CN109648087A - A kind of preparation method and applications of alkali metal ball - Google Patents
A kind of preparation method and applications of alkali metal ball Download PDFInfo
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- CN109648087A CN109648087A CN201811524561.6A CN201811524561A CN109648087A CN 109648087 A CN109648087 A CN 109648087A CN 201811524561 A CN201811524561 A CN 201811524561A CN 109648087 A CN109648087 A CN 109648087A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F2009/0804—Dispersion in or on liquid, other than with sieves
- B22F2009/0812—Pulverisation with a moving liquid coolant stream, by centrifugally rotating stream
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Abstract
The present invention provides a kind of preparation method and applications of alkali metal ball, the preparation method includes: that high-order stirred tank is added in atent solvent, bulk alkali metal is added in stirred tank, agitating and heating is warming up to above 5-30 DEG C of alkali metal fusing point, melt alkali metal, it forms ball and is scattered in atent solvent, open high-order stirred tank bottom discharge port, contain the inflow of alkali metal ball dispersion liquid in the low level stirred tank of cold solvent in advance, stirring makes alkali metal ball be fully cooled solidification, obtains alkali metal ball product.Alkali metal ball preparation method of the invention is simple, efficient, granularity is controllable and uniform, and atent solvent can be recycled, safety and environmental protection.
Description
Technical field
The present invention relates to alkali metal particles preparation fields, and in particular to a kind of preparation method and applications of alkali metal ball.
Background technique
Common alkali metal includes lithium metal, metallic sodium, metallic potassium etc., and the organo-metallic compound purposes of these alkali metal is wide
It is general.For example, butyl lithium, naphthalene lithium are for causing anionic polymerization, luxuriant sodium is used to prepare a variety of cyclopentadinyl compounds.In general, organic
Alkali metal compound is made by alkali metal and corresponding organic compound reaction.Specifically, naphthalene sodium is molten by the tetrahydrofuran of naphthalene
Liquid reacts acquisition with metallic sodium, and luxuriant sodium reacts preparation with metallic sodium by cyclopentadiene, and butyl lithium then passes through lithium metal and chloro fourth
Alkane reacts to obtain.Above-mentioned reaction is generally implemented at low temperature, to ensure that reaction process is controllable.Meanwhile in order to make reaction smoothly into
Row, needs for alkali metal to be cut into small pieces, and increases specific surface area, to improve reaction efficiency.The process of cutting alkali metal is easy to lead
The problems such as causing alkali metal that oxidation, moisture absorption reaction occurs, and easily drop and unexpected fire accidents occur.There is a kind of substitution to cut
The method cut is one-pot heating/solvent quenching method, such as the preparation of sodium sand.One-pot heating/solvent quenching method prepares the tool of sodium sand
Body technology is that agitating and heating melts in atent solvent by metallic sodium block, is dispersed into liquid metal sodium in atent solvent small
Ball is mixed into cryogenic inert solvent into system then while being kept stirring, make system temperature be down to metallic sodium fusing point with
Under, promote liquid metal sodium bead to solidify, obtains sodium sand.The outstanding problem of this technique be sodium sand partial size be difficult to control, and often
Cause metal sodium sand poly- and even agglomerates.Although can heat up again, which makes metallic sodium liquefy again, is dispersed into bead, then again
Add cold solvent solidification.But increase with repetitive operation number, system quantity of solvent is more and more, seriously affects preparation efficiency.
As it can be seen that organic alkali metal synthesizes field, there is an urgent need to a kind of easy, efficient, size tunable spherical alkali metal particles
Manufacturing method.
Summary of the invention
The invention proposes a kind of preparation method and applications of alkali metal ball, can obtain size tunable, epigranular
Spherical alkali metal product, the present invention can overcome one-pot heating/solvent quenching method defect using double kettle methods, significantly improve alkali
The manufacture efficiency of metal ball shaped particle.In double kettle methods of the invention, high-order hot kettle implements the heating droplet treatment of alkali metal, low level
Cold kettle implements the cooling and solidifying of alkali metal drop, and the partial size of alkali metal ball is adjusted by hot kettle agitator speed, in hot kettle and cold kettle
Decentralized medium using atent solvent as alkali metal ball.
Realize the technical scheme is that
A kind of preparation method of alkali metal ball, steps are as follows: using double kettle method preparations, the i.e. hot kettle of a high position of heating fusing alkali metal
With the cold kettle of low level of cooling alkali metal ball, the partial size of alkali metal ball is adjusted by hot kettle agitator speed, and the hardening of alkali metal ball
It is realized in cold kettle, wherein using decentralized medium of the atent solvent as alkali metal ball, the alkali metal packet in hot kettle and cold kettle
Lithium metal, metallic sodium and metallic potassium are included, the alkali metal mean diameter of a ball modification scope being prepared is 0.1-6mm, and granularity is divided
Cloth is uniform, without poly- and particle.
The atent solvent includes one of kerosene, paraffin oil, diesel oil, conduction oil, white oil or a variety of, and atent solvent is all
It is very hydrophobic organic oils, it can be ensured that wherein moisture content is extremely low, is unlikely to when preparing alkali metal ball because water participates in reacting
And consume alkali metal.Mixed solvent can be used in the present invention, but for the ease of solvent recovery cycle use, the present invention preferably makes
With a kind of single scheme of solvent.
The ball preparation method of the alkali metal, the specific steps are as follows:
(1) atent solvent is added in high-order hot kettle, agitating and heating is warming up to above 5-30 DEG C of alkali metal fusing point, with protection gas
Body is bubbled 10-30min in stirred tank bottom, with the moisture in removing system,;
(2) atent solvent is added in the cold kettle of low level, agitating and heating is warming up to 105-120 DEG C, with protective gas in stirred tank
Bottom is bubbled 10-30min, with the moisture in removing system, is then cooled to solvent temperature not higher than 40 DEG C;
(3) bulk alkali metal is added in the hot kettle of a high position of step (1), maintaining temperature is above 5-30 DEG C of alkali metal fusing point,
5-30min is stirred, alkali metal is melted and is dispersed into ball in atent solvent;
(4) while step (3) maintains stirring, low level described in steps for importing (2) is cold while hot for the mixture that step (3) is obtained
In kettle, wherein the speed of agitator of the cold kettle of low level is that 20-300 turns/min, and liquid alkali metal ball enters hardening by cooling immediately after cold kettle,
Maintain cold kettle stirring until hot kettle completes blowing, 10 ~ 60min of this process mixing time;
(5) while maintaining stirring, the material in the cold kettle of low level is cooled to room temperature, solid base metal ball is obtained and inertia is molten
The dispersed mixture of agent;
(6) product of filtration step (5) to get arrive solid base metal ball.
The weight ratio of atent solvent and bulk alkali metal is (2-20) in the high-order hot kettle of the step (3): 1, speed of agitator
Turn/min for 100-2000.
Atent solvent and atent solvent volume ratio in the cold kettle of step (2) low level are 1:(1- in the high-order hot kettle of the step (1)
4), preferably 1:(2-3).
Bulk alkali metal is lithium metal, metallic sodium and metallic potassium in the step (3).
Solid base metal ball impregnates storage, filtering filter using atent solvent (i.e. above-mentioned atent solvent) in the step (6)
Liquid is recycled as atent solvent.
Application of the alkali metal ball in preparation naphthalene sodium, luxuriant sodium, luxuriant potassium, butyl lithium and naphthalene lithium.
In step (1) and (2), hot kettle is located at higher position, and cold kettle is located at lower position, and material can be made by weight
Power flows into cold kettle from hot kettle, so that alkali will not be advantageously implemented because using delivery pump that alkali metal droplet size is caused to change
The control of metal ball partial size.The present invention does not limit the difference in height of hot kettle and cold kettle, as long as the dispersion liquid of alkali metal ball can smoothly flow
Enter cold kettle.The present invention does not limit the internal diameter of diversion pipe between high-order hot kettle bottom discharge port and the cold kettle of low level, but water conservancy diversion
Bore should be sufficiently large, to guarantee that the dispersed mixture of liquid alkali metal ball and atent solvent can be flowed into smoothly from hot kettle
Cold kettle, such as tube inner diameter should be not less than 10mm.In the present invention, air and tide in kettle can be driven away using protective gas bubbling
Gas, avoid alkali metal occur oxidation and with the side reaction of water and be consumed, it is often more important that protective gas completely cuts off air, can be true
Protect the purity of alkali metal ball.The temperature of atent solvent should not be higher than 40 DEG C in cold kettle, may insure that hot kettle material obtains fastly in this way
Quickly cooling but, cools and solidifies liquid alkali metal ball in time, keeps uniform particle sizes, avoids occurring to gather simultaneously.In order to ensure hot from a high position
The material that kettle enters the cold kettle of low level can obtain effective temperature-reducing, and molten drop is promoted to be quickly cooled down solidification, and the cold kettle of low level is added
Atent solvent volume should at least be no less than the atent solvent volume that high-order hot kettle is added, and therefore, high-order hot kettle is added lazy
Property the ratio between solvent volume and the atent solvent volume that is added of the cold kettle of low level be 1:(1-4), preferably 1:(2-3).The cold kettle of low level
Otherwise middle solvent adding amount also should not influence metal ball preparation efficiency, and increase solvent recovery cycle load too much.
The weight ratio of step (3) atent solvent and alkali metal is (2-20): 1, preferably (4-10): 1, excessive inertia is molten
Agent will lead to the decline of alkali metal ball preparation efficiency, and if too little solvent, the alkali metal ball particle concentration of dispersion are too high, easy hair
Raw coalescence, influences the uniformity of metal ball granularity.This step speed of agitator is critically important, and revolving speed is too low, and shearing force is small, it is difficult to real
Effective dispersion of existing liquid alkali metal, the formation of unfavorable alkali metal ball, revolving speed increase, and alkali metal size droplet diameter reduces.But if
Revolving speed too high basic metal size droplet diameter is too small, and product is difficult to be collected by filtration, and can be too fast because of reaction speed in subsequent applications
And it is difficult to control reaction process.Therefore, suitable speed of agitator is that 100-2000 turns/min, preferably 200-1500 in the present invention
Turn/min, further preferably 300-900 turns/min, and specific revolving speed can control target according to alkali metal ball particle size and be subject to
It determines.
The inventive process provides the average diameter modification scope of alkali metal ball, specific granule size modification scope is
0.1-6 millimeters, and even particle size distribution, without poly- and particle.The alkali metal good dispersion of this particle size range has good flow
Property, convenient for taking, also it is conducive to subsequent using alkali metal ball as the reaction of raw material.Final products form of the invention is dispersed in inertia
Alkali metal ball in solvent, atent solvent play the role of completely cutting off air.For the ratio of alkali metal ball and solvent in product, originally
Invention is not specifically limited, but to taking conveniently, the content of atent solvent, which should reach pass through, rocks or mild agitation
The finely dispersed ratio of metal ball Effective Suspension can just be made.
The present invention provides the applications of the alkali metal ball, and alkali metal ball is especially used as to the original of chemical reaction
Material, including it is applied to preparation naphthalene sodium, luxuriant sodium, luxuriant potassium, butyl lithium, naphthalene lithium.
The beneficial effects of the present invention are:
(1) alkali metal ball preparation method provided by the invention overcomes existing one-pot heating/solvent quenching method and alkali metal often occurs
The defect and rework operation that ball gathers and bonds, alkali metal ball preparation efficiency significantly improve, and pass through the tune of hot kettle speed of agitator
The control of alkali metal spherolite diameter may be implemented in section.
(2) alkali metal ball preparation method simple process of the invention, preparation efficiency is high, and atent solvent dosage is few, is recycled
It uses, safety and environmental protection.
(3) gained alkali metal ball is uniform in size, and surface is smooth, good fluidity, good dispersion, convenient for taking, is widely used.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
The preparation of metallic sodium ball, steps are as follows:
High-order hot kettle is added in 40L(32kg) paraffin oil, agitating and heating is warming up to 125 DEG C, is bubbled with nitrogen in stirred tank bottom
15min, with the moisture and air in removing system.The cold kettle of low level is added in 60L(48kg) paraffin oil, agitating and heating is warming up to
105 DEG C, 10min is bubbled in stirred tank bottom with nitrogen and is then cooled to 35 DEG C with the moisture and air in removing system.It will
High-order hot kettle is added in the reguline metal 8kg sodium, and maintaining temperature is 125 DEG C, stirs 25min in 400 turns/min, makes metal sodium fusion simultaneously
It is dispersed into ball.It opens hot kettle bottom discharge port to import the material of hot kettle in the cold kettle of low level, while keeping cold kettle speed of agitator
For 90 turns/min, make liquid metal sodium ball hardening by cooling.About 15min, hot kettle material all import cold kettle, will be in the cold kettle of low level
Material be cooled to room temperature, excess of solvent (after collection for be recycled) is filtered to remove, then by gained metallic sodium ball and 8kg stone
Wax oil mixing is packed into pail pack.It is measured through optical microscopy, metallic sodium bulb diameter is between 1.6 ~ 1.8mm, and sodium ball is in symmetrical
Spherical, surface-brightening.
Embodiment 2
The preparation of metal potash bulb, steps are as follows:
High-order hot kettle is added in 30L(24kg) kerosene, agitating and heating is warming up to 110 DEG C, is bubbled with nitrogen in stirred tank bottom
20min, with the moisture and air in removing system.The cold kettle of low level is added in 50L(40kg) kerosene, agitating and heating is warming up to 105
DEG C, 15min, which is bubbled, in stirred tank bottom with nitrogen is then cooled to 30 DEG C with the moisture and air in removing system.By 6kg
High-order hot kettle is added in reguline metal potassium, and maintaining temperature is 110 DEG C, stirs 10min, makes metal potash fusion and be dispersed into ball.It beats
It opens hot kettle bottom discharge port to import the material of hot kettle in the cold kettle of low level, while keeping cold kettle speed of agitator is 65 turns/min, is made
Liquid metal potash bulb hardening by cooling.Material in the cold kettle of low level is cooled to room temperature, excess of solvent is filtered to remove and (is recycled after collection
Using), gained metal potash bulb is mixed with 5kg kerosene then and is packed into pail pack.It is measured through optical microscopy, metallic potassium bulb diameter
Between 2.1 ~ 2.3mm, potash bulb is in symmetrical spherical, surface-brightening.
Embodiment 3
The preparation of metallic sodium ball, steps are as follows:
High-order hot kettle is added in 20L(16kg) paraffin oil, agitating and heating is warming up to 127 DEG C, is bubbled with nitrogen in stirred tank bottom
30min, with the moisture and air in removing system.The cold kettle of low level is added in 80L(64kg) paraffin oil, agitating and heating is warming up to
120 DEG C, 30min is bubbled in stirred tank bottom with nitrogen and is then cooled to 39 DEG C with the moisture and air in removing system.It will
High-order hot kettle is added in the reguline metal 0.8kg sodium, and maintaining temperature is 127 DEG C, stirs 30min in 100 turns/min, makes metal sodium fusion
And it is dispersed into ball.It opens hot kettle bottom discharge port to import the material of hot kettle in the cold kettle of low level, while cold kettle stirring being kept to turn
Speed is 20 turns/min, makes liquid metal sodium ball hardening by cooling.About 10min, hot kettle material all imports cold kettle, by the cold kettle of low level
In material be cooled to room temperature, excess of solvent (after collection for be recycled) is filtered to remove, then by gained metallic sodium ball and 1kg
Paraffin oil mixing is packed into pail pack.It is measured through optical microscopy, metallic sodium bulb diameter is between 5.8 ~ 6mm, and sodium ball is in symmetrical
Spherical, surface-brightening.
Embodiment 4
The preparation of lithium metal ball, steps are as follows:
High-order hot kettle is added in 20L(17kg) white oil, agitating and heating is warming up to 185 DEG C, is bubbled with argon gas in stirred tank bottom
10min, with the moisture and air in removing system.The cold kettle of low level is added in 20L(17kg) white oil, agitating and heating is warming up to 110
DEG C, 10min, which is bubbled, in stirred tank bottom with argon gas is then cooled to 35 DEG C with the moisture and air in removing system.It will
High-order hot kettle is added in the reguline metal 8.5kg lithium, and maintaining temperature is 185 DEG C, stirs 5min in 2000 turns/min, melts lithium metal
And it is dispersed into ball.It opens hot kettle bottom discharge port to import the material of hot kettle in the cold kettle of low level, while cold kettle stirring being kept to turn
Speed is 300 turns/min, makes liquid metal lithium ball hardening by cooling.About 60min, hot kettle material all imports cold kettle, and low level is cold
Material in kettle is cooled to room temperature, and is filtered to remove excess of solvent (after collection for be recycled), then by gained lithium metal ball with
The mixing of 10kg white oil is packed into pail pack and is then sealed with the air in argon gas displacement bucket.It is measured through optical microscopy, lithium metal
Bulb diameter is between 0.1 ~ 0.12mm, and lithium ball is spherical in shape, surface-brightening.
Embodiment 5
The preparation of naphthalene sodium, steps are as follows:
It taking 13g naphthalene that reactor is added, 100mL tetrahydrofuran is added into reactor, simultaneously magnetic agitation is completely dissolved naphthalene to nitrogen charging,
1 gained metallic sodium ball 2.3g of embodiment is added and obtained bottle green sodium naphthalene solution in room temperature magnetic agitation 2 hours.It is golden in reactor
Belong to sodium ball to completely disappear.
Comparative example 1
One-pot heating/solvent quenching method prepares metallic sodium ball, and steps are as follows:
Stirred tank is added in 40L(32kg) paraffin oil, agitating and heating is warming up to 125 DEG C, is bubbled with nitrogen in stirred tank bottom
15min, with the moisture and air in removing system.High-order hot kettle is added in the reguline metal 8kg sodium, maintaining temperature is 125 DEG C, in
400 turns/min stirs 25min, makes metal sodium fusion and is dispersed into ball.By 60L(48kg) room temperature under conditions of maintaining stirring
Stirred tank is added in paraffin oil, makes the cooling solidification of metallic sodium ball.Material is cooled to room temperature.The above process tests 3 times, has twice
Because room temperature paraffin oil charging rate is partially slow, causes metallic sodium drop cooling not in time, generate a large amount of agglomerations, almost do not obtain sodium
Sand.Sodium sand is only once obtained, but has mixed the poly- and metallic sodium of a large amount of irregular shapes, product poor fluidity, discharging is stranded
It is difficult.
Comparative example 2
The preparation of naphthalene sodium, steps are as follows:
Embodiment 5 is repeated, wherein metallic sodium replaces the metallic sodium ball of embodiment 1 with the sodium sand of comparative example 1.Room temperature magnetic agitation 2
Hour, bottle green sodium naphthalene solution is obtained, still there is sodium sand particle residual in reactor.
Embodiment 1 to embodiment 4 the result shows that, it is high that double kettle methods of the invention prepare alkali metal ball success rate, product ball
Shape form is good, surface-brightening, epigranular, good fluidity.Traditional one-pot heating/solvent quenching it can be seen from comparative example 1
Method poor controllability, gained metal sodium sand particle shape is uneven, there is obvious poly- and phenomenon, final products flowing property is not good enough.It is right
When ratio 2 and the bright use 1 gained sodium sand of comparative example of 5 comparison table of embodiment prepare naphthalene sodium, still there is sodium sand particle in reactor
Residual illustrates that sodium sand reaction is not thorough, this is consequence caused by bulky grain sodium sand specific surface area is smaller, depletion rate is slow.Obviously,
One-pot heating/solvent is quenched method not only poor controllability, and effect is also poor when the subsequent applications of product.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of alkali metal ball, it is characterised in that steps are as follows: using double kettle method preparations, i.e. heating fusing alkali gold
The hot kettle of a high position of category and the cold kettle of low level of cooling alkali metal, wherein using atent solvent as alkali in high-order hot kettle and the cold kettle of low level
The decentralized medium of metal ball, the alkali metal mean diameter of a ball modification scope being prepared are 0.1-6mm.
2. the ball preparation method of alkali metal according to claim 1, it is characterised in that: the atent solvent include kerosene,
One of paraffin oil, diesel oil, conduction oil, white oil are a variety of.
3. the ball preparation method of alkali metal of any of claims 1 or 2, it is characterised in that specific step is as follows:
(1) atent solvent is added in high-order hot kettle, agitating and heating is warming up to above 5-30 DEG C of alkali metal fusing point, with protection gas
Body is bubbled 10-30min in stirred tank bottom;
(2) atent solvent is added in the cold kettle of low level, agitating and heating is warming up to 105-120 DEG C, with protective gas in stirred tank
Bottom is bubbled 10-30min, is then cooled to solvent temperature not higher than 40 DEG C;
(3) bulk alkali metal is added in the hot kettle of a high position of step (1), maintaining temperature is above 5-30 DEG C of alkali metal fusing point,
5-30min is stirred, alkali metal is melted and is dispersed into liquid alkali metal ball in atent solvent;
(4) while step (3) maintains stirring, the liquid alkali metal ball that step (3) is obtained is while hot described in steps for importing (2)
In the cold kettle of low level, the speed of agitator of the cold kettle of low level is that 20-300 turns/min, and liquid alkali metal ball enters cooling immediately hard after cold kettle
Change, mixing time 10-60min;
(5) while maintaining stirring, the material in the cold kettle of low level is cooled to room temperature, solid base metal ball is obtained and inertia is molten
The dispersed mixture of agent;
(6) product of filtration step (5) to get arrive solid base metal ball.
4. the preparation method of alkali metal ball according to claim 3, it is characterised in that: in the high-order hot kettle of the step (3)
The weight ratio of atent solvent and bulk alkali metal is (2-20): 1, speed of agitator is that 100-2000 turns/min.
5. the preparation method of alkali metal ball according to claim 3, it is characterised in that: in the high-order hot kettle of the step (1)
Atent solvent volume ratio is 1:(1-4 in atent solvent and the cold kettle of step (2) low level).
6. the preparation method of alkali metal ball according to claim 3, it is characterised in that: blocky alkali gold in the step (3)
Belong to is lithium metal, metallic sodium and metallic potassium.
7. the preparation method of alkali metal ball according to claim 3, it is characterised in that: the protective gas is argon gas or nitrogen
Gas.
8. the preparation method of alkali metal ball according to claim 3, it is characterised in that: solid base gold in the step (6)
Belong to ball and impregnate storage using atent solvent, filter liquor is recycled as atent solvent.
9. application of the alkali metal ball as claimed in claim 3 in preparation naphthalene sodium, luxuriant sodium, luxuriant potassium, butyl lithium and naphthalene lithium.
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CN116688867A (en) * | 2023-08-07 | 2023-09-05 | 内蒙古默锐能源材料有限公司 | Liquid metal micro quantitative feeding device and use method thereof |
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