CN105906536A - Trifluoromethanesulfinate purification method - Google Patents
Trifluoromethanesulfinate purification method Download PDFInfo
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- CN105906536A CN105906536A CN201610341314.7A CN201610341314A CN105906536A CN 105906536 A CN105906536 A CN 105906536A CN 201610341314 A CN201610341314 A CN 201610341314A CN 105906536 A CN105906536 A CN 105906536A
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- Prior art keywords
- solvent
- sodium trifluoromethanesulfinate
- purification
- sodium
- trifluoromethanesulfinate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C313/00—Sulfinic acids; Sulfenic acids; Halides, esters or anhydrides thereof; Amides of sulfinic or sulfenic acids, i.e. compounds having singly-bound oxygen atoms of sulfinic or sulfenic groups replaced by nitrogen atoms, not being part of nitro or nitroso groups
- C07C313/02—Sulfinic acids; Derivatives thereof
- C07C313/04—Sulfinic acids; Esters thereof
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a trifluoromethanesulfinic acid purification method. The method comprises the following steps: mixing and stirring a sodium trifluoromethanesulfinate industrial product, anhydrous magnesium sulfate and a solvent, carrying out suction filtration while stirring, collecting the filtrate, putting a filter cake in an original stirred reaction kettle, further adding the solvent, carrying out suction filtration while stirring, collecting the filtrate, collecting all the filtrates and filtrate solutions after leaching and putting all the filtrates and filtrate solutions after leaching in the kettle, carrying out reduced-pressure drying, recovering the solvent, adding deionized water to obtain a sodium trifluoromethanesulfinate water solution; then sending the sodium trifluoromethanesulfinate water solution to a dryer for spray drying, thus obtaining the sodium trifluoromethanesulfinate powder product with content of 95% or above. The method has the beneficial effects that high content sodium trifluoromethanesulfinate is extracted from the sodium trifluoromethanesulfinate industrial product by using the solvent and high content sodium trifluoromethanesulfinate without inorganic salts, such as bromide ions, is obtained after the solvent is removed, thus meeting the production requirements of lithium ion battery electrolyte bis(trifluoromethane)sulfonimide lithium salt.
Description
Technical field
Subject of the present invention is the method for purification of trifluoromethanesulpacidc acidc.
It is contemplated that prepare highly purified trifluoromethanesulpacidc acidc salt, and more particularly prepare
The alkali metal salt of trifluoromethanesulpacidc acidc.
Background technology
The metropolitan atmospheric pollution of China can not be ignored, petrol car discharge be primary pollution source it
One, existing 16 cities of China are put into global atmosphere and pollute among 20 the most serious cities.
The owning amount of China's automobile now is every 1,000 10 automobiles for each person, and the volume of holding will become
10 times of ground increase, thus in order to save the energy and reduce the discharge capacity of carbon dioxide, electric automobile
Will slowly become a kind of trend and the certainty of development of automobile.Exploitation electric automobile, its maximum
Technical bottleneck or vehicle-mounted electrochmical power source.Vehicular power system has been new forms of energy by country location
The core technology of automobile, " 12 " period developing china of lithium battery is classified as it
One of emerging strategic industries.Electrolyte is that the big critical material of lithium ion battery four is (positive pole, negative
One of pole, barrier film, electrolyte), it is known as " blood " of lithium ion battery, the most just
Play the effect of conduction electronics between negative pole, be that lithium ion battery obtains high voltage, high specific energy etc.
The guarantee of advantage.Electrolyte typically (is led at present by highly purified organic solvent, electrolyte lithium salt
If lithium hexafluoro phosphate, LiPF6), the raw material such as necessary additive, under certain condition, press
Certain proportion is formulated.Selecting to the performance impact of lithium ion battery very of electrolyte
Greatly, it must be that chemical stability is the most especially under higher current potential and higher temperature environment
In be not susceptible to decompose, there is higher ionic conductivity (> 10-3S/cm), and to anode and cathode
Material must be inert, can not invade rotten they.Double trifluoromethanesulfonimide lithiums
(C2F6LiNO4S2) it is the novel organic bath lithium salts of application in a kind of lithium ion battery,
There is higher electrochemical stability and electrical conductivity.And at higher voltages to aluminum collector
There is no corrosiveness.Its electrolyte solution being made into.Electrical conductivity is up to 1.0 × 10-2S/em,
At-30 DEG C, electrical conductivity is also 10-3More than s/cm.Have compared with traditional electrolyte matter LiPF6 with
Lower advantage: improve SEI film, stablize both positive and negative polarity interface, do not react with water, gas can be suppressed
Generate, the flatulence problem of battery will not be produced, improve cycle performance, high-temperature behavior and storage property
Energy.
Sodium trifluoromethanesulfinate (CF3NaO2S) is to produce double trifluoromethanesulfonimide lithium
Primary raw material, its production method be mainly in autoclave, with bromotrifluoromethane as raw material,
Sodium hydrosulfite is agent, with sodium dihydrogen phosphate as nertralizer, is simultaneously introduced water, acetonitrile, at height
Pressure is synthesized acquisition.The content of Sodium trifluoromethanesulfinate industrial goods is only at present
60-70%, wherein impurity is mainly the inorganic salts such as disodium hydrogen phosphate, sodium bromide, sodium sulfite,
Owing to it is difficult to purify, on existing market, the Sodium trifluoromethanesulfinate without high-load is sold.Double three
The production of fluoromethane sulfimide lithium, needs without inorganic salt, and the most the height of bromine ion-containing does not contains
The Sodium trifluoromethanesulfinate of amount.If China Patent No. is 200880118035.8 to disclose one
Plant the method preparing trifluoromethanesulpacidc acidc, although it can prepare high-purity trifluoromethyl Asia sulphur
Acid, but it uses more inorganic salt, it is difficult to purify, cause preparation process complicated, system
Standby inefficiency.The producing equipment that used and to prepare raw material more, preparation cost is higher, and
And serious waste phenomenon, be not suitable for large-scale promotion and use.
Therefore need exploitation one badly and can meet lithium ion battery electrolyte double fluoroform sulphonyl Asia
Amine lithium produces to be needed, and there are the Sodium trifluoromethanesulfinate industrial goods of preferable economic worth
Method of purification, i.e. a kind of trifluoromethanesulpacidc acidc method of purification.
Summary of the invention
1, problem to be solved
For the above-mentioned problems in the prior art, the present invention provides a kind of trifluoromethyl Asia sulphur
Acid method of purification, it extracts height by using solvent from Sodium trifluoromethanesulfinate industrial goods
The Sodium trifluoromethanesulfinate of content, obtains after desolvation containing without the height of the inorganic salts such as bromide ion
The Sodium trifluoromethanesulfinate of amount, meets the double trifluoromethanesulfonimide of lithium ion battery electrolyte
Lithium production requirement.
2, technical scheme
In order to solve the problems referred to above, the technical solution adopted in the present invention is as follows:
Described a kind of trifluoromethanesulpacidc acidc method of purification, described method of purification includes walking as follows
Rapid:
(1) in stirred autoclave, dry Sodium trifluoromethanesulfinate industrial goods it are sequentially added into
And anhydrous magnesium sulfate；
(2) in described stirred autoclave, add solvent again, stir under the conditions of 20-30 DEG C
0.5-1.0h, releases solution and carries out sucking filtration, collect the filtrate that sucking filtration obtains, and put back to by filter cake
In former stirred autoclave；
(3) step described in repetitive operation (2) is at least one times；
(4) equipped with in the stirred autoclave of filter cake, solvent is added, at 20-30 DEG C of bar
Stir 0.5-1.0h under part, release solution and carry out sucking filtration, filter cake with after a small amount of eluent solvent,
Remove filter cake；
(5) gained filtrate after described step (4) sucking filtration and the filtrate after drip washing are placed in stirring
In reactor, evaporated under reduced pressure, recycling design, and deionized water is added in stirred autoclave still,
Sodium trifluoromethanesulfinate solid is dissolved, obtains Sodium trifluoromethanesulfinate aqueous solution；
(6) deliver to exsiccator is sprayed by the Sodium trifluoromethanesulfinate aqueous solution of gained
It is dried, obtains the mass fraction content Sodium trifluoromethanesulfinate powder-product more than 95%.
Preferably, Sodium trifluoromethanesulfinate industrial goods described in step (1) and step (2),
The mass ratio of anhydrous magnesium sulfate and solvent is 15:1:25.
Preferably, during described in step (4), the consumption of solvent is step (2), solvent for use is used
0.6 times of amount.
Preferably, the mass fraction of Sodium trifluoromethanesulfinate industrial goods described in step (1)
Content is 60-70%.
Preferably, described solvent is ethyl acetate or acetonitrile.
Preferably, the addition of deionized water described in step (5) is described in step (1)
3-4 times of Sodium trifluoromethanesulfinate industrial goods addition.
Preferably, in described step (3), step (2) described in repetitive operation is preferably once.
3, beneficial effect
Compared to prior art, the invention have the benefit that
(1) present invention uses solvent to extract height from Sodium trifluoromethanesulfinate industrial goods to contain
The Sodium trifluoromethanesulfinate of amount, obtains the high-load without inorganic salts such as bromide ions after desolvation
Sodium trifluoromethanesulfinate, meet the double trifluoromethanesulfonimide lithium of lithium ion battery electrolyte
Production requirement；
(2) method of purification low cost of the present invention, yield is high, Sodium trifluoromethanesulfinate
Product content is up in more than 95%, and institute's refined product without inorganic salts such as bromide ions, can meet
The double trifluoromethanesulfonimide lithium production requirement of lithium ion battery electrolyte, also can meet ethiprole
Production requirement；
(3) method of purification of the present invention can not only prepare high-purity trifluoromethyl sulfinic acid,
Meet the double trifluoromethanesulfonimide lithium production requirement of lithium ion battery electrolyte, and purified product
Without inorganic salts such as bromide ions in product, the equipment for purifying and the purification cost of material that are used are low, and
Solvent can recycle, and reduces waste, also have that operational approach is simple, preparation process simple,
The advantage that preparation efficiency is high, is suitable for large-scale promotion and uses.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described below.
A kind of trifluoromethanesulpacidc acidc method of purification, described method of purification comprises the steps:
(1) be sequentially added in stirred autoclave mass fraction content be 60-70% be dried three
Methyl fluoride sulfinic acid sodium industrial goods and anhydrous magnesium sulfate；
(2) in described stirred autoclave, add solvent again, stir under the conditions of 20-30 DEG C
0.5-1.0h, releases solution and carries out sucking filtration, collect the filtrate that sucking filtration obtains, and put back to by filter cake
In former stirred autoclave；
(3) step described in repetitive operation (2) is at least one times；
(4) equipped with in the stirred autoclave of filter cake, solvent is added, at 20-30 DEG C of bar
Stir 0.5-1.0h under part, release solution and carry out sucking filtration, filter cake with after a small amount of eluent solvent,
Remove filter cake；
(5) gained filtrate after described step (4) sucking filtration and the filtrate after drip washing are placed in stirring
In reactor, evaporated under reduced pressure, recycling design, and deionized water is added in stirred autoclave still,
Sodium trifluoromethanesulfinate solid is dissolved, obtains Sodium trifluoromethanesulfinate aqueous solution；
(6) deliver to exsiccator is sprayed by the Sodium trifluoromethanesulfinate aqueous solution of gained
It is dried, obtains the mass fraction Sodium trifluoromethanesulfinate powder-product more than 95%.
It should be noted that Sodium trifluoromethanesulfinate described in step (1) and step (2)
The mass ratio of industrial goods, anhydrous magnesium sulfate and solvent is 15:1:25.Described in step (4) molten
The consumption of agent is in step (2) 0.6 times of solvent for use consumption.Described solvent is acetic acid second
Ester or acetonitrile.The addition of deionized water described in step (5) is described in step (1) three
3-4 times of methyl fluoride sulfinic acid sodium industrial goods addition.Repetitive operation in described step (3)
Described step (2) is preferably once.
Embodiment 1
At one equipped with in the 2000ml there-necked flask of agitator, add 60-70% trifluoromethyl
Sulfinic acid sodium industrial goods 300g, anhydrous magnesium sulfate 20g, ethyl acetate solvent 500g, 20-30 DEG C
Lower stirring 0.5h, stops stirring, and discharging is filtered, filtrate collection, and filter cake is put back in flask,
In flask, add 500g ethyl acetate solvent, at 20-30 DEG C, stir 0.5h, stop stirring
Mixing, discharging is filtered, and filtrate collection, filter cake is put back in flask again, adds 300g acetic acid
Ethyl ester solvent, stirs 0.5h at 20-30 DEG C, stops stirring, and discharging is filtered, filtrate collection,
Filter cake, with a small amount of ethyl acetate solvent drip washing, is removed filter cake, is collected three filtrate and drip washing
Filtrate solutions, with rotation steam negative pressure be evaporated, reclaim ethyl acetate solvent, recycle, will
1000g deionized water adds in still, is dissolved by Sodium trifluoromethanesulfinate solid, obtains fluoroform
Base sulfinic acid sodium water solution, Sodium trifluoromethanesulfinate aqueous solution send exsiccator to carry out spray dried
Dry, obtain the Sodium trifluoromethanesulfinate product of content more than 95%.
Based on above-mentioned, the present invention uses solvent to extract from Sodium trifluoromethanesulfinate industrial goods
The Sodium trifluoromethanesulfinate of high-load, obtains the height without inorganic salts such as bromide ions after desolvation
The Sodium trifluoromethanesulfinate of content, meets the double fluoroform sulphonyl of lithium ion battery electrolyte sub-
Amine lithium production requirement；Method of purification low cost of the present invention, yield is high, trifluoromethyl Asia sulphur
Acid sodium product content is up in more than 95%, and institute's refined product without the inorganic salts such as bromide ion, energy
Meet the double trifluoromethanesulfonimide lithium production requirement of lithium ion battery electrolyte, also can meet fluorine
The production requirement of worm nitrile；It can not only prepare high-purity trifluoromethyl sulfinic acid, meet lithium from
Without bromine in sub-cell electrolyte double trifluoromethanesulfonimide lithium production requirement, and institute's refined product
The inorganic salts such as ion, the equipment for purifying used and purification cost of material are low, and solvent is permissible
Recycle, reduce waste, also have that operational approach is simple, preparation process simple, preparation effect
The advantage that rate is high, is suitable for large-scale promotion and uses.
Embodiment 2
At one equipped with in the 2000ml there-necked flask of agitator, add 60-70% trifluoromethyl
Sulfinic acid sodium industrial goods 300g, anhydrous magnesium sulfate 20g, acetonitrile solvent 500g, at 20-30 DEG C
Stirring 0.5h, stops stirring, and discharging is filtered, filtrate collection, and filter cake is put back in flask, to
Flask adds 500g acetonitrile solvent, at 20-30 DEG C, stirs 0.5h, stop stirring, go out
Material filters, filtrate collection, and filter cake is put back in flask again, adds 300g acetonitrile solvent,
Stirring 0.5h at 20-30 DEG C, stop stirring, discharging is filtered, filtrate collection, and filter cake is with few
The acetonitrile solvent drip washing of amount, removes filter cake, collects three filtrate and the Filtrate solutions of drip washing,
Steam negative pressure with rotation to be evaporated, reclaim acetonitrile solvent, recycle, 1000g deionized water is added
Enter in still, Sodium trifluoromethanesulfinate solid dissolved, obtains Sodium trifluoromethanesulfinate aqueous solution,
Sodium trifluoromethanesulfinate aqueous solution send exsiccator to be spray-dried, and obtains content more than 95%
Sodium trifluoromethanesulfinate product.
Embodiment 3
In a 2L reactor, add 60-70% Sodium trifluoromethanesulfinate industrial goods
300kg, anhydrous magnesium sulfate 20kg, ethyl acetate solvent 500kg, stir 0.5h at 20-30 DEG C,
Stopping stirring, discharging is filtered, filtrate collection, and filter cake is put back in flask, adds in flask
500k g ethyl acetate solvent, stirs 0.5h at 20-30 DEG C, stops stirring, and discharging is filtered,
Filtrate collection, filter cake is put back in flask again, adds 300kg ethyl acetate solvent,
Stirring 0.5h at 20-30 DEG C, stop stirring, discharging is filtered, filtrate collection, and filter cake is with a small amount of
Ethyl acetate solvent drip washing, remove filter cake, collect three filtrate and the Filtrate solutions of drip washing
In reactor, evaporated under reduced pressure, recycling design ethyl acetate, recycle, by 1000kg
Deionized water adds in still, is dissolved by Sodium trifluoromethanesulfinate solid, obtains trifluoromethyl Asia sulphur
Acid sodium aqueous solution, Sodium trifluoromethanesulfinate aqueous solution send exsiccator to be spray-dried, and must contain
The Sodium trifluoromethanesulfinate powder-product of amount more than 95%.
Schematically being described the present invention and embodiment thereof above, this description does not limit
Property processed, actual structure is not limited thereto.So, if those of ordinary skill in the art
Enlightened by it, in the case of without departing from the invention objective, design without creative
The frame mode similar to this technical scheme and embodiment, all should belong to the protection model of the present invention
Enclose.
Claims (7)
1. a trifluoromethanesulpacidc acidc method of purification, it is characterised in that described method of purification
Comprise the steps:
(1) in stirred autoclave, dry Sodium trifluoromethanesulfinate industrial goods it are sequentially added into
And anhydrous magnesium sulfate；
(2) in described stirred autoclave, add solvent again, stir under the conditions of 20-30 DEG C
0.5-1.0h, releases solution and carries out sucking filtration, collect the filtrate that sucking filtration obtains, and put back to by filter cake
In former stirred autoclave；
(3) step described in repetitive operation (2) is at least one times；
(4) equipped with in the stirred autoclave of filter cake, solvent is added, at 20-30 DEG C of bar
Stir 0.5-1.0h under part, release solution and carry out sucking filtration, filter cake with after a small amount of eluent solvent,
Remove filter cake；
(5) gained filtrate after described step (4) sucking filtration and the filtrate after drip washing are placed in stirring
In reactor, evaporated under reduced pressure, recycling design, and deionized water is added in stirred autoclave still,
Sodium trifluoromethanesulfinate solid is dissolved, obtains Sodium trifluoromethanesulfinate aqueous solution；
(6) deliver to exsiccator is sprayed by the Sodium trifluoromethanesulfinate aqueous solution of gained
It is dried, obtains the mass fraction Sodium trifluoromethanesulfinate powder-product more than 95%.
A kind of trifluoromethanesulpacidc acidc method of purification the most according to claim 1, it is special
Levy and be, Sodium trifluoromethanesulfinate industrial goods, nothing described in step (1) and step (2)
The mass ratio of water magnesium sulfate and solvent is 15:1:25.
A kind of trifluoromethanesulpacidc acidc method of purification the most according to claim 1, it is special
Levy and be, solvent for use consumption during the consumption of solvent is step (2) described in step (4)
0.6 times.
A kind of trifluoromethanesulpacidc acidc method of purification the most according to claim 1, it is special
Levying and be, described in step (1), the mass fraction of Sodium trifluoromethanesulfinate industrial goods is
60-70%.
5. according to a kind of trifluoromethanesulpacidc acidc purification side described in any one of claim 1-4
Method, it is characterised in that described solvent is ethyl acetate or acetonitrile.
A kind of trifluoromethanesulpacidc acidc method of purification the most according to claim 1, it is special
Levying and be, the addition of deionized water described in step (5) is trifluoro described in step (1)
3-4 times of methyl sulfinic acid sodium industrial goods addition.
A kind of trifluoromethanesulpacidc acidc method of purification the most according to claim 1, it is special
Levying and be, in described step (3), step (2) described in repetitive operation is preferably once.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610341314.7A CN105906536A (en) | 2016-05-20 | 2016-05-20 | Trifluoromethanesulfinate purification method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610341314.7A CN105906536A (en) | 2016-05-20 | 2016-05-20 | Trifluoromethanesulfinate purification method |
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ID=56748370
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748916A (en) * | 2016-12-28 | 2017-05-31 | 江苏托球农化股份有限公司 | A kind of production technology of Sodium trifluoromethanesulfinate |
| CN113976014A (en) * | 2021-10-29 | 2022-01-28 | 江苏优普生物化学科技股份有限公司 | High-content sodium trifluoromethanesulphinate refining equipment and manufacturing method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101878195A (en) * | 2007-11-27 | 2010-11-03 | 罗地亚管理公司 | Method for preparing trifluoromethanesulphinic acid |
| CN101878196A (en) * | 2007-11-27 | 2010-11-03 | 罗地亚管理公司 | Method for preparing a trifluoromethanesulphinic acid salt. |
| CN102105444A (en) * | 2008-07-30 | 2011-06-22 | 中央硝子株式会社 | Process for producing perfluoroalkanesulfinic acid salt |
-
2016
- 2016-05-20 CN CN201610341314.7A patent/CN105906536A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101878195A (en) * | 2007-11-27 | 2010-11-03 | 罗地亚管理公司 | Method for preparing trifluoromethanesulphinic acid |
| CN101878196A (en) * | 2007-11-27 | 2010-11-03 | 罗地亚管理公司 | Method for preparing a trifluoromethanesulphinic acid salt. |
| CN102105444A (en) * | 2008-07-30 | 2011-06-22 | 中央硝子株式会社 | Process for producing perfluoroalkanesulfinic acid salt |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748916A (en) * | 2016-12-28 | 2017-05-31 | 江苏托球农化股份有限公司 | A kind of production technology of Sodium trifluoromethanesulfinate |
| CN113976014A (en) * | 2021-10-29 | 2022-01-28 | 江苏优普生物化学科技股份有限公司 | High-content sodium trifluoromethanesulphinate refining equipment and manufacturing method thereof |
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Application publication date: 20160831 |