CN104681861B - The synthetic method of double chlorine sulfimide salts - Google Patents
The synthetic method of double chlorine sulfimide salts Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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Abstract
The invention discloses the synthetic method of a kind of pair of chlorine sulfimide salt, comprises the steps：（One）Under nitrogen protection, double chlorine sulfimides are added dropwise in aprotic organic solvent and are diluted the organic solution for obtaining double chlorine sulfimides, temperature is controlled in dilution for 0 DEG C～15 DEG C, the moisture Control of aprotic organic solvent is in 25～100ppm；（Two）Alkali metal salt is added in above-mentioned organic solution, 80 DEG C～140 DEG C are then heated slowly to while stirring, the moisture Control of alkali metal salt is 1 in the mol ratio of 50～100ppm, double chlorine sulfimides and alkali metal salt:1～1:1.1, organic solution is obtained after reaction；（Three）Under nitrogen protection, organic solution is filtered to get filtrate, and concentrated solution will be concentrated to give；（Four）By concentrated solution crystallization, filter, be dried, that is, obtaining highly purified pair of chlorine sulfimide salt.Said method is simple, and preparation cost is cheap；Products obtained therefrom purity and yield are higher, and moisture content is extremely low.
Description
Technical field
The invention belongs to lithium ion battery electrolyte synthesis field, and in particular to the intermediate of the double fluorine sulfimide salts of synthesis
The preparation method of double chlorine sulfimide alkali metal salts.
Background technology
Some fluorine-containing electrolyte have the conductivity of superelevation so as in the electrification such as secondary lithium battery and super capacitor
Learn and have important application on energy storage material and device.The lithium ion battery electrolyte of commercialization at present is mainly hexafluorophosphoric acid
Lithium, as some new electrolytic salts that improve of the performance requirements such as the safety to battery arise at the historic moment.For example, double fluoroforms
Base sulfimide lithium (LiTFSI), LiBF4 (LiBF4), double fluorine Lithium bis (oxalate) borates (LiODFB), and double fluorine sulphonyl Asia
Amine lithium (LiFSI) etc..These lithium salts have higher heat stability, wider electrochemical window；Wherein double fluorine sulfimide lithiums
(LiFSI) there is the advantage of uniqueness in electric conductivity and electrode corrosion, become the emphasis of current exploitation.
Due to the great water absorption of double fluorine sulfimide alkali metal salts and thermal instability, by the synthesis of general acid-base neutralization
Method --- i.e. using double fluorine sulfimides (HFSI) and alkali metal hydroxide or carbonate compound neutralization, it is impossible to prepare high-purity
Anhydrous pair of fluorine sulfimide alkali metal salt.And anhydrous pair of chlorine sulfimide alkali metal salt is anhydrous pair of fluorine sulfimide alkali gold of synthesis
The important source material of category salt.
J. Taraba（J. Taraba and Z. Zak, Inorg. Chem. 2006,45, 3695-3700）Utilize
Double chlorine sulfimides synthesize the acetonitrile solution of double chlorine sulfimide potassium in acetonitrile solvent with the potassium chloride being dried, and precipitate through benzene
Crystallize or dichloromethane precipitation Crystallization method are prepared for the double chlorine sulfimide salts containing solvent molecule respectively：KN
(SO2Cl)2·(1/2)CH3CN and KN (SO2Cl)2·(1/6)CH2Cl2, highly polar acetonitrile is made used in the course of reaction
For solvent, and the highly acid of double chlorine sulfimides (HCSI) can make solvent acetonitrile decompose, and the cyanic acid (HCN) of product severe toxicity is changed
Compound.Therefore the method is dfficult to apply in actual production.Paul（Ram chand paul et al J. inorg.
Nucl. Chem., 1977. Vol. 39. pp. 441-442）Double chlorine sulfimides and alkali metal chloride are utilized then four
In carbon chloride solution, back flow reaction prepares the alkali metal salt of anhydrous pair of chlorine sulfimide, this method avoid hypertoxic Organic substance cyanic acid
Generation, but as the alkali metal salt of double chlorine sulfimides is insoluble in carbon tetrachloride, constitute heterogeneous reaction, while generating double
The alkali metal salt of chlorine sulfimide can be coated on raw material alkali metal chloride surface, prevent the carrying out of reaction, ultimately result in product
Purity is not high, and yield is extremely low.
The content of the invention
It is an object of the invention to provide a kind of purity and yield it is higher, and suitable for the anhydrous double of industrialized production
The preparation method of chlorine sulfimide salt.The anhydrous pair of chlorine sulfimide salt is for preparing the important of anhydrous pair of fluorine sulfimide salt
Intermediate.
Described double chlorine sulfimide salts can be represented by the formula：MN(SO2Cl)2, abbreviation MCSI, wherein M be Li, Na, K,
One kind in Rb, Cs.
For achieving the above object, the technical solution used in the present invention is：The synthesis of described double chlorine sulfimide salts
Method, comprises the steps：（One）Under nitrogen protection, double chlorine sulfimides are added dropwise in aprotic organic solvent carry out it is dilute
The organic solution for obtaining double chlorine sulfimides is released, it is 0 DEG C～15 DEG C that temperature is controlled in dilution, the water of aprotic organic solvent
Sub-control system is in 25～100ppm；（Two）Alkali metal salt is added in above-mentioned organic solution, is then heated slowly to while stirring
80 DEG C～140 DEG C, the moisture Control of alkali metal salt is 1 in the mol ratio of 50～100ppm, double chlorine sulfimides and alkali metal salt:
1～1:1.1, the organic solution of double chlorine sulfimide salts is obtained after reaction；（Three）Under nitrogen protection, by double chlorine sulfimide salts
Organic solution filter to get filtrate, and filtrate is concentrated to give into concentrated solution；（Four）Concentrated solution is crystallized, solid is filtered, is dried,
Highly purified pair of chlorine sulfimide salt is obtained.
Further, the synthetic method of aforesaid pair of chlorine sulfimide salt, wherein, aprotic organic solvent is selected from following thing
One kind in matter：Dimethyl carbonate, diethyl carbonate, ethyl acetate.
Further, the synthetic method of aforesaid pair of chlorine sulfimide salt, wherein, the consumption of aprotic organic solvent is double
3～8 times of moles of chlorine sulfimide；It is highly preferred that the consumption of aprotic organic solvent is 5 times moles of double chlorine sulfimides
Amount.If extension rate is too high, the yield of double chlorine sulfimide salts in N-process is directly affected, if contrary extension rate mistake
It is low, it is unfavorable for the control of exothermic heat of reaction in N-process and the purity of product.
Further, the synthetic method of aforesaid pair of chlorine sulfimide salt, wherein, alkali metal salt is in following material
It is a kind of：Lithium chloride, Sodium Chloride, potassium chloride, Rubinorm (Ifi)., cesium chloride.
Further, the synthetic method of aforesaid pair of chlorine sulfimide salt, wherein, step（One）In by low temperature water-bath
Method controls the temperature of dilution.In practical operation, dilution course of dissolution is absorbed from 0 DEG C～10 DEG C of circulator baths
Heat release, can also by slowing down rate of addition, the means such as to be stirred too fast to prevent temperature in dilution from rising.
Further, the synthetic method of aforesaid pair of chlorine sulfimide salt, wherein, step（Two）In double chlorine sulfimides and
The mol ratio of alkali metal salt is 1:1.02～1:1.05, temperature is heated to 100 DEG C～130 DEG C, and the response time is 4～7 hours.
Further, the synthetic method of aforesaid pair of chlorine sulfimide salt, wherein, step（Three）In concentrate the filtrate to
60%～30% and obtain concentrated solution.The temperature control concentrated in practical operation is at 95 DEG C or so.
Further, the synthetic method of aforesaid pair of chlorine sulfimide salt, wherein, step（Four）The temperature of middle drying is
100 DEG C～120 DEG C, the dry time is 8～12 hours.Preferably it is dried under vacuum in practical operation, crystallizes
Temperature control between -10 DEG C～10 DEG C.
The invention has the beneficial effects as follows：Preparation process of the present invention is simple, and preparation cost is cheap；Products obtained therefrom
Purity and yield are higher, and moisture content is extremely low.
Specific embodiment
Below by specific embodiment, the invention will be further described, but the present invention is not limited in following enforcements
Example.
Embodiment 1：Double chlorine sulfimide potassium（KN(SO2Cl)2, abbreviation KCSI）Preparation.
Under the conditions of nitrogen protection and circulator bath, double chlorine sulfimides of 428 grams (2mol) are slowly added dropwise into acutely
In 900g dimethyl carbonate (10mol) solvent of stirring, it is 12 DEG C to control to dilute temperature from 5 DEG C of circulator baths.
Then dry 152g (2.04mol) potassium chloride (moisture 58ppm) is added to into above-mentioned solution at ambient temperature
In, 125 DEG C are slowly heated under agitation, are reacted 4 hours.
Reacting liquid filtering is obtained into 1400g reactant liquors after reaction, then 840g is concentrated under the conditions of 95 DEG C.
Above-mentioned concentrated solution is cooled to into 5 DEG C, is crystallized, vacuum drying obtains nothing in 12 hours under the conditions of 100 DEG C after filtration
The double chlorine sulfimide potassium 451g of water, yield 88.9%, moisture are 20ppm.
Embodiment 2：Double chlorine sulfimide sodium（NaN(SO2Cl)2, abbreviation NaCSI）Preparation.
Under the conditions of nitrogen protection and circulator bath, double chlorine sulfimides of 428g (2mol) are slowly added dropwise into acutely stirring
In 900g dimethyl carbonate (10mol) solvent mixed, it is 12 DEG C to control to dilute temperature from 8 DEG C of circulator baths.
Then dry 120g (2.04mol) Sodium Chloride (moisture 64ppm) is added to into above-mentioned solution at ambient temperature
In, 125 DEG C are slowly heated under agitation, are reacted 4 hours.
Reacting liquid filtering is obtained into 1380g reactant liquors after reaction, then 830g is concentrated under the conditions of 95 DEG C.
Above-mentioned concentrated solution is cooled to into 5 DEG C, is crystallized, vacuum drying obtains nothing in 12 hours under the conditions of 100 DEG C after filtration
The double chlorine sulfimide sodium 401g of water, yield 84.4%, moisture are 44ppm.
Embodiment 3：Double chlorine sulfimide lithiums（LiN(SO2Cl)2, abbreviation LiCSI）Preparation.
Under the conditions of nitrogen protection and circulator bath, double chlorine sulfimides of 428g (2mol) are slowly added dropwise into acutely stirring
In 900g dimethyl carbonate (10mol) solvent mixed, it is 5 DEG C to control to dilute temperature from 2 DEG C of circulator baths.
Then dry 86.5g (2.04mol) lithium chloride (moisture 57ppm) is added to into above-mentioned solution at ambient temperature
In, 125 DEG C are slowly heated under agitation, are reacted 4 hours.
Reacting liquid filtering is obtained into 1420g reactant liquors after reaction, then 860g is concentrated under the conditions of 95 DEG C.
Above-mentioned concentrated solution is cooled to into 5 DEG C, is crystallized, vacuum drying obtains nothing in 12 hours under the conditions of 100 DEG C after filtration
Double chlorine sulfimide lithiums 378g of water, yield 85.6%, moisture are 58ppm.
Embodiment 4：Double chlorine sulfimide potassium（KN(SO2Cl)2, abbreviation KCSI）Preparation.
Under the conditions of nitrogen protection and circulator bath, double chlorine sulfimides of 428 grams (2mol) are slowly added dropwise into acutely
In 880g ethyl acetate (10mol) solvent of stirring, it is 12 DEG C to control to dilute temperature from 9 DEG C of circulator baths.
Then dry 152g (2.04mol) potassium chloride (moisture 65ppm) is added to into above-mentioned solution at ambient temperature
In, 125 DEG C are slowly heated under agitation, are reacted 4 hours.
Reacting liquid filtering is obtained into 1380g reactant liquors after reaction, then 830g is concentrated under the conditions of 95 DEG C.
Above-mentioned concentrated solution is cooled to into -5 DEG C, is crystallized, vacuum drying obtains nothing in 12 hours under the conditions of 100 DEG C after filtration
The double chlorine sulfimide potassium 478g of water, yield 94.2%, moisture are 46ppm.
Embodiment 5：Double chlorine sulfimide sodium（NaN(SO2Cl)2, abbreviation NaCSI）Preparation.
Under the conditions of nitrogen protection and circulator bath, double chlorine sulfimides of 428g (2mol) are slowly added dropwise into acutely stirring
In 880g ethyl acetate (10mol) solvent mixed, it is 12 DEG C to control to dilute temperature from 5 DEG C of circulator baths.
Then dry 120g (2.04mol) Sodium Chloride (moisture 55ppm) is added to into above-mentioned solution at ambient temperature
In, 125 DEG C are slowly heated under agitation, are reacted 4 hours.
Reacting liquid filtering is obtained into 1360g reactant liquors after reaction, then 805g is concentrated under the conditions of 95 DEG C.
Above-mentioned concentrated solution is cooled to into -5 DEG C, is crystallized, vacuum drying obtains nothing in 12 hours under the conditions of 100 DEG C after filtration
The double chlorine sulfimide sodium 423g of water, yield 89.5%, moisture are 52ppm.
Embodiment 6：Double chlorine sulfimide lithiums（LiN(SO2Cl)2, abbreviation LiCSI）Preparation.
Under the conditions of nitrogen protection and circulator bath, double chlorine sulfimides of 428g (2mol) are slowly added dropwise into acutely stirring
In 880g ethyl acetate (10mol) solvent mixed, it is 5 DEG C to control to dilute temperature from 5 DEG C of circulator baths.
Then dry 86.5g (2.04mol) lithium chloride (moisture 49ppm) is added to into above-mentioned solution at ambient temperature
In, 125 DEG C are slowly heated under agitation, are reacted 4 hours.
Reacting liquid filtering is obtained into 1405g reactant liquors after reaction, then 812g is concentrated under the conditions of 95 DEG C.
Above-mentioned concentrated solution is cooled to into -5 DEG C, is crystallized, vacuum drying obtains nothing in 12 hours under the conditions of 100 DEG C after filtration
Double chlorine sulfimide lithiums 406g of water, yield 92.6%, moisture are 57ppm.
Claims (8)
1. the synthetic method of pair chlorine sulfimide salt, it is characterised in that：Comprise the steps：（One）Under nitrogen protection, will be double
Chlorine sulfimide is diluted the organic solution for obtaining double chlorine sulfimides in being added dropwise to aprotic organic solvent, in dilution
Temperature is controlled for 0 DEG C～15 DEG C, the moisture Control of aprotic organic solvent is in 25～100ppm；（Two）Alkali metal salt is added
In the organic solution stated, be then heated slowly to 80 DEG C～140 DEG C while stirring, the moisture Control of alkali metal salt 50～
The mol ratio of 100ppm, double chlorine sulfimides and alkali metal salt is 1:1～1:1.1, double chlorine sulfimide salts are obtained after reaction
Organic solution；（Three）Under nitrogen protection, the organic solution of double chlorine sulfimide salts is filtered to get filtrate, and filtrate is concentrated to give
To concentrated solution；（Four）Concentrated solution is crystallized, solid is filtered, is dried, that is, obtain highly purified pair of chlorine sulfimide salt；Above-mentioned
The one kind of aprotic organic solvent in following material：Dimethyl carbonate, diethyl carbonate, ethyl acetate.
2. the synthetic method of according to claim 1 pair of chlorine sulfimide salt, it is characterised in that：Aprotic organic solvent
Consumption is 3～8 times of moles of double chlorine sulfimides.
3. the synthetic method of according to claim 2 pair of chlorine sulfimide salt, it is characterised in that：Aprotic organic solvent
Consumption is 5 times of moles of double chlorine sulfimides.
4. the synthetic method of according to claim 1 pair of chlorine sulfimide salt, it is characterised in that：Alkali metal salt is selected from following
One kind in material：Lithium chloride, Sodium Chloride, potassium chloride, Rubinorm (Ifi)., cesium chloride.
5. the synthetic method of according to claim 1 pair of chlorine sulfimide salt, it is characterised in that：Step（One）In pass through water
The method of bath controls the temperature of dilution.
6. the synthetic method of according to claim 1 pair of chlorine sulfimide salt, it is characterised in that：Step（Two）In double chlorine sulphurs
The mol ratio of acid imide and alkali metal salt is 1:1.02～1:1.05, temperature is heated to 100 DEG C～130 DEG C, the response time be 4～
7 hours.
7. the synthetic method of according to claim 1 pair of chlorine sulfimide salt, it is characterised in that：Step（Three）It is middle by filtrate
It is concentrated into 60%～30% and obtains concentrated solution.
8. the synthetic method of according to claim 1 pair of chlorine sulfimide salt, it is characterised in that：Step（Four）Middle drying
Temperature is 100 DEG C～120 DEG C, and the dry time is 8～12 hours.
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| CN1450052A (en) * | 2003-04-30 | 2003-10-22 | 华中科技大学 | Ternary sulfonimine alkali salt and synthesis method thereof |
| CN102557996A (en) * | 2012-02-03 | 2012-07-11 | 苏州氟特电池材料有限公司 | Asymmetric fluorine-containing sulfimide alkali metal salt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450052A (en) * | 2003-04-30 | 2003-10-22 | 华中科技大学 | Ternary sulfonimine alkali salt and synthesis method thereof |
| CN102557996A (en) * | 2012-02-03 | 2012-07-11 | 苏州氟特电池材料有限公司 | Asymmetric fluorine-containing sulfimide alkali metal salt and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| (1/2)CH3CN, KN(SO2Cl)2∙(1/6)CH2Cl2, and [PCl4][N(SO2Cl)2.《Inorganic Chemistry》.2006,第45卷(第9期), * |
| CHEMISTRY OF IMIDOBIS(SULPHURYL CHLORIDE)-II SOME NOVEL DERIVATIVES OF IMIDOBIS(SULPHURYL CHLORIDE);RAM CHAND PAUL等;《Journal of Inorganic and Nuclear Chemistry》;19771231;第39卷;第441-442页 * |
| J. Taraba等.Novel Cation [N(SO2NMe3)2]+ and Its Synthesis and Crystal Structure. Dichloride of Imido-bis(sulfuric) Acid HN(SO2Cl)2. Part 1. Crystal Structures of KN(SO2Cl)2∙ * |
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