CN104925765A - Preparation method for difluorosulfimide lithium salt - Google Patents
Preparation method for difluorosulfimide lithium salt Download PDFInfo
- Publication number
- CN104925765A CN104925765A CN201510261089.1A CN201510261089A CN104925765A CN 104925765 A CN104925765 A CN 104925765A CN 201510261089 A CN201510261089 A CN 201510261089A CN 104925765 A CN104925765 A CN 104925765A
- Authority
- CN
- China
- Prior art keywords
- lithium
- preparation
- fluorine sulfimide
- described step
- alkaline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
- C01B21/0935—Imidodisulfonic acid; Nitrilotrisulfonic acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/086—Compounds containing nitrogen and non-metals and optionally metals containing one or more sulfur atoms
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
- C01B21/096—Amidosulfonic acid; Salts thereof
Abstract
The invention relates to the field of lithium batteries and lithium capacitors, in particular to a preparation method for difluorosulfimide lithium salt and application of the difluorosulfimide lithium salt. The preparation method for the difluorosulfimide lithium salt, provided by the invention, comprises the following steps: (1) performing fluorination reaction: synthetizing midbody difluorosulfimide from dichlorosulfimide and hydrogen fluoride under the action of a catalyst; (2) performing reaction between the difluorosulfimide obtained in the step 1 and alkaline lithium, and performing solid-liquid separation after the reaction to obtain an LiFSI product. The preparation method for the difluorosulfimide lithium salt, provided by the invention, is low in cost, few in by-product and simple in post-treatment, and the quality and the purity of the product are ensured, therefore the preparation method which is capable of obtaining the high-quality and high-purity product and is economic and practical is provided; the preparation method is suitable for industrial production.
Description
Technical field
The present invention relates to lithium cell and lithium capacitor area, particularly relate to the preparation method and its usage of a kind of pair of fluorine sulfimide lithium salts.
Background technology
In the periodic table of elements, fluorine is the maximum element of electronegativity.After often introducing fluorine element in a compound, its physics and chemistry character generation noticeable change, also therefore, many fluorine-containing lithium compounds, as two trifluoromethanesulfonimide lithium (LiTFSI) and lithium hexafluoro phosphate (LiPF
6), be widely used in the electric property improving battery and electric capacity.US Patent No. 5916475 discloses a kind of than LiTFSI and LiPF
6there is better thermostability and chemical stability, the fluorine-containing lithium salts of higher electroconductibility and lower erosion rate---two fluorine sulfimide lithium (LiFSI), and be considered to likely replace LiPF
6the two fluoro lithium salts of one, in lithium cell and ultracapacitor, will splendid application prospect be had.
The synthetic method of most of LiFSI is all first synthesize two chlorine sulfimide (HClSI), then (M is 11-15 race with MFn, 4-6 period element) reaction, prepare the salt intermediate of two fluorine sulfimides of corresponding metal or organic bases, then with LiOH or Li
2cO
3carry out cation exchange reaction and obtain LiFSI (US2013331609, US2012041233, EP2415757, US2011034716), the shortcoming of these methods is, permutoid reaction is difficult to after reaching a balance carry out completely, and the intermediate MSFI that unreacted is complete (M refers to metallic cation, organic base cation) be difficult to be separated completely with LiSFI completely, obtain the product of high-quality.
And adopt HClSI directly to react when preparing LiFSI (US2004097757) with LiF, macro-corrosion gas HF can be produced, while excessive LiF and LiFSI be also not easy to be separated.
Although also have report, with two fluorine sulfimide potassium (KFSI) of purifying and LiClO
4metal exchange prepares LiFSI, but in product, potassium ion is often very high, have impact on its practical application, and LiClO
4with the KClO generated
4, all there is certain risk of explosion (Electrochimical Acta, 2012,66, PP.320-324, Polyhedron, 2006,25, PP.1292-1298, CN101747242, CN101747243, CN101654229).In addition, due to LiClO
4general needs participate in reaction little over amount, but due to himself water absorbability strong, cause final product to contain a small amount of LiClO
4cannot remove, the purity of the finished product LiFSI cannot be ensured.
US8377406 disclose in aqueous two fluorine sulfimide (HFSI) directly and Quilonum Retard react the method preparing LiFSI, but also there is obvious deficiency in the method, very exothermic when HFSI is water-soluble, thus cause the decomposition of HFSI, the method that this patent have employed very low temperature (-78 DEG C) the preparation HFSI aqueous solution solve HFSI water-soluble time very exothermic technical problem, but such a process increases a large amount of energy consumption, more importantly, LiFSI has extraordinary water-soluble, extraction efficiency is very low, is not suitable for suitability for industrialized production.
JP2013091524 has carried out comparatively systematic research to the stability of LiFSI, find that LiFSI is in the environment of temperature more than 40 DEG C, decomposition rate is accelerated, and moisture is larger, decompose faster, therefore, this area uses reagent cheap and easy to get in the urgent need to one, to be swift in response and thoroughly, yield is high, few and the method for the two fluorine sulfimide lithium salts of easily removing, the synthesis preparation that lithium salts not easily decomposes, post processing mode is easy of by product, thus significantly reduce the cost of product, and make it be more suitable for suitability for industrialized production.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of preparation method of two fluorine sulfimide lithium salts (LiFSI), for solving the problems of the prior art.
For achieving the above object and other relevant objects, the invention provides a kind of preparation method of two fluorine sulfimide lithium salts (LiFSI), comprise the steps:
(1) fluoridation: by two chlorine sulfimide (HClSI) and the two fluorine sulfimide (HFSI) of hydrogen fluoride (HF) synthetic intermediate under catalyst action;
(2) two for step 1 gained fluorine sulfimide (HFSI) is reacted with alkaline, lithium, reacted rear solid-liquid separation, namely obtained LiFSI product.
The reaction equation of described step 1 is as follows:
Preferably, in described step 1, the concrete grammar of fluoridation is: HClSI, catalyzer are placed in reaction unit, passes into HF gas and reacts.
Preferably, in described step 1, catalyzer is preferably lewis acid, is more preferably SbCl
5, TiCl
4, SnCl
4, MoCl
5in one or more combination.
Preferably, in described step 1, the mol ratio of HClSI and catalyzer is preferably 1:0.05 ‰ ~ 1:1 ‰, is more preferably 1:0.1 ‰ ~ 1:0.5 ‰.
Preferably, in described step 1, HClSI and HF mol ratio is preferably 1:1.4 ~ 1:4, is more preferably 1:1.7 ~ 1:2.
Preferably, in described step 1, the temperature of reaction of reaction system is react at 90 ~ 110 DEG C, reacts at being more preferably 100 ~ 105 DEG C.
Preferably, in described step 1, by HClSI and HF synthetic intermediate HFSI under catalyst action, react HF and the HCl gas in rear removing reaction system, obtained intermediate double fluorine sulfimide.
Preferred, the method for HF and the HCl gas in described removing reaction system is for distilling reaction system or advertising reaction system and distill.
Preferred further, temperature when advertising is room temperature, and the time of advertising is 10-20 hour, and described distillation is underpressure distillation.
Preferably, in described step (2), described alkaline, lithium is LiOH, LiHCO
3or Li
2cO
3in one or more combination.
Preferably, in HFSI and alkaline, lithium, the mol ratio of lithium is preferably 1:0.8 ~ 1:1, is more preferably 1:0.9 ~ 1:0.98.
When alkaline, lithium is LiOH, reaction equation is as follows:
When alkaline, lithium is Li
2cO
3time, reaction equation is as follows:
When alkaline, lithium is Li
2hCO
3time, reaction equation is as follows:
Preferably, in described step (2), joined in alkaline, lithium solvent system by step 1 products therefrom, and adding and/or preferably cooling reaction system in reaction process, preferred feed postition is for dripping.
Preferred, the temperature of reaction of reaction system is react at 0 ~ 20 DEG C, reacts at being more preferably 0 ~ 5 DEG C.
Preferred, the solvent in described alkaline, lithium solvent system is low polar solvent, is more preferably hexane, hexanaphthene, methylene dichloride, ethylene dichloride, toluene, dimethylbenzene, chlorobenzene, one or more the combination in dichlorobenzene.
Preferably, in described step (2), two for step 1 gained fluorine sulfimide (HFSI) is reacted with alkaline, lithium, after having reacted, in reaction system, drips SOCl
2with the moisture in the system of having reacted, solid-liquid separation, namely obtains LiFSI product.
Preferred, drip SOCl
2carry out under room temperature condition.
Preferably, in described step (2), two for step 1 gained fluorine sulfimide (HFSI) is reacted with alkaline, lithium, reacted rear solid-liquid separation gained LiFSI product and also carried out making beating process.
Preferred, described making beating process concrete grammar be: solid-liquid separation gained LiFSI is added making beating solvent and metal ion remover carry out making beating process, namely obtain the LiFSI product of purifying.
Preferred further, described making beating solvent is low polar solvent, is more preferably hexane, hexanaphthene, methylene dichloride, ethylene dichloride, toluene, dimethylbenzene, chlorobenzene, one or more the combination in dichlorobenzene.
Further preferred, described metal ion remover is selected from one or more the combination also in-18-hat-6 of 12-crown-4,15-hat-5,18-hat-6, bicyclohexane.
Two fluorine sulfimide lithium salts (LIFSI) preparation methods involved in the present invention, have following advantage:
1. be fluorination reagent with HF, cost is low, and raw material is easy to get, and fluoridize under catalyst action thoroughly, the by product brought is few, and by product HCl only need with Alkali absorption; Reaction terminates most HF and HCl in rear system and can be advertised by nitrogen and take away, and remaining a small amount of is removed by distillation, thus ensure that purity and the quality of intermediate HFSI.
2. with two fluorine sulfimide (HFSI) and LiOH or LiHCO
3, Li
2cO
3reaction, speed is fast, and thoroughly, the by product of generation is water (water is very good to the solubleness of LiFSI, has water to there is product and is difficult to separate out), can by SOCl in reaction
2leniently remove at low temperatures, product can be made slowly to separate out after moisture removing, make separation become simple, generate by product SO simultaneously
2, HCl (also has CO
2) all absorbed by buck, there is not the by product of other complexity.
3., simultaneously because the equivalents of two fluorine sulfimide (HFSI) is greater than the equivalents of lithium, ensure that all alkaline, lithium are all by complete reaction, excessive HFSI owing to being liquid, with SOCl remaining in system
2(liquid), SO
2(gas), HCl (gas) or CO
2(gas) can be filtered and pull an oar removing, thus ensure that the purity of product.
4. because product is extremely responsive to temperature, under high temperature, product very easily decomposes, and therefore the present invention successfully avoids warming operation at crucial salt-forming steps, thus ensures quality and the purity of product.
5 the present invention adopt non-aqueous system, and the three wastes are few, and yield is high, and all solvents can facilitate recovery, economical and practical; The metal ions such as the potassium adopting crown ether likely to introduce in removing system during aftertreatment and sodium, can improve quality and the performance of LiFSI.
Visible, the invention provides and a kind ofly can obtain high-quality high purity product and economical and practical preparation method, be applicable to suitability for industrialized production.
Embodiment
Inventor with hydrogen fluoride (HF) and two chlorine sulfimide (HClSI) for raw material, fluoridize under catalyst action and obtain intermediate double fluorine sulfimide (HFSI), the latter reacts with the alkaline, lithium of certain equivalent and prepares the highly purified LiFSI of high-quality (two fluorine sulfimide lithium salts, CAS:171611-11-3) product, thus provide a kind of simple efficient method to prepare high-quality LiFSI, complete the present invention on this basis.
The invention provides a kind of preparation method of two fluorine sulfimide lithium salts (LiFSI), comprise the steps:
(1) fluoridation: by two chlorine sulfimide (HClSI) and the two fluorine sulfimide (HFSI) of hydrogen fluoride (HF) synthetic intermediate under catalyst action, reaction equation is as follows:
In described step 1, the concrete grammar of fluoridation is: HClSI, catalyzer are placed in reaction unit, passes into HF gas and reacts.
In described step 1, catalyzer is preferably lewis acid, is more preferably SbCl
5, TiCl
4, SnCl
4, MoCl
5in one or more combination, the mol ratio of HClSI and catalyzer is preferably 1:0.05 ‰ ~ 1:1 ‰, is more preferably 1:0.1 ‰ ~ 1:0.5 ‰.
In described step 1, HClSI and HF mol ratio is preferably 1:1.4 ~ 1:4, is more preferably 1:1.7 ~ 1:2.
In described step 1, the temperature of reaction of reaction system is preferably reacts at 90 ~ 110 DEG C, reacts at being more preferably 100 ~ 105 DEG C.Those skilled in the art can according to the Process flowchart reaction times of reacting in reaction system, and the preferred reaction times is 15 ~ 25 hours.
In described step 1, by HClSI and HF synthetic intermediate HFSI under catalyst action, react HF and the HCl gas in rear removing reaction system, obtained intermediate double fluorine sulfimide.The method of HF and the HCl gas in described removing reaction system is preferably distilled reaction system or advertises reaction system and distill, in a preferred embodiment, the method of HF and the HCl gas in removing reaction system for first to advertise reaction system, then is distilled.Temperature when advertising is preferably room temperature, advertise one or more the combination that available gas includes but not limited in nitrogen, various rare gas elementes etc., those skilled in the art can regulate according to the acidity of the size of reaction system, tail gas etc. the amount that passes into and advertise gas and advertise the time, and preferably the time of advertising is 10-20 hour.The actual conditions of described distillation is not particularly limited, and only otherwise to goal of the invention of the present invention produces and limits, be preferably underpressure distillation.
(2) salt-forming reaction: two for step 1 gained fluorine sulfimide (HFSI) is reacted with alkaline, lithium, has reacted rear solid-liquid separation, namely obtained LiFSI product.
In described step (2), described alkaline, lithium is preferably LiOH, LiHCO
3or Li
2cO
3in one or more combination, in HFSI and alkaline, lithium, the mol ratio of lithium is preferably 1:0.8 ~ 1:1, is more preferably 1:0.9 ~ 1:0.98.Described LiOH can be LiOHH
2o.
When alkaline, lithium is LiOH, reaction equation is as follows:
When alkaline, lithium is Li
2cO
3time, reaction equation is as follows:
When alkaline, lithium is Li
2hCO
3time, reaction equation is as follows:
In described step (2), preferably joined in alkaline, lithium solvent system by step 1 products therefrom, and adding and/or preferably cooling reaction system in reaction process, preferred feed postition is for dripping.Preferred, the temperature of reaction of reaction system is react at 0 ~ 20 DEG C, reacts at being more preferably 0 ~ 5 DEG C.Those skilled in the art can according to the Process flowchart reaction times of reacting in reaction system, and the preferred reaction times is 1 ~ 5 hour.Solvent in described alkaline, lithium solvent system is preferably low polar solvent, specifically includes but not limited to hexane, hexanaphthene, methylene dichloride, ethylene dichloride, toluene, dimethylbenzene, chlorobenzene, one or more the combination in dichlorobenzene.Those skilled in the art can according to practical situation, and the consumption of solvent in adjustment alkaline, lithium solvent system, preferable amount is 3 ~ 4 times of product LiFSI weight.
In described step (2), be preferably and two for step 1 gained fluorine sulfimide (HFSI) is reacted with alkaline, lithium, after having reacted, in reaction system, drip SOCl
2with the moisture in the system of having reacted, solid-liquid separation, namely obtains LiFSI product.Drip SOCl
2carry out under being preferable over room temperature condition, those skilled in the art can according to the practical situation adjustment SOCl of reaction system
2consumption, preferably, HFSI and SOCl
2mol ratio is 1:0.5 ~ 1:4, more preferably for LiOHH
2o is 1:2.4 ~ 1:3.2, for LiHCO
3for 1:1.2 ~ 1:1.6, for Li
2cO
3for 1:0.6 ~ 1:0.8.
In described step (2), two for step 1 gained fluorine sulfimide (HFSI) is reacted with alkaline, lithium, react rear solid-liquid separation gained LiFSI product and also carry out making beating process, described making beating process concrete grammar be: solid-liquid separation gained LiFSI is added making beating solvent and metal ion remover carry out making beating process, namely obtain the LiFSI product of purifying.Described making beating solvent is preferably low polar solvent, specifically includes but not limited to hexane, hexanaphthene, methylene dichloride, ethylene dichloride, toluene, dimethylbenzene, chlorobenzene, one or more the combination in dichlorobenzene.Those skilled in the art can according to practical situation, and the consumption of adjustment making beating solvent, preferable amount is 3 ~ 6 times of LiFSI weight.Described metal ion remover can select each metal ion species remover in this area, preferred metal ion remover include but not limited to 12-crown-4,15-hat-5,18-hat-6, bicyclohexane also-18-hat-6 in one or more combination.Those skilled in the art can according to practical situation, and the consumption of adjustment metal ion remover, the consumption of preferred metal ion remover is 0.02% ~ 0.2% of LiFSI weight.
The present invention also provides the preparation method of described pair of fluorine sulfimide lithium salts in the purposes of two fluorine sulfimide lithium salts preparation field.
The preparation method of LiFSI provided by the present invention adopts the mode of HF catalytic fluorination to obtain HClSI, the latter and alkaline, lithium complete reaction, through the aftertreatment of simple economy, can purify and obtain the highly purified LiFSI product of high-quality.The method reactions steps is simple, cost reasonable, is applicable to extensive industrialization.
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Notice, in the following example, the concrete processing unit that indicates or device all adopt conventional equipment in this area or device.
In addition should be understood that the one or more method stepss mentioned in the present invention do not repel and can also to there is additive method step or can also insert additive method step before and after described combination step between these steps clearly mentioned, except as otherwise noted; Will also be understood that, the relation that is connected between the one or more equipment/devices mentioned in the present invention is not repelled and can also to be there are other equipment/devices or can also insert other equipment/devices before and after described clustered aggregates/device between these two equipment/devices clearly mentioned, except as otherwise noted.And, except as otherwise noted, the numbering of various method steps is only the convenient tool differentiating various method steps, but not be ordering or the enforceable scope of restriction the present invention of restriction various method steps, the change of its relativeness or adjustment, when changing technology contents without essence, when being also considered as the enforceable category of the present invention.
Experiment: mix obtained HClSI by literature procedure (CN103935970, US2011034716, US4350685) by the thionamic acid be purchased, thionyl chloride, chlorsulfonic acid, other reagent is all from being purchased.
Embodiment 1
In 1000mL reaction flask, add HClSI 1235g, SbCl
50.5g, is warming up to 100-105 DEG C, slowly passes into HF gas and be about 230g under stirring, and react and be cooled to room temperature after 20 hours, advertise nitrogen 15 hours, obtain crude product and be about 900g, short steaming obtains product 865.6g, yield 82.8%.
Embodiment 2
In 1000mL reaction flask, add HClSI 1230g, MoCl
50.47g, is warming up to 100-105 DEG C, slowly passes into HF gas and be about 216g under stirring, and react and be cooled to room temperature after 22 hours, advertise nitrogen 15 hours, obtain crude product and be about 896g, short steaming obtains product 864.8g, yield 83.1%.
Embodiment 3
In 1000mL reaction flask, add ethylene dichloride 543g, LiOHH
2o 42.0g, is cooled to 0-5 DEG C, stirs the two fluorine sulfimide (HFSI, embodiment 1) of lower dropping 192.5g, stirs 2h, be then warming up to 20-25 DEG C, drip 357g SOCl
2, stir 16h.Filter, filter cake 600g ethylene dichloride and 0.17g 18-are preced with-6 and pull an oar, and obtain product 169.2g, yield 90.4% after filtration, drying.
Detected result is: AAS (ppm): Na:5.6, K:2.3, Fe<1, Ca<1.IC(ppm)：Cl
-：4.7，F
-：27，SO
4 2-：17
Embodiment 4
In 1000mL reaction flask, add toluene 550g, Li
2cO
336g, is cooled to 0-5 DEG C, stirs the two fluorine sulfimide (HFSI, embodiment 2) of lower dropping 181g, stirs 2h, be then warming up to 20-25 DEG C, drip 95g SOCl2, stir 16h.Filter, filter cake 600g toluene and 0.15g 15-are preced with-5 and pull an oar, and obtain product 170.6g, yield 91.2% after filtration, drying.
Detected result is: AAS (ppm): Na:3.7, K:3.5, Fe<1, Ca<1.IC(ppm)：Cl
-：7.8，F
-：14，SO4
2-：20
Embodiment 5
In 1000mL reaction flask, add cyclohexane 500g, LiHCO
368g, is cooled to 0-5 DEG C, stirs the two fluorine sulfimide (HFSI, embodiment 1) of lower dropping 188.5g, stirs 2h, be then warming up to 20-25 DEG C, drip 161g SOCl
2, stir 16h.Filter, filter cake 550g cyclohexane and 0.17g 18-are preced with-6 and pull an oar, and obtain product 170.2g, yield 91.0% after filtration, drying.
Detected result is: AAS (ppm): Na:4.4, K:3.0, Fe<1, Ca<1.IC(ppm)：Cl
-：6.1，F
-：21，SO
4 2-：15
In sum, the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (9)
1. a preparation method for two fluorine sulfimide lithium salts, comprises the steps:
(1) fluoridation: by two chlorine sulfimide and the two fluorine sulfimide of hydrogen fluoride synthetic intermediate under catalyst action;
(2) two for step 1 gained fluorine sulfimide and alkaline, lithium are reacted, reacted rear solid-liquid separation, namely obtained LiFSI product.
2. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 1, is characterized in that, in described step 1, the concrete grammar of fluoridation is: HClSI, catalyzer are placed in reaction unit, passes into HF gas and reacts.
3. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 1, is characterized in that, in described step 1, catalyzer is lewis acid;
And/or in described step 1, the mol ratio of HClSI and catalyzer is 1:0.05 ‰ ~ 1:1 ‰;
And/or in described step 1, HClSI and HF mol ratio is 1:1.4 ~ 1:4;
And/or in described step 1, the temperature of reaction of reaction system is react at 90 ~ 110 DEG C.
4. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 1, is characterized in that, in described step 1, by HClSI and HF synthetic intermediate HFSI under catalyst action, has reacted HF and the HCl gas in rear removing reaction system.
5. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 4, is characterized in that, the method for HF and the HCl gas in described removing reaction system is for distilling reaction system or advertising reaction system and distill.
6. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 5, is characterized in that, temperature when advertising is room temperature;
And/or described distillation is underpressure distillation.
7. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 1, is characterized in that, in described step 2, described alkaline, lithium is LiOH, LiHCO
3or Li
2cO
3in one or more combination;
And/or in described step 2, in HFSI and alkaline, lithium, the mol ratio of lithium is 1:0.8 ~ 1:1;
And/or in described step 2, joined by step 1 products therefrom in alkaline, lithium solvent system, the solvent in described alkaline, lithium solvent system is low polar solvent;
And/or in described step 2, the temperature of reaction of reaction system is react at 0 ~ 20 DEG C;
And/or, in described step 2, two for step 1 gained fluorine sulfimide and alkaline, lithium are reacted, after having reacted, in reaction system, drips SOCl
2with the moisture in the system of having reacted, then solid-liquid separation.
8. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 1, it is characterized in that, in described step 2, two for step 1 gained fluorine sulfimide and alkaline, lithium are reacted, react rear solid-liquid separation gained LiFSI product and also carry out making beating process, described making beating process concrete grammar be: solid-liquid separation gained LiFSI is added making beating solvent and metal ion remover carry out making beating process, namely obtain the LiFSI product of purifying.
9. the preparation method of a kind of pair of fluorine sulfimide lithium salts as claimed in claim 8, is characterized in that, described making beating solvent is low polar solvent;
And/or, described metal ion remover be selected from 12-crown-4,15-hat-5,18-hat-6, bicyclohexane also-18-hat-6 in one or more combination.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510261089.1A CN104925765B (en) | 2015-05-21 | 2015-05-21 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| KR1020177030220A KR101890787B1 (en) | 2015-05-21 | 2016-02-04 | Process for producing lithium bisfluorosulfonylimide |
| PCT/CN2016/073420 WO2016184176A1 (en) | 2015-05-21 | 2016-02-04 | Preparation method for bis-(fluoro-sulfonyl) imide lithium salt |
| JP2017568463A JP6391081B2 (en) | 2015-05-21 | 2016-02-04 | Method for producing lithium bis (fluorosulfonyl) imide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510261089.1A CN104925765B (en) | 2015-05-21 | 2015-05-21 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104925765A true CN104925765A (en) | 2015-09-23 |
| CN104925765B CN104925765B (en) | 2017-08-08 |
Family
ID=54113239
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510261089.1A Active CN104925765B (en) | 2015-05-21 | 2015-05-21 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP6391081B2 (en) |
| KR (1) | KR101890787B1 (en) |
| CN (1) | CN104925765B (en) |
| WO (1) | WO2016184176A1 (en) |
Cited By (32)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731399A (en) * | 2016-04-29 | 2016-07-06 | 多氟多化工股份有限公司 | Preparation method of difluoro-sulfonyl imide lithium |
| CN105836719A (en) * | 2016-04-29 | 2016-08-10 | 南京远淑医药科技有限公司 | Method for synthesizing imidodisulfuryl fluoride lithium salt with methyl aromatic amine |
| CN105858626A (en) * | 2016-03-31 | 2016-08-17 | 南京远淑医药科技有限公司 | A preparing method of lithium bis(fluorosulfonyl)imide |
| CN105967159A (en) * | 2016-04-29 | 2016-09-28 | 南京远淑医药科技有限公司 | Method for preparing lithium bis(fluorosulfonyl)imide from aromatic methyl amine |
| CN106006586A (en) * | 2016-05-27 | 2016-10-12 | 上海康鹏科技有限公司 | Preparation method of potassium bis(fluorosulfonyl)imide |
| CN106044728A (en) * | 2016-05-27 | 2016-10-26 | 上海康鹏科技有限公司 | Preparation method of imidodisulfuryl fluoride lithium salt |
| WO2016184176A1 (en) * | 2015-05-21 | 2016-11-24 | 上海康鹏科技有限公司 | Preparation method for bis-(fluoro-sulfonyl) imide lithium salt |
| CN106241757A (en) * | 2016-07-27 | 2016-12-21 | 上海康鹏科技有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| WO2017080831A1 (en) * | 2015-11-13 | 2017-05-18 | Lonza Ltd | Method for the preparation of bis(fluorosulfonyl)-imide and of its salts |
| CN106800280A (en) * | 2016-12-29 | 2017-06-06 | 衢州康鹏化学有限公司 | It is a kind of double（Fluorosulfonyl）The preparation method of inferior amine salt |
| CN106976849A (en) * | 2017-04-20 | 2017-07-25 | 江苏国泰超威新材料有限公司 | A kind of method of purification of pair of fluorine sulfimide lithium |
| CN107055493A (en) * | 2017-05-10 | 2017-08-18 | 浙江永太科技股份有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| WO2017204225A1 (en) * | 2016-05-26 | 2017-11-30 | 森田化学工業株式会社 | Method for producing bis(fluorosulfonyl)imide alkali metal salt and bis(fluorosulfonyl)imide alkali metal salt composition |
| WO2017204303A1 (en) * | 2016-05-27 | 2017-11-30 | 株式会社日本触媒 | Method for producing bis(fluorosulfonyl)imide alkali metal salt |
| CN107633955A (en) * | 2016-06-07 | 2018-01-26 | 罗伯特·博世有限公司 | The hybrid super capacitor of service life with raising |
| CN107662908A (en) * | 2017-10-27 | 2018-02-06 | 江苏理文化工有限公司 | A kind of preparation method of double fluorine sulfimide lithiums |
| CN108002355A (en) * | 2017-12-20 | 2018-05-08 | 厦门大学 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| WO2018174574A1 (en) * | 2017-03-22 | 2018-09-27 | 제이투에이치바이오텍(주) | Method for preparing ultrapure fluorosulfonyl imide with metal cation removed |
| CN109264682A (en) * | 2017-07-18 | 2019-01-25 | 九江天赐高新材料有限公司 | A kind of preparation method of high-purity difluoro sulfimide |
| CN109264683A (en) * | 2018-10-16 | 2019-01-25 | 广州理文科技有限公司 | A kind of extraction and purification method of bis- (fluorine sulphonyl) imines |
| CN109592655A (en) * | 2019-01-17 | 2019-04-09 | 上海如鲲新材料有限公司 | A kind of method that catalytic fluorination efficiently prepares double fluorine sulfimides |
| CN109721037A (en) * | 2019-03-11 | 2019-05-07 | 上海如鲲新材料有限公司 | A kind of new process of double fluorine sulfimide salts |
| CN109776362A (en) * | 2019-03-08 | 2019-05-21 | 如鲲(山东)新材料科技有限公司 | A kind of new process of double trifluorosulfonimide salt |
| CN109923063A (en) * | 2016-12-08 | 2019-06-21 | 阿科玛法国公司 | Dry and bis- (fluorosulfonyl) the acid imide lithium salts of purifying methods |
| CN110407184A (en) * | 2019-08-27 | 2019-11-05 | 刘大凡 | A kind of preparation method of double fluorine sulfimide alkali metal salts |
| CN111057079A (en) * | 2019-12-16 | 2020-04-24 | 江苏华盛锂电材料股份有限公司 | Purification method of lithium bis (oxalato) borate and lithium bis (oxalato) borate |
| EP3825278A1 (en) | 2019-11-20 | 2021-05-26 | Shanghai Rolechem Co., Ltd. | Method for preparing high-purity bisfluorosulfonylimide salt |
| CN113979454A (en) * | 2021-11-23 | 2022-01-28 | 山东永浩新材料科技有限公司 | Preparation method of fluorosulfonic acid alkali metal salt |
| CN114804043A (en) * | 2022-05-17 | 2022-07-29 | 临沂小篆新材料科技有限公司 | Process for preparing lithium bis (fluorosulfonyl) imide |
| WO2022199643A1 (en) * | 2021-03-26 | 2022-09-29 | 广州理文科技有限公司 | Synthesis method for bis(fluorosulfonyl)imide |
| CN115448267A (en) * | 2022-09-19 | 2022-12-09 | 安徽新宸新材料有限公司 | Method for preparing lithium bis (fluorosulfonyl) imide |
| CN115974015A (en) * | 2022-12-28 | 2023-04-18 | 无锡威孚环保催化剂有限公司 | Synthetic method of sodium bis (fluorosulfonyl) imide |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017096333A1 (en) * | 2015-12-04 | 2017-06-08 | Coorstek Fluorochemicals, Inc. | Process for producing hydrogen bis(fluorosulfonyl)imide |
| FR3081866B1 (en) | 2018-06-01 | 2020-05-08 | Arkema France | PROCESS FOR THE PREPARATION OF A SALT OF IMIDES CONTAINING A FLUOROSULFONYL GROUP |
| KR102259985B1 (en) * | 2019-03-28 | 2021-06-03 | 주식회사 천보 | Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content |
| KR102285464B1 (en) * | 2019-03-28 | 2021-08-03 | 주식회사 천보 | Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content |
| US11267707B2 (en) | 2019-04-16 | 2022-03-08 | Honeywell International Inc | Purification of bis(fluorosulfonyl) imide |
| FR3095439B1 (en) * | 2019-04-25 | 2021-04-02 | Arkema France | Process for the preparation of bis (fluorosulfonyl) imide |
| CN110155967A (en) * | 2019-06-18 | 2019-08-23 | 山东安博新材料研究院有限公司 | A kind of preparation method of double fluorine sulfimide lithiums |
| CN110745795B (en) * | 2019-11-07 | 2022-08-26 | 兰州大学 | Method for synthesizing lithium bis (fluorosulfonyl) imide by using electrochemistry |
| CN112978690B (en) * | 2019-12-18 | 2022-12-09 | 浙江蓝天环保高科技股份有限公司 | Water removal and screening method for powdery lithium bis (fluorosulfonyl) imide |
| CN111620315A (en) * | 2020-07-22 | 2020-09-04 | 上海华谊（集团）公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
| CN112479165B (en) * | 2020-11-27 | 2023-08-08 | 湖北迈可凯科技有限公司 | Method for synthesizing lithium difluorosulfimide by one-step method |
| KR20220156229A (en) | 2021-05-18 | 2022-11-25 | 임광민 | Mass Production Method of Metal bis(fluorosulfonyl)imide |
| US20230178804A1 (en) * | 2021-12-02 | 2023-06-08 | Honeywell International Inc. | Processes for producing lithium bis(fluorosulfonyl) imide |
| KR20230085823A (en) | 2021-12-07 | 2023-06-14 | 주식회사 이브이에스텍 | Economical Mass Production Method of Metal bis(fluorosulfonyl)imide solution |
| CN114436226A (en) * | 2021-12-30 | 2022-05-06 | 石家庄康坦福化工科技有限公司 | Preparation and application of potassium bis (fluorosulfonyl) imide |
| CN114560452B (en) * | 2022-03-29 | 2023-06-23 | 多氟多新材料股份有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
| CN116022748B (en) * | 2022-12-16 | 2024-02-27 | 山东惟普新能源有限公司 | Water removal method for aqueous lithium bis (fluorosulfonyl) imide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8377406B1 (en) * | 2012-08-29 | 2013-02-19 | Boulder Ionics Corporation | Synthesis of bis(fluorosulfonyl)imide |
| CN103910346A (en) * | 2013-01-05 | 2014-07-09 | 江苏华盛精化工股份有限公司 | Method for preparing bis(fluorosulfonyl)imide |
| CN103935970A (en) * | 2014-03-24 | 2014-07-23 | 深圳新宙邦科技股份有限公司 | Preparation methods of bis(fluorosulfonyl)imide and alkali metal salts thereof |
| CN104495767A (en) * | 2014-11-21 | 2015-04-08 | 湖南有色郴州氟化学有限公司 | Preparation method of lithium bis(fluorosulfonyl)amide |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2998297B1 (en) * | 2012-11-22 | 2014-11-14 | Arkema France | PROCESS FOR PREPARING SALT OF IMIDES CONTAINING FLUOROSULFONYL GROUP |
| US8722005B1 (en) * | 2013-07-26 | 2014-05-13 | Boulder Ionics Corporation | Synthesis of hydrogen bis(fluorosulfonyl)imide |
| FR3020060B1 (en) * | 2014-04-18 | 2016-04-01 | Arkema France | PREPARATION OF IMIDES CONTAINING FLUOROSULFONYL GROUP |
| JP6691740B2 (en) * | 2015-04-24 | 2020-05-13 | ステラケミファ株式会社 | Method for producing fluorosulfonylimide compound |
| CN104925765B (en) * | 2015-05-21 | 2017-08-08 | 上海康鹏科技有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
-
2015
- 2015-05-21 CN CN201510261089.1A patent/CN104925765B/en active Active
-
2016
- 2016-02-04 WO PCT/CN2016/073420 patent/WO2016184176A1/en active Application Filing
- 2016-02-04 JP JP2017568463A patent/JP6391081B2/en active Active
- 2016-02-04 KR KR1020177030220A patent/KR101890787B1/en active IP Right Grant
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8377406B1 (en) * | 2012-08-29 | 2013-02-19 | Boulder Ionics Corporation | Synthesis of bis(fluorosulfonyl)imide |
| CN103910346A (en) * | 2013-01-05 | 2014-07-09 | 江苏华盛精化工股份有限公司 | Method for preparing bis(fluorosulfonyl)imide |
| CN103935970A (en) * | 2014-03-24 | 2014-07-23 | 深圳新宙邦科技股份有限公司 | Preparation methods of bis(fluorosulfonyl)imide and alkali metal salts thereof |
| CN104495767A (en) * | 2014-11-21 | 2015-04-08 | 湖南有色郴州氟化学有限公司 | Preparation method of lithium bis(fluorosulfonyl)amide |
Cited By (51)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016184176A1 (en) * | 2015-05-21 | 2016-11-24 | 上海康鹏科技有限公司 | Preparation method for bis-(fluoro-sulfonyl) imide lithium salt |
| WO2017080831A1 (en) * | 2015-11-13 | 2017-05-18 | Lonza Ltd | Method for the preparation of bis(fluorosulfonyl)-imide and of its salts |
| CN108349737A (en) * | 2015-11-13 | 2018-07-31 | 隆萨有限公司 | The method for being used to prepare bis- (fluorosulfonyl)-acid imides and its salt |
| CN105858626A (en) * | 2016-03-31 | 2016-08-17 | 南京远淑医药科技有限公司 | A preparing method of lithium bis(fluorosulfonyl)imide |
| CN105731399A (en) * | 2016-04-29 | 2016-07-06 | 多氟多化工股份有限公司 | Preparation method of difluoro-sulfonyl imide lithium |
| CN105836719A (en) * | 2016-04-29 | 2016-08-10 | 南京远淑医药科技有限公司 | Method for synthesizing imidodisulfuryl fluoride lithium salt with methyl aromatic amine |
| CN105967159A (en) * | 2016-04-29 | 2016-09-28 | 南京远淑医药科技有限公司 | Method for preparing lithium bis(fluorosulfonyl)imide from aromatic methyl amine |
| CN105967159B (en) * | 2016-04-29 | 2018-06-01 | 南京远淑医药科技有限公司 | A kind of method for preparing imidodisulfuryl fluoride lithium salt using fragrant methyl amine |
| CN105836719B (en) * | 2016-04-29 | 2018-06-01 | 南京远淑医药科技有限公司 | A kind of method for synthesizing imidodisulfuryl fluoride lithium salt using fragrant methyl amine |
| CN105731399B (en) * | 2016-04-29 | 2018-03-27 | 多氟多化工股份有限公司 | A kind of preparation method of double fluorine sulfimide lithiums |
| CN109311669A (en) * | 2016-05-26 | 2019-02-05 | 森田化学工业株式会社 | The manufacturing method of double fluorine sulfimide alkali metal salts and double fluorine sulfimide alkali metal salt compositions |
| CN109311669B (en) * | 2016-05-26 | 2022-04-19 | 株式会社日本触媒 | Method for producing alkali metal salt of bis (fluorosulfonyl) imide, and alkali metal salt composition of bis (fluorosulfonyl) imide |
| WO2017204225A1 (en) * | 2016-05-26 | 2017-11-30 | 森田化学工業株式会社 | Method for producing bis(fluorosulfonyl)imide alkali metal salt and bis(fluorosulfonyl)imide alkali metal salt composition |
| WO2017204303A1 (en) * | 2016-05-27 | 2017-11-30 | 株式会社日本触媒 | Method for producing bis(fluorosulfonyl)imide alkali metal salt |
| CN106044728B (en) * | 2016-05-27 | 2018-07-27 | 上海康鹏科技有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| CN109415209A (en) * | 2016-05-27 | 2019-03-01 | 株式会社日本触媒 | The preparation method of two (fluorosulfonyl) imine alkali metal salts |
| JPWO2017204303A1 (en) * | 2016-05-27 | 2019-03-22 | 株式会社日本触媒 | Process for producing bis (fluorosulfonyl) imide alkali metal salt |
| CN109415209B (en) * | 2016-05-27 | 2022-09-27 | 株式会社日本触媒 | Process for producing bis (fluorosulfonyl) imide alkali metal salt |
| CN106044728A (en) * | 2016-05-27 | 2016-10-26 | 上海康鹏科技有限公司 | Preparation method of imidodisulfuryl fluoride lithium salt |
| CN106006586A (en) * | 2016-05-27 | 2016-10-12 | 上海康鹏科技有限公司 | Preparation method of potassium bis(fluorosulfonyl)imide |
| CN107633955A (en) * | 2016-06-07 | 2018-01-26 | 罗伯特·博世有限公司 | The hybrid super capacitor of service life with raising |
| CN106241757B (en) * | 2016-07-27 | 2018-09-18 | 上海康鹏科技有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| CN106241757A (en) * | 2016-07-27 | 2016-12-21 | 上海康鹏科技有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| CN109923063B (en) * | 2016-12-08 | 2023-08-15 | 阿科玛法国公司 | Method for drying and purifying lithium bis (fluorosulfonyl) imide salt |
| CN109923063A (en) * | 2016-12-08 | 2019-06-21 | 阿科玛法国公司 | Dry and bis- (fluorosulfonyl) the acid imide lithium salts of purifying methods |
| CN106800280A (en) * | 2016-12-29 | 2017-06-06 | 衢州康鹏化学有限公司 | It is a kind of double（Fluorosulfonyl）The preparation method of inferior amine salt |
| WO2018174574A1 (en) * | 2017-03-22 | 2018-09-27 | 제이투에이치바이오텍(주) | Method for preparing ultrapure fluorosulfonyl imide with metal cation removed |
| CN106976849A (en) * | 2017-04-20 | 2017-07-25 | 江苏国泰超威新材料有限公司 | A kind of method of purification of pair of fluorine sulfimide lithium |
| CN107055493A (en) * | 2017-05-10 | 2017-08-18 | 浙江永太科技股份有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| CN109264682A (en) * | 2017-07-18 | 2019-01-25 | 九江天赐高新材料有限公司 | A kind of preparation method of high-purity difluoro sulfimide |
| CN109264682B (en) * | 2017-07-18 | 2019-11-29 | 九江天赐高新材料有限公司 | A kind of preparation method of high-purity difluoro sulfimide |
| CN107662908A (en) * | 2017-10-27 | 2018-02-06 | 江苏理文化工有限公司 | A kind of preparation method of double fluorine sulfimide lithiums |
| CN108002355A (en) * | 2017-12-20 | 2018-05-08 | 厦门大学 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| CN108002355B (en) * | 2017-12-20 | 2019-10-22 | 厦门大学 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| CN109264683B (en) * | 2018-10-16 | 2021-07-27 | 广州理文科技有限公司 | Method for extracting and purifying bis (fluorosulfonyl) imide |
| CN109264683A (en) * | 2018-10-16 | 2019-01-25 | 广州理文科技有限公司 | A kind of extraction and purification method of bis- (fluorine sulphonyl) imines |
| CN109592655A (en) * | 2019-01-17 | 2019-04-09 | 上海如鲲新材料有限公司 | A kind of method that catalytic fluorination efficiently prepares double fluorine sulfimides |
| CN109776362A (en) * | 2019-03-08 | 2019-05-21 | 如鲲(山东)新材料科技有限公司 | A kind of new process of double trifluorosulfonimide salt |
| CN109776362B (en) * | 2019-03-08 | 2022-02-15 | 如鲲(山东)新材料科技有限公司 | Novel process of bis (trifluorosulfonyl) imide salt |
| CN109721037A (en) * | 2019-03-11 | 2019-05-07 | 上海如鲲新材料有限公司 | A kind of new process of double fluorine sulfimide salts |
| CN110407184A (en) * | 2019-08-27 | 2019-11-05 | 刘大凡 | A kind of preparation method of double fluorine sulfimide alkali metal salts |
| CN110407184B (en) * | 2019-08-27 | 2021-04-06 | 刘大凡 | Preparation method of bis (fluorosulfonyl) imide alkali metal salt |
| EP3825278A1 (en) | 2019-11-20 | 2021-05-26 | Shanghai Rolechem Co., Ltd. | Method for preparing high-purity bisfluorosulfonylimide salt |
| CN111057079A (en) * | 2019-12-16 | 2020-04-24 | 江苏华盛锂电材料股份有限公司 | Purification method of lithium bis (oxalato) borate and lithium bis (oxalato) borate |
| WO2022199643A1 (en) * | 2021-03-26 | 2022-09-29 | 广州理文科技有限公司 | Synthesis method for bis(fluorosulfonyl)imide |
| CN113979454A (en) * | 2021-11-23 | 2022-01-28 | 山东永浩新材料科技有限公司 | Preparation method of fluorosulfonic acid alkali metal salt |
| CN113979454B (en) * | 2021-11-23 | 2023-09-26 | 山东永浩新材料科技有限公司 | Preparation method of alkali metal fluorosulfonate |
| CN114804043A (en) * | 2022-05-17 | 2022-07-29 | 临沂小篆新材料科技有限公司 | Process for preparing lithium bis (fluorosulfonyl) imide |
| CN115448267A (en) * | 2022-09-19 | 2022-12-09 | 安徽新宸新材料有限公司 | Method for preparing lithium bis (fluorosulfonyl) imide |
| CN115448267B (en) * | 2022-09-19 | 2023-04-07 | 安徽新宸新材料有限公司 | Method for preparing lithium bis (fluorosulfonyl) imide |
| CN115974015A (en) * | 2022-12-28 | 2023-04-18 | 无锡威孚环保催化剂有限公司 | Synthetic method of sodium bis (fluorosulfonyl) imide |
Also Published As
| Publication number | Publication date |
|---|---|
| KR101890787B1 (en) | 2018-08-22 |
| WO2016184176A1 (en) | 2016-11-24 |
| CN104925765B (en) | 2017-08-08 |
| KR20170131524A (en) | 2017-11-29 |
| JP2018520981A (en) | 2018-08-02 |
| JP6391081B2 (en) | 2018-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104925765A (en) | Preparation method for difluorosulfimide lithium salt | |
| CN106044728B (en) | A kind of preparation method of imidodisulfuryl fluoride lithium salt | |
| EP3381923B1 (en) | Novel method for preparing lithium bis(fluorosulfonyl)imide | |
| JP6694394B2 (en) | Preparation of imide containing fluorosulfonyl group | |
| CN113135554A (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN106276829B (en) | A kind of synthetic method of double fluorine sulfimide lithiums | |
| CN106006586B (en) | A kind of preparation method of double fluorine sulfimide potassium | |
| CN107055493B (en) | A kind of preparation method of imidodisulfuryl fluoride lithium salt | |
| CN103524387A (en) | Preparation method of imidodisulfuryl fluoride lithium salt | |
| CN106241757A (en) | A kind of preparation method of imidodisulfuryl fluoride lithium salt | |
| CN104310327A (en) | Method of manufacturing phosphorous pentafluoride and hexafluorophosphate | |
| CN107720717B (en) | Preparation method of lithium difluorophosphate | |
| CN108155434B (en) | Method for recovering lithium from waste electrolyte of lithium ion battery | |
| CN105175452B (en) | A kind of preparation method of phosphonitrile oroalkane sulfonyl imine alkali metal salt | |
| WO2016017389A1 (en) | Method for producing difluorophosphate | |
| JP2014062036A (en) | Method for producing lithium difluorophosphate | |
| CN103259040B (en) | Organotin fluoride is utilized to prepare the method for high-purity lithium difluorophosphate | |
| CN104671224B (en) | The synthetic method of double fluorine sulfimide salt | |
| EP1976048B1 (en) | Method for producing electrolyte solution for lithium ion battery and lithium ion battery using same | |
| TWI439414B (en) | Method for producing hexafluorophosphate | |
| JP6199117B2 (en) | Method for producing difluorophosphate | |
| KR20200049164A (en) | Very efficient Method for preparing lithium bis(fluorosulfonyl)imide | |
| CN105947998B (en) | A kind of method that imidodisulfuryl fluoride lithium salt is prepared using lithium nitride | |
| CN106430257A (en) | Preparation method of porous high-activity LiF and preparation method of LiFSI | |
| CN107244662B (en) | A kind of preparation method of bis- (fluorosulfonyl) imides |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 200331 No. 200, Wuwei Road, Shanghai, Putuo District Applicant after: SHANGHAI KANGPENG TECHNOLOGY CO., LTD. Applicant after: Quzhou Kangpeng Chemical Co., Ltd. Address before: 200331 No. 200, Wuwei Road, Shanghai, Putuo District Applicant before: Shanghai Kangpeng Chemical Co., Ltd. Applicant before: Quzhou Kangpeng Chemical Co., Ltd. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 2003-1 Building No. 200, 2891 Lane, Qilian Mountain South Road, Putuo District, Shanghai Co-patentee after: Quzhou Kangpeng Chemical Co., Ltd. Patentee after: Shanghai Kangpeng Science and Technology Co., Ltd. Address before: 2003 2001 No. 200 Wuwei Road, Putuo District, Shanghai Co-patentee before: Quzhou Kangpeng Chemical Co., Ltd. Patentee before: SHANGHAI KANGPENG TECHNOLOGY CO., LTD. |