System for producing bis (fluorosulfonyl) imide organic alkali salt
Through the reactor system of wire-flow stirring components connected in series and high-speed shear stirring components, the problem of amplification of production capacity in the prior art will be solved, and the production of high selectivity and high throughput difluorosulfonimide organic alkali salts is achieved, with lower energy consumption and more economical equipment costs.
Patent Information
- Application Number
- CN202421249114.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-03
- Publication Date
- 2025-05-09
- Estimated Expiration
- 2034-06-03
AI Technical Summary
The existing batch kettle reactors and microchannel continuous flow reactors are difficult to meet the safety requirements of amplification of production capacity when producing bisfluorosulfonimide organic alkali salts. At the same time, the equipment costs are high, the failure rate is high, and the maintenance costs are high.
The reactor system that uses a series-connected jig-flow stirring component and a high-speed shear stirring component is used to disperse the initial material through jig-flow stirring component, and the high-speed shear stirring component crushes solids, achieving high selectivity and high-throughput reactions.
Under the conditions of lower energy consumption and equipment cost, high selectivity and high throughput preparation of difluorosulfonimide organic alkali salts are achieved. The equipment cost is more economical than that of microchannel reactors or pipeline reactors and has higher safety than kettle reaction equipment.
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Figure CN222842073U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the field of chemical product production, in particular to a system for producing bisfluorosulfonyl imide organic alkali salt by taking ammonia and sulfuryl fluoride as raw materials. Background Art
[0002] Lithium bis(fluorosulfonyl)imide (LiFSI) is a new type of electrolyte lithium salt, which is considered to be the most likely electrolyte lithium salt to replace lithium hexafluorophosphate, and has become the focus of attention in the battery field. At present, the LiFSI synthesis route reported by the industry includes using sulfuryl fluoride as the initialization raw material, first synthesizing bis(fluorosulfonyl)imide, and then exchanging it with lithium hydroxide to prepare lithium bis(fluorosulfonyl)imide.
[0003] At present, using ammonia and sulfuryl fluoride as starting materials, the following three types of reactors are mainly used to produce bis(fluorosulfonyl)imide: (1) traditional intermittent kettle reaction; (2) microchannel continuous flow reactor, such as CN202310067861 reported that the production using a microchannel reactor can obtain good reaction purity and yield; (3) pipeline continuous flow, such as CN115140716A reported that bis(fluorosulfonyl)imide is synthesized by pipeline reaction.
[0004] However, in order to meet the production capacity requirements, the traditional intermittent kettle reactor must increase the reaction vessel and the amount of material processed in a single batch, and the destructiveness after loss of control increases sharply. In an environment with increasingly stringent safety supervision, it is difficult to meet the safety requirements of capacity expansion. Moreover, as a battery electrolyte, it has high quality requirements such as impurities. It is not easy for traditional intermittent kettle reactors to meet the requirements of quality, safety and production capacity at the same time. The microchannel continuous flow reactor is limited by the size of the pipeline, and the flux of a single reactor is limited. To achieve amplification, it is necessary to set up reaction equipment in parallel, resulting in high equipment costs. At the same time, the increase in the number of equipment will lead to higher failure rates and high maintenance costs. At present, the pipeline continuous flow reactors that can meet the process requirements on the market are generally expensive, and the reaction flux is also limited, which cannot meet the process requirements.
[0005] Therefore, there is an urgent need to provide a new system for producing bis(fluorosulfonyl)imide organic base salts. Utility Model Content
[0006] The utility model aims to provide an economical and safe production system of bisfluorosulfonyl imide organic alkali salt, and can prepare bisfluorosulfonyl imide organic alkali salt with high selectivity and high throughput.
[0007] To achieve the above object, the utility model provides a system for producing a bis(fluorosulfonyl)imide organic alkali salt, the system comprising:
[0008] at least one upstream reactor including a jet flow agitation element and at least one downstream reactor including a high shear agitation element connected in series;
[0009] The jet flow stirring component is used to disperse the initial material entering the upstream reactor; the high-speed shear stirring component is used to crush the solid in the downstream reactor.
[0010] In an embodiment of the present utility model, the upstream reactor is used to carry out a reaction to generate a bisfluorosulfonyl imide organic base salt;
[0011] The downstream reactor receives the intermediate material output from the upstream reactor and continues the reaction of generating the bisfluorosulfonyl imide organic base salt.
[0012] In the utility model, the upstream reactor is used to add initial materials to generate a reaction of generating a bisfluorosulfonyl imide organic alkali salt, such as introducing ammonia, sulfuryl fluoride and organic amine in the presence of an organic solvent to generate a reaction, and the organic amine used is triethylamine. The jet flow stirring component evenly disperses the initial materials entering the upstream reactor to promote the main reaction of generating a bisfluorosulfonyl imide organic alkali salt. The downstream reactor receives the intermediate materials discharged from the upstream reactor and continues the main reaction of generating a bisfluorosulfonyl imide organic alkali salt. The intermediate materials include the raw materials, products and organic solvents listed in the reaction formulas (1)-(7) in the upstream reactor, such as products such as bisfluorosulfonyl imide organic alkali salt, ammonium salt, monofluorosulfonamide and other intermediates, and initial materials that have not reacted when output to the downstream reactor. The high-speed shear stirring component unit breaks the solids in the downstream reactor, such as solid ammonium salts such as ammonium fluoride generated due to poor solubility in the organic solvent, and promotes the above-mentioned main reaction in the downstream reactor to continue to proceed in the positive direction.
[0013] In an embodiment of the present invention, the system further comprises: a time-delay reactor located downstream of the downstream reactor.
[0014] In an embodiment of the present invention, the upstream reactor, the downstream reactor and the delayed reactor are each independently selected from a kettle continuous flow reactor, a tubular continuous flow reactor and a tubular-kettle continuous flow reactor.
[0015] In an embodiment of the present invention, the upstream reactor, the downstream reactor and the delayed reactor are each independently selected from a kettle continuous flow reactor, a tubular continuous flow reactor and a tubular-kettle continuous flow reactor.
[0016] In an embodiment of the present invention, the upstream reactor including the jet flow stirring component includes a jet flow stirring component unit and a reactor unit, and the jet flow stirring component unit and the reactor unit are arranged independently or integratedly.
[0017] In an embodiment of the present invention, the downstream reactor including the high-speed shear stirring component includes a high-speed shear stirring component unit and a reactor unit, and the high-speed shear stirring component unit and the reactor unit are arranged independently or integratedly.
[0018] In the embodiment of the present invention, based on the direction of pushing the material forward, the material inlet of each reactor is arranged at a position behind the stirring blades of the fast flow stirring component and / or the high-speed shear stirring component. Figure 5 As shown, the rear of the stirring blade refers to the direction in which the stirring blade pushes the material forward, the front of the blade is the front, that is, the direction in which the material flows out, and the back of the blade is the rear, that is, the direction in which the material flows in. The material inlet is arranged in this way so that the inflow point of the material is located behind the stirring blade, and the material reacts after being fully stirred and dispersed by the stirring blade.
[0019] In an embodiment of the present utility model, the stirring blades of the jet flow stirring component or the high-speed shear stirring component are two-blade or three-blade.
[0020] In an embodiment of the present utility model, the initial materials include ammonia, sulfuryl fluoride and organic amine.
[0021] In an embodiment of the utility model, the system further comprises a distillation device and an extraction device connected in series, wherein the extraction device is arranged downstream of the distillation device, and the distillation device receives the crude product of the bisfluorosulfonyl organic amine salt produced after the reaction for purification operation.
[0022] In the utility model, the system for synthesizing bisfluorosulfonyl imide organic alkali salt using ammonia and sulfuryl fluoride as starting materials can realize high selectivity and high throughput preparation of bisfluorosulfonyl imide organic alkali salt under the conditions of low energy consumption and equipment cost. In the utility model, the system for preparing bisfluorosulfonyl imide organic alkali salt combines the optimization of feeding and stirring mode, etc. to achieve the reaction yield and purity equivalent to the scheme using microchannel reactor, and is better than the scheme using microchannel reactor in terms of reaction flux. Moreover, the equipment cost of the system of the utility model is more economical than that of microchannel reactor or pipeline reactor, and the safety is higher than that of kettle reaction equipment. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The present invention can be better understood by describing exemplary embodiments of the present invention in conjunction with the accompanying drawings, in which:
[0024] Figure 1 The schematic diagram of the specific embodiment of the utility model including the jet flow stirring kettle and the high shear stirring kettle is shown, wherein 1 represents the jet flow stirring kettle, 2 represents the high shear stirring kettle, 3 represents ammonia gas, 4 represents sulfuryl fluoride, 5 represents the mixed liquid, 6 represents the jet flow agitator, and 7 represents the high shear agitator.
[0025] Figure 2 The schematic diagram of the specific embodiment of the utility model includes a jet flow stirring pipeline, a high shear stirring pipeline and a delayed reaction pipeline. Among them, 21 represents the jet flow stirring pipeline, 22 represents the high shear stirring pipeline, 23 represents ammonia gas, 24 represents sulfuryl fluoride, 25 represents a mixed liquid, 26 represents a jet flow agitator, 27 represents a high shear agitator, and 28 represents a delayed reaction pipeline.
[0026] Figure 3 The schematic diagram of the specific embodiment of the utility model includes a jet flow stirring pipeline, a high shear stirring pipeline and a time-delayed reaction kettle. 31 represents the jet flow stirring pipeline, 32 represents the high shear stirring pipeline, 33 represents ammonia gas, 34 represents sulfuryl fluoride, 35 represents a mixed liquid, 36 represents a jet flow agitator, 37 represents a high shear agitator, and 38 represents a time-delayed reaction kettle.
[0027] Figure 4 The schematic diagram of the specific embodiment of the utility model including the Jet Flow stirring pipeline and the high shear stirring kettle is shown, wherein 41 represents the Jet Flow stirring pipeline, 42 represents the high shear stirring kettle, 43 represents ammonia gas, 44 represents sulfuryl fluoride, 45 represents the mixed liquid, 46 represents the Jet Flow stirrer, and 47 represents the high shear stirrer.
[0028] Figure 5 A schematic diagram showing the relationship between the stirring front and rear of the stirring blade and the advancing direction of the material in a specific embodiment of the utility model. DETAILED DESCRIPTION
[0029] Unless otherwise defined, the technical or scientific terms used in the claims and the specification shall have the common meanings understood by persons having ordinary skills in the technical field to which the present invention belongs.
[0030] As used herein, "about" to modify, for example, the amount of an ingredient in a composition, concentration, process temperature, process time, flow rate, and the like and ranges thereof, or the dimensions of a component and the like and ranges thereof, refers to variations in the numerical amount that may occur, for example, from conventional measurements and operating procedures used in making materials, compositions, complexes, concentrates, component parts, articles of manufacture or using the formulation; from accidental errors in these procedures; from differences in the purity or composition of the manufacturing, source or starting materials used to perform the method; and similar factors.
[0031] Herein, when a numerical range is given, such as 5-25 or 5 to 25, this means at least 5 or not less than 5 and separately and independently not more than or less than 25. In some embodiments, such ranges may be independently defined as not less than 5, and separately and independently not more than 25. Values having such ranges, such as 10-15, or 10-20, also separately and independently include the lower and upper limits of the range in the same manner.
[0032] As used herein, unless otherwise specifically indicated, the "weight %" or "weight percentage" of a component is based on the total weight of the composition or object containing the component. The term "include" or "comprising" and similar words mean that the elements or objects appearing before "include" or "comprising" include the elements or objects listed after "include" or "comprising" and their equivalent elements, and do not exclude other elements or objects.
[0033] In the utility model, in the reaction of preparing bisfluorosulfonyl imide organic alkali salt with sulfuryl fluoride and ammonia as starting raw materials, except two main reactions 1-2 described below, there is also a balance of ammonium salt and triethylamine salt. Although theoretically triethylamine alkalinity is stronger than ammonia, in organic solvents, ammonium salt has poor solubility and is easily precipitated in the system, and the initial equilibrium moves to the ammonium salt. In order to make full use of ammonia, the dispersion problem of ammonium salt is involved. As can be seen from the reaction formula, side reactions may occur in raw materials, intermediates or products in the main reaction. Fortunately, among several sulfonylation reagents, raw material sulfuryl fluoride has higher activity, which makes it more feasible to suppress side reactions and also reduces difficulty. The following shows the relevant reaction of synthesizing bisfluorosulfonyl imide organic alkali salt with sulfuryl fluoride and ammonia as starting raw materials.
[0034]
[0035] Based on further research on the above content, the inventor of the utility model unexpectedly found that the use of fast and highly dispersed Jet Flow stirring components, and the optional inlet of the material in the kettle is placed behind the stirring blades of the Jet Flow stirring component, so that the material falls or the inflow point is located behind the stirring blades of the Jet Flow stirring component and / or the high-speed shear stirring component, so that the material is quickly mixed, thereby improving the selectivity and reaction rate of the reaction. In addition, adding a high-speed shear stirring component unit to the reaction process to crush the ammonium fluoride solid can increase the specific surface area and reaction rate of the ammonium fluoride solid, greatly accelerating the reaction process. It should be emphasized that the Jet Flow stirring component described in the utility model is not limited to the Jet Flow agitator and Jet Flow mixer that are already commercially available, but can also be other equivalent components that can achieve the same or similar functions, which are not exhaustively listed here. Similarly, the high-speed shear stirring component unit can not only select high-shear agitators, high-shear emulsifiers, high-shear dispersers, etc., but can also be other equivalent components that can achieve the same or similar functions, which are not exhaustively listed here. In the present invention, the jet flow stirring component and / or the high-speed shear stirring component unit can be installed in the reactor or in the pipeline. If necessary, the reactor / pipeline can be added at the same time to extend the reaction time, so as to achieve a good reaction effect and reaction flux. In comparison, the method of directly installing the stirring component in the reactor is more concise. Of course, the reactor can also be regarded as a relatively large pipeline to a certain extent.
[0036] In a specific embodiment, the system for producing bis-monofluorosulfonamide amine salt adopts a production method of kettle continuous flow or pipeline kettle series continuous flow, and the (fast) jet flow stirring is used as a dispersion method for the reaction materials. At the same time, the high-speed shear stirring component unit crushes the solids produced by the reaction, which can accelerate the reaction speed. In some specific embodiments, the jet flow stirring component can be installed in a kettle or a pipeline, and the high-speed shear stirring component unit can also be installed in a kettle or a pipeline. Usually, a reaction unit containing a jet flow stirring component and a reaction unit containing a high-speed shear stirring component unit are connected in series to form a continuous reaction device. In some specific embodiments, downstream of the continuous reaction device composed of the above, a reactor or a pipeline can be further used to extend the reaction time. The preferred method is to use a reactor. In some specific embodiments, the material inlet in each device is arranged behind the stirring component (relative to the direction in which the stirring pushes the material forward). In some specific embodiments, the maximum speed of the jet flow stirring component and the high-speed shear stirring component unit can be set to 3000rpm (revolutions per minute), which can usually be 100-3000rpm, 500-2500rpm or 1000-2000rpm. Figure 1-Figure 4 In the more specific example of the production system of the present invention, the jet flow stirring component and the high-speed shear stirring component units used are a jet flow stirrer and a high shear stirrer respectively.
[0037] like Figure 1 As shown, the utility model provides a system for producing bis(fluorosulfonyl)imide organic base salt, comprising a series-connected jet flow stirring kettle 1 and a high shear stirring kettle 2. The jet flow stirring kettle comprises a reactor with a pre-integrated stirring paddle, and a jet flow stirrer 6 installed on the reactor, the stirring blades of the jet flow stirrer are as shown in FIG. Figure 1 As shown, it is a three-blade stirring blade. The stirring paddle extends vertically into the reactor from the top center of the reactor. The Jet Flow agitator is installed on the upper part of the reactor and extends obliquely into the reactor so that its stirring blades are close to the stirring paddle. The material inlet of the Jet Flow agitator is located between the Jet Flow agitator and the stirring paddle installation position, so that the inflow point of the material entering from the material inlet is located behind the stirring blade of the Jet Flow agitator, so that it is fully dispersed. The high shear stirring reactor includes a reactor with a pre-integrated stirring paddle, and a high shear agitator 7 installed on the reactor. The high shear agitator is installed on the upper part of the corresponding reactor and extends obliquely into the reactor so that its stirring blades are close to the stirring paddle. Figure 1 As shown, the stirring blade is a three-blade stirring blade. In this system, the reactants ammonia 3 and sulfuryl fluoride 4 and the mixed solution 5 (including solvent and organic base, etc.) are first introduced into the Jet Flow stirring tank 1 and are fully dispersed and reacted by the Jet Flow agitator. The generated reaction liquid is drawn out from the Jet Flow stirring tank 1 and then passed into the subsequent downstream high shear stirring tank 2 in series. After the reaction, the reaction liquid can continue to undergo operations such as distillation and continuous extraction after being drawn out from the high shear stirring tank 2.
[0038] like Figure 2 As shown, the present invention provides a system for producing bis(fluorosulfonyl)imide organic base salt, comprising a series-connected jet flow stirring pipeline 21, a high shear stirring pipeline 22 and a delayed reaction pipeline 28. The jet flow stirring pipeline comprises a reaction pipeline body, and a jet flow stirrer 26 mounted on the reaction pipeline body. The stirring blades of the jet flow stirrer are as shown in FIG. Figure 2 As shown, it is a three-blade stirring blade. The Jet Flow agitator extends vertically into the reaction pipe body from the top center thereof. The material inlet of the Jet Flow agitator is located on the side wall of the reaction pipe body between the installation position of the Jet Flow agitator and its stirring blades, so that the inflow point of the material entering from the material inlet is located behind the stirring blades of the Jet Flow agitator, so that it is fully dispersed. The high shear stirring pipe also includes a reaction pipe body and a high shear agitator 27 installed on the reaction pipe body. The high shear agitator extends vertically into the reaction pipe body from the top center thereof, as shown in FIG. Figure 2As shown, the stirring blade of the high shear agitator is a three-blade stirring blade. In this system, the reactants ammonia 23 and sulfuryl fluoride 24 and the mixed solution 25 (including solvents and organic bases, etc.) are first introduced into the fast-flow stirring pipe 21, and are fully dispersed and reacted by the fast-flow agitator. The generated reaction liquid is drawn out from the fast-flow stirring pipe 21 and passed into the subsequent downstream high shear stirring pipe 22 in series. In order to fully react, it is drawn out from the high shear stirring pipe 22 and passed into the subsequent delayed reaction pipe 28 in series. The reaction liquid after the delayed reaction can continue to undergo operations such as distillation and continuous extraction.
[0039] like Figure 3 As shown, the utility model provides a system for producing bis(fluorosulfonyl)imide organic base salt, specifically: the system comprises a series-connected fast-flow stirring pipeline 31, a high-shear stirring pipeline 32 and a time-delayed reaction kettle 38. The fast-flow stirring pipeline comprises a reaction pipeline body, and a fast-flow stirrer 36 installed on the reaction pipeline body, and the stirring blades of the fast-flow stirrer are as shown in FIG. Figure 3 As shown, it is a three-blade stirring blade. The Jet Flow agitator extends vertically into the reaction pipe body from the top center thereof. The material inlet of the Jet Flow agitator pipe is located on the side wall of the reaction pipe body between the installation position of the Jet Flow agitator and the stirring blades, so that the inflow point of the material entering from the material inlet is located behind the stirring blades of the Jet Flow agitator, so that the material is fully dispersed. The high shear stirring pipe also includes a reaction pipe body and a high shear agitator 37 installed on the reaction pipe body. The high shear agitator extends vertically into the reaction pipe body from the top center thereof, as shown in FIG. Figure 3 As shown, the stirring blade of the high shear agitator is a three-blade stirring blade. In this system, the reactants ammonia 33 and sulfuryl fluoride 34 and the mixed liquid 35 (including solvents and organic bases, etc.) are first introduced into the Jet Flow stirring pipe 31, and are fully dispersed and reacted by the Jet Flow agitator. The generated reaction liquid is drawn out from the Jet Flow stirring pipe 31 and passed into the subsequent downstream high shear stirring pipe 32 in series. In order to fully react, it is drawn out from the high shear stirring pipe 32 and passed into the subsequent delayed reaction kettle 38 in series. The reaction liquid after the delayed reaction can continue to undergo operations such as distillation and continuous extraction.
[0040] like Figure 4 As shown, the present invention provides a system for producing bis(fluorosulfonyl)imide organic alkali salt, comprising a series-connected jet flow stirring pipeline 41 and a high shear stirring kettle 42. The jet flow stirring pipeline comprises a reaction pipeline body, and a jet flow stirrer 46 mounted on the pipeline body. The stirring blades of the jet flow stirrer are as shown in FIG. Figure 4As shown, it is a three-blade stirring blade. The Jet Flow agitator extends vertically into the reaction pipe body from the top center thereof. The material inlet of the Jet Flow agitator pipe is located on the side wall of the reaction pipe body between the installation position of the Jet Flow agitator and its stirring blades, so that the inflow point of the material entering from the material inlet is located behind the stirring blades of the Jet Flow agitator, so that it is fully dispersed. The high shear stirring kettle includes a reactor with a pre-integrated stirring paddle, and a high shear agitator 47 installed on the reactor. The high shear agitator is installed on the upper part of the corresponding reactor and extends obliquely into the reactor so that its stirring blades are close to the stirring paddles, as shown in FIG. Figure 4 As shown, the stirring blade is a three-blade stirring blade. In this system, the reactants ammonia 43 and sulfuryl fluoride 44 and the mixed solution 45 (including solvents and organic bases, etc.) are first introduced into the Jet Flow stirring pipe 41 and are fully dispersed and reacted by the Jet Flow agitator. The generated reaction liquid is drawn out from the Jet Flow stirring pipe 41 and then passed into the subsequent downstream high shear stirring kettle 42 in series. After the reaction, the reaction liquid can continue to undergo operations such as distillation and continuous extraction after being drawn out from the high shear stirring kettle 42.
[0041] Figure 5 Shows the above Figure 1-Figure 4 In the system of the utility model including the implementation mode, the relationship between the rear and front of the stirring blade of the (jet flow and high shear) agitator and the forward direction of the material is: based on the direction in which the stirring blade pushes the material forward, the front of the blade is the front, that is, the direction in which the material flows out, and the back of the blade is the rear, that is, the direction in which the material flows in.
[0042] Example
[0043] In the present utility model, Examples 1-8 adopt the following general process to produce bis(fluorosulfonyl)imide organic base salts.
[0044] 1. Mixed reaction
[0045] First, a solvent (e.g., acetonitrile) is introduced into an upstream reactor including a jet flow stirring component, a jet flow stirrer is turned on, and the temperature in each reaction unit is maintained. At the same time, ammonia, sulfuryl fluoride, an organic base (e.g., triethylamine) and a solvent are introduced in proportion. After the reaction, the reaction solution is introduced into a high shear stirring reaction device. In Table 1, the organic base and sulfuryl fluoride are measured in equivalents (eq), ammonia is measured in grams per minute (g / min) and equivalents (eq), and the solvent is measured in the ratio of solvent / organic base, for example, 1.5v means that the volume ratio of solvent / organic base is 1.5.
[0046] 2. Crushing
[0047] The solvent is introduced into the downstream reactor including the high shear stirrer in advance to ensure that the stirring operation is in the solvent. After the high shear stirrer is turned on, the reaction liquid produced in the above mixing reaction is introduced, and after being crushed, it is optionally introduced into the delayed reaction device, or directly introduced into the pre-distillation device.
[0048] 3. Delayed response
[0049] The delayed reaction device can be set up separately or integrated with the high shear stirring reaction device. After the delayed reaction, the reaction liquid is introduced into the pre-distillation device.
[0050] 3. Pre-distillation
[0051] In the pre-distillation device, the reaction liquid is removed from the reaction solvent and then introduced into the continuous extraction device.
[0052] 4. Continuous extraction
[0053] After continuous extraction of the reaction concentrate after distillation, the organic phase is introduced into a distillation device.
[0054] 5. Post-distillation
[0055] The reaction liquid after continuous extraction is then subjected to post-distillation to remove the reaction solvent, thereby obtaining a high-purity bis(fluorosulfonyl)imide organic base salt.
[0056]
[0057] Measurement Standards
[0058] Reaction liquid solid
[0059] In the present invention, the solid content of the reaction solution is measured by visual inspection and filtering and weighing; the solid content is measured as a mass percentage relative to the final product.
[0060] Ionic impurities in reaction solution
[0061] In the present invention, the ionic impurities in the reaction solution are detected by ion chromatography. The ionic impurities in the reaction solution include fluoride ions, monofluorosulfonate ions (from the hydrolysis of excess sulfuryl fluoride), bisfluorosulfonamide ions (FSI - ) other unexpected impurity ions; the content of impurity ions is expressed as relative FSI - The weight percentage is measured.
[0062] Product Purity
[0063] In the utility model, the purity of the product is detected by ion chromatography and calculated by normalization method.
[0064] Product yield
[0065] In the utility model, the product yield is calculated after the content is measured by an external standard method using an ion chromatograph.
[0066] Although the utility model has been described in conjunction with specific embodiments, it will be appreciated by those skilled in the art that many modifications and variations may be made to the utility model. Therefore, it is to be appreciated that the intent of the claims is to cover all such modifications and variations within the true concept and scope of the utility model.
Claims
1. A system for producing bis(fluorosulfonyl)imide organic base salt, characterized in that: The system includes: at least one upstream reactor including a jet flow agitation element and at least one downstream reactor including a high shear agitation element connected in series; The jet flow stirring component is used to disperse the initial material entering the upstream reactor; the high-speed shear stirring component is used to crush the solid in the downstream reactor.
2. The system according to claim 1, characterized in that The upstream reactor is used for performing a reaction to generate a bisfluorosulfonyl imide organic base salt; The downstream reactor receives the intermediate material output from the upstream reactor and continues the reaction of generating the bisfluorosulfonyl imide organic base salt.
3. The system according to claim 1 or 2, wherein: The system further comprises: a time delay reactor located downstream of the downstream reactor.
4. The system according to claim 1 or 2, wherein: The upstream reactor, the downstream reactor and the delayed reactor are each independently selected from a tank continuous flow reactor, a tubular continuous flow reactor and a tubular-tank continuous flow reactor.
5. The system according to claim 1 or 2, wherein: The upstream reactor including the jet flow stirring component includes a jet flow stirring component unit and a reactor unit, and the jet flow stirring component unit and the reactor unit are arranged independently or integratedly.
6. The system according to claim 1 or 2, wherein: The downstream reactor including the high-speed shear stirring component includes a high-speed shear stirring component unit and a reactor unit, and the high-speed shear stirring component unit and the reactor unit are arranged independently or integratedly.
7. The system according to claim 1, wherein: Based on the direction of pushing the material forward, the material inlet of each reactor is arranged at a position behind the stirring blades of the jet flow stirring component and / or the high-speed shear stirring component.
8. The system according to claim 1 or 7, wherein: The stirring blades of the jet flow stirring component or the high speed shear stirring component are two-blade or three-blade.
9. The system according to claim 3, wherein: The delayed reactor comprises a high-speed shear stirring component unit and a reactor unit, and the high-speed shear stirring component unit and the reactor unit are arranged independently or integratedly.
Citation Information
Patent Citations
Preparation method of bis (fluorosulfonyl) imine compound, bis (fluorosulfonyl) imine ionic liquid and bis (fluorosulfonyl) imine lithium
CN115140716A
Method for high-selectivity synthesis of bis (fluorosulfonyl) imide triethylamine salt
CN116281895A