Synthesis device of diethyl fluorophosphate

Abstract

The utility model discloses a synthesis device of diethyl fluorophosphate. The synthesis device comprises a reaction kettle, a three-in-one dryer and a rectifying tower, wherein the reaction kettle is respectively connected with a diethyl carbonate solvent pipeline, a diethyl chlorophosphate feeding pipeline and a potassium fluoride feeding pipeline, and a discharge hole of the reaction kettle is connected with the three-in-one dryer; the filtrate dried by the three-in-one dryer is conveyed to a rectifying tower, and a diethyl fluorophosphate product is extracted from a product extraction port after rectification of the rectifying tower; the device disclosed by the utility model is suitable for large-scale industrial application, and the extracted diethyl fluorophosphate product is high in purity and few in byproducts.

Description

Technical Field

[0001] The utility model belongs to the field of preparation of lithium ion battery electrolytes, and particularly relates to a synthesis device for diethyl fluorophosphate. Background Art

[0002] As a new type of green energy, lithium ion batteries are widely used in many fields due to their advantages such as high working voltage, environmental protection and pollution-free, light weight, and no memory effect. With the strong support of the country for the new energy vehicle industry, the market demand for lithium ion batteries is also increasing. When the negative electrode material is first lithiated, a solid electrolyte interface (SEI) film will be formed. The SEI film will undergo dynamic rupture and recombination during the cycling process, resulting in film thickening and continuous decomposition of the electrolyte, leading to a decrease in battery capacity or even failure.

[0003] It has been confirmed by research that diethyl fluorophosphate (CAS No.: 358-74-7), as an electrolyte additive, can first undergo redox reaction on the electrode surface prior to the electrolyte, generating a stable and dense protective film to avoid continuous decomposition of the electrolyte on the surface of the positive electrode material, thereby improving the cycling performance of lithium batteries. However, at present, there is only a laboratory-level synthesis device for diethyl fluorophosphate in China, and there is a lack of industrial synthesis devices.

[0004] Therefore, the applicant hopes to propose a synthesis device for diethyl fluorophosphate that can be applied industrially to solve the above technical problems. Summary of the Invention

[0005] In view of this, the purpose of the utility model is to provide a synthesis device for diethyl fluorophosphate, which is suitable for large-scale industrial application, and the produced diethyl fluorophosphate product has high purity and few by-products.

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

[0007] A synthesis device for diethyl fluorophosphate includes a reaction kettle, a three-in-one dryer, and a rectification column; wherein, the reaction kettle is respectively connected to a carbonic acid diethyl ester solvent pipeline, a diethyl chlorophosphate incoming material pipeline, and a potassium fluoride incoming material pipeline, and the discharge port of the reaction kettle is connected to the three-in-one dryer; the filtrate after being dried by the three-in-one dryer is transported to the rectification column, and the diethyl fluorophosphate product is taken out from the product extraction port after the rectification of the rectification column.

[0008] Preferably, an intermediate tank is provided on the filtrate pipeline between the three-in-one dryer and the rectification column.

[0009] Preferably, a filtrate output end and a filter residue discharge end are respectively provided at the bottom of the three-in-one dryer, and a gas-phase output end is provided at the upper end of the three-in-one dryer; wherein, the gas-phase output end is connected to a drying filter, and the output end of the drying filter is connected to a condenser for condensation treatment; the output end of the condenser is connected to the intermediate tank to achieve a recovery effect.

[0010] Preferably, the filter residue of the drying filter is discharged externally through a filter residue outlet end; a refrigerant outlet and a refrigerant inlet are respectively provided at the upper and lower ends of the condenser.

[0011] Preferably, the refrigerant of the condenser is 5°C cold water.

[0012] Preferably, the diethyl carbonate solvent pipeline, the diethyl chlorophosphate feed pipeline, and the potassium fluoride feed pipeline are respectively connected to the upper end of the reaction kettle, and the discharge port is located at the bottom of the reaction kettle.

[0013] Preferably, a jacket is provided on the outer periphery of the reaction kettle; wherein, a heat medium outlet and a heat medium inlet are respectively provided at the upper and lower ends of the jacket.

[0014] Preferably, the heat medium of the jacket is 80°C hot water, which is used to control the internal temperature of the reaction kettle within the expected temperature range.

[0015] Preferably, the distillation column is a vacuum distillation column; wherein, the product extraction port is arranged on the side wall of the distillation column and is connected to a side-draw product pipeline.

[0016] Preferably, the top of the distillation column is connected to a solvent recovery pipeline, and its bottom is connected to a residual liquid discharge pipeline.

[0017] It should be noted that the synthesis process mechanism adopted by the synthesis device of diethyl fluorophosphate is: potassium fluoride and diethyl chlorophosphate are used for synthesis reaction in a solvent environment, and this synthesis process belongs to the common knowledge of those skilled in the art.

[0018] The present invention provides a synthesis device of diethyl fluorophosphate mainly composed of a reaction kettle A, a three-in-one dryer B, and a distillation column F, which is suitable for large-scale industrial application, and the produced diethyl fluorophosphate product has high purity and few by-products. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic structural diagram of the synthesis device of diethyl fluorophosphate under the specific embodiment of the present invention.

[0020] Reference numerals: Reactor A, Diethyl carbonate solvent pipeline a1, Diethyl chlorophosphate feed pipeline a2, Potassium fluoride feed pipeline a3, Discharge port a4, Tail gas treatment pipeline a5, Triad dryer B, Dry filter C, Condenser D, Intermediate tank E, Rectifying column F, Product extraction port f0, Side draw product pipeline f1, Solvent recovery pipeline f2, Residual liquid discharge pipeline f3. Detailed implementation mode

[0021] This embodiment provides a synthesis device for diethyl fluorophosphate, including a reactor, a triad dryer and a rectifying column; wherein, the reactor is respectively connected with a diethyl carbonate solvent pipeline, a diethyl chlorophosphate feed pipeline and a potassium fluoride feed pipeline, and the discharge port of the reactor is connected with the triad dryer; the filtrate after being dried by the triad dryer is transported to the rectifying column, and the diethyl fluorophosphate product is extracted from the product extraction port after the rectifying effect of the rectifying column.

[0022] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0023] Please refer to Figure 1 As shown, a synthesis device for diethyl fluorophosphate includes a reactor A, a triad dryer B and a rectifying column F; wherein, the reactor A is respectively connected with a diethyl carbonate solvent pipeline a1, a diethyl chlorophosphate feed pipeline a2 and a potassium fluoride feed pipeline a3, and the discharge port a4 of the reactor A is connected with the triad dryer B; the filtrate after being dried by the triad dryer B is transported to the rectifying column F, and the diethyl fluorophosphate product is extracted from the product extraction port f0 after the rectifying effect of the rectifying column F;

[0024] Preferably, in order to control the internal temperature of the reactor A within the expected temperature range and improve the synthesis efficiency, in this embodiment, a jacket is provided on the outer periphery of the reactor A; wherein, a heat medium outlet and a heat medium inlet are respectively provided at the upper and lower ends of the jacket; specifically preferably, in this embodiment, the heat medium of the jacket is 80°C hot water, which is used to control the internal temperature of the reactor A within the expected temperature range (50 - 55°C); further, in actual implementation, the heat medium inlet is for the input of 80°C hot water, and the heat medium outlet is for the output of 70°C hot water.

[0025] Preferably, for the convenience of pipeline layout, in this embodiment, the diethyl carbonate solvent pipeline a1, the diethyl chlorophosphate incoming material pipeline a2, and the potassium fluoride incoming material pipeline a3 are respectively connected to the upper end of the reaction kettle A, and the discharge port a4 is located at the bottom of the reaction kettle A; Further preferably, a tail gas treatment pipeline a5 is also connected to the upper end of the reaction kettle A.

[0026] To improve the synthesis efficiency, specifically preferably, in this embodiment, a stirring device is provided in the reaction kettle A. The applicant's recommended optimal raw material ratio is n(diethyl chlorophosphate):n(potassium fluoride)=1:1.5, and the usage amount of diethyl carbonate is 3 times the mass of potassium fluoride; Of course, those skilled in the art can make conventional selections based on common knowledge, and this part of the content is not considered as the innovative content of this application.

[0027] Preferably, to further improve the product yield, in this embodiment, an intermediate tank E is provided on the filtrate pipeline between the triple dryer B and the distillation column F; The bottom of the triple dryer B is respectively provided with a filtrate output end and a filter residue discharge end, and a gas phase output end is provided at the upper end of the triple dryer B; Among them, the gas phase output end is connected to the drying filter C, and the output end of the drying filter C is connected to the condenser D for condensation treatment; The output end of the condenser D is connected to the intermediate tank E to achieve the recycling effect.

[0028] Preferably, in this embodiment, the filter residue of the drying filter C is discharged externally through the filter residue outlet end; The upper and lower ends of the condenser D are respectively provided with a refrigerant outlet and a refrigerant inlet; Among them, specifically preferably, in this embodiment, the refrigerant of the condenser D is 5°C cold water. Further, in actual implementation, the refrigerant inlet is for the input of 5°C cold water, and the refrigerant outlet is for the output of 10°C cold water.

[0029] Preferably, in this embodiment, the distillation column F is a vacuum distillation column; Among them, the product extraction port f0 is arranged on the side wall of the distillation column F and is connected to the side extraction product pipeline f1; Further preferably, in this embodiment, the top of the distillation column F is connected to the solvent recovery pipeline f2, and its bottom is connected to the residual liquid discharge pipeline f3.

[0030] To further illustrate the implementation process of this embodiment, the applicant also proposes the following specific embodiments:

[0031] 260 kg of diethyl carbonate is added to reactor A from the tank farm through a flow meter, and the stirring device of reactor A is started; diethyl chlorophosphate and potassium fluoride are respectively added to reactor A through the diethyl chlorophosphate feed pipeline a2 and the potassium fluoride feed pipeline a3, and the reaction is carried out while maintaining stirring; hot water is introduced into the jacket of the reactor to control the temperature in reactor A at 50 °C; reactor A is connected to the relief main pipe through the tail gas treatment pipeline a5; after the reaction is qualified, the synthesized material enters the three-in-one dryer B through the discharge port a4 for negative pressure drying and filtration, the filter residue is collected and treated through the filter residue discharge end, the liquid phase is directly introduced into the intermediate tank E, and at the same time, the gas phase is filtered through the drying filter C and condensed by the condenser D and recovered into the intermediate tank E; then, the intermediate tank E feeds the rectification column F at a feed rate of 52 kg / h, and negative pressure rectification is carried out through the rectification column F. Among them, the solvent is recovered and reused through the solvent recovery pipeline f2, the bottom of the tower is a small amount of by-products, which are discharged through the bottom-connected residual liquid discharge pipeline f3, and the side-drawn product of the side-drawn product pipeline f1 is a diethyl fluorophosphate product with a purity of more than 99.8%.

[0032] For those skilled in the art, it is obvious that the present utility model is not limited to the details of the above 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, from any point of view, the embodiments should be regarded as exemplary and non-restrictive. 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 included in the present utility model. Any reference signs in the claims should not be regarded as limiting the claimed rights involved.

[0033] 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. This narrative way of the 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 diethyl fluorophosphate, characterized in that, It includes a reactor (A), a three-in-one dryer (B) and a rectification column (F); among them, The reactor (A) is respectively connected to a diethyl carbonate solvent pipeline (a1), a diethyl chlorophosphate feed pipeline (a2) and a potassium fluoride feed pipeline (a3), and the discharge port (a4) of the reactor (A) is connected to the three-in-one dryer (B); the filtrate after being dried by the three-in-one dryer (B) is transported to the rectification column (F), and the diethyl fluorophosphate product is taken out from the product extraction port after the rectification of the rectification column (F).

2. The synthesis device of diethyl fluorophosphate according to claim 1, characterized in that, An intermediate tank (E) is provided on the filtrate pipeline between the three-in-one dryer (B) and the rectification column (F).

3. The synthesis device of diethyl fluorophosphate according to claim 2, characterized in that, The bottom of the three-in-one dryer (B) is respectively provided with a filtrate output end and a filter residue discharge end, and the upper end of the three-in-one dryer (B) is provided with a gas phase output end; among them, This gas phase output end is connected to a drying filter (C), and the output end of the drying filter (C) is connected to a condenser (D) for condensation treatment; The output end of the condenser (D) is connected to the intermediate tank (E) to achieve a recycling effect.

4. The synthesis device of diethyl fluorophosphate according to claim 3, characterized in that The filter residue of the drying filter (C) is discharged externally through the filter residue outlet end; the upper and lower ends of the condenser (D) are respectively provided with a refrigerant outlet and a refrigerant inlet.

5. The synthesis device of diethyl fluorophosphate according to claim 4, characterized in that, The refrigerant of the condenser (D) uses cold water at 5°C.

6. The synthesis device of diethyl fluorophosphate according to claim 1, characterized in that, The diethyl carbonate solvent pipeline (a1), the diethyl chlorophosphate feed pipeline (a2) and the potassium fluoride feed pipeline (a3) are respectively connected to the upper end of the reactor (A), and the discharge port (a4) is located at the bottom of the reactor (A).

7. The synthesis device of diethyl fluorophosphate according to claim 1 or 5, characterized in that A jacket is provided on the outer periphery of the reactor (A); among them, the upper and lower ends of the jacket are respectively provided with a heat medium outlet and a heat medium inlet.

8. The synthesis device of diethyl fluorophosphate according to claim 7, characterized in that, The heat medium of the jacket uses hot water at 80°C to control the internal temperature of the reactor (A) within the expected temperature range.

9. The synthesis device of diethyl fluorophosphate according to claim 1, wherein The rectification column (F) is a negative pressure rectification column; among them, the product extraction port (f0) is arranged on the side wall of the rectification column (F) and is connected to a side extraction product pipeline (f1).

10. The synthesis device of diethyl fluorophosphate according to claim 9, characterized in that, The top of the rectification column (F) is connected to a solvent recovery pipeline (f2), and its bottom is connected to a residue discharge pipeline (f3).

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