CN118306951A - Preparation method of sodium fluorosulfonate - Google Patents
Preparation method of sodium fluorosulfonate Download PDFInfo
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- CN118306951A CN118306951A CN202410522458.7A CN202410522458A CN118306951A CN 118306951 A CN118306951 A CN 118306951A CN 202410522458 A CN202410522458 A CN 202410522458A CN 118306951 A CN118306951 A CN 118306951A
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- XCXLEIPEAAEYTF-UHFFFAOYSA-M sodium fluorosulfate Chemical compound [Na+].[O-]S(F)(=O)=O XCXLEIPEAAEYTF-UHFFFAOYSA-M 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical group O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 31
- 239000011734 sodium Substances 0.000 claims abstract description 31
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 24
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 21
- 239000011737 fluorine Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 46
- 238000006243 chemical reaction Methods 0.000 claims description 41
- 235000013024 sodium fluoride Nutrition 0.000 claims description 23
- 239000011775 sodium fluoride Substances 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 22
- 239000003960 organic solvent Substances 0.000 claims description 17
- 239000012043 crude product Substances 0.000 claims description 14
- -1 sodium halide Chemical class 0.000 claims description 11
- BFXAWOHHDUIALU-UHFFFAOYSA-M sodium;hydron;difluoride Chemical compound F.[F-].[Na+] BFXAWOHHDUIALU-UHFFFAOYSA-M 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000011343 solid material Substances 0.000 claims description 9
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 3
- 239000000010 aprotic solvent Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 4
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims 2
- 229910000104 sodium hydride Inorganic materials 0.000 claims 1
- 239000012312 sodium hydride Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 4
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- 159000000000 sodium salts Chemical class 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application discloses a preparation method of sodium fluorosulfonate, which comprises the steps of reacting a fluorine source, a sodium source and a sulfonic acid source, wherein the sulfonic acid source is sulfur trioxide. The method has the advantages of easily available raw materials, simple preparation method and capability of obviously improving the yield of the product sodium fluorosulfonate.
Description
Technical Field
The invention relates to the technical field of chemical preparation, in particular to a preparation method of sodium fluorosulfonate.
Background
With the rapid development of lithium ion battery-driven electric automobiles, the application of lithium ion batteries has been expanded from portable electronic products to aspects affecting the social development, and the rapid development of lithium ion batteries is limited by limited lithium resources, so that sodium and lithium are metal elements in the same main group and different periods, have similar chemical characteristics, have very wide application prospects, and are hopeful to replace lithium with sodium.
At present, related researches on sodium ion batteries are mature, and as the cycle performance of the sodium ion batteries needs to be improved, the researches on the sodium ion batteries are mainly focused on the design and modification of anode and cathode materials, and the researches on electrolyte are less. And the electrolyte is an important component of the battery, and has an important influence on the battery performance.
Sodium fluorosulfonate can be used as a main component of sodium ion battery electrolyte, but reports on synthesis of sodium fluorosulfonate are less, and the existing method for synthesizing sodium fluorosulfonate is low in yield of sodium fluorosulfonate, so that raw material utilization and cost reduction are not facilitated.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a preparation method of sodium fluorosulfonate, which improves the yield of sodium fluorosulfonate.
The invention is realized in the following way:
In a first aspect, the invention provides a method for preparing sodium fluorosulfonate, which comprises the steps of reacting a fluorine source, a sodium source and a sulfonic acid source, wherein the sulfonic acid source is sulfur trioxide.
In an alternative embodiment, the sodium source is selected from at least one of sodium halides, sodium salts of organic acids, sodium salts of inorganic acids, sodium metals, and sodium hydrides;
Preferably, sodium fluoride is used as both the fluorine source and the sodium source.
In an alternative embodiment, the molar ratio of fluorine in the fluorine source, sodium in the sodium source, to sulfur trioxide is (0.9-1.1): (0.9-1.1): 1.
In an alternative embodiment, the reaction is carried out under non-aqueous solvent conditions;
Preferably, the nonaqueous solvent is an aprotic solvent;
preferably, the nonaqueous solvent is at least one of dimethyl carbonate and propylene carbonate;
preferably, the nonaqueous solvent is dimethyl carbonate;
preferably, the ratio of the total mass of the reactants to the addition amount of the nonaqueous solvent is 1 (4-10) g/ml.
In an alternative embodiment, the reaction is carried out under catalytic conditions, the catalyst being sodium hydrogen fluoride;
preferably, the addition amount of the sodium hydrogen fluoride is 8-10% of the mass of the hydrogen fluoride.
In an alternative embodiment, the reaction temperature is 60 ℃ to 80 ℃ and the reaction time is 8 hours to 12 hours.
In an alternative embodiment, concentrating after the reaction is completed to obtain a crude product, and purifying the crude product to obtain sodium fluorosulfonate;
Preferably, the temperature of the concentration step is from 55 ℃ to 70 ℃.
In an alternative embodiment, mixing and dissolving the crude product and an organic solvent to obtain an organic solution, standing the organic solution at (-8) - (-10) DEG C for 8-12 hours, and then carrying out solid-liquid separation to obtain a solid material containing sodium fluorosulfonate;
In an alternative embodiment, the ratio of crude product to organic solvent is 1 (18-22) g/ml;
Preferably, the dissolution temperature is 60 ℃ to 80 ℃;
Preferably, the obtained solid material is dried to obtain sodium fluorosulfonate;
preferably, the organic solvent is at least one of methanol and ethanol.
In alternative embodiments, the reaction process and/or purification step is performed under an inert atmosphere.
The invention has the following beneficial effects:
the sodium fluorosulfonate is prepared by utilizing the reaction of sulfur trioxide, a sodium source and a fluorine source, the raw materials are easy to obtain, the preparation method is simple, and the yield of the product sodium fluorosulfonate can be obviously improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a PXRD diagram of sodium fluorosulfonate;
FIG. 2 is a fluorine spectrum of sodium fluorosulfonate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The application provides a preparation method of sodium fluorosulfonate, which comprises the steps of reacting a fluorine source, a sodium source and a sulfonic acid source, wherein the sulfonic acid source is sulfur trioxide.
The sodium fluorosulfonate is prepared by utilizing the reaction of sulfur trioxide, a sodium source and a fluorine source, the raw materials are easy to obtain, the preparation method is simple, and the yield of the product sodium fluorosulfonate can be obviously improved.
The sulfur trioxide in the embodiment can be obtained by heating fuming sulfuric acid, and can also be prepared by other ways. In the present embodiment, since corrosive components such as HF may be produced as a byproduct due to the presence of the fluorine source, the reaction vessel needs to be resistant to HF corrosion, and specifically, a polytetrafluoroethylene reaction bottle may be selected, and a common glass reaction bottle may not be used.
In an alternative embodiment, the sodium source is selected from at least one of sodium halides, sodium salts of organic acids, sodium salts of inorganic acids, sodium metals, and sodium hydrides;
Preferably, sodium fluoride is used as both the fluorine source and the sodium source.
Sodium fluoride contains sodium and fluorine at the same time, does not contain other elements, does not introduce impurity elements, is beneficial to improving the utilization rate of raw materials, and is convenient for the subsequent separation and purification of sodium fluosulfonate.
The reaction principle of sodium fluoride and sulfur trioxide to form sodium fluorosulfonate is as follows:
S03+NaFNaOS02F
In an alternative embodiment, the molar ratio of fluorine in the fluorine source, sodium in the sodium source, to sulfur trioxide is (0.9-1.1): (0.9-1.1): 1, when sodium fluoride is used as the fluorine source and the sodium source, the molar ratio of sodium fluoride to sulfur trioxide is (0.9-1.1): 1.
The slightly excessive sulfur trioxide can improve the utilization rate of sodium fluoride and the yield of products, and unreacted SO 3 remains more than the above proportion reaction, SO that the amount of organic solvent for cleaning is increased, and the cost is correspondingly increased; if the ratio is higher than the above range, unreacted sodium source remains and the purity of sodium fluorosulfonate tends to be low. Specifically, the molar ratio of sodium fluoride to sulfur trioxide may be 0.90:1, 0.95:1, 1.00:1, 1.05:1, 1.10:1, etc.
In an alternative embodiment, the reaction is carried out under non-aqueous solvent conditions;
Preferably, the nonaqueous solvent is an aprotic solvent;
preferably, the nonaqueous solvent is at least one of dimethyl carbonate and propylene carbonate;
preferably, the nonaqueous solvent is dimethyl carbonate;
Preferably, the ratio of the total mass of the reactants to the added amount of the nonaqueous solvent is 1 (4-10) g/ml, and specifically may be any value between 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10g/ml or 1 (4-10) g/ml.
In the embodiment, on one hand, sulfur trioxide and sodium fluoride are adopted to react, so that the reaction is more severe and potential safety hazards are generated, therefore, a solvent is introduced into a reaction system, the reaction intensity is reduced, and the controllability and the safety of the reaction are improved; on the other hand, if the solvent amount is too small, a part of sodium fluorosulfonate that is not soluble in the solvent will adhere to the surface of sodium fluoride as sodium fluorosulfonate is formed, preventing the reaction of sodium fluoride with sulfur trioxide that is soluble in the solvent, and therefore the solvent amount needs to be sufficient to dissolve the product sodium fluorosulfonate.
The solvent may be omitted if safety is not a concern.
In an alternative embodiment, the reaction is carried out under catalytic conditions, the catalyst being sodium hydrogen fluoride;
Preferably, the sodium hydrogen fluoride is added in an amount of 8% to 10% by mass of hydrogen fluoride, and specifically may be any value between 8%, 8.5%, 9%, 9.5%, 10%, or 8% to 10%.
In this embodiment, since the amount of the solvent added is large in order to dissolve sodium fluorosulfonate, the reaction rate is greatly reduced. The fluorosulfonic acid serving as a catalyst can generate fluorosulfonic acid in a system, the fluorosulfonic acid and a fluorine source can react rapidly, and further the reaction rate is improved, but the existence of sodium bifluoride has little influence on the yield of sodium fluorosulfonate.
In an alternative embodiment, the reaction temperature is 60 ℃ to 80 ℃ and the reaction time is 8 hours to 12 hours to complete the reaction. Specifically, the reaction temperature may be 60 ℃, 65 ℃, 70 ℃, 75 ℃,80 ℃ or any value between 60 ℃ and 80 ℃; the reaction time may be 8h, 9h, 10h, 11h, 12h or any value between 8h and 12h.
The method and the order of addition of the reaction mixture are not particularly limited, but the preferable method of addition is, in terms of easy adjustment of the mass of sulfur trioxide to be introduced and easy adjustment of the reaction temperature: sulfur trioxide and reaction solvent are added to the reaction vessel followed by sodium fluoride and sodium bifluoride.
In an alternative embodiment, concentrating after the reaction is completed to obtain a crude product, and purifying the crude product to obtain sodium fluorosulfonate;
Preferably, the temperature of the concentration step is from 55 ℃ to 70 ℃.
The purpose of the concentration is to remove the waste water solvent, the specific temperature being related to the boiling point of the non-aqueous solvent. In some embodiments, the concentration is performed in a vacuum drying oven at 55-70deg.C and 0.8-0.9MPa, and drying under vacuum conditions to improve drying efficiency.
In an alternative embodiment, the crude product is mixed with an organic solvent to be dissolved to obtain an organic solution, the organic solution is placed at (-8) DEG C- (-10) DEG C and is kept stand for 8-12 h, and then solid-liquid separation is carried out to obtain a solid material containing sodium fluorosulfonate.
At low temperature, the solubility of sodium fluorosulfonate in organic solvent is reduced, so that the sodium fluorosulfonate is continuously separated out to obtain purer solid material containing a certain amount of organic solvent. Specifically, the temperature at which sodium fluorosulfonate is precipitated from the organic solution may be any value between (-8) °c, (-8.5) °c, (-9) °c, (-9.5) °c, (-10) °c, or (-8) °c- (-10) °c, and the standing time may be any value between 8h, 9h, 10h, 11h, 12h, or 8h-12 h.
In alternative embodiments, the ratio of crude product to organic solvent is 1 (18-22) g/ml, specifically may be any value between 1:18g/ml, 1:19g/ml, 1:20g/ml, 1:21g/ml, 1:22g/ml, or 1 (18-22) g/ml;
Preferably, the dissolution temperature is 60 ℃ to 80 ℃, in particular can be 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ or any value between 60 ℃ to 80 ℃;
Preferably, the obtained solid material is dried to obtain sodium fluorosulfonate;
preferably, the organic solvent is at least one of methanol and ethanol.
On the one hand, the introduction of the organic solvent is to enable sodium fluorosulfonate in the solid material to be fully dissolved, so that impurities or residual waste water solvent in the solid material are removed, and therefore the consumption of the organic solvent is not required to be too small; on the other hand, if the amount of the organic solvent is too large, the amount of sodium fluorosulfonate dissolved in the organic solvent increases, and therefore, the amount of the organic solvent to be added needs to be set appropriately.
In alternative embodiments, the reaction process and/or purification step is performed under an inert atmosphere.
Specifically, the inert atmosphere may be nitrogen or argon, in order to mainly avoid the contact of the reaction system with moisture in the outside air.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The embodiment provides a preparation method of sodium fluorosulfonate, which comprises the following steps:
(1) Under the condition of introducing nitrogen, 9.2g (115 mmol) of sulfur trioxide is introduced into a polytetrafluoroethylene reaction flask, 60ml of dimethyl carbonate is added into the reaction vessel, 5.07g (120.75 mmol) of sodium fluoride and 0.7129g (11.5 mmol) of sodium bifluoride are added, namely, the molar ratio of sodium fluoride to sulfur trioxide is 1.05:1, and the mixture is reacted for 10 hours at 70 ℃. After the reaction, it was directly concentrated to obtain 13.96g of a crude product.
(2) Under the protection of nitrogen, 500ml of absolute ethyl alcohol is added into the crude product, the solid is completely dissolved at 70 ℃, after stirring for about 30min, the crude product is placed in a refrigerator at-18 ℃ for 12h, white crystals are separated out, filter residues are reserved after suction filtration and are dried, and 11.5g (94.3 mmol, yield 82% and purity 99.8%) of sodium fluorosulfonate is obtained.
The PXRD pattern of sodium fluorosulfonate prepared in this example is shown in fig. 1, and it can be seen that 3 distinct diffraction peaks in the pattern are attributed to sodium fluorosulfonate.
The fluorine spectrum of the sodium fluorosulfonate prepared in this example is shown in FIG. 2, and it can be seen that a single peak appears at a chemical shift of 40.5ppm, which is attributed to the resonance absorption peak of fluorine atoms in sodium fluorosulfonate.
Example 2
This example provides a method for preparing sodium fluorosulfonate, which differs from example 1 only in that: the amount of sodium fluoride used was 126.5mmol. Namely: the molar ratio of sodium fluoride to sulfur trioxide was 1.1:1.
The result showed that the yield of sodium fluorosulfonate was 75% and the purity was 99.5%.
Example 3
This example provides a method for preparing sodium fluorosulfonate, which differs from example 1 only in that: the amount of sodium fluoride used was 103.5mmol. Namely: the molar ratio of sodium fluoride to sulfur trioxide was 0.9:1.
The result showed that the yield of sodium fluorosulfonate was 62% and the purity was 99.6%.
Example 4
This example provides a method for preparing sodium fluorosulfonate, which differs from example 1 only in that: the reaction temperature in the step (1) is 60 ℃.
The result showed that the yield of sodium fluorosulfonate was 48% and the purity was 99.6%.
Example 5
This example provides a method for preparing sodium fluorosulfonate, which differs from example 1 only in that: the reaction temperature in the step (1) is 80 ℃.
The result showed that the yield of sodium fluorosulfonate was 77% and the purity was 99.5%.
Example 6
This example provides a method for preparing sodium fluorosulfonate, which differs from example 1 only in that: the reaction temperature in the step (1) is 70 ℃, the reaction time is 8 hours, and the dosage of sodium fluoride is 120.75mmol, namely: the molar ratio of sodium fluoride to sulfur trioxide was 1.05:1.
The result showed that the yield of sodium fluorosulfonate was 60% and the purity was 99.6%.
Example 7
This example provides a method for preparing sodium fluorosulfonate, which differs from example 1 only in that: the reaction temperature is 70 ℃, the reaction time is 12 hours, and the dosage of sodium fluoride is 120.75mmol, namely: the molar ratio of sodium fluoride to sulfur trioxide was 1.05:1.
The result showed that the yield of sodium fluorosulfonate was 68% and the purity was 99.5%.
Example 8
This example provides a method for preparing sodium fluorosulfonate, which differs from example 1 only in that: sodium hydrogen fluoride was not added.
The result showed that the yield of sodium fluorosulfonate was 65% and the purity was 99.5%.
In summary, the invention provides a preparation method of sodium fluorosulfonate, which uses raw materials which are easy to obtain and process, can prepare sodium fluorosulfonate by a simple method, and simultaneously remarkably improves the yield of sodium fluorosulfonate.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the sodium fluorosulfonate is characterized by comprising the step of reacting a fluorine source, a sodium source and a sulfonic acid source, wherein the sulfonic acid source is sulfur trioxide.
2. The method for producing sodium fluorosulfonate according to claim 1, wherein the sodium source is at least one of sodium halide, sodium organic acid, sodium inorganic acid, sodium metal and sodium hydride;
Preferably, sodium fluoride is used as both the fluorine source and the sodium source.
3. The method for producing sodium fluorosulfonate according to claim 1, wherein the molar ratio of fluorine in the fluorine source, sodium in the sodium source, and sulfur trioxide is (0.9-1.1): (0.9-1.1): 1.
4. The method for producing sodium fluorosulfonate according to claim 1, wherein the reaction is performed under nonaqueous solvent conditions;
Preferably, the nonaqueous solvent is an aprotic solvent;
preferably, the nonaqueous solvent is at least one of dimethyl carbonate and propylene carbonate;
preferably, the nonaqueous solvent is dimethyl carbonate;
preferably, the ratio of the total mass of the reactants to the addition amount of the nonaqueous solvent is 1 (4-10) g/ml.
5. The method for preparing sodium fluorosulfonate according to claim 1, wherein the reaction is performed under a catalyst condition, the catalyst being sodium hydrogen fluoride;
preferably, the addition amount of the sodium hydrogen fluoride is 8-10% of the mass of the hydrogen fluoride.
6. The method for preparing sodium fluorosulfonate according to claim 1, wherein the reaction temperature is 60 ℃ to 80 ℃ and the reaction time is 8h to 12h.
7. The method for preparing sodium fluorosulfonate according to claim 1, wherein after the reaction is completed, concentration is performed to obtain a crude product, and purification is performed to obtain sodium fluorosulfonate;
Preferably, the temperature of the concentration step is from 55 ℃ to 70 ℃.
8. The method for preparing sodium fluorosulfonate according to claim 7, wherein the crude product is mixed with an organic solvent to obtain an organic solution, the organic solution is placed at (-8) - (-10) deg.c for 8-12 h, and then solid-liquid separation is performed to obtain a solid material containing sodium fluorosulfonate.
9. The method for producing sodium fluorosulfonate according to claim 8, wherein the ratio of the crude product to the organic solvent is 1 (18-22) g/ml;
Preferably, the dissolution temperature is 60 ℃ to 80 ℃;
Preferably, the obtained solid material is dried to obtain sodium fluorosulfonate;
preferably, the organic solvent is at least one of methanol and ethanol.
10. The method of preparing sodium fluorosulfonate according to claim 7, wherein the reaction process and/or the purification step are performed under an inert atmosphere.
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