CN217756905U - Preparation process system of lithium bis (fluorosulfonyl) imide - Google Patents
Preparation process system of lithium bis (fluorosulfonyl) imide Download PDFInfo
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- CN217756905U CN217756905U CN202222204081.XU CN202222204081U CN217756905U CN 217756905 U CN217756905 U CN 217756905U CN 202222204081 U CN202222204081 U CN 202222204081U CN 217756905 U CN217756905 U CN 217756905U
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Abstract
The utility model relates to the technical field of lithium battery material preparation, and discloses a process system for preparing bis (fluorosulfonyl) imide lithium, which comprises a continuous chlorination unit A, a continuous fluorination unit B, a continuous salifying unit C, a product purification unit D and a tail gas treatment unit E; the utility model discloses utilize the modularization production, adopt stable three-step method technology production difluoride sulfimide lithium, chlorination, fluorination and salification process are gone on step by step, have avoided chlorination and have fluoridized the safety problem that one step of going on existing among the prior art, can realize serialization production, and the accessory substance is few, and rate of raw materials utilization improves, and the volume of solid useless mixed salt reduces by a wide margin, and the environmental protection waste liquid also reduces to some extent, and complete system equipment is less, easy operation, and the accessory substance is less, and the equipment investment tradition technology can reduce more than 20%.
Description
Technical Field
The utility model relates to a lithium battery material preparation technical field, concretely relates to lithium bifluorosulfonyl imide preparation process system.
Background
With the rapid development of society, china has become the first major consumer nation of petroleum, but because of limited energy, the stability is always tested due to environmental changes, and the development of new energy sources of 'replacing oil with electricity and storing electricity by staggering peaks' is more beneficial to long-term development. With the rapid development of economy and the popularization of automobiles in China, environmental pollution is prominent day by day, and the development of new energy batteries becomes a necessary way for sustainable development due to tail gas discharged by traditional automobiles and environmental pollution caused by traditional lead-acid batteries. And the lithium cell possesses excellent product property ability, and especially energy density is high, and cycle number is high, and safety ring protects etc for energy storage type lithium electricity is triggered the explosive type and is increased, "photovoltaic power generation, battery energy storage, terminal application" merge the energy electronic industry chain of innovation and accelerate development step by step, and light stores up integratively, and the integration of energy storage of staggering peak accelerates the construction.
In consideration of the factors of battery cost, safety performance and the like, lithium hexafluorophosphate (LiPF 6) is the lithium battery solute lithium salt which is most widely used commercially, however, in the using process, liPF6 also has the problems of poor thermal stability, easy hydrolysis and the like, and the battery capacity is rapidly attenuated, and potential safety hazards are brought. The solute lithium salt lithium bifluorosulfonyl imide (LIFSI) of the novel electrolyte has the physicochemical properties far better than those of LiPF 6: higher thermal stability-the melting point of LiFSI is 145 ℃, the decomposition temperature is higher than 200 ℃; better conductivity and good high-rate discharge performance; better thermodynamic stability-the LiFSI electrolyte has good compatibility with two main components of the SEI film, and only has a displacement reaction with partial components at 160 ℃. LiFSI can become the best substitute for improving the defects of LiPF6, and accords with the development trend of future electrolytes.
The prior art for LiFSI preparation generally involves: synthesis of bis (chlorosulfonyl) imide, preparation of bis (fluorosulfonyl) imide by fluorination reaction (using bis (chlorosulfonyl) imide, potassium fluoride and triethylamine as raw materials), and lithiation using LiOH or LiCO 3 As raw material), such as CN110217763A, in a method for preparing lithium bis (fluorosulfonyl) imide, which is disclosed by the specification, thionyl chloride, sulfamic acid, chlorosulfonic acid and an incubator are reacted together in a reaction kettle at a certain temperature to generate the lithium bis (fluorosulfonyl) imideAnd reacting amine with the suspension of the polar solvent, lithium carbonate and thionyl chloride to generate suspension of the lithium bis (fluorosulfonyl) imide, and filtering and drying to obtain a finished product.
The whole process is complex, more equipment is used, the fluorination step not only can rapidly release heat in a large amount, but also involves high-risk raw materials, so that the entrance threshold is higher, the operation can only be intermittently performed due to safety, and the problems of more byproducts and high three wastes caused by adopting potassium fluoride as the raw material cause very high preparation cost of the whole process. Therefore, a LiFSI preparation process system which has lower preparation cost and less three wastes and can be continuously and safely produced is needed.
SUMMERY OF THE UTILITY MODEL
The utility model discloses there is the accessory substance many to LIFSI's production preparation technology among the prior art, and the problem that the three wastes are high provides a neotype difluoride sulfonyl imide lithium preparation process systems, and this system adopts stable three-step process to replace traditional potassium fluoride with hydrogen fluoride, cost such as raw and other materials consumption, manual work, depreciation descend by a wide margin, and the volume of solid useless mixed salt reduces by a wide margin, and the environmental protection waste liquid also reduces to some extent, and cost reduction is more than 20%.
In order to achieve the above object, the utility model adopts the following technical scheme:
a process system for preparing lithium bis (fluorosulfonyl) imide comprises a continuous chlorination unit A, a continuous fluorination unit B, a continuous salt forming unit C, a product purification unit D and a tail gas treatment unit E;
the continuous chlorination unit A comprises a solid phase mixer A1, a chlorination reaction kettle A2, a chlorination gas-liquid separation tower A3 and a solvent recovery tower A4 which are connected in sequence;
the continuous fluorination unit B comprises a fluorination reaction kettle B1, a fluorination gas-liquid separation tower B2, an impurity removal kettle B3, a film evaporator B4 and a rectifying tower B5 which are connected in sequence;
the continuous salifying unit C comprises a dissolving kettle C1, a salifying reactor C2, a salifying gas-liquid separation tower C3, a dehydration kettle C4, a solvent evaporator C5 and a solvent recovery tower C6 which are connected in sequence,
the product purification unit D comprises a continuous crystallizer D1 and a dryer D2 which are connected in sequence;
a gas-phase discharge port of the chlorination gas-liquid separation tower A3 is connected with the tail gas treatment unit E, and a liquid-phase discharge port is connected with the fluorination reaction kettle B1;
a gas-phase discharge port of the fluorination gas-liquid separation tower B2 is connected with the tail gas treatment unit E, and a liquid-phase discharge port is connected with the impurity removal kettle B3; the discharge hole of the rectifying tower B5 is connected with the dissolving kettle C1;
salify vapour and liquid separator C3's gaseous phase discharge gate is connected with tail gas processing unit E, and the liquid phase discharge gate is connected with dehydration cauldron C4, and solvent evaporator C5 gaseous phase discharge gate is connected with tail gas processing unit E, and the liquid phase discharge gate is connected with continuous crystallizer D1.
The utility model discloses utilize the modularization production, adopt stable three-step method technology production difluoride sulfimide lithium, chlorination, fluorination and salification process go on step by step, have avoided chlorination and have fluoridized the safety problem that one step of going on existence among the prior art, can realize serialization production, and the accessory substance is few, and material utilization improves, and the volume of solid useless mixed salt reduces by a wide margin, and the environmental protection waste liquid also reduces to some extent.
Preferably, the continuous chlorination unit a further comprises a solvent recovery tower A4 connected with a liquid phase discharge port of the chlorination gas-liquid separation tower A3, the solvent recovered in the solvent recovery tower A4 is used for recycling the chlorination reaction kettle A2, and the liquid phase discharge port is connected with the fluorination reaction kettle B1. In the reaction process, the thionyl chloride can be recycled back to the chlorination reaction kettle for recycling through the solvent recovery tower, so that the utilization rate of raw materials is improved, and the cost and the production amount of waste liquid are reduced.
Preferably, the continuous salt-forming unit C further comprises a solvent recovery tower C6 connected with a gas-phase discharge port of the solvent evaporator C5, the solvent recovered in the solvent recovery tower C6 is used for recycling the dissolution kettle C1, and the recovered liquid phase returns to the dehydration kettle C4 for continuous dehydration. Similarly, acetonitrile solution mixed with part of lithium bis (fluorosulfonyl) imide in a discharge port of the solvent evaporator C5 is recovered through a solvent recovery tower, acetonitrile can return to the dissolution kettle for continuous use, and liquid-phase lithium bis (fluorosulfonyl) imide mixed solution can return to the dehydration kettle for continuous dehydration, so that the acetonitrile raw material utilization rate and the product yield are improved.
Preferably, the fluorinating agent added in the fluorination reaction kettle B1 is hydrogen fluoride. The utility model discloses a traditional potassium fluoride is replaced to hydrogen fluoride, can reduce material cost by a wide margin, and produced accessory substance is HCl, adopt alkali to absorb can, compare in prior art potassium fluoride treatment cost lower, economic benefits is higher.
Preferably, the tail gas treatment unit E comprises a water absorption tower E1, an alkali absorption tower E2 and a refrigerator E3 connected in sequence. Gas phase product HCl/SO of continuous chlorination unit A 2 Absorbing the mixed gas with water in a water absorption tower E1 to obtain hydrochloric acid as a byproduct, and the rest contains SO 2 Absorbing sulfur dioxide with caustic soda through an alkali absorption tower E2 to obtain sodium sulfite; in the continuous fluorination unit B, hydrogen fluoride is used as a raw material, and gas-phase products are excessive hydrogen fluoride and a byproduct hydrogen chloride, and tail gas treatment can also be realized through a water absorption tower, an alkali absorption tower and a refrigerator.
Preferably, said product purification unit D further comprises a packaging machine D3 connected to the dryer.
Preferably, the solid phase mixer is preceded by a continuous grinder A5 for grinding the sulfamic acid feed.
Preferably, the continuous chlorination unit A comprises at least two chlorination reaction kettles A2 connected in series. So as to realize the continuous chlorination production of the raw materials in the whole process and ensure the process yield.
Preferably, the continuous fluorination unit B comprises at least two fluorination reaction kettles B1 connected in series. So as to realize continuous chlorination production of the intermediate product in the whole process and guarantee the process yield.
Compared with the prior art, the utility model discloses following beneficial effect has:
the utility model discloses a stable three-step process production difluoride sulfimide lithium, chloridize, it goes on with salification process substep to fluoridize, the safety problem who exists is carried out in one step to chloridize among the having avoided prior art and fluoridize, can realize serialization production, the accessory substance is few, material utilization improves, and use HF as the reagent of fluoridizing, and is with low costs, the raw materials is easily obtained, the accessory substance can be handled through simple tail gas processing apparatus, the volume of solid useless mixed salt reduces by a wide margin, the environmental protection waste liquid also reduces to some extent, whole system equipment is less, and easy operation, the accessory substance is less, the equipment investment can reduce more than 20% than traditional technology.
Drawings
FIG. 1 is a schematic diagram of the preparation of bis (chlorosulfonyl) imide in the process system for preparing lithium bis (fluorosulfonyl) imide in example 1.
Fig. 2 is a schematic diagram of preparation of lithium bis (chlorosulfonyl) imide from bis (chlorosulfonyl) imide in the process for preparation of lithium bis (fluorosulfonyl) imide in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention can be modified or substituted by other modifications without departing from the spirit and scope of the present invention, and all such modifications and substitutions are intended to be covered by the present invention.
Example 1
A preparation process system of lithium bis (fluorosulfonyl) imide is shown in figures 1 and 2 and comprises a continuous chlorination unit A, a continuous fluorination unit B, a continuous salt formation unit C, a product purification unit D and a tail gas treatment unit E;
the continuous chlorination unit A comprises a solid phase mixer A1, at least two chlorination reaction kettles A2 (only one whole is shown as a representation) connected in series, a chlorination gas-liquid separation tower A3 and a solvent recovery tower A4 which are connected in sequence; the continuous fluorination unit B comprises at least two serially connected fluorination reaction kettles B1 (only one whole is drawn as a representation), a fluorination gas-liquid separation tower B2, an impurity removal kettle B3, a film evaporator B4 and a rectifying tower B5 which are sequentially connected; the continuous salifying unit C comprises a dissolving kettle C1, a salifying reactor C2, a salifying gas-liquid separation tower C3, a dehydration kettle C4, a solvent evaporator C5 and a solvent recovery tower C6 which are connected in sequence; the product purification unit D comprises a continuous crystallizer D1, a dryer D2 and a packaging machine D3 which are connected in sequence; the tail gas treatment unit E comprises a water absorption tower E1, an alkali absorption tower E2 and a refrigerator E3 which are connected in sequence.
A continuous grinding machine A5 is arranged in front of the solid-phase mixer and is used for grinding the sulfamic acid raw material; the gas phase discharge port of the chlorination gas-liquid separation tower A3 is connected with the tail gas treatment unit E, the liquid phase discharge port is connected with the solvent recovery tower A4, the recovered solvent in the solvent recovery tower A4 is used for recycling the chlorination reaction kettle A2, and the liquid phase discharge port is connected with the fluorination reaction kettle B1.
A gas-phase discharge port of the fluorination gas-liquid separation tower B2 is connected with the tail gas treatment unit E, and a liquid-phase discharge port is connected with the impurity removal kettle B3; the discharge hole of the rectifying tower B5 is connected with the dissolving kettle C1;
a gas-phase discharge port of the salified gas-liquid separator C3 is connected with the tail gas treatment unit E, a liquid-phase discharge port is connected with the dehydration kettle C4, a gas-phase discharge port of the solvent evaporator C5 is connected with the solvent recovery tower C6, and a liquid-phase discharge port is connected with the continuous crystallizer D1; the solvent recovered in the solvent recovery tower C6 is used for recycling the dissolving kettle C1, and the recovered liquid phase returns to the dehydration kettle C4 for continuous dehydration.
The whole preparation process of the lithium bis (fluorosulfonyl) imide comprises the following steps: grinding sulfamic acid by a continuous grinding machine A5, mixing the sulfamic acid with chlorosulfonic acid in a solid-phase mixer A1, then allowing the mixture and thionyl chloride to enter a chlorination reactor A2 for continuous reaction to prepare a mixed liquid containing the bischlorosulfonimide, separating the mixed liquid by a chlorination gas-liquid separation tower A3, separating the mixed gas of hydrogen chloride and sulfur dioxide in tail gas and sending the mixed gas to a tail gas treatment unit E, sending the rest liquid to a solvent recovery tower A4, sending the thionyl chloride solvent into the chlorination reactor A2 for recycling, and sending the rest bischlorosulfonimide mixed liquid to a continuous fluorination unit B.
The method comprises the steps of feeding a dichlorosulfimide mixed solution prepared by a continuous chlorination unit A into a series-connected fluorination reaction kettle B1 to continuously react with anhydrous hydrogen fluoride to obtain a mixed liquid containing the dichlorosulfimide, feeding the mixed liquid into a fluorination gas-liquid separation tower B2, separating excessive hydrogen fluoride and a byproduct hydrogen chloride mixed gas, feeding the mixed gas into a tail gas treatment unit E, feeding the residual liquid into an impurity removal kettle B3, adding an auxiliary agent to remove impurities, purifying by using a thin film evaporator B4 and a rectifying tower B5, and feeding a dichlorosulfimide product into a continuous salification unit C.
The bis-fluorosulfonyl imide product prepared by the continuous fluorination unit B is dissolved in acetonitrile solvent and lithium carbonateStirring the mixture in a kettle C1, feeding the mixture into a salt-forming reactor C2 connected in series for continuous reaction to prepare mixed liquid containing lithium bis (fluorosulfonyl) imide, feeding the mixed liquid into a salt-forming gas-liquid separation tower C3, and separating CO 2 And (3) sending the liquid to a tail gas treatment unit E, dehydrating the liquid through a dehydration kettle C4, obtaining a refined lithium bis (fluorosulfonyl) imide liquid through a solvent evaporator C5, feeding redundant gas-phase products in the solvent evaporator C5 into a solvent recovery tower C6, recovering the recovered acetonitrile for reacting with salifying to serve as a solvent, returning the liquid phase containing the lithium bis (fluorosulfonyl) imide to the dehydration kettle for continuous dehydration, and feeding the refined lithium bis (fluorosulfonyl) imide liquid obtained by the solvent evaporator C5 into a product purification unit D.
After the refined lithium bis (fluorosulfonyl) imide liquid is crystallized and purified by a continuous crystallizer D1, the crystals are sent to a dryer D2 for drying, and the dryer D2 can take away CO by adopting nitrogen 2 And (3) gas is generated to obtain a dry lithium bis (fluorosulfonyl) imide product, and the dry lithium bis (fluorosulfonyl) imide product is sent to a packaging machine D3 for product sub-packaging to obtain a final lithium bis (fluorosulfonyl) imide product.
Wherein the tail gas treatment unit E comprises a water absorption tower E1, an alkali absorption tower E2, a refrigerator E3, HCL/SO 2 The mixed gas is absorbed by water through a water absorption tower E1 to obtain by-product hydrochloric acid, and the rest contains SO 2 Absorbing the sulfur dioxide with caustic soda by an alkali absorption tower E2 to obtain sodium sulfite.
The reaction temperature of the chlorination procedure is 120-140 ℃, and the molar ratio of sulfamic acid, thionyl chloride and chlorosulfonic acid is 1: 2-2.4: 1 to 1.3, and the yield of the bis (chlorosulfonyl) imide is 95 percent based on sulfamic acid;
fluorination step reaction temperature: 100-140 ℃, and the molar ratio of the bischlorosulfonimide to the hydrogen fluoride is 1:2 to 3, the yield of the bis (fluorosulfonyl) imide is 97 percent based on the bis (chlorosulfonyl) imide;
reaction temperature in the salt forming process: at 0-40 ℃, the molar ratio of the bis-fluorosulfonyl imide to the lithium carbonate is 1:0.5 to 0.8, and the yield of the lithium bis (fluorosulfonyl) imide is 96 percent based on the lithium bis (fluorosulfonyl) imide;
the utility model discloses adopting stable three-step process technology can realize the reliable and stable production of difluoride sulfonyl imide lithium in succession, drop into cost such as hydrogen fluoride raw and other materials consumption, manual work, depreciation by a wide margin, the volume of solid useless mixed salt reduces by a wide margin, and the environmental protection waste liquid also reduces to some extent, and the equipment investment can reduce more than 20% than more than traditional technology.
Claims (9)
1. A preparation process system of lithium bis (fluorosulfonyl) imide is characterized by comprising a continuous chlorination unit A, a continuous fluorination unit B, a continuous salt formation unit C, a product purification unit D and a tail gas treatment unit E;
the continuous chlorination unit A comprises a solid phase mixer A1, a chlorination reaction kettle A2 and a chlorination gas-liquid separation tower A3 which are connected in sequence; the continuous fluorination unit B comprises a fluorination reaction kettle B1, a fluorination gas-liquid separation tower B2, an impurity removal kettle B3, a film evaporator B4 and a rectifying tower B5 which are connected in sequence; the continuous salifying unit C comprises a dissolving kettle C1, a salifying reactor C2, a salifying gas-liquid separation tower C3, a dehydration kettle C4 and a solvent evaporator C5 which are connected in sequence; the product purification unit D comprises a continuous crystallizer D1 and a dryer D2 which are connected in sequence;
a gas-phase discharge port of the chlorination gas-liquid separation tower A3 is connected with the tail gas treatment unit E, and a liquid-phase discharge port is connected with the fluorination reaction kettle B1; a gas phase discharge port of the fluorination gas-liquid separation tower B2 is connected with a tail gas treatment unit E, and a liquid phase discharge port is connected with an impurity removal kettle B3; the discharge hole of the rectifying tower B5 is connected with the dissolving kettle C1; salify vapour and liquid separator C3's gaseous phase discharge gate is connected with tail gas processing unit E, and the liquid phase discharge gate is connected with dehydration cauldron C4, and solvent evaporator C5 gaseous phase discharge gate is connected with tail gas processing unit E, and the liquid phase discharge gate is connected with continuous crystallizer D1.
2. The lithium bis (fluorosulfonyl) imide preparation process system according to claim 1, wherein said continuous chlorination unit a further comprises a solvent recovery column A4 connected to a liquid phase discharge port of the chlorination gas-liquid separation column A3, wherein the solvent recovered in the solvent recovery column A4 is used for recycling of the chlorination reactor A2, and the liquid phase discharge port is connected to the fluorination reactor B1.
3. The lithium bis (fluorosulfonyl) imide preparation process system according to claim 1, wherein said continuous salt formation unit C further comprises a solvent recovery column C6 connected to a gas phase discharge port of the solvent evaporator C5, the solvent recovered in the solvent recovery column C6 is used for recycling of the dissolution tank C1, and the recovered liquid phase is returned to the dehydration tank C4 for continuous dehydration.
4. The lithium bis (fluorosulfonyl) imide preparation process system according to claim 1, wherein the fluorinating agent added to fluorination reaction vessel B1 is hydrogen fluoride.
5. The lithium bis (fluorosulfonyl) imide preparation process system according to claim 1, wherein said tail gas treatment unit E comprises a water absorption tower E1, an alkali absorption tower E2, and a refrigerator E3, which are connected in sequence.
6. The lithium bis (fluorosulfonyl) imide preparation process system of claim 1 wherein said product purification unit D further comprises a packaging machine D3 connected to a dryer.
7. The lithium bis (fluorosulfonyl) imide preparation process system of claim 1 wherein said solid phase mixer is preceded by a continuous grinder A5 for grinding sulfamic acid feed stock.
8. The lithium bis (fluorosulfonyl) imide preparation process system according to claim 1, wherein said continuous chlorination unit a comprises at least two chlorination reactors A2 connected in series.
9. The lithium bis (fluorosulfonyl) imide preparation process system according to claim 1, wherein said continuous fluorination unit B comprises at least two fluorination reaction vessels B1 connected in series.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117263146A (en) * | 2023-11-23 | 2023-12-22 | 万华化学集团股份有限公司 | Continuous production device system and production method for liquid difluoro sulfonyl imide salt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117263146A (en) * | 2023-11-23 | 2023-12-22 | 万华化学集团股份有限公司 | Continuous production device system and production method for liquid difluoro sulfonyl imide salt |
| CN117263146B (en) * | 2023-11-23 | 2024-01-30 | 万华化学集团股份有限公司 | Continuous production device system and production method for liquid difluoro sulfonyl imide salt |
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