CN115991460A - Preparation method and application of dichloro sulfonyl imide - Google Patents
Preparation method and application of dichloro sulfonyl imide Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical group ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 title claims abstract description 18
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 claims abstract description 44
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 36
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000002912 waste gas Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 23
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 21
- 238000006276 transfer reaction Methods 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 13
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 13
- 238000012546 transfer Methods 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims description 58
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 26
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 26
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 14
- ATMIHASMQFJNLZ-UHFFFAOYSA-N dichloro(imino)-$l^{4}-sulfane Chemical compound ClS(Cl)=N ATMIHASMQFJNLZ-UHFFFAOYSA-N 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 8
- 229910001416 lithium ion Inorganic materials 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910000856 hastalloy Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910000792 Monel Inorganic materials 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 14
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 7
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000001804 emulsifying effect Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 235000011837 pasties Nutrition 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- BHHYHSUAOQUXJK-UHFFFAOYSA-L zinc fluoride Chemical compound F[Zn]F BHHYHSUAOQUXJK-UHFFFAOYSA-L 0.000 description 2
- FIADVASZMLCQIF-UHFFFAOYSA-N 2,2,4,4,6,6,8,8-octamethyl-1,3,5,7,2,4,6,8-tetrazatetrasilocane Chemical compound C[Si]1(C)N[Si](C)(C)N[Si](C)(C)N[Si](C)(C)N1 FIADVASZMLCQIF-UHFFFAOYSA-N 0.000 description 1
- ZJPPTKRSFKBZMD-UHFFFAOYSA-N [Li].FS(=N)F Chemical compound [Li].FS(=N)F ZJPPTKRSFKBZMD-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GBFOVGYSKHACRD-UHFFFAOYSA-N dichloro-imino-oxo-lambda6-sulfane Chemical compound ClS(Cl)(=N)=O GBFOVGYSKHACRD-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method and application of dichloro sulfonyl imide. The preparation method comprises the following steps: (1) Grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride to obtain a raw material mixed solution; (2) Carrying out mass transfer and heat transfer reaction on the raw material mixed solution in the step (1) to obtain a dichloro sulfonyl imide mixed solution; (3) And (3) sequentially carrying out gas-liquid separation and nitrogen introduction treatment on the mixed solution of the dichlorsulfonylimide in the step (2) to obtain a dichlorsulfonylimide solution and acid waste gas, distilling the dichlorsulfonylimide solution to obtain the dichlorsulfonylimide, and sequentially carrying out pressurization, rectification and separation, oxidation and chemical synthesis reaction on the acid waste gas to obtain chlorosulfonic acid. In the process of preparing the dichloro sulfonyl imide, the waste gas and the waste liquid are treated, so that the preparation cost is greatly reduced, the high-purity dichloro sulfonyl imide is obtained, and the raw material utilization rate of the dichloro sulfonyl imide is improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, relates to a preparation method of dichloro-sulfonyl-imide, and particularly relates to a preparation method and application of dichloro-sulfonyl-imide.
Background
Lithium ion batteries, which are widely used chemical energy sources, are widely studied in the world, mainly comprise a positive electrode, a negative electrode and an electrolyte, and lithium bis (fluorosulfonyl) imide, which is a key high-performance material in lithium ion batteries, has extremely high industrial application value.
The lithium bis (fluorosulfonyl) imide becomes the novel lithium salt with the fastest industrialization progress due to the beneficial properties such as structural stability and electrochemical properties. Compared with lithium hexafluorophosphate, lithium bis (fluorosulfonyl) imide has the following advantages: 1) The anion radius of the lithium bis (fluorosulfonyl) imide is larger, so that the lithium ions are more easily dissociated and removed, and the conductivity of the lithium ion battery is further improved; 2) When the temperature is higher than 200 ℃, the lithium bis (fluorosulfonyl) imide can still exist stably, decomposition does not occur, the thermal stability is good, and the safety performance of the low-ion battery is further improved; 3) The electrolyte taking lithium bis (fluorosulfonyl) imide as electrolyte maintains good compatibility with positive and negative electrode materials, and can obviously improve the high and low temperature performance of the lithium ion battery.
Currently, as an important intermediate for synthesizing lithium difluorosulfimide, the economic value is high, and therefore, the purity of the bischlorosulfimide and the low-cost industrial production are important.
CN111099566a discloses a method for preparing co-produced bis-chlorosulfonyl imide acid and lithium bis-fluorosulfonyl imide. And adding sulfuryl chloride into the first solvent, then dropwise adding octamethyl cyclotetrasilazane, reacting, and purifying to obtain the dichloro sulfonyl imide acid. The purification method comprises distilling off the residual raw materials and byproducts, distilling off the first solvent, and recycling the distilled byproducts. However, simple distillation does not completely remove by-products, and the purity of the produced bischlorosulfonimide is not high.
In CN103524387A, sulfamic acid, thionyl chloride and chlorosulfonic acid are reacted to generate a difluoro sulfonimide compound, thionyl chloride and anhydrous lithium salt are directly added for reaction to obtain the dichloro sulfonimide lithium salt, and anhydrous zinc fluoride is utilized for fluorination reaction to obtain the difluoro sulfonimide salt, but the byproduct generated in the process of synthesizing the dichloro sulfonimide is high, the purity of the product is low, the waste of raw materials is serious, and the industrialized production is not facilitated.
Therefore, how to prepare the dichlorsulfoximine efficiently and at low cost in a large scale is an important research direction in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method and application of dichloro sulfonyl imide.
To achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a preparation method of the dichloro sulfonyl imide, which comprises the following steps:
(1) Grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride to obtain a raw material mixed solution;
(2) Carrying out mass transfer and heat transfer reaction on the raw material mixed solution in the step (1) to obtain a dichloro sulfonyl imide mixed solution;
(3) Sequentially carrying out gas-liquid separation and nitrogen introduction treatment on the mixed solution of the dichloro sulfimide in the step (2) to obtain a dichloro sulfimide solution and acid waste gas; distilling the bischlorosulfimide solution to obtain the bischlorosulfimide; and (3) sequentially carrying out pressurized rectification separation, oxidation and chemical synthesis reaction on the acid waste gas. Chlorosulfonic acid is obtained.
Grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride, wherein the blending is accompanied with a grinding process, and particularly, the sulfamic acid in a solid phase is fully ground, so that three raw materials can be fully mixed and uniformly dispersed to form a raw material mixed solution with good uniformity, the reaction rate in the step (2) is further improved, and the reaction time is shortened; and then through the mass and heat transfer reaction in the step (2), particularly the mass and heat transfer of a solid-liquid interface is generated between sulfamic acid and chlorosulfonic acid/thionyl chloride, the efficiency of mass and heat transfer is greatly improved, the reaction time is reduced, and the generation rate of the dichlorosulfimide is improved. In the step (3), a large amount of acid waste gas is generated in the process of synthesizing the dichlorosulfimide, and meanwhile, by-products hydrochloric acid and sodium sulfite are generated, so that the method has no economic value. The invention separates high-purity sulfur dioxide gas and hydrogen chloride gas through pressurized rectification, oxidizes sulfur dioxide to sulfur trioxide, then reacts with hydrogen chloride to produce chlorosulfonic acid, and the chlorosulfonic acid is recycled and reused as a raw material for the first step of reaction. The synthesis process greatly reduces the waste of raw materials and the pollution to the environment.
As a preferable technical scheme of the invention, the feeding mole ratio of chlorosulfonic acid, sulfamic acid and thionyl chloride in the step (1) is 1: (0.8-1.5): (2-8), wherein 0.8-1.5 may be 0.9, 1, 1.1, 1.2, 1.3, 1.4, 1.5, etc., and 2-8 may be 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, etc.; the molar ratio may be 1:1:2. 1:1.2:2. 1:1.5: 2. 1:1: 3. 1:1.2: 3. 1:1.2:2.5, 1:1.5: 2. 1:1.5:3 or 1:1.5:4, etc., but are not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the grinding blending of step (1) is performed in a compounding device provided with an emulsion pump.
Preferably, the time for the milling and blending in the step (1) is 1 to 15 hours, for example, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours or 14 hours, etc., and more preferably 5 to 12 hours.
As a preferable technical scheme of the invention, the mixture of chlorosulfonic acid, sulfamic acid and thionyl chloride is circularly ground in a mixing device provided with an emulsifying pump so as to fully crush and emulsify materials; the grinding and blending time is 1-2h, and the grain diameter can reach 200-300 mu m; the grinding and blending time is 5 hours, and the grain diameter can reach 80-100 mu m; the grinding and blending time is 10 hours, and the grain diameter can reach 30-50 mu m; the grinding and blending time is 12 hours and can reach 20-30 mu m; the economy of continuing the milling is not high. Thus, the most preferred time for the grind blending is 12 hours.
Preferably, the atmosphere of the blending in step (1) is a nitrogen atmosphere.
Preferably, the temperature of the milling and blending in step (1) is 10 to 45 ℃, wherein the temperature may be 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ or the like, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the sulfamic acid after the grinding and blending in step (1) has a particle size of <100 μm, wherein the particle size may be 5 μm, 10 μm, 15 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 99 μm, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the mass and heat transfer reaction of step (2) is carried out in a dynamic tubular reactor.
As a preferable embodiment of the present invention, the length of the dynamic tube reactor is 500 to 10000mm, wherein the length may be 500mm, 1000mm, 2000mm, 3000mm, 4000mm, 5000mm, 6000mm, 7000mm, 8000mm, 9000mm or 10000mm, etc., but not limited to the recited values, other non-recited values within the numerical range are equally applicable.
Preferably, the equivalent diameter of the dynamic tubular reactor is 50-800 mm, wherein the diameter may be 50mm, 100mm, 200mm, 300mm, 400mm, 500mm, 600mm, 700mm or 800mm, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the inner wall material of the dynamic tube reactor comprises any one of silicon carbide, 316L stainless steel, hastelloy C-276 alloy or Monel alloy.
As a preferable technical scheme of the invention, the feeding flow rate of the raw material mixed solution in the step (2) is 0.1-50L/min, wherein the feeding flow rate can be 0.1L/min, 1L/min, 5L/min, 10L/min, 15L/min, 20L/min, 25L/min, 30L/min, 35L/min, 40L/min, 45L/min or 50L/min, and the like, but the raw material mixed solution is not limited to the listed values, and other non-listed values in the range of the values are applicable.
Preferably, the temperature of the mass and heat transfer reaction in the step (2) is 75 to 150 ℃, wherein the temperature may be 80 ℃, 90 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, or the like, but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the time of the mass and heat transfer reaction in the step (2) is 5-120 min, wherein the time can be 5min, 10min, 15min, 20min, 25min or 30min, etc., but is not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
As a preferred embodiment of the present invention, the gas-liquid separation in step (3) is performed in a gas-liquid separator.
Preferably, the constant temperature ageing treatment is carried out in the gas-liquid separation in the step (3).
Preferably, the temperature of the constant temperature aging treatment is 75 to 150 ℃, wherein the temperature can be 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃ or the like, but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the constant temperature aging treatment is performed for 0.1 to 10 hours, wherein the time can be 0.1 hour, 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours or 10 hours, etc., but the method is not limited to the listed values, and other non-listed values in the range of the values are equally applicable.
Preferably, the nitrogen gas in the nitrogen passing treatment has a water content of <50ppm, wherein the water content may be 5ppm, 10ppm, 15ppm, 20ppm, 25ppm, 30ppm, 35ppm, 40ppm, 45ppm or 49ppm, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In a preferred embodiment of the present invention, the pressure of the distillation in the step (3) may be, for example, 200Pa, 500Pa, 800Pa, 1kPa, 2kPa, 3kPa, 4kPa, 5kPa, 6kPa, 7kPa, 8kPa, 9kPa, etc., but the distillation pressure is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
The distillation temperature in the step (3) is preferably 50 to 150 ℃, and may be, for example, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃, or 140 ℃, but is not limited to the values listed, and other values not listed in the range are equally applicable.
As a preferred embodiment of the present invention, the acid waste gas in step (3) includes sulfur dioxide (gas) and hydrogen chloride (gas).
Preferably, sulfur dioxide (gas) and hydrogen chloride (gas) are respectively obtained after the separation of the pressure rectification in the step (3).
Preferably, the temperature of the pressure distillation in the step (3) is-50 ℃ to-10 ℃, and for example, it may be-45 ℃, -40 ℃, -35 ℃, -30 ℃, -25 ℃, -20 ℃, -15 ℃, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
The pressure of the pressure distillation in the step (3) is preferably 0.2 to 1.5MPa, and may be, for example, 0.3MPa, 0.5MPa, 0.8MPa, 1MPa, 1.2MPa, or 1.4MPa, etc., but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the pressure rectification in step (3) is performed in a pressure rectification column, and the packing mode of the pressure rectification column is optional structured packing, but is not limited to the mode.
Preferably, the rectifying tower diameter of the pressure rectification in the step (3) is 200 mm-1000 mm, wherein the tower diameter can be 200mm, 400mm, 600mm, 800mm, 1000mm and the like, but is not limited to the listed values, and other non-listed values in the range of the values are equally applicable.
Preferably, the column height of the pressure rectification column in the step (3) is 3000mm to 20000mm, wherein the column height can be 3000mm, 4000mm, 6000mm, 8000mm, 10000mm, 15000mm, 20000mm and the like, but is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the oxidation of step (3) is performed on the sulfur dioxide to obtain sulfur trioxide.
Preferably, the oxidising agent comprises oxygen; preferably, the air (which contains oxygen) is mixed with sulfur dioxide and then oxidized to obtain sulfur trioxide.
Preferably, the oxidation is carried out in the presence of a catalyst comprising vanadium pentoxide.
The oxidation temperature is preferably 250 to 500 ℃, and may be 260 ℃, 280 ℃, 300 ℃, 320 ℃, 345 ℃, 350 ℃, 380 ℃, 400 ℃, 420 ℃, 450 ℃, 480 ℃, or the like, for example, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the oxidation process of sulfur dioxide is a continuous process, and the specific method comprises the following steps: sulfur dioxide and air are introduced into a reaction device, and oxidation is carried out by adopting a method of three-conversion and two-absorption (three-conversion and two-absorption) in the presence of a catalyst (vanadium pentoxide), so that the sulfur dioxide is fully converted into sulfur trioxide.
In the invention, sulfur trioxide obtained by catalytic oxidation of sulfur dioxide is absorbed by sulfuric acid to obtain fuming sulfuric acid, and the sulfur trioxide is evaporated from the fuming sulfuric acid and used for subsequent reactions.
Preferably, the mass fraction (purity) of the sulfur trioxide is 99% or more, wherein the mass fraction may be 99%, 99.1%, 99.2%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8%, 99.9% or 100% or the like, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the mass fraction (purity) of the hydrogen chloride (gas) is not less than 98%, wherein the mass fraction may be 98%, 98.2%, 98.4%, 98.6%, 98.9%, 99%, 99.2v, 99.4%, 99.6%, 99.8% or 100%, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the sulfur trioxide (gas) and hydrogen chloride (gas) are subjected to the chemical synthesis of step (3) to obtain chlorosulfonic acid.
In the invention, a part of hydrogen chloride gas participates in the preparation of chlorosulfonic acid, and the rest part is absorbed by water to obtain hydrochloric acid for recovery.
Preferably, the chemical synthesis reaction of step (3) is carried out in a synthesis column.
Preferably, the temperature of the chemical synthesis reaction in the step (3) is 125 to 200 ℃, wherein the reaction temperature may be 130 ℃, 135 ℃, 140 ℃, 145 ℃, 155 ℃, 156 ℃, 157 ℃, 158 ℃, 159 ℃, 160 ℃, 161 ℃, 162 ℃, 163 ℃, 164 ℃, 165 ℃, 170 ℃, 180 ℃, 190 ℃, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the process of performing chemical synthesis reaction on the sulfur trioxide and the hydrogen chloride in the step (3) to obtain chlorosulfonic acid is a continuous process, and the process can be a gas-phase process or a liquid-phase process; wherein, the gas phase process specifically comprises: carrying out chemical synthesis reaction on sulfur trioxide (gas) obtained by oxidation and HCl gas to obtain chlorosulfonic acid; the liquid phase process specifically comprises the following steps: absorbing sulfur trioxide obtained by oxidation by sulfuric acid to obtain fuming sulfuric acid; HCl is introduced into fuming sulfuric acid, chemical synthesis reaction is carried out under the condition of liquid phase, chlorosulfonic acid (dissolved in sulfuric acid) is obtained, and chlorosulfonic acid is obtained through conventional separation modes such as distillation and the like.
Preferably, the molar ratio of sulfur trioxide to hydrogen chloride in the chemical synthesis is 1: (0.8-1.2), wherein the molar ratio may be 1:0.8, 1:0.9, 1:0.95, 1:1, 1:1.05, 1:1.08, 1:1, 1:1.12, 1:1.14, 1:1.16, 1:1.18, or 1:1.2, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the chlorosulfonic acid of step (3) is recovered for use in step (1).
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) The feed mole ratio was 1: (0.8-1.5): grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride in a mixing device with an emulsion pump at the temperature of 10-45 ℃ to obtain a raw material mixed solution;
(2) Carrying out mass transfer and heat transfer reaction on the raw material mixed solution in the step (1) at the temperature of 75-150 ℃ for 5-120 min to obtain a dichloro sulfonyl imide mixed solution;
(3) Sequentially carrying out constant-temperature aging treatment on the mixed solution of the dichloro-sulfonyl-imide in the step (2) at the temperature of 75-150 ℃ for 0.1-10 h, and carrying out gas-liquid separation and nitrogen introducing treatment to obtain a dichloro-sulfonyl-imide solution and acid waste gas;
distilling the bischlorosulfimide solution at 50-150 ℃ to obtain the bischlorosulfimide;
the acidic waste gas is subjected to pressurized rectification separation at the temperature of minus 50 ℃ to minus 15 ℃ and the pressure of 0.2 to 1.5MPa, and sulfur dioxide and hydrogen chloride are respectively obtained; oxidizing the sulfur dioxide to obtain sulfur trioxide; and (3) carrying out chemical synthesis reaction on the sulfur trioxide and hydrogen chloride to obtain chlorosulfonic acid, wherein the chlorosulfonic acid is recycled in the step (1).
The second object of the invention is to provide an application of the preparation method of the dichlorinated sulfimide, which is applied to the field of lithium ion batteries.
Preferably, the preparation method of the dichloro-sulphonyl-imine is applied to synthesis of difluoro-sulphonyl-imine salts.
Compared with the prior art, the invention has the following beneficial effects:
the preparation process of the dichlorsulfimide is convenient to operate, continuous and efficient, the purity of the product can reach more than or equal to 98.5%, and the raw material utilization rate is close to 99.5% (sulfamic acid) and 99% (chlorosulfonic acid); the process is carried out by treating waste gas and waste liquid, the obtained chlorosulfonic acid can be continuously used as a starting material, the utilization rate of the material is greatly improved, the preparation cost is reduced, the influence of waste gas and waste liquid on the environment is reduced, and the whole preparation system has the characteristics of convenience, high efficiency, environmental protection and the like.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The terms "comprising," "including," "having," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
"optional" or "any" means that the subsequently described event or event may or may not occur, and that the description includes both cases where the event occurs and cases where the event does not.
The indefinite articles "a" and "an" preceding an element or component of the invention are not limited to the requirement (i.e. the number of occurrences) of the element or component. Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component includes the plural reference unless the amount clearly dictates otherwise.
The description of the terms "one embodiment," "some embodiments," "exemplarily," "specific examples," or "some examples," etc., herein described means that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this document, the schematic representations of the above terms are not necessarily for the same embodiment or example.
The technical features of the respective embodiments of the present invention may be combined with each other as long as they do not collide with each other.
In the following specific embodiments of the invention, the length of the pipeline of the dynamic tubular reactor is 1000mm, the equivalent diameter is 150mm, and the inner wall material is Hastelloy C-276 alloy.
In the following specific embodiments of the present invention, the pressure rectification process of the obtained acid waste gas is performed in a pressure rectification tower; introducing sulfur dioxide obtained by pressurized rectification and air into a reaction device, and oxidizing by adopting a three-to-two-absorption method in the presence of a catalyst (vanadium pentoxide) to fully convert the sulfur dioxide into sulfur trioxide; and absorbing the sulfur trioxide by sulfuric acid to obtain fuming sulfuric acid, and heating the fuming sulfuric acid to obtain the high-purity sulfur trioxide. The sulfur trioxide is reacted with HCl (obtained by the aforementioned pressurized distillation) to obtain chlorosulfonic acid.
Example 1
The embodiment provides a preparation method of dichloro sulfonyl imide, which comprises the following steps:
(1) The feed mole ratio was 1:1.2:2.2, grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride in a mixing kettle provided with an emulsifying pump at the temperature of 22 ℃ for 12 hours to obtain pasty liquid, namely raw material mixed liquid;
(2) Carrying out mass and heat transfer reaction at 115 ℃ and a feeding flow rate of 10L/min on the raw material mixed solution in the step (1) in a dynamic tubular reactor to obtain a dichloro sulfimide mixed solution;
(3) Sequentially performing constant-temperature aging treatment on the mixed solution of the bischlorosulfimide in the step (2) at the temperature of 120 ℃ for 7 hours, and performing gas-liquid separation and nitrogen introducing treatment to obtain a bischlorosulfimide solution and acid waste gas;
distilling the bischlorosulfonimide solution at the centrifugal speed of 2500rpm, the pressure of 100Pa and the temperature of 90 ℃ to obtain the bischlorosulfonimide;
sequentially carrying out pressurized rectification separation (the temperature of pressurized rectification is-30 ℃ and the pressure is 0.8 MPa) on the acid waste gas to respectively obtain sulfur dioxide and hydrogen chloride; mixing sulfur dioxide with air, and fully oxidizing at 345 ℃ under the catalysis of vanadium pentoxide to obtain sulfur trioxide; and (3) carrying out chemical synthesis reaction on the sulfur trioxide and hydrogen chloride at 160 ℃ to obtain chlorosulfonic acid, wherein the chlorosulfonic acid is recycled in the step (1).
Example 2
The embodiment provides a preparation method of dichloro sulfonyl imide, which comprises the following steps:
(1) The feed mole ratio was 1:1:2.5 grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride in a mixing kettle provided with an emulsifying pump at 20 ℃ for 12 hours to obtain pasty liquid, namely raw material mixed liquid;
(2) Carrying out mass and heat transfer reaction on the raw material mixed solution in the step (1) in a dynamic tubular reactor at the temperature of 100 ℃ and the feeding flow rate of 15mL/min to obtain a dichloro-sulfonyl-imide mixed solution;
(3) Sequentially carrying out heat preservation ageing treatment on the mixed solution of the dichloro sulfimide in the step (2) at 110 ℃ for 10 hours, and carrying out gas-liquid separation and nitrogen introducing treatment to obtain a dichloro sulfimide solution and acid waste gas;
distilling the bischlorosulfonimide solution at a centrifugal speed of 500rpm, a pressure of 500Pa and a temperature of 75 ℃ to obtain the bischlorosulfonimide;
sequentially carrying out pressurized rectification separation (the temperature of pressurized rectification is-30 ℃ and the pressure is 0.8 MPa) on the acid waste gas to respectively obtain sulfur dioxide and hydrogen chloride; mixing sulfur dioxide with air, and fully oxidizing at 340 ℃ under the catalysis of vanadium pentoxide to obtain sulfur trioxide; and (3) carrying out chemical synthesis reaction on the sulfur trioxide and hydrogen chloride at 150 ℃ to obtain chlorosulfonic acid, wherein the chlorosulfonic acid is recycled in the step (1).
Example 3
The embodiment provides a preparation method of dichloro sulfonyl imide, which comprises the following steps:
(1) The feed mole ratio was 1:1.5:2, grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride in a mixing kettle provided with an emulsifying pump at the temperature of 25 ℃ to obtain pasty liquid, wherein the time is 12 hours, namely raw material mixed liquid;
(2) Carrying out mass and heat transfer reaction with the temperature of 130 ℃ and the feeding flow rate of 15L/min on the raw material mixed solution in the step (1) in a dynamic tubular reactor to obtain a dichloro sulfimide mixed solution;
(3) Sequentially performing gas-liquid separation and nitrogen introducing treatment on the mixed solution of the bischlorosulfimide in the step (2) at the constant temperature of 130 ℃ for 10 hours to obtain a bischlorosulfimide solution and acid waste gas;
distilling the bischlorosulfonimide solution at a centrifugal speed of 5000rpm, a pressure of 400Pa and a temperature of 60 ℃ to obtain the bischlorosulfonimide;
sequentially carrying out pressurized rectification separation (the temperature of pressurized rectification is-30 ℃ and the pressure is 0.8 MPa) on the acid waste gas to respectively obtain sulfur dioxide and hydrogen chloride; the sulfur dioxide is mixed with air and fully oxidized at 350 ℃ under the catalysis of vanadium pentoxide to obtain sulfur trioxide; and (3) carrying out chemical synthesis reaction on the sulfur trioxide and hydrogen chloride at 165 ℃ to obtain chlorosulfonic acid, wherein the chlorosulfonic acid is recycled in the step (1).
Example 4
This example was the same as example 1 except that the time for the polish blending in step (1) was set to 2 hours.
Example 5
This example is identical to example 1 except that the temperature of the mass and heat transfer reaction in step (2) is replaced with 90 ℃.
Example 6
This example is identical to example 1 except that the temperature of the mass and heat transfer reaction described in step (2) is replaced with 140 ℃.
Example 7
In this example, the conditions were the same as in example 1 except that the feed rate of the raw material mixture for the mass and heat transfer reaction in step (2) was replaced with 2L/min.
Example 8
In this example, the conditions were the same as in example 1 except that the feed rate of the raw material mixture for the mass and heat transfer reaction in step (2) was replaced with 18L/min.
Comparative example 1
The comparative example was conducted under the same conditions as in example 1 except that the acid off-gas in step (3) was not treated.
The raw material utilization and purity were calculated for the bischlorosulfonimide of examples 1 to 8 and comparative example 1, and the calculated structures are shown in Table 1.
The method for calculating the utilization rate of the raw materials comprises the following steps: (1) Sulfamic acid utilization, dividing the mole number of the obtained product by the mole number of sulfamic acid added; (2) The chlorosulfonic acid utilization rate is divided by the mole number of the obtained product by the mole number of the input chlorosulfonic acid; (3) The utilization rate of thionyl chloride is divided by the mole number of the obtained product divided by the mole number of the thionyl chloride added.
TABLE 1
As can be seen from the above table, in example 4, compared with example 1, the grinding and blending time of the raw materials is shorter, resulting in that the particle size of sulfamic acid in the raw material mixed solution is larger than 100 μm, the contact degree and the reaction degree of materials in the mass and heat transfer reaction are affected, the mass and heat transfer efficiency is reduced, the utilization rate of sulfamic acid is reduced, and the purity of the bischlorosulfimide is reduced. The excessive or low temperature during the mass and heat transfer in examples 5-6 has the problem of excessive byproduct generation during the preparation process, thereby resulting in reduced purity and raw material utilization of the bischlorosulfimide. In the mass transfer and heat transfer reactions in examples 7 to 8, when the feed rate of the raw material mixed solution is too high or too low, the reaction time of mass transfer and heat transfer is too long, resulting in the production of byproducts in the preparation overcharge, and thus, the purity of the bischlorosulfonimide and the utilization rate of the raw material are lowered. The acid waste gas generated in the preparation process of the dichlorsulfonyl imide is not treated in the comparative example 1, the obtained acid waste gas cannot be recycled in the system again, resources are wasted, the environment is not protected, and meanwhile, the dichlorsulfonyl imide is not utilized in the comparative example 1, so that the utilization rate of raw materials is reduced.
The applicant states that the invention is illustrated by the above embodiments, but the invention is not limited to the above embodiments, i.e. it does not mean that the invention has to be carried out in dependence of the above embodiments. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (10)
1. A method for preparing bischlorosulfonimide, which is characterized by comprising the following steps:
(1) Grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride to obtain a raw material mixed solution;
(2) Carrying out mass transfer and heat transfer reaction on the raw material mixed solution in the step (1) to obtain a dichloro sulfonyl imide mixed solution;
(3) Sequentially carrying out gas-liquid separation and nitrogen introduction treatment on the mixed solution of the dichloro sulfimide in the step (2) to obtain a dichloro sulfimide solution and acid waste gas;
distilling the bischlorosulfonimide solution to obtain the bischlorosulfonimide;
and sequentially carrying out pressurization rectification separation, oxidation and chemical synthesis reaction on the acid waste gas to obtain chlorosulfonic acid.
2. The process according to claim 1, wherein the feed molar ratio of chlorosulfonic acid, sulfamic acid and thionyl chloride in step (1) is 1: (0.8-1.5): (2-8);
preferably, the grinding and blending of step (1) is performed in a mixing device provided with an emulsion pump;
preferably, the time of the grinding and blending in the step (1) is 1 to 15 hours, more preferably 5 to 12 hours;
preferably, the milling and blending atmosphere of step (1) is a nitrogen atmosphere;
preferably, the temperature of the grinding and blending in the step (1) is 10-45 ℃;
preferably, the particle size of sulfamic acid after the grinding blending in step (1) is <100 μm.
3. The process according to claim 1 or 2, wherein the mass and heat transfer reaction of step (2) is carried out in a dynamic tubular reactor;
preferably, the length of the dynamic tubular reactor is 500-10000 mm;
preferably, the equivalent diameter of the dynamic tubular reactor is 50-800 mm;
preferably, the inner wall material of the dynamic tube reactor comprises any one of silicon carbide, 316L stainless steel, hastelloy C-276 alloy or Monel alloy.
4. A production method according to any one of claims 1 to 3, wherein the feed flow rate of the raw material mixture in step (2) is 0.1 to 50L/min;
preferably, the temperature of the mass and heat transfer reaction in the step (2) is 75-150 ℃;
preferably, the time of the mass and heat transfer reaction in the step (2) is 5-120 min.
5. The process according to any one of claims 1 to 4, wherein the gas-liquid separation in step (3) is performed in a gas-liquid separator;
preferably, the constant temperature ageing treatment is carried out in the gas-liquid separation in the step (3);
preferably, the temperature of the constant temperature ageing treatment is 75-150 ℃;
preferably, the constant temperature ageing treatment is carried out for 0.1-10 hours;
preferably, the nitrogen gas in the nitrogen-passing treatment has a water content of <50ppm.
6. The process according to any one of claims 1 to 5, wherein the pressure of the distillation in step (3) is 100Pa to 10kPa;
preferably, the temperature of the distillation in step (3) is 50 to 150 ℃.
7. The process according to any one of claims 1 to 6, wherein the acid waste gas of step (3) comprises sulfur dioxide and hydrogen chloride;
preferably, sulfur dioxide and hydrogen chloride are respectively obtained after the pressurized rectification separation in the step (3);
preferably, the temperature of the pressurized rectification in the step (3) is-50 ℃ to-10 ℃;
preferably, the pressure of the pressurized rectification in the step (3) is 0.2-1.5 MPa;
preferably, the diameter of the rectifying tower of the pressure rectification in the step (3) is 200 mm-1000 mm;
preferably, the height of the rectifying tower of the pressure rectification in the step (3) is 3000 mm-20000 mm.
8. The method of claim 7, wherein the oxidizing of the sulfur dioxide in step (3) is performed to obtain sulfur trioxide;
preferably, the oxidising agent comprises oxygen;
preferably, the oxidation is carried out in the presence of a catalyst comprising vanadium pentoxide;
preferably, the temperature of the oxidation is 250-500 ℃;
preferably, the sulfur trioxide and the hydrogen chloride undergo the chemical synthesis reaction of the step (3) to obtain chlorosulfonic acid;
preferably, the chemical synthesis reaction of step (3) is carried out in a synthesis column;
preferably, the temperature of the chemical synthesis reaction in the step (3) is 125-200 ℃;
preferably, the molar ratio of sulfur trioxide to hydrogen chloride in the chemical synthesis is 1: (0.8-1.2);
preferably, the chlorosulfonic acid of step (3) is recovered for use in step (1).
9. The preparation method according to any one of claims 1 to 8, characterized in that the preparation method comprises the steps of:
(1) The feed mole ratio was 1: (0.8-1.5): grinding and blending chlorosulfonic acid, sulfamic acid and thionyl chloride in a mixing device with an emulsion pump at the temperature of 10-45 ℃ to obtain a raw material mixed solution;
(2) Carrying out mass transfer and heat transfer reaction on the raw material mixed solution in the step (1) at the temperature of 75-150 ℃ for 5-120 min to obtain a dichloro sulfonyl imide mixed solution;
(3) Sequentially carrying out constant-temperature aging treatment on the mixed solution of the dichloro-sulfonyl-imide in the step (2) at the temperature of 75-150 ℃ for 0.1-10 h, and carrying out gas-liquid separation and nitrogen introducing treatment to obtain a dichloro-sulfonyl-imide solution and acid waste gas;
distilling the bischlorosulfimide solution at 50-150 ℃ to obtain the bischlorosulfimide;
the acidic waste gas is subjected to pressurized rectification separation at the temperature of minus 50 ℃ to minus 15 ℃ and the pressure of 0.2 to 1.5MPa, and sulfur dioxide and hydrogen chloride are respectively obtained; oxidizing the sulfur dioxide to obtain sulfur trioxide; and (3) carrying out chemical synthesis reaction on the sulfur trioxide and hydrogen chloride to obtain chlorosulfonic acid, wherein the chlorosulfonic acid is recycled in the step (1).
10. Use of the method for the preparation of bischlorosulfonimide according to any of claims 1 to 9, characterized in that the method for the preparation is applied in the field of lithium ion batteries;
preferably, the preparation method of the dichloro-sulphonyl-imine is applied to synthesis of difluoro-sulphonyl-imine salts.
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| WO2020109720A1 (en) * | 2018-11-28 | 2020-06-04 | Arkema France | Process for producing lithium bis(fluorosulfonyl)imide salt |
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