阅读说明：本技术 双氟磺酰亚胺的清洁生产工艺 (Clean production process of bis (fluorosulfonyl) imide ) 是由 李光辉 张泰铭 孙庆民 王军 杨建玲 孙健 王永 薛居强 于 2021-09-14 设计创作，主要内容包括：本发明涉及双氟磺酰亚胺生产技术领域,具体涉及一种双氟磺酰亚胺的清洁生产工艺。所述的双氟磺酰亚胺的清洁生产工艺,使用间歇反应釜作为预反应装置,微通道反应器作为主反应装置,微通道反应器包含串联的第一温区和第二温区,两个温区均包含多个串联的反应模块；先将氨基磺酸、三氧化硫、氯化亚砜加入间歇反应釜进行反应,得到预反应液,然后将预反应液打入第一温区进行反应,得到双氯反应料液,再将双氯反应料液和氟化氢液体同时打入第二温区进行反应,得到双氟反应料液,经减压精馏,得到高纯度双氟磺酰亚胺产品。本发明基于微通道反应器,从双氯磺酰亚胺的合成开始,经过氟化氢高效氟代反应,精馏提纯得到高纯度双氟磺酰亚胺产品。(The invention relates to the technical field of production of bis (fluorosulfonyl) imide, and particularly relates to a clean production process of bis (fluorosulfonyl) imide. The clean production process of the bis (fluorosulfonyl) imide uses an intermittent reaction kettle as a pre-reaction device, a microchannel reactor as a main reaction device, the microchannel reactor comprises a first temperature zone and a second temperature zone which are connected in series, and the two temperature zones comprise a plurality of reaction modules which are connected in series; firstly, sulfamic acid, sulfur trioxide and thionyl chloride are added into a batch reactor to react to obtain a pre-reaction liquid, then the pre-reaction liquid is injected into a first temperature zone to react to obtain a bis-chlorine reaction liquid, then the bis-chlorine reaction liquid and a hydrogen fluoride liquid are injected into a second temperature zone simultaneously to react to obtain a bis-fluorine reaction liquid, and a high-purity bis-fluorine sulfimide product is obtained through reduced pressure rectification. The invention is based on a microchannel reactor, and a high-purity bis (fluorosulfonyl) imide product is obtained by starting from the synthesis of bis (chlorosulfonyl) imide, performing high-efficiency fluorination reaction of hydrogen fluoride, and rectifying and purifying.)

1. A clean production process of bis (fluorosulfonyl) imide is characterized by comprising the following steps: a batch reaction kettle is used as a pre-reaction device, a microchannel reactor is used as a main reaction device, the microchannel reactor comprises a first temperature zone and a second temperature zone which are connected in series, and the two temperature zones comprise a plurality of reaction modules which are connected in series; the method comprises the following steps:

(1) adding sulfamic acid, sulfur trioxide and thionyl chloride into an intermittent reaction kettle, starting stirring, and reacting at a certain temperature and pressure to obtain a pre-reaction solution;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of the microchannel reactor for reaction, and obtaining a dichlorine reaction liquid from an outlet;

(3) the reaction liquid enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out from a lower liquid outlet and is pumped into a reaction module of a second temperature zone, meanwhile, the hydrogen fluoride liquid is pumped into the reaction module of the second temperature zone for reaction, and the difluoride reaction liquid is obtained from an outlet;

(4) and (3) allowing the difluoride reaction liquid to enter a gas-liquid separation tank, discharging gas from an upper gas outlet to a fluorine-chlorine separation condenser, allowing the reaction liquid to flow out of a lower liquid outlet, and pumping the reaction liquid into a rectifying tower for reduced pressure rectification to obtain a high-purity difluoride sulfimide product.

2. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (1), the molar ratio of sulfamic acid, sulfur trioxide and thionyl chloride is 1:1 (2-2.5).

3. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (1), the reaction temperature is 90-120 ℃, the reaction pressure is 0.1-0.7MPa, and the reaction time is 1-6 h.

4. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (2), the first temperature zone is provided with 4-10 series modules, the reaction time of a single module is 5-15s, and the total reaction time of the temperature zone is 20-150 s.

5. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (2), the reaction temperature of the first temperature zone is 120-.

6. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (3), the molar ratio of the hydrogen fluoride to the aminosulfonic acid in the step (1) is (2-10): 1.

7. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (3), 4-10 series-connected modules are arranged in the second temperature zone, the reaction time of a single module is 2-6s, and the reaction (retention) time of the temperature zone is 8-60 s.

8. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (3), the reaction temperature of the second temperature zone is 90-120 ℃, and the reaction pressure is 0.5-1.2 MPa.

9. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (4), the gas is a mixed gas of hydrogen chloride and hydrogen fluoride, and the hydrogen fluoride liquid obtained by separation in the fluorine-chlorine separation condenser is recycled to the step (3) for reaction.

10. The clean production process of bis-fluorosulfonylimide according to claim 1, characterized in that: in the step (4), the pressure of the reduced pressure distillation is 2-5mmHg, and the collecting temperature of the bis (fluorosulfonyl) imide fraction is 112-115 ℃.

Technical Field

The invention relates to the technical field of production of bis (fluorosulfonyl) imide, and particularly relates to a clean production process of bis (fluorosulfonyl) imide.

Background

The lithium ion battery has the excellent characteristics of high working voltage, high energy density, long cycle life, rapid charge and discharge and the like, is widely applied to the fields of various mobile electric appliances, automobiles and the like at present, is developing to the field of wind energy and solar energy storage, and the related manufacturing industry faces the expansion and pressure of productivity and technical level.

The most widely used electrolyte lithium salt in current lithium batteries is lithium hexafluorophosphate, which has a small fluorine atom radius and a PF₆ ^-The high-temperature resistant HF gas phase-change material has proper radius, good ionic conductivity and electrochemical stability, but has the defects of weak high-temperature resistance, easy decomposition when meeting water and HF gas generation after decomposition at 60-80 ℃. The lithium bis (fluorosulfonyl) imide has good thermal stability and chemical stability, and has excellent performances of unique electrode material compatibility, low viscosity, low melting point, high conductivity and the like, and is considered to possibly replace LiPF₆The new generation of lithium ion battery electrolyte.

The production scheme for lithium bis (fluorosulfonyl) imide generally comprises: the method comprises three steps of synthesis of the bischlorosulfonimide, fluorination and salification. The fluorination section is the step with the highest technical difficulty, and the technical level of the fluorination section not only directly influences the quality of a final product, but also determines the technological indexes such as safety, environmental protection and the like. The mainstream fluorination process adopted in China at present is divided into a fluoride salt method and a hydrogen fluoride method.

Patent CN106006586B discloses a method for preparing potassium bis (fluorosulfonyl) imide, wherein the preparation of bis (fluorosulfonyl) imide takes bis (chlorosulfonyl) imide and hydrogen fluoride as raw materials, and the fluorination reaction is completed under the action of a catalyst, which has the main problems of danger and low efficiency. The fluorination reaction is one of the national regulated dangerous processes, and the intermittent production process has extremely high danger, so that the policy encourages the development and popularization of a microchannel continuous flow process, and the intrinsic safety of the process is improved. As the reaction is a gas-liquid two-phase reaction of hydrogen fluoride gas and bischlorosulfonimide, the mass transfer efficiency in the traditional reaction kettle is extremely low, so that the reaction time is as long as 10-25 hours, the production cost is increased, and the danger coefficient is also increased.

Patent CN101747242B discloses a method for preparing alkali metal salts of bis-fluorosulfonyl imide, wherein the bis-fluorosulfonyl imide is prepared by carrying out fluorination reaction on bis-chlorosulfonyl imide and antimony trifluoride serving as raw materials. The process has the advantage of high process safety, but the problems of rare metal resource consumption, byproduct fluorine-containing antimony chloride waste salt and the like are also outstanding, and other similar processes using fluoride salt as a fluorination reagent have similar problems. Although the process still occupies the domestic mainstream production line, under the development trend of green chemical industry and clean process, the process should be gradually eliminated and replaced.

In summary, under the background of the rapid expansion of market demand, the development of the process level of the bis-fluorosulfonyl imide is also urgent, and the problems of process safety and cleanness need to be solved more perfectly.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: the clean production process of the bis (fluorosulfonyl) imide is based on a microchannel reactor, and a high-purity bis (fluorosulfonyl) imide product is obtained by starting from the synthesis of the bis (fluorosulfonyl) imide, performing high-efficiency fluorination reaction of hydrogen fluoride, and rectifying and purifying.

The clean production process of the bis (fluorosulfonyl) imide uses an intermittent reaction kettle as a pre-reaction device, uses a microchannel reactor as a main reaction device, and comprises a first temperature zone and a second temperature zone which are connected in series, wherein the two temperature zones comprise a plurality of reaction modules which are connected in series; the method comprises the following steps:

(1) adding sulfamic acid, sulfur trioxide and thionyl chloride into an intermittent reaction kettle, starting stirring, and reacting at a certain temperature and pressure to obtain a pre-reaction solution;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of the microchannel reactor for reaction, and obtaining a dichlorine reaction liquid from an outlet;

(3) the reaction liquid enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out from a lower liquid outlet and is pumped into a reaction module of a second temperature zone, meanwhile, the hydrogen fluoride liquid is pumped into the reaction module of the second temperature zone for reaction, and the difluoride reaction liquid is obtained from an outlet;

(4) and (3) allowing the difluoride reaction liquid to enter a gas-liquid separation tank, discharging gas from an upper gas outlet to a fluorine-chlorine separation condenser, allowing the reaction liquid to flow out of a lower liquid outlet, and pumping the reaction liquid into a rectifying tower for reduced pressure rectification to obtain a high-purity difluoride sulfimide product.

In the step (1), the molar ratio of sulfamic acid, sulfur trioxide and thionyl chloride is 1:1 (2-2.5).

In the step (1), the reaction temperature is 90-120 ℃, the reaction pressure is 0.1-0.7MPa, and the reaction time is 1-6 h.

In the step (2), the first temperature zone is provided with 4-10 series modules, the reaction (residence) time of a single module is 5-15s, and the total reaction (residence) time of the temperature zone is 20-150 s.

In the step (2), the reaction temperature of the first temperature zone is 120-.

In the step (3), the molar ratio of the hydrogen fluoride to the aminosulfonic acid in the step (1) is (2-10): 1.

In the step (3), 4-10 series-connected modules are arranged in the second temperature zone, the reaction (retention) time of a single module is 2-6s, and the reaction (retention) time of the temperature zone is 8-60 s.

In the step (3), the reaction temperature of the second temperature zone is 90-120 ℃, and the reaction pressure is 0.5-1.2 MPa.

In the step (4), the gas is a mixed gas of hydrogen chloride and hydrogen fluoride, and the hydrogen fluoride liquid obtained by separation in the fluorine-chlorine separation condenser is recycled to the step (3) for reaction.

In the step (4), the pressure of the reduced pressure distillation is 2-5mmHg, and the collecting temperature of the bis (fluorosulfonyl) imide fraction is 112-115 ℃.

As a preferable scheme, the clean production process of the bis (fluorosulfonyl) imide comprises the following steps:

(1) adding quantitative sulfamic acid, sulfur trioxide and thionyl chloride into an intermittent reaction kettle, controlling the temperature to be 90-120 ℃, starting stirring, adjusting and controlling the pressure in the kettle to be 0.1-0.7MPa by adopting a back pressure valve, and reacting for 1-6 hours;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of the microchannel reactor through a material transfer pump, wherein the reaction temperature is 120-150 ℃, the reaction pressure is 0.5-1.5MPa, the temperature zone is provided with 4-10 series modules, the reaction (retention) time of a single module is 5-15s, and the reaction (retention) time of the temperature zone is 20-150 s;

(3) the dichlorine reaction feed liquid flows out of a first temperature zone, enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out of a lower liquid outlet, is pumped into a reaction module of a second temperature zone through a material transfer pump, and hydrogen fluoride liquid is pumped into the reaction module to carry out mixed reaction, wherein the reaction temperature is 90-120 ℃, the reaction pressure is 0.5-1.2MPa, the temperature zone is provided with 4-10 series modules, the reaction (retention) time of a single module is 2-6s, and the reaction (retention) time of the temperature zone is 8-60 s;

(4) and the defluorination reaction liquid flows out of the continuous flow reactor and enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and flows to a fluorine-chlorine separation condenser, and the reaction liquid flows out of a lower liquid outlet and is pumped into a rectifying tower through a material transfer pump for reduced pressure rectification to obtain the high-purity defluorination sulfimide product.

Compared with the prior art, the invention has the following beneficial effects:

(1) the process of the invention develops the continuous flow production process of the bis (fluorosulfonyl) imide based on the microchannel reactor, and fills the blank of the continuous flow process in the bis (fluorosulfonyl) imide production industry;

(2) the fluorination process belongs to a 'dangerous process' specified by the state, and the traditional process method has great safety risk, the invention adopts the microchannel reactor to reduce the reaction liquid holdup to below 1kg, the intrinsic safety is greatly improved, and the microchannel reactor greatly improves the mass and heat transfer effects of gas phase and liquid phase in a reaction system, thereby preventing dangerous accidents caused by heat accumulation;

(3) the invention adopts sulfur trioxide to replace chlorosulfonic acid in the traditional process to synthesize the intermediate bischlorosulfonimide, improves the reaction activity and the utilization rate of raw materials, adopts pre-reaction to finish most reactions of the working section, then uses a microchannel reactor to improve the reaction temperature and pressure, quickly finishes the residual reaction, and obviously improves the production efficiency;

(4) the intermediate bischlorosulfimide and hydrogen fluoride are in gas-liquid two phases in the traditional reaction process, the microchannel reactor used by the invention can obviously improve the mass transfer efficiency of the gas-liquid two phases, not only reduces the usage amount of the hydrogen fluoride, but also greatly shortens the fluorination reaction time;

(5) compared with the fluoride salt fluorination process, the process has the advantages that no fluorine-containing waste salt is generated, and the cleanness is higher; compared with the hydrofluoride fluorination process of the traditional batch process, the method does not need to use a catalyst, avoids the introduction of impurities and the generation of three wastes, has higher product purity, and can recycle the excessive hydrofluoride.

Detailed Description

The present invention is further described in the following examples, which should not be construed as limiting the scope of the invention, but rather as providing those skilled in the art with the benefit of the present disclosure with additional inventive concepts and features described herein.

The purity detection method of the product of the bis-fluorosulfonyl imide comprises the following steps:

(1) and (3) measuring N: adding water into a sample, fully hydrolyzing, titrating by using a sodium nitrite solution, and taking starch potassium iodide as an indicator;

(2) f, measurement: diluting the sample with dilute alkaline water, heating for full hydrolysis, and measuring the content of fluorine ions by a fluorine electrode through potentiometric titration;

(3) if F%/N% >2, calculating the purity of the sample by N%; if F%/N% < 2, the sample purity is calculated as F%.

Example 1

The clean production process of the bis (fluorosulfonyl) imide provided by the invention uses an intermittent reaction kettle as a pre-reaction device, uses a microchannel reactor as a main reaction device, and comprises a first temperature zone and a second temperature zone which are connected in series, wherein both temperature zones comprise 6 reaction modules which are connected in series; the method comprises the following steps:

(1) adding 97.1g (1mol) of sulfamic acid, 273.7g (2.3mol) of thionyl chloride and 80g (1mol) of sulfur trioxide into an intermittent reaction kettle, controlling the temperature to be 110 ℃, starting stirring, regulating and controlling the pressure in the kettle to be 0.4MPa by adopting a back pressure valve, and reacting for 3 hours;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of a microchannel reactor at 49.2g/min through a material transfer pump, wherein the reaction temperature is 135 ℃, the reaction pressure is 0.75MPa, the temperature zone is provided with 6 series modules, the reaction (retention) time of a single module is 10s, and the reaction (retention) time of the temperature zone is 60 s;

(3) the dichlorine reaction liquid flows out of a first temperature zone, enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a reaction module of a second temperature zone through a material transfer pump, meanwhile, hydrogen fluoride liquid is pumped into the reaction module, the molar ratio of hydrogen fluoride to aminosulfonic acid in the step (1) in the reaction liquid is 6:1, the total flow rate of two materials is 98.4g/min, the reaction temperature is 105 ℃, the reaction pressure is 0.8MPa, the temperature zone is provided with 6 series modules, the reaction (retention) time of a single module is 5s, and the reaction (retention) time of the temperature zone is 30 s;

(4) the defluorination reaction liquid flows out from the continuous flow reactor and enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a fluorine-chlorine separation condenser, the reaction liquid flows out from a lower liquid outlet, the reaction liquid is pumped into a rectifying tower through a material transfer pump, and 112-115 ℃ fraction is collected under the pressure of 2-5mmHg, so that the high-purity defluorination sulfimide product is obtained, wherein the product yield is 94.05 percent, and the product purity is 99.9 percent.

Example 2

The clean production process of the bis (fluorosulfonyl) imide provided by the invention uses an intermittent reaction kettle as a pre-reaction device, uses a microchannel reactor as a main reaction device, and comprises a first temperature zone and a second temperature zone which are connected in series, wherein both temperature zones comprise 4 reaction modules which are connected in series; the method comprises the following steps:

(1) adding 97.1g (1mol) of sulfamic acid, 238g (2.0mol) of thionyl chloride and 80g (1mol) of sulfur trioxide into an intermittent reaction kettle, controlling the temperature to be 90 ℃, starting stirring, regulating and controlling the pressure in the kettle to be 0.2MPa by adopting a back pressure valve, and reacting for 1 hour;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of a microchannel reactor at 49.2g/min through a material transfer pump, wherein the reaction temperature is 120 ℃, the reaction pressure is 0.5MPa, the temperature zone is provided with 4 series modules, the reaction (retention) time of a single module is 5s, and the reaction (retention) time of the temperature zone is 20 s;

(3) the dichlorine reaction liquid flows out of a first temperature zone, enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a reaction module of a second temperature zone through a material transfer pump, meanwhile, hydrogen fluoride liquid is pumped into the reaction module, the molar ratio of hydrogen fluoride to aminosulfonic acid in the step (1) in the reaction liquid is 2:1, the total flow rate of two materials is 98.4g/min, the reaction temperature is 90 ℃, the reaction pressure is 0.5MPa, the temperature zone is provided with 4 series modules, the reaction (retention) time of a single module is 2s, and the reaction (retention) time of the temperature zone is 8 s;

(4) the defluorination reaction liquid flows out from the continuous flow reactor and enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and flows to a fluorine-chlorine separation condenser, the reaction liquid flows out from a lower liquid outlet, the reaction liquid is pumped into a rectifying tower through a material transfer pump, and 112-115 ℃ fraction is collected under the pressure of 2-5mmHg, so that the high-purity defluorination sulfimide product is obtained, the product yield is 90.6 percent, and the product purity is 98.5 percent.

Example 3

The clean production process of the bis (fluorosulfonyl) imide provided by the invention uses an intermittent reaction kettle as a pre-reaction device, uses a microchannel reactor as a main reaction device, and comprises a first temperature zone and a second temperature zone which are connected in series, wherein both the two temperature zones comprise 10 reaction modules which are connected in series; the method comprises the following steps:

(1) adding 97.1g (1mol) of sulfamic acid, 297.5g (2.5mol) of thionyl chloride and 80g (1mol) of sulfur trioxide into an intermittent reaction kettle, controlling the temperature to be 120 ℃, starting stirring, adjusting and controlling the pressure in the kettle to be 0.7MPa by adopting a back pressure valve, and reacting for 6 hours;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of a microchannel reactor at 49.2g/min through a material transfer pump, wherein the reaction temperature is 150 ℃, the reaction pressure is 1.5MPa, the temperature zone is provided with 10 series modules, the reaction (retention) time of a single module is 10s, and the reaction (retention) time of the temperature zone is 100 s;

(3) the dichlorine reaction liquid flows out of a first temperature zone, enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a reaction module of a second temperature zone through a material transfer pump, meanwhile, hydrogen fluoride liquid is pumped into the reaction module, the molar ratio of hydrogen fluoride to aminosulfonic acid in the step (1) in the reaction liquid is 10:1, the total flow rate of two materials is 98.4g/min, the reaction temperature is 120 ℃, the reaction pressure is 1.2MPa, the temperature zone is provided with 10 series modules, the reaction (retention) time of a single module is 5s, and the reaction (retention) time of the temperature zone is 50 s;

(4) the defluorination reaction liquid flows out of the continuous flow reactor and enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and flows to a fluorine-chlorine separation condenser, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a rectifying tower through a material transfer pump, and 112-115 ℃ fraction is collected under the pressure of 2-5mmHg, so that the high-purity defluorination sulfimide product is obtained, wherein the product yield is 96.1 percent, and the product purity is 99.5 percent.

Example 4

The clean production process of the bis (fluorosulfonyl) imide provided by the invention uses an intermittent reaction kettle as a pre-reaction device, uses a microchannel reactor as a main reaction device, and comprises a first temperature zone and a second temperature zone which are connected in series, wherein the two temperature zones respectively comprise 8 and 6 reaction modules which are connected in series; the method comprises the following steps:

(1) adding 97.1g (1mol) of sulfamic acid, 273.7g (2.3mol) of thionyl chloride and 80g (1mol) of sulfur trioxide into an intermittent reaction kettle, controlling the temperature to be 100 ℃, starting stirring, regulating and controlling the pressure in the kettle to be 0.3MPa by adopting a back pressure valve, and reacting for 3 hours;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of a microchannel reactor at 49.2g/min through a material transfer pump, wherein the reaction temperature is 130 ℃, the reaction pressure is 0.6MPa, the temperature zone is provided with 8 series modules, the reaction (retention) time of a single module is 10s, and the reaction (retention) time of the temperature zone is 80 s;

(3) the dichlorine reaction liquid flows out of a first temperature zone, enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a reaction module of a second temperature zone through a material transfer pump, meanwhile, hydrogen fluoride liquid is pumped into the reaction module, the molar ratio of hydrogen fluoride to aminosulfonic acid in the step (1) in the reaction liquid is 8:1, the total flow rate of two materials is 98.4g/min, the reaction temperature is 105 ℃, the reaction pressure is 0.8MPa, the temperature zone is provided with 6 series modules, the reaction (retention) time of a single module is 5s, and the reaction (retention) time of the temperature zone is 30 s;

(4) the defluorination reaction liquid flows out from the continuous flow reactor and enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a fluorine-chlorine separation condenser, the reaction liquid flows out from a lower liquid outlet, the reaction liquid is pumped into a rectifying tower through a material transfer pump, and 112-115 ℃ fraction is collected under the pressure of 2-5mmHg, so that the high-purity defluorination sulfimide product is obtained, the product yield is 95.0 percent, and the product purity is 99.8 percent.

Comparative example 1

Adding 97.1g (1mol) of sulfamic acid, 273.7g (2.3mol) of thionyl chloride and 117g (1mol) of chlorosulfonic acid into a reaction kettle, starting stirring, starting a condenser reflux device, controlling the temperature to be 130 ℃, reacting for 24 hours, distilling at normal pressure to remove excessive thionyl chloride, and carrying out reduced pressure distillation to collect 90-105 ℃ fraction to obtain 192.2g of bischlorosulfonimide liquid, wherein the reaction yield is 88% and the product purity is 98.0%.

107.5g (0.5mol) of bischlorosulfonimide liquid and 0.1g of antimony pentachloride catalyst are added into a tetrafluoro reaction bottle, the temperature is raised to 100-105 ℃, 24g of HF gas is slowly introduced under stirring, the temperature is reduced to room temperature after the reaction is carried out for 20 hours, the reaction liquid is rectified, and the 112-115 ℃ fraction is collected under the pressure of 2-5mmHg, so that 92.45g of a comparative product is obtained, the yield is 88 percent, and the purity is 98.0 percent.

Comparative example 2

The comparative example also uses a batch reactor as a pre-reaction device, and a microchannel reactor as a main reaction device, and comprises a first temperature zone and a second temperature zone which are connected in series, wherein both the two temperature zones comprise 2 reaction modules which are connected in series;

(1) adding 97.1g (1mol) of sulfamic acid, 238g (2.0mol) of thionyl chloride and 80g (1mol) of sulfur trioxide into an intermittent reaction kettle, controlling the temperature to be 90 ℃, starting stirring, regulating and controlling the pressure in the kettle to be 0.2MPa by adopting a back pressure valve, and reacting for 1 hour;

(2) pumping the pre-reaction liquid into a reaction module of a first temperature zone of a microchannel reactor at 49.2g/min through a material transfer pump, wherein the reaction temperature is 120 ℃, the reaction pressure is 0.5MPa, the temperature zone is provided with 2 series modules, the reaction (retention) time of a single module is 5s, and the reaction (retention) time of the temperature zone is 10 s;

(3) the dichlorine reaction feed liquid flows out of a first temperature zone, enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a reaction module of a second temperature zone through a material transfer pump, meanwhile, hydrogen fluoride liquid is pumped into the reaction module, the molar ratio of hydrogen fluoride to aminosulfonic acid in the step (1) in the reaction liquid is 2:1, the total flow rate of two materials is 98.4g/min, the reaction temperature is 90 ℃, the reaction pressure is 0.5MPa, the temperature zone is provided with 2 series modules, the reaction (retention) time of a single module is 2s, and the reaction (retention) time of the temperature zone is 4 s;

(4) the defluorination reaction liquid flows out from the continuous flow reactor and enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a fluorine-chlorine separation condenser, the reaction liquid flows out from a lower liquid outlet, the reaction liquid is pumped into a rectifying tower through a material transfer pump, and 112-115 ℃ fraction is collected under the pressure of 2-5mmHg, so that the high-purity defluorination sulfimide product is obtained, the product yield is 81.6 percent, and the product purity is 96.5 percent.

Comparative example 3

The comparative example directly enters a microchannel reactor as a reaction device without adopting a pre-reaction device, and comprises a first temperature zone and a second temperature zone which are connected in series, wherein the two temperature zones respectively comprise 4 reaction modules which are connected in series;

(1)97.1g (1mol) of sulfamic acid, 238g (2.0mol) of thionyl chloride and 80g (1mol) of sulfur trioxide are added into a premixer and stirred uniformly;

(2) pumping the premixed material liquid into a reaction module of a first temperature zone of the microchannel reactor at 49.2g/min through a material transfer pump, wherein the reaction temperature is 120 ℃, the reaction pressure is 0.5MPa, the temperature zone is provided with 4 series modules, the reaction (retention) time of a single module is 5s, and the reaction (retention) time of the temperature zone is 20 s;

(3) the dichlorine reaction liquid flows out of a first temperature zone, enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and goes to a tail gas treatment system, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a reaction module of a second temperature zone through a material transfer pump, meanwhile, hydrogen fluoride liquid is pumped into the reaction module, the molar ratio of hydrogen fluoride to aminosulfonic acid in the step (1) in the reaction liquid is 2:1, the total flow rate of two materials is 98.4g/min, the reaction temperature is 90 ℃, the reaction pressure is 0.5MPa, the temperature zone is provided with 4 series modules, the reaction (retention) time of a single module is 2s, and the reaction (retention) time of the temperature zone is 8 s;

(4) the defluorination reaction liquid flows out of the continuous flow reactor and enters a gas-liquid separation tank, gas is discharged from an upper gas outlet and flows to a fluorine-chlorine separation condenser, the reaction liquid flows out of a lower liquid outlet, the reaction liquid is pumped into a rectifying tower through a material transfer pump, and 112-115 ℃ fraction is collected under the pressure of 2-5mmHg, so that the high-purity defluorination sulfimide product is obtained, the product yield is 75.3 percent, and the product purity is 96.2 percent.