Synthesizer of sodium difluoro (oxalato) borate

Abstract

The utility model discloses a synthesis device of sodium difluoro (oxalato) borate, comprising a reaction kettle which is respectively connected with a sodium tetrafluoroborate raw material tank, an oxalic acid raw material tank, a dimethyl carbonate raw material tank and a silicon tetrachloride dropwise adding tank; wherein a discharging port of the reaction kettle is connected into a crystallization kettle, a solid material treated by the crystallization kettle is connected into a dryer, and a discharging end of the dryer conveys a dried sodium difluoro (oxalato) borate finished product to a product storage tank; the industrial synthesis device for sodium difluoro (oxalato) borate changes the current situation that an industrial synthesis device for sodium difluoro (oxalato) borate is lacked in the prior art, promotes large-scale industrial synthesis application of sodium difluoro (oxalato) borate, is simple in structure and easy to implement, saves manpower and material resources, and effectively saves production cost.

Description

Technical Field

[0001] The utility model belongs to the field of electrolyte preparation, and particularly relates to a synthesis device for sodium difluoro(oxalato)borate. Background Technique

[0002] In recent years, with the rapid development of China's battery industry, electrochemical energy storage has also developed rapidly following the trend. The market demand is increasing. When using batteries for energy storage, sodium-ion batteries are the best choice, and sodium-ion batteries are cheaper than lithium-ion batteries. The supply and demand relationship of sodium resources is stable, and the price fluctuates little. Sodium has a very high content in the earth's crust, and its crustal abundance is more than 1000 times that of lithium. The advantages of sodium-ion batteries are stable electrochemical performance and better safety. Sodium and lithium are both elements in the first main group, and the characteristic is that the monovalent positive ions have better stability and higher solution conductivity. In contrast, sodium has a higher atomic number, larger atomic and ionic radii, lower electronegativity and first ionization energy, which makes sodium ions more stable and has higher ionic conductivity.

[0003] The stability and high conductivity of sodium ions also bring better fast charging and low-temperature operation performance to sodium-ion batteries. The higher molar ionic conductivity of sodium ions makes the charging efficiency higher; at the same time, the higher stability of sodium ions enables sodium-ion batteries to be charged at a higher power without easily causing battery damage or safety accidents; in addition, the internal resistance of sodium-ion batteries is slightly higher during operation. If a short circuit occurs, the heat generation is smaller, the temperature rise is lower, and the accident rate is reduced. The stability of sodium ions also makes it more difficult for sodium to precipitate at low temperatures, giving it better low-temperature safety than lithium-ion batteries; it can enhance the resistance of energy storage power stations to temperature interference and improve the stability of their operation. Sodium-ion battery additives can effectively improve battery performance, inhibit the decline of the initial energy of the battery, increase the initial discharge capacity, reduce the battery swelling after high-temperature storage, improve the charge-discharge performance of the battery, and the cycle times. Sodium difluoro(oxalato)borate can be used as an additive for sodium-ion battery electrolytes and can improve the high-temperature performance of sodium-ion batteries.

[0004] Currently, the publicly disclosed patents and papers are basically about the laboratory-level synthesis technology of sodium difluoro(oxalato)borate by Guan Hongyu, and there is no device technology for industrialization. Moreover, the existing preparation technologies have defects such as low purity, low yield, and many by-products; therefore, the applicant hopes to develop a synthesis device for sodium difluoro(oxalato)borate suitable for industrial-scale applications. Summary of the Invention

[0005] In view of this, the purpose of the utility model is to provide a synthesis device for sodium difluoro(oxalato)borate, which changes the current situation that there is a lack of industrial synthesis devices for sodium difluoro(oxalato)borate in the existing technology, promotes the large-scale industrial synthesis application of sodium difluoro(oxalato)borate, and has a simple structure, is easy to implement, saves manpower and material resources, and effectively saves production costs.

[0006] The technical solution adopted by the utility model is as follows:

[0007] A synthesis device for sodium difluoro(oxalato)borate includes a reaction kettle, which is respectively connected to a sodium tetrafluoroborate raw material tank, an oxalic acid raw material tank, a dimethyl carbonate raw material tank and a silicon tetrachloride dropping tank; wherein, the discharge port of the reaction kettle is connected to a crystallization kettle, and the solid material after being processed by the crystallization kettle is connected to a dryer, and the discharge end of the dryer transports the dried sodium difluoro(oxalato)borate finished product to a product storage tank.

[0008] Preferably, the reaction kettle is provided with a stirrer.

[0009] Preferably, a reaction kettle jacket is provided on the outer periphery of the reaction kettle, a heat medium inlet is provided at the lower end of the reaction kettle jacket, and a heat medium outlet is provided at the upper end thereof.

[0010] Preferably, a solvent raw material transfer pump is provided between the dimethyl carbonate raw material tank and the reaction kettle.

[0011] Preferably, a crystallization kettle jacket is provided on the outer periphery of the crystallization kettle, a refrigerant inlet is provided at the lower end of the crystallization kettle jacket, and a refrigerant outlet is provided at the upper end thereof.

[0012] Preferably, the crystallization kettle is a crystallization and filtration integrated crystallization kettle; wherein, the solid material after being filtered by the crystallization kettle is connected to a dryer.

[0013] Preferably, the filtrate after being filtered by the crystallization kettle is transported to the reaction kettle through a solvent recovery tank.

[0014] Preferably, a mother liquor reuse pump is provided between the solvent recovery tank and the reaction kettle.

[0015] Preferably, the dryer adopts a double-cone dryer.

[0016] Preferably, a heat medium inlet and a heat medium outlet are respectively provided on both sides of the double-cone dryer.

[0017] When this application is in operation, sodium tetrafluoroborate and oxalic acid are respectively transported to the reaction kettle through the sodium tetrafluoroborate raw material tank and the oxalic acid raw material tank. Dimethyl carbonate is transported to the reaction kettle through the dimethyl carbonate raw material tank and stirred. Silicon tetrachloride is added dropwise to the reaction kettle through the silicon tetrachloride dropping tank. After the reaction is completed, the reaction solution is transported to the crystallization kettle for crystallization. The solid material after filtration is added to the dryer for drying. After drying, the obtained sodium difluorooxalate finished product enters the product storage tank. The filtrate after crystallization and filtration enters the solvent recovery tank, and then the mother liquor is transported to the reaction kettle through the mother liquor recycling pump for recycling. This utility model changes the current situation that the existing technology lacks an industrial synthesis device for sodium difluorooxalate, promotes the large-scale industrial synthesis application of sodium difluorooxalate, has a simple structure, is easy to implement, saves manpower and material resources, and effectively reduces production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is a schematic structural diagram of the synthesis device for sodium difluorooxalate under the specific embodiment of this application;

[0019] Reference numerals: Sodium tetrafluoroborate raw material tank V101, oxalic acid raw material tank V102, dimethyl carbonate raw material tank V103, silicon tetrachloride dropping tank V104, reaction kettle R101, crystallization kettle R102, dryer D101, solvent recovery tank V105, product storage tank V106, solvent raw material transfer pump P101, mother liquor recycling pump P102, hot medium inlet HWS, hot medium outlet HWR, cold medium inlet CWS, cold medium outlet CWR. SPECIFIC EMBODIMENTS

[0020] This embodiment provides a synthesis device for sodium difluorooxalate, including a reaction kettle, and the reaction kettle is respectively connected to a sodium tetrafluoroborate raw material tank, an oxalic acid raw material tank, a dimethyl carbonate raw material tank, and a silicon tetrachloride dropping tank; wherein, the discharge port of the reaction kettle is connected to the crystallization kettle, and the solid material after being processed by the crystallization kettle is connected to the dryer, and the discharge end of the dryer transports the dried sodium difluorooxalate finished product to the product storage tank.

[0021] In order to enable those skilled in the art to better understand the technical solutions in this utility model, the following will clearly and completely describe the technical solutions in the embodiments of this utility model with reference to the accompanying drawings in the embodiments of this utility model. Obviously, the described embodiments are only a part of the embodiments of this utility model, rather than all the embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those of ordinary skill in the art without making creative efforts shall fall within the protection scope of this utility model.

[0022] Please refer to Figure 1As shown in the figure, a synthesis device for sodium difluoro(oxalato)borate includes a reaction kettle R101, which is respectively connected to a sodium tetrafluoroborate raw material tank V101, an oxalic acid raw material tank V102, a dimethyl carbonate raw material tank V103 and a silicon tetrachloride dropping tank V104; among them, the discharge port of the reaction kettle R101 is connected to a crystallization kettle R102, and the solid material processed by the crystallization kettle R102 is connected to a dryer D101, and the discharge end of the dryer D101 transports the dried sodium difluoro(oxalato)borate finished product to a product storage tank V106.

[0023] Preferably, in order to facilitate the full reaction of sodium difluoro(oxalato)borate, in this embodiment, the reaction kettle R101 is provided with a stirrer M for stirring and mixing the raw materials located in the reaction kettle R101;

[0024] Preferably, in this embodiment, the outer periphery of the reaction kettle R101 is provided with a reaction kettle jacket, the lower end of the reaction kettle jacket is provided with a heat medium inlet HWS, and the upper end is provided with a heat medium outlet HWR; further preferably, in this embodiment, the temperature of the reaction kettle R101 is controlled at a constant temperature of 28 - 35 °C through the heat medium in the reaction kettle jacket, and specifically preferably controlled at 30 °C;

[0025] Preferably, in order to achieve the efficient transportation of the dimethyl carbonate raw material, in this embodiment, a solvent raw material transfer pump P101 is provided between the dimethyl carbonate raw material tank V103 and the reaction kettle R101;

[0026] Preferably, in this embodiment, the outer periphery of the crystallization kettle R102 is provided with a crystallization kettle jacket, the lower end of the crystallization kettle jacket is provided with a refrigerant inlet CWS, and the upper end is provided with a refrigerant outlet CWR; further preferably, in this embodiment, the temperature of the crystallization kettle R102 is controlled at 10 - 20 °C through the refrigerant in the crystallization kettle jacket, which is conducive to an efficient crystallization effect; further preferably, in this embodiment, the crystallization kettle R102 is a crystallization and filtration integrated crystallization kettle; among them, the solid material filtered by the crystallization kettle R102 is connected to the dryer D101.

[0027] Preferably, in order to facilitate the recycling of the solvent, in this embodiment, the filtrate filtered by the crystallization kettle R102 is transported to the reaction kettle R101 through a solvent recovery tank V105; further preferably, in order to achieve the efficient recovery of the mother liquor, in this embodiment, a mother liquor reuse pump P102 is provided between the solvent recovery tank V105 and the reaction kettle R101.

[0028] Preferably, in the present embodiment, the dryer D101 is a double-cone dryer; among them, preferably, the two sides of the double-cone dryer (with a dryer jacket provided on its outer periphery) are respectively provided with a heat medium inlet HWS and a heat medium return HWR, and the temperature of the dryer D101 is controlled at 90-100 degrees Celsius through the heat medium in the dryer jacket, which is beneficial to the drying effect of sodium difluoroborate oxalate.

[0029] To further illustrate the implementation effect of this embodiment, the applicant further provides the following specific implementation process:

[0030] The reaction kettle R101 is used for the synthesis of sodium difluoroborate oxalate. The synthesis process includes: sodium tetrafluoroborate and oxalic acid are respectively fed into the reaction kettle R101 from the raw material storage tanks (i.e., the sodium tetrafluoroborate raw material tank V101 and the oxalic acid raw material tank V102), and then dimethyl carbonate is added through the dimethyl carbonate raw material tank V103 and stirred evenly. The reaction kettle R101 is controlled to stir at a constant temperature of 30 degrees Celsius through the heat medium. Silicon tetrachloride is added dropwise to the reaction kettle R101 through the silicon tetrachloride dropping tank V104 for reaction. The dropping time is controlled within 1-2 hours, and the temperature is controlled at 30-40 degrees Celsius. Sodium difluoroborate oxalate is generated by the reaction. After the dropping is completed, it is kept warm for 1 hour, and the remaining amount of the raw materials is detected. After the reaction is qualified, it enters the crystallization and filtration integrated crystallization kettle R102. The temperature of the crystallization kettle R102 is controlled to drop to 10-20 degrees Celsius through the refrigerant for cooling crystallization, filtration, and the solvent is recovered and enters the solvent recovery tank V105, and the mother liquor reuse pump P102 realizes reusing. The filter cake enters the double-cone dryer D101 for drying, and the temperature is controlled at a constant temperature of 90-95 degrees Celsius through the heat medium for vacuum drying. After drying, the finished product of sodium difluoroborate oxalate enters the product storage tank V106. After detection, the purity of the finished product of sodium difluoroborate oxalate is above 99.7%, and there are few by-products.

[0031] For those skilled in the art, it is obvious that the present utility model is not limited to the details of the above-mentioned exemplary embodiments, and without departing from the spirit or basic characteristics of the present utility model, the present utility model can be implemented in other specific forms. Therefore, in any regard, the embodiments should be regarded as exemplary and non-limiting. The scope of the present utility model is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be encompassed within the present utility model. Any reference signs in the claims should not be regarded as limiting the claims involved.

[0032] In addition, it should be understood that although this specification is described according to the embodiments, not every embodiment only contains an independent technical solution. The narrative way of this specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A synthesis device for sodium difluorooxalatoborate, characterized in that: The invention comprises a reactor (R101), wherein the reactor (R101) is respectively connected to a sodium tetrafluoroborate raw material tank (V101), an oxalic acid raw material tank (V102), a dimethyl carbonate raw material tank (V103) and a silicon tetrachloride dropping tank (V104); wherein the discharge port of the reactor (R101) is connected to a crystallization reactor (R102), the solid material treated by the crystallization reactor (R102) is connected to a dryer (D101), and the discharge end of the dryer (D101) transports the dried sodium difluorooxalatoborate finished product to a product storage tank (V106).

2. The synthesis device of sodium difluorooxalatoborate according to claim 1, characterized in that: The reactor (R101) is provided with a stirrer (M).

3. The synthesis device of sodium difluorooxalatoborate according to claim 1, characterized in that: A reactor jacket is provided on the outer periphery of the reactor (R101), a heat medium source (HWS) is provided at the lower end of the reactor jacket, and a heat medium return (HWR) is provided at the upper end thereof.

4. The synthesis device of sodium difluorooxalatoborate according to claim 1, characterized in that: A solvent raw material delivery pump (P101) is provided between the dimethyl carbonate raw material tank (V103) and the reaction kettle (R101).

5. The synthesis device of sodium difluorooxalatoborate according to claim 1, characterized in that: The outer periphery of the crystallization kettle (R102) is provided with a crystallization kettle jacket, the lower end of the crystallization kettle jacket is provided with a refrigerant source (CWS), and the upper end thereof is provided with a refrigerant return (CWR).

6. The synthesis device of sodium difluorooxalatoborate according to claim 1, characterized in that: The crystallization kettle (R102) is a two-in-one crystallization and filtration kettle; wherein the solid material filtered by the crystallization kettle (R102) is connected to the dryer (D101).

7. The synthesis device of sodium difluorooxalatoborate according to claim 6, characterized in that: The filtrate filtered through the crystallization kettle (R102) is transported to the reaction kettle (R101) via the solvent recovery tank (V105).

8. The synthesis device of sodium difluorooxalatoborate according to claim 7, characterized in that: A mother liquor recycling pump (P102) is provided between the solvent recovery tank (V105) and the reaction kettle (R101).

9. The synthesis device of sodium difluorooxalatoborate according to claim 1, characterized in that: The dryer (D101) is a double cone dryer.

10. The synthesis device of sodium difluorooxalatoborate according to claim 9, characterized in that: The two sides of the double cone dryer are respectively provided with a heat medium supply (HWS) and a heat medium return (HWR).

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