download PDFInfo
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- CN106008563A CN106008563A CN201610344341.XA CN201610344341A CN106008563A CN 106008563 A CN106008563 A CN 106008563A CN 201610344341 A CN201610344341 A CN 201610344341A CN 106008563 A CN106008563 A CN 106008563A
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- solid impurity
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- organometallic reagent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic System
- C07F3/06—Zinc compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/24—Feed or discharge mechanisms for settling tanks
- B01D21/2444—Discharge mechanisms for the classified liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/26—Separation of sediment aided by centrifugal force or centripetal force
- B01D21/262—Separation of sediment aided by centrifugal force or centripetal force by using a centrifuge
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic System
- C07F1/02—Lithium compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic System
- C07F3/02—Magnesium compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Centrifugal Separators (AREA)
Abstract
The invention discloses a method for removing solid impurities in an organic metal reagent solution. The method comprises the following steps of (1) under the conditions of insert gas protection and air isolation, separating solid impurities from an organic metal reagent clear solution in a mode of natural sedimentation or centrifugal sedimentation of the organic metal reagent solution containing metal impurities; (b) guiding out the clear solution in a way of maintaining the insert gas protection and air isolation conditions to obtain the organic metal reagent solution subjected to solid impurity removal. The method for removing solid impurities in the organic metal reagent solution has the following beneficial effects that under the insert gas protection condition, the solid impurities in the organic metal reagent solution can be effectively removed by a natural sedimentation or centrifugal sedimentation method, so that the technical problem of reagent quality reduction due to solid impurity existence in the organic metal reagent solution is solved.
Description
Technical field
The present invention relates to the method for purification of a kind of solution.
Background technology
Organo-metallic compound, also known as metallo-organic compound, refers to organic group (such as alkyl, aromatic radical)
In carbon and metallic atom directly in conjunction with the general name of material, this compounds is generally of the anti-of uniqueness
Should be active, it is widely used in the fields such as organic chemistry, polymer chemistry, materials chemistry, life sciences.Often
The organometallic reagent seen includes organic alkali metal reagent, organic alkaline earth metal reagent, organic zinc reagent, has
Machine aluminon, organoboron reagent, organic cadion, organic mercury reagent, organic beryllon, organotin reagent
Or Organic leadP reagent etc..Such reagent preserves the most as a solution, convenient storage and use, solvent Chang Xuan
From in alkanes or ethers etc..
But, organometallic reagent solution is often mixed with variable amount of solid impurity.On the one hand, solid impurity comes
Come from the preparation process of organometallic reagent.Such as, organomagnesium reagent (i.e. Grignard reagent) is acutely
Organic halogen is added drop-wise in the organic solvent containing magnesium metal in the case of stirring reaction prepare, often
Magnesium metal include magnesium chips, magnesium powder, MAG block etc..One layer of magnesium oxide is often wrapped up on the surface of magnesium metal, in system
Become solid small particles impurity during standby organomagnesium reagent, be suspended in reaction mixture.Additionally, some
Side reaction also results in the appearance of solid impurity, is present in product solution.On the other hand, multiple organic gold
The reactivity belonging to reagent is the highest, more sensitive to water, oxygen, preparation and during storing easily
Rotten, products of metamorphism is suspended in product solution becomes solid impurity.Additionally, some organometallic reagent exists
Meeting crystallization during storage, especially organometallic reagent concentration is higher when during such phenomenon
Occur.The existence of solid impurity causes in solution effective ingredient to reduce, such as suspension Lithium hydrate in organolithium,
Suspension magnesium hydroxide, magnesium oxide etc. in Grignard reagent.Above-mentioned solid impurity is mostly alkaline matter, causes molten
Total alkali virtual height in liquid system, and effective active alkali content is on the low side, causes user cannot accurately know have
The valid density of machine metal agent solution, impact uses.
For a long time, organometallic reagent solution is mixed with the technical problem of solid impurity and has no always and reported,
There is no effective solution yet.
Summary of the invention
Embodiments of the invention are intended to overcome above technical problem, propose one can by natural subsidence or from
The method of solid impurity in the removal organometallic reagent solution of heart sedimentation.
Major part organo-metallic compound is to the oxygen in air, moisture-sensitive, apt to deteriorate, common place
Reason mode easily makes organometallic reagent rapid deterioration in processing procedure, not only can not improve organic metal
The quality of reagent solution, reduces its quality on the contrary.Additionally, organometallic reagent generally has corrosivity, should
Container in operating process, protector etc. can be damaged by corrosivity, have danger to operator, from
And more improve the difficulty of solution problem.Therefore, prior art all the time do not propose solve organometallic reagent molten
Liquid is mixed with the scheme of the technical problem of solid impurity.
In this application, inert gas refers to the gas not reacted with organometallic reagent, e.g.
Noble gas or nitrogen.
For solving above-mentioned technical problem, according to the first aspect of the invention, it is provided that a kind of organic metal of removing is tried
The method of solid impurity in agent solution, wherein, comprises the steps:
(a), under conditions of being completely cut off air by inert gas shield, organic by containing solid impurity
Metal agent solution makes solid impurity and organometallic reagent by the way of natural subsidence or centrifugal sedimentation
Settled solution separates；And
(b), be maintained at and completely cut off air by inert gas shield under conditions of, derive settled solution and obtain
To the organometallic reagent solution removing solid impurity.
According to the second aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, described inert gas is noble gas or nitrogen.
According to the third aspect of the invention we, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, described organometallic reagent includes: organic alkali metal reagent, organic alkaline earth metal reagent, have
Machine zincon, organoaluminum reagents, organoboron reagent, organic cadion, organic mercury reagent, organic beryllon,
Organotin reagent and Organic leadP reagent.
According to the fourth aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, the solvent in described organometallic reagent solution is alkane solvents, ether solvent, aromatic hydrocarbons
The mixed solvent of the one or more of which in solvent.
According to the fifth aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, step (a) including:
After preparing organometallic reagent solution, allow reactant liquor natural subsidence in reaction bulb, wherein,
After standing a period of time, solid impurity can be deposited in bottom reaction bulb, is settled solution on solid impurity.
According to the sixth aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, step (a) including:
Storing during organic metal agent solution, allowing the organometallic reagent solution containing solid impurity
Natural subsidence in a reservoir, wherein, after standing a period of time, solid impurity can be deposited in container bottom, Gu
It it is settled solution on body impurity.
According to the seventh aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, step (a) including:
Import to, in centrifuge bottle or sedimentation centrifuge, pass through by the organometallic reagent solution containing solid impurity
The mode of centrifugal rotation, makes solid impurity be deposited in centrifuge bottle or the bottom of sedimentation centrifuge or inwall.
According to the eighth aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein,
Described centrifuge bottle material is glass or rustless steel；
The inner bag material of described sedimentation centrifuge is enamel, glass, plastics or rustless steel.
According to the ninth aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, the rotating speed of described centrifugal rotation is at more than 1000r/h, and centrifugation time is more than 10 minutes.
According to the tenth aspect of the invention, it is provided that a kind of remove the side of solid impurity in organometallic reagent solution
Method, wherein, the time of described natural subsidence is 1 120 hours, such as 24 hours.
The method of solid impurity in organometallic reagent solution of removing of the present invention has compared to prior art
Following advantage: the present invention is by passing through natural subsidence by the organometallic reagent settled solution containing solid impurity
Or the mode of centrifugal sedimentation makes solid impurity separate with organometallic reagent solution, then derives clarification
Solution obtains the method removing the organometallic reagent solution of solid impurity, can effectively remove organic metal
Solid impurity in reagent solution, thus solve organometallic reagent solution exists solid impurity cause examination
The technical problem that agent quality reduces.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to enforcement
In example or description of the prior art, the required accompanying drawing used is briefly described, it should be apparent that, describe below
In accompanying drawing be only some embodiments of the present invention, for those of ordinary skill in the art, do not paying
On the premise of going out creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the flowage structure signal of the method for solid impurity in organometallic reagent solution of removing of the present invention
Figure.
Detailed description of the invention
For making the purpose of the present invention, technical scheme and advantage of greater clarity, below in conjunction with specific embodiment party
Formula referring to the drawings, the present invention is described in more detail.It should be understood that these describe the most exemplary,
And it is not intended to limit the scope of the present invention.Additionally, in the following description, eliminate known features and technology
Description, to avoid unnecessarily obscuring idea of the invention.
Here, inert gas refers to the gas not reacted with organometallic reagent, e.g. indifferent gas
Body or nitrogen.
Fig. 1 is the flowage structure signal of the method for solid impurity in organometallic reagent solution of removing of the present invention
Figure, a kind of removes the method for solid impurity in organometallic reagent solution as it is shown in figure 1, the invention provides,
It comprises the steps:
(a), under conditions of being completely cut off air by inert gas shield, organic by containing solid impurity
Metal agent solution makes solid impurity and organometallic reagent by the way of natural subsidence or centrifugal sedimentation
Settled solution separates, described inert gas e.g. noble gas or nitrogen；And
(b), be maintained at and completely cut off air by inert gas shield under conditions of, derive settled solution and obtain
To the organometallic reagent solution removing solid impurity.
The present invention effectively removes organic metal by the method using natural subsidence or centrifugal sedimentation and tries
Solid impurity in agent solution, thus solve in organometallic reagent solution because of exist solid impurity cause examination
The technical problem that agent quality reduces.
Wherein it is desired to explanation, the most generally the organometallic reagent solution containing solid impurity is used
Following method is purified: in atmosphere by the methods such as conventional filtration or centrifugally operated by solid impurity with
Solution separates, but above-mentioned processing method easily makes organometallic reagent become rapidly in processing procedure
Matter, not only the quality of organometallic reagent solution can not be improved, reduce its quality on the contrary.It should be noted that
For solving above-mentioned technical problem, the present invention removes the operating procedure (a) of solid impurity in organometallic reagent solution
(b) all carry out under conditions of inert gas shield, or under conditions of isolation air
Carrying out, described inert gas e.g. noble gas or nitrogen, the condition of described isolation air is such as
It it is vacuum environment.The present invention is eliminated containing solid impurity by the method for natural subsidence or centrifugal sedimentation
Organometallic reagent solution stores under the cryogenic conditions of anhydrous and oxygen-free, and character is relatively stable.Send out the most afterwards
Existing, its concentration of active substance did not had significant change within time several months.
When carrying out gas shield, the inert gas of employing compression, the noble gas such as compressed or nitrogen,
With nozzle, the gas of compression is sprayed to organometallic reagent solution, makes organometallic reagent solution and air insulated,
So that the operating procedure of solid impurity is in the gas shield of isolation air in removal organometallic reagent solution
Under the conditions of carry out.Described nozzle can be circular ports, or the bucket shape mouth of pipe, it is also possible to be the flat mouth of pipe, institute
Stating nozzle and can have certain area coverage, for example, circular lid, with conveniently and effectively by compressed gas
Body makes organometallic reagent solution and air insulated after spraying to organometallic reagent solution.
The present invention removes the solid in organometallic reagent solution by the method for natural subsidence or centrifugal sedimentation
Impurity, specifically can have following several situation:
The organometallic reagent solution of solid impurity will be produced by the way of natural subsidence in preparation process
The method making solid impurity carry out separating with organometallic reagent solution is as follows, i.e. step (a) including:
After preparing organometallic reagent solution, allow reactant liquor natural subsidence in reaction bulb, wherein, quiet
After putting a period of time, solid impurity can be deposited in bottom reaction bulb, is settled solution on solid impurity.
The organometallic reagent solution of solid impurity will be produced by the way of natural subsidence during storing
The method making solid impurity carry out separating with organometallic reagent solution is as follows, i.e. step (a) including:
Storing during organic metal agent solution, allowing organometallic reagent solution natural subsidence in a reservoir,
Wherein, after standing a period of time, solid impurity can be deposited in container bottom, molten for clarification on solid impurity
Liquid.
Organometallic reagent solution containing solid impurity is made solid impurity by the way of centrifugal sedimentation
The method carrying out separating with organometallic reagent solution is as follows, i.e. step (a) including: will be miscellaneous containing solid
The organometallic reagent solution of matter imports in centrifuge bottle or sedimentation centrifuge, by the way of centrifugal rotation,
Solid impurity is made to be deposited in centrifuge bottle or the bottom of sedimentation centrifuge or inwall.
In the present invention use organometallic reagent include: organic alkali metal reagent, organic alkaline earth metal reagent,
Organic zinc reagent, organoaluminum reagents, organoboron reagent, organic cadion, organic mercury reagent, organic beryllium try
Agent, organotin reagent or Organic leadP reagent.
Solvent in the organometallic reagent solution used in the present invention is alkane solvents, ether solvent, virtue
The mixed solvent of the one or more of which in varsol.Specifically, molten in organometallic reagent solution
Agent use benzene, toluene, hexamethylene, normal hexane, pentane, petroleum ether, decahydronaphthalenes, carbon tetrachloride,
Dichloromethane, ethyl chloride, dichloroethanes, 1,2-dichloropropane, chloropropane or pyridine.
In further embodiment of the present invention, centrifuge bottle material is glass or rustless steel；Sedimentation centrifuge interior
Gallbladder material is enamel, glass, plastics or rustless steel.
In further embodiment of the present invention, centrifugal sedimentation method uses sedimentation centrifuge, its centrifugal rotation
Rotating speed at more than 1000r/h, and centrifugation time is more than 10 minutes.
In further embodiment of the present invention, in natural subsidence method, the time of its natural subsidence is not specified by,
Need to determine according to practical situation the time of natural subsidence, find the scope of the time of natural subsidence in an experiment
It is 1 120 hours, such as, can be 24 hours.
Below in conjunction with concrete example, the present invention will be further described, and the most concrete example is for this is described
Bright rather than be used for limiting the scope of the present invention.
Example 1 removes the solid impurity in methyl grignard reagent
Under the protection of nitrogen, ether (0.1 liter) solution of methyl bromide (1.1 moles) is added drop-wise to containing
Ether (0.9 liter) solution of a large amount of magnesium chips (2 moles) is prepared the diethyl ether solution of methyl-magnesium-bromide.Reaction
After, reaction solution has a large amount of black suspension thing, bottom reaction bulb, has the solid impurity of 1.0 cm thicks
Precipitation.Reactant liquor stands 24 hours in reaction bulb, and black suspension thing settles, and has 1.5 bottom reaction bulb
The solid impurity precipitation of cm thick.Under conditions of nitrogen is protected, upper strata settled solution is poured into storage bottle
In, obtain the clarification diethyl ether solution of methyl-magnesium-bromide, in solution and there is no obvious solid precipitation bottom solution.
Total alkali concn 1.1 moles every liter, active alkali concentration 1.0 moles every liter.
Example 2 removes the solid impurity in diethyl zinc tetrahydrofuran solution
The bottom solid precipitation thickness of the diethyl zinc tetrahydrofuran solution storage bottle storing 5 months is 0.2 li
Rice, solution shows slightly muddy.Under nitrogen protection, this solution is imported in the glass centrifuge bottle being dried, from
The heart rotates 30 minutes, and rotating speed 4000 turns is per hour.After Li Xin, solid impurity is deposited on glass and is centrifuged
On bottle inwall.Under conditions of nitrogen is protected, the settled solution in centrifuge bottle is directed in storage bottle.Storage
Depositing in bottle is settled solution, in solution and does not has obvious solid precipitation bottom solution.
Example 3 removes the solid impurity in n-BuLi hexane solution
The bottom solid precipitation thickness of the n-BuLi hexane solution storage bottle storing 6 months is 0.1 centimetre,
Solution is muddy.Natural subsidence does not has effect to improve the clarity of solution.Under nitrogen protection, this solution is led
Enter in dry glass centrifuge bottle, centrifugal rotation 30 minutes, rotating speed 60 revs/min.After Li Xin,
Solid is deposited on glass centrifuge bottle inwall.Under conditions of nitrogen is protected, by the settled solution in centrifuge bottle
It is directed in storage bottle.Storage bottle is settled solution, in solution and there is no obvious solid precipitation bottom solution.
Example 4 removes the solid impurity in the diethyl ether solution of phenyl-magnesium-bromide
The bottom solid precipitation thickness of the diethyl ether solution storage bottle storing the phenyl-magnesium-bromide of 5 months is 0.3 li
Rice, solution is black, slightly muddy.Under nitrogen protection, this solution is imported to the sedimentation centrifuge being dried
In, the inner bag of sedimentation centrifuge is plastics, and outer wall is rustless steel.Centrifugal rotation 30 minutes, rotating speed 4000
Turn/hour.After Li Xin, solid is deposited on the inner bag of sedimentation centrifuge.Condition in nitrogen protection
Under, the settled solution in sedimentation centrifuge is directed in storage bottle.Storage bottle is settled solution, solution
Neutralize and there is no obvious solid precipitation bottom solution.
It should be appreciated that the above-mentioned detailed description of the invention of the present invention is used only for exemplary illustration or explains this
The principle of invention, and be not construed as limiting the invention.Therefore, without departing from spirit and scope of the present invention
In the case of any modification, equivalent substitution and improvement etc. done, should be included in protection scope of the present invention
Within.Additionally, claims of the present invention be intended to fall into scope and border or
Whole changes in the equivalents on this scope of person and border and modification.
Claims (10)
1. remove a method for solid impurity in organometallic reagent solution, comprise the steps:
(a), under conditions of being completely cut off air by inert gas shield, organic by containing solid impurity
Metal agent solution makes solid impurity and organometallic reagent by the way of natural subsidence or centrifugal sedimentation
Settled solution separates；And
(b), be maintained at and completely cut off air by inert gas shield under conditions of, derive settled solution and obtain
To the organometallic reagent solution removing solid impurity.
The method of solid impurity in removal organometallic reagent solution the most according to claim 1, its
In, described inert gas is noble gas or nitrogen.
The method of solid impurity in removal organometallic reagent solution the most according to claim 1, its
In, described organometallic reagent includes: organic alkali metal reagent, organic alkaline earth metal reagent, organic zinc try
Agent, organoaluminum reagents, organoboron reagent, organic cadion, organic mercury reagent, organic beryllon, organic
Tin reagent and Organic leadP reagent.
The method of solid impurity in removal organometallic reagent solution the most according to claim 1, its
In, the solvent in described organometallic reagent solution is in alkane solvents, ether solvent, aromatic hydrocarbon solvent
The mixed solvent of one or more of which.
5. according to solid impurity in the removal organometallic reagent solution according to any one of claim 14
Method, wherein, step (a) including:
After preparing organometallic reagent solution, allow reactant liquor natural subsidence in reaction bulb, wherein,
After standing a period of time, solid impurity can be deposited in bottom reaction bulb, is settled solution on solid impurity.
6. according to solid impurity in the removal organometallic reagent solution according to any one of claim 14
Method, wherein, step (a) including:
Storing during organic metal agent solution, allowing the organometallic reagent solution containing solid impurity
Natural subsidence in a reservoir, wherein, after standing a period of time, solid impurity can be deposited in container bottom, Gu
It it is settled solution on body impurity.
7. according to solid impurity in the removal organometallic reagent solution according to any one of claim 14
Method, wherein, step (a) including:
Import to, in centrifuge bottle or sedimentation centrifuge, pass through by the organometallic reagent solution containing solid impurity
The mode of centrifugal rotation, makes solid impurity be deposited in centrifuge bottle or the bottom of sedimentation centrifuge or inwall.
The method of solid impurity in removal organometallic reagent solution the most according to claim 7, its
In,
Described centrifuge bottle material is glass or rustless steel；
The inner bag material of described sedimentation centrifuge is enamel, glass, plastics or rustless steel.
The method of solid impurity in removal organometallic reagent solution the most according to claim 7, its
In, the rotating speed of described centrifugal rotation is at more than 1000r/h, and centrifugation time is more than 10 minutes.
10. miscellaneous according to solid in the removal organometallic reagent solution according to any one of claim 14
The method of matter, wherein, the time of described natural subsidence is 1 120 hours.
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| CN107556331A (en) * | 2017-09-04 | 2018-01-09 | 南京哈柏医药科技有限公司 | The production technology of RMgBr |
| CN108220935A (en) * | 2018-01-12 | 2018-06-29 | 中国工程物理研究院流体物理研究所 | A kind of solid particle is in the centrifugal sedimentation adhesion method of metal works inner periphery |
| CN111939603A (en) * | 2020-06-24 | 2020-11-17 | 东南大学 | Device for removing particulate matters in liquid metal gallium working medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107556331A (en) * | 2017-09-04 | 2018-01-09 | 南京哈柏医药科技有限公司 | The production technology of RMgBr |
| CN108220935A (en) * | 2018-01-12 | 2018-06-29 | 中国工程物理研究院流体物理研究所 | A kind of solid particle is in the centrifugal sedimentation adhesion method of metal works inner periphery |
| CN108220935B (en) * | 2018-01-12 | 2020-03-10 | 中国工程物理研究院流体物理研究所 | Centrifugal sedimentation adhesion method for solid particles on inner cylindrical surface of metal workpiece |
| CN111939603A (en) * | 2020-06-24 | 2020-11-17 | 东南大学 | Device for removing particulate matters in liquid metal gallium working medium |
| CN111939603B (en) * | 2020-06-24 | 2024-04-16 | 东南大学 | Particulate matter remove device in liquid metal gallium working medium |
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