Production device of fluoroethylene carbonate

Abstract

The utility model belongs to the technical field of lithium battery electrolyte preparation, and particularly relates to a fluoroethylene carbonate production device which comprises a chloroethylene carbonate storage tank, an anhydrous hydrogen fluoride storage tank and an antimony pentachloride storage tank, the anhydrous hydrogen fluoride storage tank is connected to the main pipeline through a second communicating pipe, and the antimony pentachloride storage tank is connected to the main pipeline through a third communicating pipe; the outlet end of the main pipeline is connected to a feed port of the tubular reactor, and a discharge port of the tubular reactor is sequentially connected with a gas-liquid separator, a crude product transfer tank, a crude product rectifying tower and a finished product rectifying tower; fluoroethylene carbonate is rectified from the tower top of the finished product rectifying tower, and the tower bottom of the finished product rectifying tower is connected with a waste tank. According to the utility model, the continuous production is realized, the yield and the utilization rate of raw materials are improved, and the production cost and the waste output are reduced.

Description

Technical Field

[0001] The utility model belongs to the technical field of lithium battery electrolyte preparation, in particular to a production device for fluoroethylene carbonate. Background Art

[0002] Fluorinated ethylene carbonate is an electrolyte additive for lithium-ion batteries. Adding it to the electrolyte can make the formed SEI film have better performance, form a tight structure layer without increasing impedance, prevent the electrolyte from further decomposing, and improve the low-temperature performance of the electrolyte. There are three main mainstream synthesis processes for fluoroethylene carbonate: 1. Chloroethylene carbonate reacts with potassium fluoride. This process has high requirements for the activity of potassium fluoride, and the utilization rate of potassium fluoride is only about 60%. The amount of solid waste generated is large, the cost of three wastes treatment is high, and the environmental pollution is large; 2. Vinyl carbonate directly reacts with fluorine gas for chlorination. Due to the strong activity and oxidizing property of fluorine gas, the yield and selectivity of this process are poor, there are more polyfluorinated products, and the production cost and waste generation are large; 3. Chloroethylene carbonate reacts with hydrogen fluoride, with low yield and low utilization rate of hydrogen fluoride, and it is difficult to achieve continuous production. Direct fluorination reaction has relatively stringent requirements on mass transfer, heat transfer, safety, etc. of the equipment and process. Due to the limitations of the equipment and process, the existing technologies have problems of complex equipment and cumbersome process to varying degrees, which in turn lead to problems such as long reaction time, low production efficiency, poor flexibility and selectivity of the process and equipment. Utility Model Content

[0003] In order to solve the problems in the above-mentioned background technology, the utility model provides a production device for fluoroethylene carbonate, which utilizes chloroethylene carbonate, anhydrous hydrogen fluoride and antimony pentachloride to prepare fluoroethylene carbonate, realizes continuous production, improves the yield and utilization rate of raw materials, and reduces production costs and waste generation.

[0004] The utility model adopts the following technical solutions:

[0005] A production device for fluoroethylene carbonate, comprising a chloroethylene carbonate storage tank, an anhydrous hydrogen fluoride storage tank and an antimony pentachloride storage tank, wherein:

[0006] The chloroethylene carbonate storage tank is connected to the main pipeline through a first connecting pipe, the anhydrous hydrogen fluoride storage tank is connected to the main pipeline through a second connecting pipe, and the antimony pentachloride storage tank is connected to the main pipeline through a third connecting pipe; the outlet end of the main pipeline is connected to the feed port of the tubular reactor, and the discharge port of the tubular reactor is sequentially connected to a gas-liquid separator, a crude product transfer tank, a crude product distillation tower, and a finished product distillation tower;

[0007] The top of the finished product distillation tower distills out fluoroethylene carbonate, and the bottom of the finished product distillation tower is connected to a waste tank.

[0008] Furthermore, the top of the gas-liquid separator is connected to the inlet end of the condenser through a fourth connecting pipe, and the condensate outlet of the condenser is connected to the main pipeline through a fifth connecting pipe.

[0009] Furthermore, the gas outlet of the condenser is connected to the bottom of the spray absorption tower through a sixth connecting pipe. The top of the spray absorption tower is provided with a plurality of downward spraying nozzles, which are connected to an external water source.

[0010] Furthermore, the top of the spray absorption tower is connected to the tail gas treatment device through a seventh connecting pipe, and the bottom of the spray absorption tower is connected to the hydrochloric acid collection tank through an eighth connecting pipe.

[0011] Furthermore, the bottom of the crude product transfer tank is connected to the crude product distillation tower through a ninth connecting pipe, and a metering pump is provided on the ninth connecting pipe.

[0012] Furthermore, a heating device and a temperature sensor are provided in the tubular reactor, and both the heating device and the temperature sensor are electrically connected to the PLC system.

[0013] Furthermore, the top of the crude product distillation tower is connected to the ethylene chlorocarbonate storage tank through a tenth connecting pipe.

[0014] Furthermore, a first feed valve is provided on the first connecting pipe, a second feed valve is provided on the second connecting pipe, and a third feed valve is provided on the third connecting pipe.

[0015] Furthermore, a first regulating valve is provided on the first connecting pipe, a second regulating valve is provided on the second connecting pipe, and a third regulating valve is provided on the third connecting pipe.

[0016] Compared with the prior art, the beneficial effects of the utility model are:

[0017] The production device structure and process of fluoroethylene carbonate of the present application are relatively simple, and fluoroethylene carbonate is prepared by using chloroethylene carbonate, anhydrous hydrogen fluoride and antimony pentachloride, with a short reaction time, realizing continuous production, improving the yield and utilization rate of raw materials, and reducing production costs and waste generation. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0019] Figure 1 It is a schematic diagram of the overall structure of the production device of the utility model;

[0020] Wherein: 1-ethylene chlorocarbonate storage tank, 2-anhydrous hydrogen fluoride storage tank, 3-antimony pentachloride storage tank, 4-first connecting pipe, 5-second connecting pipe, 6-third connecting pipe, 7-main pipeline, 8-tubular reactor, 9-gas-liquid separator, 10-crude product transfer tank, 11-crude product distillation tower, 12-finished product distillation tower, 13-fourth connecting pipe, 14-condenser, 15-fifth connecting pipe, 16-sixth connecting pipe, 17-spray absorption tower, 18-seventh connecting pipe, 19-eighth connecting pipe, 20-ninth connecting pipe, 21-tenth connecting pipe, 22-first feed valve, 23-second feed valve, 24-third feed valve. DETAILED DESCRIPTION

[0021] The following will be combined with the drawings in the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work belong to the protection scope of the utility model.

[0022] The following is combined with Figure 1 And specific embodiments describe the present invention in detail.

[0023] like Figure 1 As shown, the utility model provides a production device for fluoroethylene carbonate, comprising a chloroethylene carbonate storage tank 1, an anhydrous hydrogen fluoride storage tank 2 and an antimony pentachloride storage tank 3, wherein: the chloroethylene carbonate storage tank 1 is connected to a main pipeline 7 through a first connecting pipe 4, the anhydrous hydrogen fluoride storage tank 2 is connected to the main pipeline 7 through a second connecting pipe 5, and the antimony pentachloride storage tank 3 is connected to the main pipeline 7 through a third connecting pipe 6; the outlet end of the main pipeline 7 is connected to the feed port of a tubular reactor 8, that is, chloroethylene carbonate, anhydrous hydrogen fluoride and antimony pentachloride are mixed and enter the tubular reactor 8 together to react to prepare fluoroethylene carbonate, and the discharge port of the tubular reactor 8 is connected to a gas-liquid separator 9, a crude product transfer tank 10, a crude product distillation tower 11 and a finished product distillation tower 12 in sequence, and through the above process, the top of the finished product distillation tower 12 is distilled to produce electronic grade fluoroethylene carbonate, and the bottom of the finished product distillation tower 12 is connected to a waste tank, so that the kettle residue in the finished product distillation tower 12 enters the waste tank.

[0024] The structure and process of the production device in the embodiment of the present application are relatively simple. Vinyl fluoride carbonate is prepared by using vinyl chlorinated carbonate, anhydrous hydrogen fluoride and antimony pentachloride. The reaction time is short, continuous production is achieved, the yield and raw material utilization rate are improved, and the production cost and waste generation are reduced.

[0025] Specifically, the top of the gas-liquid separator 9 of this embodiment is connected to the inlet end of the condenser 14 through the fourth connecting pipe 13, and the condensate outlet of the condenser 14 is connected to the main pipeline 7 through the fifth connecting pipe 15. The gas-liquid separator 9 is mainly used for gas-liquid phase separation of the outlet material of the tubular reactor 8. The liquid phase is unreacted chloroethylene carbonate and the target product fluoroethylene carbonate, and the gas phase is by-product hydrogen chloride, unreacted anhydrous hydrogen fluoride and antimony pentachloride. The gas phase is introduced into the condenser 14 through the fourth connecting pipe 13, and the anhydrous hydrogen fluoride and antimony pentachloride are condensed into liquid and enter the main pipeline 7 through the fifth connecting pipe 15 to participate in the next reaction. The arrangement of the gas-liquid separator 9 and the condenser 14 realizes the recycling of anhydrous hydrogen fluoride and antimony pentachloride.

[0026] Specifically, the gas outlet of the condenser 14 is connected to the bottom of the spray absorption tower 17 through the sixth connecting pipe 16. The top of the spray absorption tower 17 is provided with a plurality of downward spraying nozzles, which are connected to an external water source. The hydrogen chloride in the gas phase has a low boiling point and is not condensed. The gas phase hydrogen chloride is introduced into the spray absorption tower 17 through the sixth connecting pipe 16. Water is sprayed downward through the nozzle on the spray absorption tower 17 to absorb the gas phase hydrogen chloride as a by-product hydrochloric acid, which is then transported to the hydrochloric acid collection tank through the eighth connecting pipe 19. The top of the spray absorption tower 17 is connected to the tail gas treatment device through the seventh connecting pipe 18, and the generated tail gas is introduced into the tail gas treatment device.

[0027] Specifically, the bottom of the crude product transfer tank 10 in this embodiment is connected to the crude product distillation tower 11 through a ninth connecting pipe 20 , and a metering pump is provided on the ninth connecting pipe 20 , and the flow rate is accurately adjusted by the metering pump.

[0028] Specifically, a heating device and a temperature sensor are provided in the tubular reactor 8 in this embodiment, and both the heating device and the temperature sensor are electrically connected to the PLC system. When the temperature in the tubular reactor 8 reaches above 90°, the material is introduced therein for reaction.

[0029] Specifically, the top of the crude product distillation tower 11 in this embodiment is connected to the ethylene chlorocarbonate storage tank 1 through the tenth connecting pipe 21, and the unreacted ethylene chlorocarbonate is recovered into the ethylene chlorocarbonate storage tank 1 for repeated use.

[0030] Specifically, in this embodiment, the first connecting pipe 4 is provided with a first feed valve 22 and a first regulating valve, the second connecting pipe 5 is provided with a second feed valve 23 and a second regulating valve, and the third connecting pipe 6 is provided with a third feed valve 23 and a third regulating valve. The feed valve is used to open the corresponding connecting pipe, and the regulating valve is used to adjust the ratio of the raw materials.

[0031] The utility model realizes the recycling of anhydrous hydrogen fluoride and antimony pentachloride through the gas-liquid separator 9 and the condenser 14. At the same time, the unreacted chloroethylene carbonate is recycled through the connection of the crude product distillation tower 11 and the chloroethylene carbonate storage tank 1, which greatly improves the utilization rate of raw materials, has a high product yield, and reduces waste, thereby realizing the continuous production of fluoroethylene carbonate.

[0032] The working principle of the utility model is briefly described below: first, the raw materials are transported to the chloroethylene carbonate storage tank 1, the anhydrous hydrogen fluoride storage tank 2 and the antimony pentachloride storage tank 3 respectively, then, the heating device of the tubular reactor 8 is started, when the temperature in the tubular reactor 8 reaches above 90°, the first feed valve 22, the second feed valve 23 and the third feed valve 24 are opened, and the raw materials enter the tubular reactor 8 to start the reaction. After a certain reaction time, the outlet material of the tubular reactor 8 enters the gas-liquid separator 9 for gas-liquid phase separation, and the gas phase is condensed by the condenser 14, so that the anhydrous hydrogen fluoride and antimony pentachloride are condensed into liquid and enter the main pipeline 7 again through the fifth connecting pipe 15. The non-condensable gaseous hydrogen chloride is introduced into the bottom of the spray absorption tower 17, and the top of the spray absorption tower 17 is sprayed with tap water to prepare by-product hydrochloric acid, and the gas at the top of the spray absorption tower 17 is sent to the tail gas treatment device for alkali spray absorption; the liquid discharge of the gas-liquid separator 9 enters the crude product transfer tank 10 for temporary storage, and is transported to the crude product distillation tower 11 through a metering pump, and the chloroethylene carbonate recovered by the crude product distillation tower 11 is transported to the chloroethylene carbonate storage tank 1 for standby use, and the crude fluoroethylene carbonate enters the finished product distillation tower 12, and finally electronic grade fluoroethylene carbonate is extracted at the top of the finished product distillation tower 12, and the kettle residue at the bottom is transported to the waste tank as hazardous waste.

[0033] The utility model is further described above with the help of specific embodiments, but it should be understood that the specific description here should not be construed as limiting the essence and scope of the utility model. Various modifications made to the above embodiments by ordinary technicians in this field after reading this specification are all within the scope of protection of the utility model.

Claims

1. A production device for fluoroethylene carbonate, characterized in that: Including ethylene chloride storage tanks, anhydrous hydrogen fluoride storage tanks and antimony pentachloride storage tanks, of which: The ethylene chloride storage tank is connected to the main pipeline through a first connecting pipe, the anhydrous hydrogen fluoride storage tank is connected to the main pipeline through a second connecting pipe, and the antimony pentachloride storage tank is connected to the main pipeline through a third connecting pipe; the outlet end of the main pipeline is connected to the feed port of the tubular reactor, and the outlet of the tubular reactor is sequentially connected to a gas-liquid separator, a crude product transfer tank, a crude product distillation tower, and a finished product distillation tower; The top of the finished product distillation tower distills out fluoroethylene carbonate, and the bottom of the finished product distillation tower is connected to a waste tank.

2. The production device of fluoroethylene carbonate according to claim 1, characterized in that: The top of the gas-liquid separator is connected to the inlet end of the condenser through a fourth connecting pipe, and the condensate outlet of the condenser is connected to the main pipeline through a fifth connecting pipe.

3. The production device of fluoroethylene carbonate according to claim 2, characterized in that: The gas outlet of the condenser is connected to the bottom of the spray absorption tower through a sixth connecting pipe. The top of the spray absorption tower is provided with a plurality of downward spraying nozzles, and the nozzles are connected to an external water source.

4. The production device of fluoroethylene carbonate according to claim 3, characterized in that: The top of the spray absorption tower is connected to the tail gas treatment device through the seventh connecting pipe, and the bottom of the spray absorption tower is connected to the hydrochloric acid collection tank through the eighth connecting pipe.

5. The production device of fluoroethylene carbonate according to claim 1, characterized in that: The bottom of the crude product transfer tank is connected to the crude product distillation tower via a ninth connecting pipe, and a metering pump is disposed on the ninth connecting pipe.

6. The production device of fluoroethylene carbonate according to claim 1, characterized in that: A heating device and a temperature sensor are arranged in the tubular reactor, and both the heating device and the temperature sensor are electrically connected to the PLC system.

7. The production device of fluoroethylene carbonate according to claim 1, characterized in that: The top of the crude product distillation tower is connected to the ethylene chlorocarbonate storage tank through a tenth connecting pipe.

8. The production device of fluoroethylene carbonate according to claim 1, characterized in that: The first connecting pipe is provided with a first feed valve, the second connecting pipe is provided with a second feed valve, and the third connecting pipe is provided with a third feed valve.

9. The production device of fluoroethylene carbonate according to claim 1, characterized in that: The first communicating pipe is provided with a first regulating valve, the second communicating pipe is provided with a second regulating valve, and the third communicating pipe is provided with a third regulating valve.

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