Production device of lithium bis (fluorosulfonyl) imide

Abstract

The utility model discloses a production device of lithium bis (fluorosulfonyl) imide. The production device comprises a first reaction kettle, a second reaction kettle and a third reaction kettle which are sequentially connected in series, a sulfuryl chloride feeding pipe and a sulfuryl fluoride discharging pipe are arranged at the top of the first reaction kettle, the bottom of the first reaction kettle is connected with a first filter, the first filter is respectively connected with a potassium chloride storage tank and the first reaction kettle, and sulfuryl fluoride is connected with a second reaction kettle; the top of the second reaction kettle is provided with an ammonia feeding pipe and connected with a gas holder, and the bottom of the second reaction kettle is connected with a second filter which is respectively connected with the third reaction kettle and a calcium fluoride storage tank; the top of the third reaction kettle is connected with a second reaction kettle, the bottom of the third reaction kettle is connected with a third filter, and the third filter is respectively connected with a lithium fluoride storage tank and a subsequent purifying and drying device of the lithium bis (fluorosulfonyl) imide; each of the first reaction kettle, the second reaction kettle and the third reaction kettle is provided with a stirring device and a temperature control device. The method is simple to operate, safe, environment-friendly, free of emission of three wastes, free of pollution to the environment and suitable for large-scale production.

Description

Technical Field

[0001] The utility model relates to a production device for lithium bis(fluorosulfonyl)imide, belonging to the technical field of chemical industry. Background Art

[0002] Electrolyte lithium salts, as new energy storage materials for lithium-ion batteries, have been widely used in the electronics field. Lithium bis(fluorosulfonyl)imide has good thermal stability, chemical stability, long service life, high safety and environmental friendliness, and is considered to be a new generation of lithium-ion battery electrolyte with very promising prospects. In the conventional process for producing lithium bis(fluorosulfonyl)imide, a non-protonic polar solvent is used, with sulfuryl fluoride and ammonia as raw materials and triethylamine as a catalyst, to carry out a condensation reaction to prepare bis(fluorosulfonyl)imide triethylamine salt, which is then reacted with lithium hydroxide to prepare lithium bis(fluorosulfonyl)imide. However, the post-processing step of this process produces a large amount of wastewater, the recovery of triethylamine is difficult, and the product loss is relatively high. When triethylamine is replaced by silicon dioxide and calcium oxide, the above problems are solved. However, the solid waste and waste gas generated in the reaction are directly discharged, which not only wastes resources but also pollutes the environment and needs further solution. Utility Model Content

[0003] The technical problem to be solved by the utility model is to provide a production device for lithium bis(fluorosulfonyl)imide products which can ensure good production operation and does not discharge "three wastes".

[0004] In order to solve the above technical problems, the utility model discloses a production device for lithium bis(fluorosulfonyl)imide, which comprises a No. 1 reactor, a No. 2 reactor and a No. 3 reactor connected in series in sequence; a sulfuryl chloride feed pipe and a sulfuryl fluoride discharge pipe are arranged on the top of the No. 1 reactor, and a discharge port at the bottom is connected to the No. 1 filter through a pipeline, the No. 1 filter is respectively connected to a potassium chloride storage tank and is connected to the middle and lower part of the No. 1 reactor through a solvent sleeve pipe, and the sulfuryl fluoride discharge pipe is connected to the lower part of the No. 2 reactor; an ammonia feed pipe is arranged on the top of the No. 2 reactor. The pipe is connected to the gas cabinet through the silicon tetrafluoride discharge pipe, the bottom is connected to the No. 2 filter through a pipe, and the No. 2 filter is connected to the top of the No. 3 reactor and the calcium fluoride storage tank through pipes; the top of the No. 3 reactor is connected to the top of the No. 2 reactor through an ammonia return pipe, and the bottom of the No. 3 reactor is connected to the No. 3 filter through a pipe, and the No. 3 filter is connected to the lithium fluoride storage tank and the subsequent purification and drying device of lithium bis(fluorosulfonyl)imide; the No. 1 reactor, the No. 2 reactor and the No. 3 reactor are all equipped with a stirring device and a temperature control device.

[0005] Furthermore, the ammonia return pipe is connected to the ammonia feed pipe or is arranged in parallel with the ammonia feed pipe.

[0006] Furthermore, a solvent and potassium fluoride are placed in the No. 1 reactor; a solvent, silicon dioxide and calcium oxide are placed in the No. 2 reactor; and a solvent and lithium salt are placed in the No. 3 reactor.

[0007] Furthermore, the filter No. 1, filter No. 2 and filter No. 3 are all closed filters.

[0008] Furthermore, flow meters are provided on the sulfuryl chloride feed pipe, the sulfuryl fluoride discharge pipe, the ammonia feed pipe, the ammonia return pipe and the silicon tetrafluoride discharge pipe.

[0009] Furthermore, the temperature control device includes a reactor jacket, which is connected to a steam system or a cooling brine system.

[0010] Furthermore, the heating temperature of the steam system is 20 to 100°C, and the cooling temperature of the cooling brine system is -25 to 0°C.

[0011] Furthermore, the feed port of the sulfuryl chloride feed pipe is a dropping port.

[0012] The present invention utilizes the properties of the reactants and products produced during the preparation of lithium bis(fluorosulfonyl)imide. Three reactors are installed, each with a corresponding filter to separate the substances. This effectively ensures the smooth operation of the preparation reaction, allows the solvent used in the production process to be recycled and reused, and sells and reuses the solid waste and waste gas generated during the reaction as co-products. The preparation device of the present invention is simple to operate, safe and environmentally friendly, eliminates the "three wastes" (waste, waste gas, and waste gas) emissions, and is environmentally friendly. It is suitable for large-scale production and achieves the goal of industrialized co-production of waste-to-wealth. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 This is a structural diagram of an embodiment of the present invention;

[0014] Figure 2 This is a structural diagram of another embodiment method of the present invention.

[0015] Numbers in the figure: 1-Reactor No. 1; 1.1-Stirring paddle; 2-Reactor No. 2; 2.1-Stirring paddle; 3-Reactor No. 3; 3.1-Stirring paddle; 4-Filter No. 1; 5-Filter No. 2; 6-Filter No. 3; 7-Gas cabinet; 8-Solvent casing pipe; 9-Ammonia return pipe; 10-Potassium chloride storage tank; 11-Calcium fluoride storage tank; 12-Lithium fluoride storage tank. DETAILED DESCRIPTION

[0016] The present invention will be further explained below in conjunction with the following examples. The following examples are only used to illustrate the present invention, but are not intended to limit the scope of the present invention.

[0017] Example 1

[0018] like Figure 1 、 Figure 2 As shown, the production device of lithium bis(fluorosulfonyl)imide of the present invention includes a No. 1 reactor 1, a No. 2 reactor 2 and a No. 3 reactor 3 connected in series, and each reactor is equipped with a stirring device, a temperature control device and a filter.

[0019] Specifically, a sulfuryl chloride feed pipe with a flowmeter is provided on the top of the No. 1 reactor 1, and the bottom discharge port is connected to the No. 1 filter 4 through a pipeline. The No. 1 filter 4 is respectively connected to the potassium chloride storage tank 10 through a pipeline and to the middle and lower part of the No. 1 reactor 1 through a solvent sleeve pipe 8. The top of the No. 1 reactor 1 is also connected to the lower part of the No. 2 reactor 2 through a sulfuryl fluoride discharge pipe, and a flowmeter is provided on the sulfuryl fluoride discharge pipe. Reactor No. 2 is topped with an ammonia feed pipe with a flowmeter. Its top is also connected to a gas cabinet 7 via a silicon tetrafluoride discharge pipe with a flowmeter. The bottom of Reactor No. 2 is connected via a pipe to Filter No. 2, which is in turn connected to the top of Reactor No. 3 and a calcium fluoride storage tank 11. Reactor No. 3 is topped with an ammonia return pipe 9 with a flowmeter to the top of Reactor No. 2. The bottom of Reactor No. 3 is connected via a pipe to Filter No. 3, which is connected via pipes to a lithium fluoride storage tank 12 and subsequent purification and drying equipment for lithium bis(fluorosulfonyl)imide. Reactors No. 1, 2, and 3 are all equipped with a stirring device and a temperature control device. The temperature control device includes a reactor jacket connected to either a steam system or a cooling brine system. The steam system has a heating temperature of 20 to 100°C, while the cooling brine system has a cooling temperature of -25 to 0°C. Filters No. 1, 5, and 6 are all sealed filters. The feed port of the sulfuryl chloride feed pipe is a dropping port.

[0020] Ammonia return pipe 9 is directly connected to ammonia feed pipe, and then flows into No. 2 reactor 2 (such as Figure 1 As shown) or arranged in parallel with the ammonia feed pipe, directly connected to the No. 2 reactor 2 ((as shown Figure 2 shown).

[0021] The flow meter of the present invention, as well as some necessary conventional components such as thermometers, valves, pumps, etc. are not shown in the figures, but are still included according to the required functions.

[0022] When using this apparatus to produce lithium bis(fluorosulfonyl)imide, a solvent (acetonitrile) and potassium fluoride are placed in reactor No. 1, a solvent (acetonitrile), silicon dioxide, and calcium oxide are placed in reactor No. 2, and a solvent (diethyl carbonate) and a lithium salt (such as lithium carbonate) are placed in reactor No. 3. Stirring paddles 1.1, 2.1, and 3.1 are turned on.

[0023] Sulfuryl chloride is added dropwise to reactor No. 1 via a sulfuryl chloride feed pipe. The reaction proceeds under stirring and at a controlled temperature. The resulting sulfuryl fluoride is then passed from the top through a sulfuryl fluoride discharge pipe into reactor No. 2. After the reaction in reactor No. 1 is complete, the bottom discharge port is opened, allowing a mixture of the solvent and the generated potassium chloride to enter filter No. 1 through a pipe. After filtration, the solvent is returned to the lower middle portion of reactor No. 1 via solvent recycle pipe 8 and recycles into reactor No. 1. The potassium chloride then enters a potassium chloride storage tank 10 as a product.

[0024] Ammonia enters the No. 2 reactor 2 through the ammonia feed pipe, and the reaction is carried out at a certain temperature under stirring. The silicon tetrafluoride gas generated by the reaction enters the gas cabinet 7 through the silicon tetrafluoride discharge pipe and is stored as a product. After the reaction in the No. 2 reactor 2 is completed, the mixture enters the No. 2 filter 5 through the pipeline from the bottom discharge port. After filtration, calcium fluoride enters the calcium fluoride storage tank 11 as a product, and the filtrate directly enters the No. 3 reactor 3. The ammonia generated by the reaction in the No. 3 reactor 3 is returned to the No. 2 reactor 2 through the ammonia return pipe 9 and can continue to participate in the reaction. After the reaction in the No. 3 reactor 3 is completed, the mixture enters the No. 3 filter 6 through the pipeline from the bottom discharge port, and the lithium fluoride obtained by filtration enters the lithium fluoride storage tank 12 as a product. The target product, crude lithium bis(fluorosulfonyl)imide, enters the subsequent purification and drying system for treatment to obtain the product.

Claims

1. A production device for lithium bis(fluorosulfonyl)imide, characterized in that: The production device comprises a No. 1 reactor (1), a No. 2 reactor (2) and a No. 3 reactor (3) which are sequentially connected in series; a sulfuryl chloride feed pipe and a sulfuryl fluoride discharge pipe are arranged on the top of the No. 1 reactor (1); a bottom discharge port is connected to a No. 1 filter (4) through a pipeline; the No. 1 filter (4) is respectively connected to a potassium chloride storage tank (10) and is connected to the middle and lower part of the No. 1 reactor (1) through a solvent sleeve pipe (8); the sulfuryl fluoride discharge pipe is connected to the lower part of the No. 2 reactor (2); an ammonia feed pipe is arranged on the top of the No. 2 reactor (2) and is connected to a gas cabinet (7) through a silicon tetrafluoride discharge pipe; a bottom discharge port is connected to a No. 1 filter (4) through a pipeline; a potassium chloride storage tank (10) is connected to the middle and lower part of the No. 1 reactor (1) through a solvent sleeve pipe (8); a sulfuryl fluoride discharge pipe is connected to the lower part of the No. 2 reactor (2); an ammonia feed pipe is arranged on the top of the No. 2 reactor (2) and is connected to a gas cabinet (7) through a silicon tetrafluoride discharge pipe; a bottom discharge port is connected to a No. 1 filter (4) through a pipeline; a potassium chloride storage tank (10) is connected to the No. 1 filter (4) through a solvent sleeve pipe (8); a sulfuryl fluoride discharge pipe is connected to a bottom discharge port; a potassium chloride storage tank (10) is connected to the No. 1 filter (4) through a solvent sleeve pipe (8); a potassium chloride storage tank (10) is connected to the No. 1 filter (1 ... The first reactor (1) is connected to the second filter (5) through a pipeline, and the second filter (5) is connected to the top of the third reactor (3) and the calcium fluoride storage tank (11) through pipelines; the top of the third reactor (3) is connected to the top of the second reactor (2) through an ammonia return pipe (9), and the bottom of the third reactor (3) is connected to the third filter (6) through a pipeline, and the third filter (6) is connected to the lithium fluoride storage tank (12) and the subsequent purification and drying device of lithium bis(fluorosulfonyl)imide; the first reactor (1), the second reactor (2) and the third reactor (3) are all equipped with a stirring device and a temperature control device.

2. The production device of lithium bis(fluorosulfonyl)imide according to claim 1, characterized in that: The ammonia return pipe (9) is connected to the ammonia feed pipe or is arranged in parallel with the ammonia feed pipe.

3. The production device of lithium bis(fluorosulfonyl)imide according to claim 1, characterized in that: The first reactor (1) contains a solvent and potassium fluoride; the second reactor (2) contains a solvent, silicon dioxide and calcium oxide; and the third reactor (3) contains a solvent and lithium salt.

4. The production device of lithium bis(fluorosulfonyl)imide according to claim 1, characterized in that: The first filter (4), the second filter (5) and the third filter (6) are all closed filters.

5. The production device of lithium bis(fluorosulfonyl)imide according to claim 1 or 2, characterized in that: Flow meters are provided on the sulfuryl chloride feed pipe, the sulfuryl fluoride discharge pipe, the ammonia feed pipe, the ammonia return pipe (9) and the silicon tetrafluoride discharge pipe.

6. The production device of lithium bis(fluorosulfonyl)imide according to claim 1, characterized in that: The temperature control device includes a reactor jacket connected to a steam system or a cooling brine system.

7. The production device of lithium bis(fluorosulfonyl)imide according to claim 6, characterized in that: The heating temperature of the steam system is 20~100℃, and the cooling temperature of the cooling brine system is -25~0℃.

8. The production device of lithium bis(fluorosulfonyl)imide according to claim 1, characterized in that: The feed port of the sulfuryl chloride feed pipe is a dropping port.

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