A continuous flow reaction device and a method for the flow synthesis of bis(fluorosulfonyl)imide based on the device

A reaction device, fluorosulfonyl technology, applied in the direction of separation methods, feeding devices, chemical instruments and methods, etc., can solve the problems of difficult separation of by-products, high safety risks, high energy consumption, etc., to shorten the reaction time and reduce by-products Response, low energy consumption effect

Active Publication Date: 2022-06-24
LEE & MAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In summary, the HFSI fluorination methods reported in these patents generally have by-products that are difficult to separate, high temperature and high pressure reaction environment, low yield, high three wastes, high energy consumption, and high safety risks. It is urgent to develop relatively safe / or simple high-yield Method for preparing high-purity HFSI with high efficiency

Method used

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  • A continuous flow reaction device and a method for the flow synthesis of bis(fluorosulfonyl)imide based on the device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] like figure 1 As shown, the continuous flow reaction device of the present invention comprises a jacket heat exchanger 1, a metering pump 2, a first microchannel reactor 3, a first gas-liquid separation system 4, a second microchannel reactor 5, The second gas-liquid separation system 6, the third micro-channel reactor 7, the third gas-liquid separation system 8, the delight tower 9 and the rectification tower 10, also include a liquid booster system 11, a mass flow meter 12 and a tail gas absorption system 13. The liquid pressurization system 11 is respectively communicated with the first microchannel reactor 3, the second microchannel reactor 5 and the third microchannel reactor 7 through the mass flow meter 12, and the liquid pressurization system 11 is connected to the mass A first shut-off valve 14 is provided between the flow meters 12, and a second micro-channel reactor 12 is provided between the mass flow meter 12 and the first micro-channel reactor 3, the secon...

Embodiment 2

[0035] Use the continuous flow reaction device of Example 1 to prepare high-purity HFSI by continuous flow, and the specific steps are as follows:

[0036] The reaction temperature of the first microchannel reactor 3, the second microchannel reactor 5 and the third microchannel reactor 7 was set to 90°C. HClSI and N,N-dimethylformamide (DMF) were mixed to form a material 1, which was charged into a jacketed heat exchanger 1 and preheated to 60°C. The amount of DMF added was 3.3% of the mass of HClSI. Anhydrous AHF is pressurized to 1.2MPa by the liquid pressurizing system 11 for standby.

[0037] The preheated material 1 in the jacket heat exchanger 1 was pumped into the first microchannel reactor 3 through the metering pump 2, and the flow rate was 24ml / min, and was heated to 90 through the preheating module of the first microchannel reactor 3. After ℃, it enters the reaction module group. When the material 1 is filled with the reaction module group, the first shut-off valve...

Embodiment 3

[0039] Use the continuous flow reaction device of Example 1 to prepare high-purity HFSI by continuous flow, and the specific steps are as follows:

[0040] The reaction temperature of the first microchannel reactor 3, the second microchannel reactor 5 and the third microchannel reactor 7 was set to 120°C. HClSI and dibutyl butyl phosphonate (DBBP) were mixed to form a material 1, which was charged into a jacketed heat exchanger 1 and preheated to 60° C., and the amount of DBBP added was 5.7% of the mass of HClSI. Anhydrous AHF is pressurized to 1.2MPa by the liquid pressurizing system 11 for standby.

[0041] The preheated material 1 in the jacket heat exchanger 1 was pumped into the first microchannel reactor 3 through the metering pump 2, and the flow rate was 24ml / min, and was heated to 120 through the preheating module of the first microchannel reactor 3. After ℃, it enters the reaction module group. When the material 1 is filled with the reaction module group, the first ...

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Abstract

The invention discloses a continuous flow reaction device and a flow synthesis method for bis(fluorosulfonyl)imide based on the device. The continuous flow reaction device includes a jacketed heat exchanger, a metering pump, a first microchannel reactor, a first gas-liquid separation system, a second microchannel reactor, a second gas-liquid separation system, and a third microchannel reactor connected in sequence. The channel reactor, the third gas-liquid separation system, light removal tower and rectification tower also include liquid pressurization system, mass flow meter and tail gas absorption system. The present invention adopts three groups of microchannel reactors + gas-liquid separation system to be connected in series, and the vaporized hydrogen fluoride is divided into three strands and injected into the first, second and third microchannel reactors respectively, and the HCl gas generated by the reaction is discharged from the system in time, reducing the reaction time. The pressure drop improves the selectivity of the reaction, and the continuous supplement of AHF makes the reaction more complete, improves the single-pass conversion rate, shortens the reaction time, and reduces the occurrence of side reactions.

Description

Technical field: [0001] The invention relates to the technical field of fluorine chemical lithium battery electrolytes, in particular to a continuous flow reaction device and a flow synthesis method of bis(fluorosulfonyl)imide based on the device. Background technique: [0002] Bis(fluorosulfonyl)imide (cas: 14984-73-7), molecular formula HN (SO 2 f) 2 , referred to as HFSI. It is a strong acid, and its salts and ionic liquids have been proven to be widely used in the field of catalysis, electrolytes, and fluorination reagents, especially its lithium salt (LiFSI) has been proven to be particularly suitable for batteries and supercapacitors. [0003] There are many LiFSI synthesis methods that have been published. For example, as recorded in patent US2004097757, LiFSI is prepared by directly reacting HClSI with lithium fluoride LiF. This method directly produces a large amount of corrosive gas hydrogen fluoride. At the same time, it is difficult to completely separate exces...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00B01J4/02B01D3/14C01B21/093
CPCB01J19/0093B01J19/0053B01J4/02B01D3/143B01D3/14C01B21/093
Inventor 岳公星翁业芹谢文健王宇陈新滋
Owner LEE & MAN CHEM CO LTD
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