CN104282954B - Prepare method and the device thereof of melting electrolyte - Google Patents
Prepare method and the device thereof of melting electrolyte Download PDFInfo
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- CN104282954B CN104282954B CN201310285930.1A CN201310285930A CN104282954B CN 104282954 B CN104282954 B CN 104282954B CN 201310285930 A CN201310285930 A CN 201310285930A CN 104282954 B CN104282954 B CN 104282954B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention relates to prepare method and the device thereof of melting electrolyte.This prepares the method for melting electrolyte, including: reaction zone will be injected into from different directions through pretreated various raw materials so that mixing after the various raw materials formation convection current of injection with the ratio of regulation；In described reaction zone, raw material mixed through convection current is heated and be reacted to give required melting electrolyte；And the whole process of described method is carried out under the reaction environment atmosphere of regulation.The method and related device thereof have time-consuming less, the uniformity high and can the feature such as preparation continuously.
Description
Technical field
The present invention relates to the preparation of electrolyte, especially, relate to a kind of method preparing melting electrolyte and device thereof.
Background technology
Along with the economic and development of society, extensive energy storage, in terms of effectively utilizing the load balancing of regenerative resource and electrical network, particularly with big city or rural area, has the most urgent demand.The energy storage technology of various types of physics and chemistry is studied, but weigh the standard that promising energy storage technology has multinomial needs to consider, such as useful life, energy and power density, self-discharge rate, the maturity etc. of impact, cycle efficieny, Capacity Cost, high rate performance and technology on environment.
In all of chemical energy storage technology, due to its high theoretical specific energy, (such as, ZEBRA battery is 790 to the reversible sode cell of middle temperature including sodium-nickel chloride battery (also known as ZEBRA battery)
Wh kg-1), the long-life, high transformation efficiency, good cyclical stability and high rate performance and the characteristic such as low preparation and maintenance cost, become one the most promising large scale static energy storage technology.
Additionally, sode cell uses β, "-aluminium oxide ceramics is as solid electrolyte, NaAlCl4Etc. middle temperature sodium ion conductor as the second phase (liquid phase) electrolyte, good stability, and it is a kind of omniseal battery, discharges without any gas in running, thus environmentally friendly, there are good practicality and generalization.
But, the large-scale commercial problem still facing some reality of sode cell needs to solve, such as in sode cell, the efficiently preparation of the second phase electrolyte is to affect battery cost and a key factor of actual application.The second phase electrolyte in sode cell, with NaAlCl4As a example by, it is common that in vacuum or protective atmosphere, at a temperature of about 200 DEG C, gained is synthesized with certain proportion by anhydrous sodium chloride and alchlor.One typical example is 50.3mol% alchlor and 49.7mol% sodium chloride salt-mixture to be loaded in glass tube, vacuumizes sealing.Temperature is controlled at about 200 DEG C, drive material containing glass tube to move and carry out zone refining, make reaction uniformly (" Rare Metals Materials and engineering ", 1994,23(6), 32-35).Whole zone refining process takes around two time-of-weeks.Such synthetic method efficiency is low, the longest, it is difficult to serialization.
At present the newest synthetic technology include machinery back-and-forth method and extrusion molding etc. (such as, United States Patent (USP) US6,824,702 and United States Patent (USP) US6,767,665), but these methods are required on motor consuming many energy, and not enough to the control power of prepared atmosphere environment.
Therefore, in the urgent need to develop a kind of simple, efficiently, low cost, can the method for the melting electrolyte of the second phase electrolyte in the preparation such as sodium electrode implemented of scale.
Summary of the invention
In view of the above, the technical problem to be solved be to provide a kind of method preparing melting electrolyte and device, the method and related device thereof have time-consuming less, the uniformity high and can the feature such as preparation continuously.
In order to solve above-mentioned technical problem, according to an aspect of the present invention, provide a kind of method preparing melting electrolyte, including: reaction zone will be injected into from different directions through pretreated various raw materials so that mixing after the various raw materials formation convection current of injection with the ratio of regulation；In described reaction zone, raw material mixed through convection current is heated and be reacted to give required melting electrolyte；And the whole process of described method is carried out under the reaction environment atmosphere of regulation.
According to the present invention, the various raw materials needed for melting electrolyte will be prepared after pretreatment, it is injected into reaction zone from different directions so that the various raw materials of injection mix after forming convection current with the ratio of regulation, the various raw materials sprayed in reaction zone can be made to mix by the mixing of this convection type, obtain the product of pure phase, and then carry out again heating with the required melting electrolyte of synthesis.And the method preparing melting electrolyte of the present invention is simple, cost is relatively low, and the selectivity for raw material is strong, additionally, be also equipped with time-consuming few and can the feature such as preparation continuously.It is applicable to fused salt and mixture several samples thereof that preparation need to synthesize under specific atmospheric conditions.
Also, in the present invention, described melting electrolyte can be the second phase electrolyte in sode cell, and described sode cell includes negative pole that metallic sodium makes and the positive pole that metal halide is made.Preferably, described sode cell includes sodium-nickel chloride battery, sodium-iron chloride battery or sodium-zinc chloride batteries.
According to the present invention, this method preparing melting electrolyte especially can be effectively applied to the second phase electrolyte preparing in sode cell.Thus, can simple by the present invention, efficiently, low cost, the second phase electrolyte can prepared to scale in sode cell, thus advantageously reduce sode cell cost so that it is there is the basis of extensive commercialization.
Further, described second phase can be selected from liquid phase or the solid phase possessing mobility.This second phase is selected from liquid phase or possesses the solid phase of mobility, the preferably solid phase of good fluidity, can improve the ion in positive electrode or electronic conductivity.
Also, in the present invention, described melting electrolyte can be sodium ion conductor fused salt and mixture thereof or sodium ion and electron mixed conductor.According to the present invention it is possible to provide ion or the quick conduction pathway of electronics.
Also, in the present invention, described raw material can be to be the form of solid-state, liquid or gaseous state, and described pretreatment can include various raw materials carrying out ball milling, air blast respectively, heating or make mist；Thus it is injected into described reaction zone from different directions with the form of particle mist, drop or steam respectively through described pretreated various raw materials.
According to the present invention, by various raw materials being carried out respectively ball milling, air blast, heating or make the pretreatment of mist, can become possess undersized raw material by various Feedstock treating, such as solid particle, drop or steam etc., such that it is able to be conducive to making various raw material spray in subsequent handling, and raw material spurts into reaction zone with undersized form and make reaction rate increase, thus reduce reaction time consumption further.
Also, in the present invention, described injection can include any one in steam injection, single point injection, multi-point injection, bank injection, sequence-injection and ECI electronic control injection.
According to the present invention, above-mentioned various different spray regime can be used effectively will to be injected into reaction zone from different directions through pretreated various raw materials, it is applied widely.
Also, in the present invention, the temperature range of described reaction zone heating is 100-1000 DEG C.
According to the present invention, the temperature range of reaction zone can be the temperature range that reaction zone material can bear, and in the present invention, the temperature range of reaction zone heating is 100-1000 DEG C, depending on the synthesis temperature needed for prepared product.
Preferably, can be heated by heating tape, heating using microwave, Resistant heating, Elema heating or Si-Mo rod heating described reaction zone is heated.
Above-mentioned various different mode of heating can be used effectively to heat raw material mixed through convection current in described reaction zone and be reacted to give required melting electrolyte, it is applied widely.
Also, in the present invention, the reaction environment atmosphere of described regulation can be air, oxygen, vacuum, hydrogen or inert atmosphere.
According to the present invention, the whole process control of this method preparing melting electrolyte is carried out under air, oxygen, vacuum, hydrogen or inert atmosphere, to be conducive to the preparation of this melting electrolyte, can be different according to required raw material and corresponding reaction condition.
Preferably, described inert atmosphere uses argon gas, nitrogen, argon hydrogen gaseous mixture or nitrogen and hydrogen mixture.
In accordance with the present invention, it is preferred that the whole process control of this method preparing melting electrolyte is carried out under an inert atmosphere, in particular by argon gas, nitrogen, argon hydrogen gaseous mixture or the inert gas of nitrogen and hydrogen mixture.With this, it is more beneficial for the preparation of this melting electrolyte.
According to a further aspect in the invention, it is provided that a kind of device for implementing the aforementioned method preparing melting electrolyte, including: with regulation ratio be separately added into the multiple feed unit through pretreated various raw materials；The multiple injection units being respectively communicated with the plurality of feed unit；The reaction member connected with the plurality of injection unit；The discharging unit connected with described reaction member；And the control climate unit that the overall reaction environment atmosphere of described device is controlled；Wherein, the various raw materials that the plurality of injection unit is received are injected in described reaction member mixing after forming convection current from different directions, and heat raw material mixed through convection current in described reaction member and be reacted to give required melting electrolyte.
According to the present invention, the various raw materials received by multiple injection units are injected in reaction member mixing after forming convection current from different directions, the various raw materials sprayed in reaction member can be made to mix, obtain the product of pure phase, and then carry out again heating with the required melting electrolyte of synthesis.And the apparatus structure preparing melting electrolyte of the present invention is simple, manufacturing cost is relatively low, and the selectivity for raw material is strong.Additionally, use this device be also equipped with time-consuming few and can the feature such as preparation continuously, such as due to the reaction member in this device can Reusability, product can be continuously available.It addition, this reaction member strong adaptability, it is adaptable to prepare the fused salt and mixture several samples thereof that need to synthesize under special atmosphere and temperature conditions, especially can be effectively applied to the second phase electrolyte preparing in sode cell.And the working service of this reaction member is convenient.From the foregoing, it will be observed that this device has extensive commercial possibility.
Also, in the present invention, described injection unit can include any one in steam injection, single point injection, multi-point injection, bank injection, sequence-injection and ECI electronic control injection system.
According to the present invention, above-mentioned various different spraying system can be used effectively will to be injected into reaction member from different directions through pretreated various raw materials, it is applied widely.
Also, in the present invention, described control climate unit can include the vavuum pump being connected respectively, and the inert gas supply source being connected with the plurality of feed unit and the plurality of injection unit respectively with the plurality of feed unit.
According to the present invention, by the vacuum action of vavuum pump, and the inert gas supply source being connected with multiple feed unit and multiple injection unit, can effectively the entirety of this device be controlled under the reaction environment atmosphere of regulation.
According to following detailed description of the invention and with reference to accompanying drawing, the above-mentioned and other objects, features and advantages of the present invention will become apparent from.
Accompanying drawing explanation
Fig. 1 shows the structural representation of an embodiment of the device for implementing the method preparing melting electrolyte according to the present invention；
Fig. 2 is according to the NaAlCl of synthesis in the embodiment 1 of the method preparing melting electrolyte of the present invention4X-ray diffractogram.
Detailed description of the invention
The method preparing melting electrolyte according to the present invention and device thereof is described in detail below in conjunction with drawings and Examples.
The present inventor proposes a kind of method preparing melting electrolyte and device thereof have passed through extensively after in-depth study.The method and implement the device of the method have time-consuming less, convection type and can the feature such as preparation continuously, it is applicable to fused salt and the preparation of mixture thereof that need to synthesize under special atmosphere and temperature conditions, especially can be effectively applied to prepare the second phase electrolyte in sode cell.
In a first aspect of the present invention, it is provided that a kind of method preparing melting electrolyte, including: reaction zone will be injected into from different directions through pretreated various raw materials so that mixing after the various raw materials formation convection current of injection with the ratio of regulation；In described reaction zone, raw material mixed through convection current is heated and be reacted to give required melting electrolyte；And the whole process of described method is carried out under the reaction environment atmosphere of regulation.The various raw materials sprayed in reaction zone can be made to mix by the mixing of this convection type, obtain the product of pure phase, and then carry out again heating with the required melting electrolyte of synthesis.
The method is simple, and cost is relatively low, and the selectivity for raw material is strong, is also equipped with time-consuming few and can the feature such as preparation continuously.Especially can be effectively applied to the second phase electrolyte preparing in sode cell.This sode cell can be such as to include negative pole that metallic sodium makes and the sode cell of the positive pole that metal halide is made.Preferably, this sode cell can include sodium-nickel chloride battery, sodium-iron chloride battery or sodium-zinc chloride batteries.And, the second phase can be selected from liquid phase or the solid phase of good fluidity.
From the foregoing, it will be observed that employing this method, simple, efficient, low cost, the second phase electrolyte can prepared to scale in sode cell, thus advantageously reduce sode cell cost so that it is there is extensive commercial basis.But the present invention is not limited to this, it is possible to being applicable to fused salt and the preparation of mixture thereof that need to synthesize under special atmosphere and temperature conditions, therefore the method range is extensive.Such as, prepared melting electrolyte can be sodium ion conductor fused salt and mixture thereof or sodium ion and electron mixed conductor etc., it is adaptable to the electrolyte of the second phase electrolyte in sode cell.
The concrete steps of the method preparing melting electrolyte according to the present invention described further below.
First, to pre-processing respectively for preparing the various raw materials needed for melting electrolyte, this raw material can be to be the form of solid-state, liquid or gaseous state, depending on the kind of raw material and ratio regard the reaction equation prepared.And this process includes the different material that is directed to above-mentioned solid-state, liquid or gaseous state, carry out ball milling, air blast the most respectively, heat or make mist, thus can become possess undersized raw material by various Feedstock treating, such as solid particle, drop or steam etc..
Then by the various raw materials of above-mentioned particle mist, drop or vapor form through pretreatment respectively to be injected into reaction zone from different directions so that the various raw materials of injection are formed after convection current mixes.Raw material is spurted into reaction zone with undersized form and reaction rate is increased, thus reduces reaction time consumption further.And the mixing of this convection type can make the various raw materials sprayed in reaction zone mix, obtain the product of pure phase.
Additionally, in this step, this injection can include any one in steam injection, single point injection, multi-point injection, bank injection, sequence-injection and ECI electronic control injection.Using above-mentioned various different spray regime effectively will be injected into reaction zone from different directions through pretreated various raw materials, it is applied widely.
Then, in reaction zone, raw material mixed through convection current is heated and be reacted to give required melting electrolyte.In this step, can be heated by heating tape, heating using microwave, Resistant heating, Elema heating or Si-Mo rod heating reaction zone is heated, it is applied widely.
Wherein, the temperature range of reaction zone can be the temperature range that reaction zone material can bear, and in the present invention, the temperature range of reaction zone heating is 100-1000 DEG C, depending on the synthesis temperature needed for prepared product.
Finally, the whole process control of the method is carried out under the reaction environment atmosphere of regulation, such as, can be air, oxygen, vacuum, hydrogen or inert atmosphere.The most under an inert atmosphere, the preparation of this melting electrolyte it is more beneficial for.This inert atmosphere can be argon gas, nitrogen, argon hydrogen gaseous mixture or nitrogen and hydrogen mixture.
Fig. 1 shows the structural representation of an embodiment of the device for implementing the aforementioned method preparing melting electrolyte according to a further aspect in the invention.Device shown in this Fig. 1 includes: being separately added into the multiple feed unit 1 through pretreated various raw materials with the ratio of regulation, in the embodiment shown in fig. 1, this feed unit 1 is hopper 1.This device also includes the multiple injection units 3 being respectively communicated with the plurality of feed unit 1；The reaction member 4 connected with the plurality of injection unit 3；And the control climate unit that the overall reaction environment atmosphere of this device is controlled.The various raw materials that multiple injection units 3 are received are injected in reaction member 4 from different directions to mix after forming convection current, and heat raw material mixed through convection current in reaction member 4 and be reacted to give required melting electrolyte.
According to the present invention, it is injected into from different directions in reaction member 4 mixing after forming convection current from the various raw materials that each feed unit 1 receives by it by multiple injection units 3, the various raw materials sprayed in reaction member 4 can be made to mix, obtain the product of pure phase, and then again this reaction member 4 is heated with the required melting electrolyte of synthesis.
In different embodiments of the invention, this injection unit 3 can include vapor injection system, single point injection system or multipoint injection system respectively.
Additionally, referring also to Fig. 1, above-mentioned reaction member 4 can carry out heating by heater 5 so that melting electrolyte needed for Material synthesis in this reaction member 4.This heater 5 can heat or the form of Si-Mo rod heating to use heating tape heating, heating using microwave, Resistant heating, Elema, but the present invention is not limited to this.And the temperature range of reaction member 4 heating is 100-1000 DEG C, depending on the temperature that synthesis temperature needed for prepared product and the material of reaction member 4 can bear.
Also, in the embodiment shown in Fig. 1, control climate unit can include respectively with multiple feed unit 1, vavuum pump 6 that i.e. hopper 1 is connected, and the inert gas supply source being connected with multiple feed unit 1 and multiple injection unit 3 respectively.By the vacuum action of vavuum pump, and the inert gas supply source being connected with multiple feed unit 1 and multiple injection unit 3, can effectively the entirety of this device be controlled under the reaction environment atmosphere of required regulation.
Additionally, also as it is shown in figure 1, this device also includes the collecting region 9 connected with above-mentioned reaction member 4, for collecting the product after coming from the synthesis in reaction member 4, i.e. required melting electrolyte.It addition, this device also includes vavuum pump 6 and the inert gas supply source being connected with collecting region 9, control under the reaction environment atmosphere of regulation with the operating process by whole device.This product collected by collecting region 9 can be discharged by discharging opening 10.Also, as it is shown in figure 1, in an embodiment of the present invention, valve 2,7,8 to be opened/closed also can be included between each feed unit 1 and each spraying system 3, between reaction member 4 and collecting region 9 and/or between collecting region 9 and discharging opening 10 respectively.
The above-mentioned of the present invention prepares the apparatus structure of melting electrolyte simply, and manufacturing cost is relatively low, and the selectivity for raw material is strong.Additionally, use this device be also equipped with time-consuming few and can the feature such as preparation continuously, such as due to the reaction member in this device can Reusability, product can be continuously available.It addition, this reaction member strong adaptability, it is adaptable to prepare the fused salt and mixture several samples thereof that need to synthesize under special atmosphere and temperature conditions, especially can be effectively applied to the second phase electrolyte preparing in sode cell.And the working service of this reaction member is convenient.From the foregoing, it will be observed that this device has extensive commercial possibility.
Employing methods and apparatus of the present invention described further below prepares each embodiment of melting electrolyte, and is all to illustrate as a example by the embodiment of the device of the method preparing melting electrolyte for enforcement using the present invention shown in Fig. 1.It should be appreciated, however, that these embodiments are merely to illustrate the present invention and are not meant to limit the scope of the invention.The test method of unreceipted actual conditions in the following example, generally according to normal condition, or according to the condition proposed by manufacturer.Except as otherwise noted, all of percentage and number are by weight.
Embodiment
1
It is in argon gas atmosphere in making whole device before using this device for the first time.By the anhydrous NaCl after ball milling and anhydrous AlCl3As raw material, feeding respectively to two hoppers 1 with the mol ratio of 1:1, close valve 2, hopper 1 vacuumizes through vavuum pump 6, and fills argon gas to keep the ar gas environment of hopper 1 by inert gas supply source.Open valve 2, make raw material enter the single point injection system as injection unit 3, drive through argon gas at this and be injected into reaction zone, i.e. reaction member 4, at 210 DEG C, react 72h.After having reacted, open valve 7, reacted sample collection is entered collecting region 9, close valve 7, open valve 8, after discharging opening 10 takes out sample, close valve 8, collecting region 9 is vacuumized by vavuum pump 6, and fill argon gas so that collecting region 9 keeps ar gas environment by inert gas supply source.
Fig. 2 is the NaAlCl of synthesis in the present embodiment 14X-ray diffractogram.The all corresponding NaAlCl of all sharp diffraction peak in figure4(standard card valut is numbered: 23-0649), therefore can be synthesized the sample of pure phase by assembly of the invention.
Embodiment
2
It is in argon gas atmosphere in making whole device before using this device for the first time.By the anhydrous AlCl after the anhydrous NaCl after ball milling and preheating3Melt, as raw material, feeds respectively to two hoppers 1 with the mol ratio of 1:1, closes valve 2, and hopper 1 vacuumizes through vavuum pump 6, and fills argon gas to keep the ar gas environment of hopper 1 by inert gas supply source.
Remaining content is all with described in embodiment 1.
The present embodiment obtains the NaAlCl of pure phase4。
Embodiment
3
It is in argon gas atmosphere in making whole device before using this device for the first time.By the anhydrous AlCl after the anhydrous NaCl after ball milling and heating sublimation3Steam, as raw material, feeds respectively to two hoppers 1 with the mol ratio of 1:1, closes valve 2, and hopper 1 vacuumizes through vavuum pump 6, and fills argon gas to keep the ar gas environment of hopper 1 by inert gas supply source.
Remaining content is all with described in embodiment 1.
The present embodiment obtains the NaAlCl of pure phase4。
Embodiment
4
It is in nitrogen atmosphere in making whole device before using this device for the first time.By the anhydrous NaCl after ball milling and anhydrous AlCl3As raw material, feeding respectively to two hoppers 1 with the mol ratio of 1:1, close valve 2, hopper 1 vacuumizes through vavuum pump 6, and fills nitrogen to keep the nitrogen environment of hopper 1 by inert gas supply source.
Remaining content is all with described in embodiment 1.
The present embodiment obtains the NaAlCl of pure phase4。
Embodiment
5
It is in argon gas atmosphere in making whole device before using this device for the first time.By the anhydrous NaCl after ball milling and anhydrous AlCl3As raw material, feeding respectively to two hoppers 1 with the mol ratio of 1:1, close valve 2, hopper 1 vacuumizes through vavuum pump 6, and fills argon gas to keep the ar gas environment of hopper 1 by inert gas supply source.Open valve 2, make raw material enter single point injection system, drive through argon gas and be injected into reaction zone, at 300 DEG C, react 48h.
Remaining content is all with described in embodiment 1.
The present embodiment obtains the NaAlCl of pure phase4。
Embodiment
6
It is in argon gas atmosphere in making whole device before using this device for the first time.By the anhydrous NaCl after ball milling and anhydrous AlCl3As raw material, feeding respectively to two hoppers 1 with the mol ratio of 1:1, close valve 2, hopper 1 vacuumizes through vavuum pump 6, and fills argon gas to keep the ar gas environment of hopper 1 by inert gas supply source.Open valve 2, make raw material enter 3 spraying systems as injection unit 3, drive through argon gas at this and be injected into reaction zone, at 210 DEG C, react 72h.
Remaining content is all with described in embodiment 1.
The present embodiment obtains the NaAlCl of pure phase4。
Embodiment
7
It is in argon gas atmosphere in making whole device before using this device for the first time.By the anhydrous NaCl after ball milling, NaBr and anhydrous AlCl3As raw material, feeding respectively to three hoppers 1 with the mol ratio of 0.75:0.25:1.15, close valve 2, hopper 1 vacuumizes through vavuum pump 6, and fills argon gas to keep the ar gas environment of hopper 1 by inert gas supply source.
Remaining content is all with described in embodiment 1.
The present embodiment obtains uniform sode cell ternary the second phase electrolyte NaBr-NaAlCl4。
Embodiment
8
It is in argon gas atmosphere in making whole device before using this device for the first time.By the anhydrous NaCl after ball milling, LiCl and anhydrous AlCl3As raw material, feeding respectively to three hoppers 1 with the mol ratio of 0.75:0.25:1.15, close valve 2, hopper 1 vacuumizes through vavuum pump 6, and fills argon gas to keep the ar gas environment of hopper 1 by inert gas supply source.
Remaining content is all with described in embodiment 1.
The present embodiment obtains uniform sode cell ternary the second phase electrolyte LiCl-NaAlCl4。
Under the objective without departing from the essential characteristic of the present invention, the present invention can be presented as various ways, therefore the embodiment in the present invention is to be illustrative rather than definitive thereof, owing to the scope of the present invention is defined by the claims rather than limited by specification, and all changes in the scope defined in claim, or the full scope of equivalents of its scope defined that fall are understood to be included in the invention.
Claims (13)
1. the method preparing melting electrolyte, it is characterised in that including:
Reaction zone will be injected into from different directions through pretreated various raw materials so that mixing after the various raw materials formation convection current of injection with the ratio of regulation；
In described reaction zone, raw material mixed through convection current is heated and be reacted to give required melting electrolyte；And
The whole process of described method is carried out under the reaction environment atmosphere of regulation.
Method the most according to claim 1, it is characterised in that described melting electrolyte is the second phase electrolyte in sode cell, described sode cell includes negative pole that metallic sodium makes and the positive pole that metal halide is made.
Method the most according to claim 2, it is characterised in that described sode cell includes sodium-nickel chloride battery, sodium-iron chloride battery or sodium-zinc chloride batteries, and described second phase is selected from liquid phase or possesses the solid phase of mobility.
Method the most according to claim 2, it is characterised in that described melting electrolyte is sodium ion conductor fused salt and mixture thereof or sodium ion and electron mixed conductor.
Method the most according to claim 1, it is characterised in that described raw material is the form of solid-state, liquid or gaseous state, described pretreatment includes various raw materials carrying out ball milling, air blast respectively, heating or make mist；Thus it is injected into described reaction zone from different directions with the form of particle mist, drop or steam respectively through described pretreated various raw materials.
Method the most according to claim 1, it is characterised in that described injection includes any one in steam injection, single point injection, multi-point injection, bank injection, sequence-injection and ECI electronic control injection.
Method the most according to claim 1, it is characterised in that the temperature range of described reaction zone heating is 100-1000 DEG C.
Method the most according to claim 7, it is characterised in that by heating tape heating, heating using microwave, Resistant heating, Elema heats or described reaction zone is heated by Si-Mo rod heating.
Method the most according to claim 1, it is characterised in that the reaction environment atmosphere of described regulation is air, oxygen, vacuum, hydrogen or inert atmosphere.
Method the most according to claim 9, it is characterised in that described inert atmosphere uses argon gas, nitrogen, argon hydrogen gaseous mixture or nitrogen and hydrogen mixture.
11. 1 kinds for implementing the device according to the method preparing melting electrolyte according to any one of aforementioned claim 1 to 10, it is characterised in that including:
It is separately added into the multiple feed unit through pretreated various raw materials with the ratio of regulation；
The multiple injection units being respectively communicated with the plurality of feed unit；
The reaction member connected with the plurality of injection unit；
The discharging unit connected with described reaction member；And
The control climate unit that the overall reaction environment atmosphere of described device is controlled；
Wherein, the various raw materials that the plurality of injection unit is received are injected in described reaction member mixing after forming convection current from different directions, and heat raw material mixed through convection current in described reaction member and be reacted to give required melting electrolyte.
12. devices according to claim 11, it is characterised in that described injection unit includes any one in vapor injection system, single point injection system, multipoint injection system, bank injection system, sequencial jet system and ECI electronic control injection system.
13. devices according to claim 11, it is characterised in that described control climate unit includes the vavuum pump being connected respectively, and the inert gas supply source being connected with the plurality of feed unit and the plurality of injection unit respectively with the plurality of feed unit.
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