CN107244662A - It is a kind of double（Fluorosulfonyl）The preparation method of imide - Google Patents
It is a kind of double（Fluorosulfonyl）The preparation method of imide Download PDFInfo
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- CN107244662A CN107244662A CN201710405380.0A CN201710405380A CN107244662A CN 107244662 A CN107244662 A CN 107244662A CN 201710405380 A CN201710405380 A CN 201710405380A CN 107244662 A CN107244662 A CN 107244662A
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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
It is more particularly to a kind of double the present invention relates to organic synthesis field（Fluorosulfonyl）The preparation method of imide.The present invention provides a kind of double（Fluorosulfonyl）The preparation method of imide, comprises the following steps：Double chlorine sulfimides and potassium bifluoride are reacted under conditions of catalyst presence, prepared double（Fluorosulfonyl）Imide.KFSI provided by the present invention preparation method is compared with traditional handicraft, and reactions steps are simpler, safety non-pollution, prepares cost rationally, due to using anhydrous response, effectively controls the introducing of moisture in product, steady quality, suitable large-scale industrial production.
Description
Technical field
The present invention relates to organic synthesis field, more particularly to a kind of preparation side of double (fluorosulfonyl) imides
Method.
Background technology
Double fluorine sulfimide potassium are as functional electric material, in molten salt battery, hard coat film, conducting film, antistatic bonding
The fields such as agent are with a wide range of applications, and its preparation method also turns into Recent study focus.
Patent JP2013087019, double chlorine sulfimides are first prepared using the reaction of sulfamic acid, chlorosulfonic acid and thionyl chloride,
Further with fluorination nak response.This method can generate a large amount of sour gas hydrogen chloride and sulfur dioxide in first step reaction,
It is unfavorable for environmental protection, second step reaction needs excessive more anhydrous potassium fluoride, and cost is high, purifying complex.
Patent WO2015143866, still using sulfamic acid, chlorosulfonic acid and the thionyl chloride for producing a large amount of sour gas
Technique prepares double chlorine sulfimides, then obtained with fluorination nak response by solvent of hydrogen fluoride.It is fluorinated hydrogen consumption equivalents excessive, system
The problem of causing high, and equally exist in environmental protection.
Patent US2012020867, is firstly generated accordingly using sulfuryl fluoride, ammonia, organic base in pressure reacting container, is made
Double fluorine sulfimide salts, then obtain product with potassium hydroxide reaction.This is used in the post processing and follow-up reaction of intermediate
Water, and double fluorine sulfimide salts have preferable solubility in water, extraction efficiency is lower, be not suitable for heavy industrialization
Production.
Patent US2013323154, is reacted using double chlorine sulfimides and ammonium chloride and double chlorine sulfimide ammonium salts is made, then
It is fluorinated, then is reacted with KOH through HF, water has equally been used in process program, extracting operation is employed, it is inefficient.
Because double fluorine sulfimide potassium have good dissolubility in water, extraction efficiency is poor, and the non-refractory in water, contains
Aqueous systems synthesis is easily caused environmental issue caused by waste water.Therefore double fluorine sulphonyl are prepared with rational cost, safely and efficiently
Imines potassium turns into this area technical problem in the urgent need to address.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of double (fluorosulfonyl) imines
The preparation method of sylvite, for solving the problems of the prior art.
In order to achieve the above objects and other related objects, the present invention provides a kind of system of double (fluorosulfonyl) imides
Preparation Method, comprises the following steps：By double chlorine sulfimides (HClSI) and potassium bifluoride (KHF2) under conditions of catalyst presence
Reaction, prepares double (fluorosulfonyl) imides, and reaction equation is as follows：
In some embodiments of the invention, one or more of the catalyst in quaternary ammonium salt, quaternary phosphonium salt, crown ether
Combination.
In some embodiments of the invention, the catalyst is selected from tetrabutylammonium chloride, TBAB, the tetrabutyl
Ammonium iodide, tetramethyl ammonium chloride, methyl tricapryl ammonium chloride, TBAH, 4-butyl ammonium hydrogen sulfate, tetraphenylphosphonibromide bromide
One or more combinations in phosphine, 18- crown-s 6,15- crown-s 5,12-crown-4.
In some embodiments of the invention, the weight ratio of the HClSI and catalyst are 1:1 ‰~1:3%.
In some embodiments of the invention, the weight ratio of the HClSI and catalyst are 1:5 ‰~1:1%.
In some embodiments of the invention, HClSI and KHF2Mol ratio be 1:0.9~1:2.
In some embodiments of the invention, HClSI and KHF2Mol ratio be 1:1~1:1.2.
In some embodiments of the invention, reaction is carried out in the presence of a solvent, and the solvent is selected from carbonic ester
One or more combinations in class, glycols, pyrrolidinone compounds, C2-C4 nitrile solvents.
In some of the invention embodiments, the solvent be selected from dimethyl carbonate, diethyl carbonate, ethylene carbonate,
One kind in triethylene glycol, diethylene glycol (DEG), 2-Pyrrolidone, 1-METHYLPYRROLIDONE, N- ethyl pyrrolidones, acetonitrile, propionitrile, butyronitrile
Or a variety of combinations.
In some embodiments of the invention, reaction temperature is 80~150 DEG C.
In some embodiments of the invention, reaction temperature is 90~120 DEG C.
In some embodiments of the invention, the post processing of reaction comprises the following steps：To reaction system after the completion of reaction
Cooled, separation of solid and liquid, liquid phase concentration, crystallization produce KFSI products.
In some embodiments of the invention, the temperature of reaction system is down to room temperature or 10~35 DEG C after the completion of reaction.
In some embodiments of the invention, the method for crystallization includes concentration and/or cooling and/or adds poor solvent.
Embodiment
The present invention has found by substantial amounts of research work, is that raw material can be hydrogenated with fluorine with double chlorine sulfimides (HClSI)
Potassium (KHF2) reaction prepares double (fluorosulfonyl) imides (KFSI) under catalyst action, so as to provide one kind
Simple efficient method prepares KFSI, and the present invention is completed on this basis.
The present invention provides a kind of preparation method of double (fluorosulfonyl) imides, comprises the following steps：By double chlorine sulphurs
Acid imide (HClSI) and potassium bifluoride (KHF2) reacted under conditions of catalyst presence, prepare double (fluorosulfonyls)
Imide, reaction equation is as follows：
In preparation method provided by the present invention, the catalyst can be one kind in quaternary ammonium salt, quaternary phosphonium salt, crown ether etc.
Or a variety of combinations, more specifically can be tetrabutylammonium chloride, TBAB, tetrabutylammonium iodide, tetramethyl ammonium chloride,
Methyl tricapryl ammonium chloride, TBAH, 4-butyl ammonium hydrogen sulfate, tetraphenylphosphonibromide bromide, 18- crown-s 6,15- crown-s 5,
One or more combinations in 12-crown-4 etc..In the embodiment of the invention, the catalyst is preferably the tetrabutyl
One or more combinations in ammonium chloride, TBAB, tetrabutylammonium iodide and tetraphenylphosphonibromide bromide etc., more preferably
Tetraphenylphosphonibromide bromide.The usage amount of the catalyst is typically catalytic amount, for example, the weight ratio of the HClSI and catalyst
Can be 1:1 ‰~1:3% or 1:5 ‰~1:1%.
In preparation method provided by the present invention, HClSI and KHF2Mol ratio can be 1:0.9~1:2, KHF2Use
Amount preferably can be equivalent or excess relative to HClSI, for example, HClSI and KHF2Mol ratio can be 1:1~1:
1.2。
In preparation method provided by the present invention, reaction can be carried out under conditions of solvent-free presence, and reaction can also
Carry out in the presence of a solvent, suitable solvent species and usage amount, which may be selected, in those skilled in the art is used for the present invention,
For example, the solvent is one or more in carbonates, glycols, pyrrolidinone compounds, C2-C4 nitrile solvents etc.
Combination.In the embodiment of the invention, the solvent can be dimethyl carbonate, diethyl carbonate, ethylene carbonate,
One in triethylene glycol, diethylene glycol (DEG), 2-Pyrrolidone, 1-METHYLPYRROLIDONE, N- ethyl pyrrolidones, acetonitrile, propionitrile, butyronitrile etc.
Kind or a variety of combinations, in preferably being dimethyl carbonate, diethyl carbonate, ethylene carbonate, triethylene glycol, diethylene glycol (DEG) etc.
One or more combinations, more preferably can be diethyl carbonate and/or triethylene glycol.For another example the weight ratio of HClSI and solvent
Can be 1:2~1:10 or 1:1.5~1:4.
In preparation method provided by the present invention, reaction temperature can be 80~150 DEG C or 90~120 DEG C.This
Art personnel can be in reaction system reaction process control the reaction time, monitoring reaction process method can be example
Such as high performance liquid chromatography (HPLC), thin-layer chromatography (TLC), the reaction time can be such as 10~40 hours.
In preparation method provided by the present invention, suitable post-processing step may be selected in those skilled in the art, to reaction
Product is purified.For example, reaction system can be cooled after completion of the reaction, separation of solid and liquid, liquid phase concentration, crystallization,
Produce KFSI products.More specifically, the temperature of reaction system can be down to room temperature or 10~35 DEG C, the mode of separation of solid and liquid can
Be filtered using filter paper, filter cloth or miillpore filter, press filtration, solid phase is the insoluble pair of unreacted raw material and/or generation
Product, the liquid phase obtained by separation of solid and liquid is typically KFSI solution, can be concentration, drop to the method that KFSI solution carries out crystallization
Temperature, add filtered after the mode such as poor solvent, crystallization, drying process, that is, obtain KFSI products.It is another specific in the present invention
In embodiment, those skilled in the art can select suitable pressure and/or temperature to be operated according to the property of solvent,
Concentration can be concentrated or be concentrated under reduced pressure using normal pressure, and the temperature of concentration can be 30-90 DEG C, be concentrated into liquor capacity and reduced 1/2
Above or when system solid formation content is more than 50%, being cooled in crystallization at 10-30 DEG C, Crystallization Process further to add not
Good solvent crystallization.The poor solvent usually for the relatively low solvent of KFSI product solubilities, for example, can be alkane, halo
One or more combinations in alkane, benzene, alkylbenzene, halogeno-benzene etc..It is described bad in the embodiment of the invention
Solvent can be hexane, hexamethylene, heptane, dichloromethane, dichloroethanes, benzene,toluene,xylene, ethylbenzene, chlorobenzene, dichloro-benzenes
One or more combinations in, the usage amount of poor solvent can be 1-10 times of HClSI weight, and preferred consumption can be with
It is 2-6 times of HClSI weight.
Another aspect of the present invention provides the preparation method of described double (fluorosulfonyl) imides in double (fluoro sulphonyl
Base) imide preparation field purposes.
KFSI provided by the present invention preparation method uses HClSI and KHF2KFSI is prepared for raw material reaction, with fluorine hydrogen
Change potassium and react obtained under conditions of catalyst presence, by the post processing of simple economy, you can purification obtains KFSI products.Should
Method is compared with traditional handicraft, and reactions steps are simpler, safety non-pollution, prepares cost rationally, due to using anhydrous response, has
Effect controls the introducing of moisture in product, steady quality, suitable large-scale industrial production.
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
It should be clear that in the following example not specifically dated process equipment or device using conventional equipment in the art or
Device.
In addition, it is to be understood that the one or more method and steps mentioned in the present invention do not repel before and after the combination step
There can also be other method step or other method step can also be inserted between the step of these are specifically mentioned, unless separately
It is described；It should also be understood that the combination annexation between the one or more equipment/devices mentioned in the present invention is not repelled
Can also have other equipment/device before and after the unit equipment/device or two equipment/devices specifically mentioning at these it
Between can also insert other equipment/device, unless otherwise indicated.Moreover, unless otherwise indicated, the numbering of various method steps is only
Differentiate the convenient tool of various method steps, rather than ordering or restriction enforceable model of the invention for limitation various method steps
Enclose, being altered or modified for its relativeness is of the invention enforceable when being also considered as in the case of without essence change technology contents
Category.
Embodiment 1
The preparation of the double chlorine sulfimides of raw material：
In 1000mL reaction bulbs, chlorosulfonic acid 582.5g, 98% dense H are added2SO45.8g, opens stirring, it is warming up to 105~
115 DEG C, chlorosulphonyl isocyanate 778.3g is added dropwise.Completion of dropping, progressively rises to 120~130 DEG C, continues stirring reaction 30h.
Vacuum distillation, to reclaim excessive chlorosulphonyl isocyanate, reclaims residue 1026g in 50g, kettle, yield 95.9%, acid number altogether
Measured value 1295mg KOH/g, calculated value 1311mg KOH/g.
Embodiment 2
The preparation of double fluorine sulfimide potassium：
To in mechanical agitation, thermometer, four mouthfuls of reaction bulbs of condenser pipe, acetonitrile 300g, KHF are added237.5g, four fourths
Base ammonium hydrogen sulfate 0.9g, room temperature, stirring is lower to be added dropwise 85.6g HClSI.Completion of dropping is warming up to backflow, and the buffered bottle of tail gas is imported
Absorbed in the NaOH aqueous solution.After back flow reaction 28 hours, filtering, filtrate decompression precipitation is concentrated, and is concentrated under reduced pressure at 60 DEG C in bottle
When volume reduces 50%, 450g dichloromethane is added into concentrate, 30min is stirred, is cooled to less than 20 DEG C, through filtering, is done
Product 74.5g, yield 85.0%, chromatography of ions detection purity 99.3% are obtained after dry.
Embodiment 3
The preparation of double fluorine sulfimide potassium：
To in mechanical agitation, thermometer, four mouthfuls of reaction bulbs of condenser pipe, diethyl carbonate 300g, KHF are added2
32.8g, TBAB 0.7g, room temperature, stirring is lower to be added dropwise 85.6g HClSI.Completion of dropping is warming up to 115~120 DEG C, tail
The buffered bottle of gas, which is imported in the NaOH aqueous solution, to be absorbed.After insulation reaction 16 hours, filtering, filtrate decompression precipitation concentration is concentrated into
When solid content is more than 50% in bottle, 450g dichloromethane is added into concentrate, 30min is stirred, less than 20 DEG C, process are cooled to
Product 83.9g, yield 95.7%, chromatography of ions detection purity 99.0% are obtained after filter, drying.
Embodiment 4
The preparation of double fluorine sulfimide potassium：
To in mechanical agitation, thermometer, four mouthfuls of reaction bulbs of condenser pipe, 1-METHYLPYRROLIDONE 300g, KHF are added2
32.8g, tetrabutylammonium chloride 1.1g, room temperature, stirring is lower to be added dropwise 85.6g HClSI.Completion of dropping is warming up to 145~150 DEG C, tail
The buffered bottle of gas, which is imported in the NaOH aqueous solution, to be absorbed.After insulation reaction 12 hours, filtering, filtrate decompression precipitation concentration is concentrated into
When solid content is more than 50% in bottle, 450g dichloromethane is added into concentrate, 30min is stirred, less than 20 DEG C, process are cooled to
Product 76.3g, yield 87.0%, chromatography of ions detection purity 99.4% are obtained after filter, drying.
Embodiment 5
The preparation of double fluorine sulfimide potassium：
To in mechanical agitation, thermometer, four mouthfuls of reaction bulbs of condenser pipe, triethylene glycol 300g, KHF are added232.8g, four
Phenyl bromide phosphine 0.9g, room temperature, stirring is lower to be added dropwise 85.6g HClSI.Completion of dropping is warming up to 100-110 DEG C, and tail gas is buffered
Bottle, which is imported in the NaOH aqueous solution, to be absorbed.After insulation reaction 20 hours, filtering, filtrate decompression precipitation concentration is concentrated into bottle and contained admittedly
When amount is more than 50%, 300g toluene is added into concentrate and is warming up to 60 DEG C of stirring 30min, less than 20 DEG C is cooled to, filters, does
Product 81.2g, yield 92.6%, chromatography of ions detection purity 99.3% are obtained after dry.
In summary, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of preparation method of double (fluorosulfonyl) imides, comprises the following steps：By double chlorine sulfimides and fluorine hydrogen
Change potassium to react under conditions of catalyst presence, prepare double (fluorosulfonyl) imides, reaction equation is as follows：
2. preparation method as claimed in claim 1, it is characterised in that the catalyst is in quaternary ammonium salt, quaternary phosphonium salt, crown ether
One or more combinations.
3. preparation method as claimed in claim 2, it is characterised in that the catalyst is selected from tetrabutylammonium chloride, the tetrabutyl
Ammonium bromide, tetrabutylammonium iodide, tetramethyl ammonium chloride, methyl tricapryl ammonium chloride, TBAH, tetrabutyl hydrogen sulfate
One or more combinations in ammonium, tetraphenylphosphonibromide bromide, 18- crown-s 6,15- crown-s 5,12-crown-4.
4. preparation method as claimed in claim 1, it is characterised in that the weight ratio of the HClSI and catalyst are 1:1 ‰~
1:3%, preferably 1:5 ‰~1:1%.
5. preparation method as claimed in claim 1, it is characterised in that the HClSI and KHF2Mol ratio be 1:0.9~1:
2, preferably 1:1~1:1.2.
6. preparation method as claimed in claim 1, it is characterised in that reaction is carried out in the presence of a solvent, described molten
One or more combinations of the agent in carbonates, glycols, pyrrolidinone compounds, C2-C4 nitrile solvents.
7. preparation method as claimed in claim 6, it is characterised in that the solvent be selected from dimethyl carbonate, diethyl carbonate,
Ethylene carbonate, triethylene glycol, diethylene glycol (DEG), 2-Pyrrolidone, 1-METHYLPYRROLIDONE, N- ethyl pyrrolidones, acetonitrile, propionitrile,
One or more combinations in butyronitrile.
8. preparation method as claimed in claim 1, it is characterised in that reaction temperature is 80~150 DEG C, preferably 90~120
℃。
9. preparation method as claimed in claim 1, it is characterised in that the post processing of reaction comprises the following steps：Reaction is completed
Reaction system is cooled afterwards, separation of solid and liquid, liquid phase concentration, crystallization produce KFSI products.
10. preparation method as claimed in claim 1, it is characterised in that the method for crystallization include concentration and/or cooling and/or
Add poor solvent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116425128A (en) * | 2023-04-18 | 2023-07-14 | 浙江中欣氟材股份有限公司 | Preparation method of anhydrous lithium bis (fluorosulfonyl) imide |
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| CN105731398A (en) * | 2016-01-25 | 2016-07-06 | 苏州氟特电池材料股份有限公司 | Preparation method of alkali metal salt of bis (fluorosulfonyl) imide |
| 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 |
| CN106219503A (en) * | 2016-07-12 | 2016-12-14 | 武汉松石科技股份有限公司 | A kind of double (fluorine sulphonyl) imines and the preparation method of alkali metal salt thereof |
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| CN103391896A (en) * | 2011-03-03 | 2013-11-13 | 日本曹达株式会社 | Manufacturing method for fluorosulfonylimide ammonium salt |
| US9233849B2 (en) * | 2011-03-03 | 2016-01-12 | Nippon Soda Co., Ltd. | Process for producing fluorine-containing sulfonylimide salt |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116425128A (en) * | 2023-04-18 | 2023-07-14 | 浙江中欣氟材股份有限公司 | Preparation method of anhydrous lithium bis (fluorosulfonyl) imide |
| CN116425128B (en) * | 2023-04-18 | 2024-06-11 | 浙江中欣氟材股份有限公司 | Preparation method of anhydrous lithium bis (fluorosulfonyl) imide |
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Address after: 2003-1 Building No. 200, 2891 Lane, Qilian Mountain South Road, Putuo District, Shanghai Co-patentee after: Zhejiang Huajing Fluorine Chemistry Technology 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: Zhejiang Huajing Fluorine Chemistry Technology Co., Ltd. Patentee before: SHANGHAI KANGPENG TECHNOLOGY CO., LTD. |
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| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20211203 Address after: 2003-1 Building No. 200, 2891 Lane, Qilian Mountain South Road, Putuo District, Shanghai Patentee after: Shanghai Kangpeng Science and Technology Co.,Ltd. Patentee after: Quzhou kangpeng Chemical Co., Ltd Address before: 2003-1 Building No. 200, 2891 Lane, Qilian Mountain South Road, Putuo District, Shanghai Patentee before: Shanghai Kangpeng Science and Technology Co.,Ltd. Patentee before: Zhejiang Huajing Fluorine Chemical Technology Co., Ltd |