An apparatus for continuous production of a bisfluorosulfonylimide intermediate

By designing a continuous production unit to directly separate products and by-products, the problem of complex post-processing in batch production was solved, achieving efficient production of bis(fluorosulfonyl)imide intermediates, improving production efficiency and reducing costs.

CN224271142UActive Publication Date: 2026-05-26LINHAI LIMIN CHEM
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
LINHAI LIMIN CHEM
Filing Date
2025-05-29
Publication Date
2026-05-26

AI Technical Summary

Technical Problem

In the existing technology, the production of bisfluorosulfonyl imide intermediates adopts an intermittent process, the post-processing is complex and the recovery of triethylamine is difficult, making it difficult to achieve continuous production.

Method used

Design a continuous production device including a feed mixer, a coil reactor, a separator, and a cooling tank. By directly separating products and byproducts, and combining a steam heating and brine cooling system, the product and unreacted raw materials can be recycled and reused.

Benefits of technology

Continuous production of bis(fluorosulfonyl)imide intermediates has been achieved, increasing production scale and capacity while reducing production costs.

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Abstract

This invention discloses an apparatus for the continuous production of bis(fluorosulfonyl)imide intermediates. The apparatus includes a feed mixer with liquid and gas feed ports. The outlet of the feed mixer is connected to the top of a coil reactor via a pipe and is also connected to the inlet of the coil inside the reactor. The outlet of the coil connects from the bottom of the reactor to the top of a separator. A cooling tank is provided outside the coil. The separator has a by-product outlet at the top and a product outlet at the bottom. A steam heater is also provided inside the separator. This apparatus can directly separate the product and by-product, thereby achieving the goal of continuous production of bis(fluorosulfonyl)imide intermediates, increasing production scale and capacity, and ensuring smooth production operation. Furthermore, this apparatus can recover and reuse unreacted raw materials and solvents during the production process, reducing production costs.
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Description

Technical Field

[0001] This utility model relates to an apparatus for the continuous production of bis(fluorosulfonyl)imide intermediates, belonging to the field of chemical equipment technology. Background Technology

[0002] Lithium-ion battery materials for new energy storage have been widely used in aerospace, marine, and computer electronics fields. Difluorosulfonyl imide, as an important intermediate in lithium-ion battery electrolytes, is considered a promising compound for preparing next-generation lithium-ion battery electrolytes. In conventional processes for producing difluorosulfonyl imide intermediates, aprotic polar solvents are used as the medium, organic amines as catalysts, and thiosulfonyl fluoride and ammonia as raw materials for a condensation reaction. Due to the involvement of multiphase reactions, complex post-processing steps, and the difficulty in recovering triethylamine, current production facilities employ batch production processes. Utility Model Content

[0003] The technical problem to be solved by this utility model is to provide an apparatus for producing bis(fluorosulfonyl)imide intermediates, which achieves continuous production and increases production capacity by directly separating the product and by-product.

[0004] To address the above technical problems, this utility model discloses an apparatus for the continuous production of bis(fluorosulfonyl)imide intermediates. The apparatus includes a feed mixer with a liquid feed port and a gas feed port. The outlet of the feed mixer is connected to the top of a coil reactor via a pipe and is connected to the inlet of the coil inside the coil reactor. The outlet of the coil is connected from the bottom of the coil reactor to the top of a separator. A cooling tank is provided outside the coil. A by-product outlet is provided at the top of the separator, and a product outlet is provided at the bottom. A steam heater is also provided inside the separator.

[0005] Furthermore, the cooling tank is the space between the coil and the outer wall of the coil reactor. The coolant inlet of the cooling tank is located at the lower part of the coil reactor, and the coolant outlet is located at the upper part of the coil reactor.

[0006] Furthermore, the coolant inlet and coolant outlet are connected to a brine cooling system.

[0007] Furthermore, the coil is 128 meters long and 1.5 centimeters in diameter.

[0008] Furthermore, the steam heater is connected to a steam heating system, with its steam inlet located at the top of the separator and its condensate outlet located at the bottom of the separator.

[0009] Furthermore, the separator is provided with a recycling outlet at the top, and the feed mixer is provided with a recycling inlet at the top. The recycling outlet and the recycling inlet are connected by a recycling pipe.

[0010] Furthermore, the steam heater is a coil-type heating tube.

[0011] Furthermore, the gas feed port is equipped with a flow meter.

[0012] The apparatus of this invention can directly separate products and byproducts, thereby achieving continuous production of bis(fluorosulfonyl)imide intermediates, increasing production scale and capacity, and ensuring smooth production operation. This apparatus can also recover and reuse unreacted raw materials and solvents from the production process, reducing production costs. Attached Figure Description

[0013] Figure 1 This is a schematic diagram of the structure of the device of the utility model.

[0014] Numbering in the diagram: 1-Coil reactor; 1.1-Coil; 1.2-Coolant inlet; 1.3-Coolant outlet; 1.4-Cooling tank; 2-Separator; 2.1-Steam heater; 2.2-Steam inlet; 2.3-Condensate outlet; 2.4-By-product outlet; 2.5-Product outlet; 2.6-Recovery and reuse outlet; 3-Feed mixer; 3.1-Liquid feed port; 3.2-Gas feed port; 4-Recovery and reuse pipe; 4.1-Recovery and reuse inlet. Detailed Implementation

[0015] The present invention will be further explained below with reference to the embodiments. The following embodiments are only used to illustrate the present invention, but are not intended to limit the scope of implementation of the present invention.

[0016] Example 1

[0017] like Figure 1 As shown, the apparatus for continuous production of bis(fluorosulfonyl)imide intermediates of this invention includes a feed mixer 3 with a liquid feed port 3.1 and a gas feed port 3.2. The outlet of the feed mixer 3 is connected to the top of a coil reactor 1 via a pipe and is connected to the inlet of the coil 1.1 inside the coil reactor 1. The outlet of the coil 1.1 is connected from the bottom of the coil reactor 1 to the top of a separator 2. A cooling tank 1.4 is provided outside the coil 1.1, which is the space between the coil 1.1 and the outer wall of the coil reactor 1. The cooling liquid inlet 1.2 is located at the lower part of the coil reactor 1, and the cooling liquid outlet 1.3 is located at the upper part of the coil reactor 1. The cooling liquid inlet 1.2 and the cooling liquid outlet 1.3 are connected to a brine cooling system. The coil 1.1 is 128 meters long and 1.5 centimeters in diameter.

[0018] The separator 2 has a by-product outlet 2.4 at the top and a product outlet 2.5 at the bottom. A steam heater 2.1 is also installed inside the separator 2. The steam heater 2.1 is connected to a steam heating system, with its steam inlet 2.2 located at the top of the separator 2 and its condensate outlet 2.3 located at the bottom. A recycling outlet 2.6 is also provided at the top of the separator 2, and a recycling inlet 4.1 is provided at the top of the feed mixer 3. The recycling outlet 2.6 and the recycling inlet 4.1 are connected by a recycling pipe 4.

[0019] The gas feed port 3.2 is equipped with a flow meter.

[0020] To clearly show the components, some parts not shown in the attached drawings, such as coils, are for illustrative purposes only and are not drawn to scale. Similarly, some common components, such as valves on pipes, are not shown in the drawings, but this does not mean they are not present.

[0021] When using this device, the raw material triethylamine and the solvent acetonitrile are added to the feed mixer 3 through the liquid feed port 3.1, while thiocyanate fluoride and ammonia are added to the feed mixer 3 through the gas feed port 3.2. After mixing in the feed mixer 3, the mixture is piped into the coil 1.1 for reaction. The cooling temperature of the cooling tank 1.4 is -15℃, and the coolant is chilled brine. After the reaction, the mixture enters the separator 2 from the bottom of the coil reactor 1. The steam heater 2.1 in the separator 2 is a coil-type heating tube. Steam at 110℃ enters the coil to heat the material in the separator 2, causing the by-products and unreacted raw materials to vaporize. The by-products are discharged from the by-product outlet 2.4, and the unreacted raw materials are discharged from the recovery outlet 2.6, and then enter the feed mixer 3 through the recovery pipe 4 and the recovery inlet 4.1 to continue the subsequent reaction.

[0022] The product is continuously released from the bottom of separator 2 and enters the purification system.

Claims

1. An apparatus for continuous production of a bisfluorosulfone imide intermediate, characterized by: The device includes a feed mixer (3) with a liquid feed port (3.1) and a gas feed port (3.2); the outlet of the feed mixer (3) is connected to the top of the coil reactor (1) through a pipe and is connected to the inlet of the coil (1.1) inside the coil reactor (1); the outlet of the coil (1.1) is connected from the bottom of the coil reactor (1) to the top of the separator (2); a cooling tank (1.4) is provided outside the coil (1.1); a by-product outlet (2.4) is provided at the top of the separator (2) and a product outlet (2.5) is provided at the bottom; a steam heater (2.1) is also provided inside the separator (2).

2. The apparatus for continuous production of bis(fluorosulfonyl)imide intermediates according to claim 1, characterized in that: The cooling tank (1.4) is the space between the coil (1.1) and the outer wall of the coil reactor (1). The coolant inlet (1.2) of the cooling tank (1.4) is located at the lower part of the coil reactor (1), and the coolant outlet (1.3) is located at the upper part of the coil reactor (1).

3. The apparatus for continuous production of bis(fluorosulfonyl)imide intermediates according to claim 2, characterized in that: The coolant inlet (1.2) and coolant outlet (1.3) are connected to the brine cooling system.

4. The apparatus for continuous production of bis(fluorosulfonyl)imide intermediates according to claim 1, characterized in that: The coil (1.1) is 128 meters long and 1.5 centimeters in diameter.

5. The apparatus for continuous production of bis(fluorosulfonyl)imide intermediates according to claim 1, characterized in that: The steam heater (2.1) is connected to the steam heating system, with its steam inlet (2.2) located at the upper part of the separator (2) and its condensate outlet (2.3) located at the lower part of the separator (2).

6. The apparatus for continuous production of bis(fluorosulfonyl)imide intermediates according to claim 1, characterized in that: The separator (2) is also provided with a recycling outlet (2.6) at the top, and the feed mixer (3) is provided with a recycling inlet (4.1) at the top. The recycling outlet (2.6) and the recycling inlet (4.1) are connected by a recycling pipe (4).

7. The apparatus for continuous production of bis(fluorosulfonyl)imide intermediates according to claim 1, characterized in that: The steam heater (2.1) is a coil-type heating tube.

8. The apparatus for continuous production of bis(fluorosulfonyl)imide intermediates according to claim 1, characterized in that: The gas feed port (3.2) is equipped with a flow meter.