CN115784178B - Preparation method of difluoro sulfimide - Google Patents
Preparation method of difluoro sulfimide Download PDFInfo
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- CN115784178B CN115784178B CN202211652016.1A CN202211652016A CN115784178B CN 115784178 B CN115784178 B CN 115784178B CN 202211652016 A CN202211652016 A CN 202211652016A CN 115784178 B CN115784178 B CN 115784178B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XPVRBHCXMWRJEY-UHFFFAOYSA-N difluoro(imino)-$l^{4}-sulfane Chemical compound FS(F)=N XPVRBHCXMWRJEY-UHFFFAOYSA-N 0.000 title claims description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 52
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical group FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008240 homogeneous mixture Substances 0.000 claims abstract description 8
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical group ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 20
- 150000003949 imides Chemical class 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000012263 liquid product Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- ATMIHASMQFJNLZ-UHFFFAOYSA-N dichloro(imino)-$l^{4}-sulfane Chemical compound ClS(Cl)=N ATMIHASMQFJNLZ-UHFFFAOYSA-N 0.000 abstract description 13
- -1 fluorosulfonyl imide Chemical class 0.000 description 16
- 238000000034 method Methods 0.000 description 14
- 239000012295 chemical reaction liquid Substances 0.000 description 13
- 230000002572 peristaltic effect Effects 0.000 description 13
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 238000004821 distillation Methods 0.000 description 7
- 238000005086 pumping Methods 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- IXPAAHZTOUOJJM-UHFFFAOYSA-N sulfuryl chloride fluoride Chemical group FS(Cl)(=O)=O IXPAAHZTOUOJJM-UHFFFAOYSA-N 0.000 description 4
- 125000003963 dichloro group Chemical group Cl* 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical group 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- FVELMKWTTMVGME-UHFFFAOYSA-N ClS(=O)(O)Cl Chemical compound ClS(=O)(O)Cl FVELMKWTTMVGME-UHFFFAOYSA-N 0.000 description 1
- 229910006095 SO2F Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- PQIOSYKVBBWRRI-UHFFFAOYSA-N methylphosphonyl difluoride Chemical group CP(F)(F)=O PQIOSYKVBBWRRI-UHFFFAOYSA-N 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- PVMUVDSEICYOMA-UHFFFAOYSA-N n-chlorosulfonylsulfamoyl chloride Chemical compound ClS(=O)(=O)NS(Cl)(=O)=O PVMUVDSEICYOMA-UHFFFAOYSA-N 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 229910021483 silicon-carbon alloy Inorganic materials 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- BFXAWOHHDUIALU-UHFFFAOYSA-M sodium;hydron;difluoride Chemical compound F.[F-].[Na+] BFXAWOHHDUIALU-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005292 vacuum distillation 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 belongs to the field of preparation of difluoro-sulfonyl imide, and particularly relates to a preparation method of difluoro-sulfonyl imide. The preparation method comprises the following steps: mixing anhydrous hydrofluoric acid, difluoro-sulfonyl imide and dichloro-sulfonyl imide to obtain a homogeneous mixture; the homogeneous mixture is reacted in a reactor to produce the difluoro-sulfonyl imide. The anhydrous hydrofluoric acid and the dichlorsulfimide are not mutually soluble, and the hydrofluoric acid and the dichlorsulfimide can be in a homogeneous state after the dichlorsulfimide is added, so that the hydrofluoric acid and the dichlorsulfimide are better contacted, and the reaction efficiency is improved.
Description
Technical Field
The invention belongs to the field of preparation of difluoro-sulfonyl imide, and particularly relates to a preparation method of difluoro-sulfonyl imide.
Background
LIFSI (lithium bis (fluorosulfonyl imide)) has a large anion structure, so that the acting force of anions and lithium ions is weak, and lithium ions are easy to be released from molecules in an organic solvent, and high freeness is presented. LIFSI has good conductivity, can be used for electrolyte of lithium secondary battery, and has very important application prospect and value. HFSI (bis-fluorosulfonyl imide) is one of the important intermediate raw materials for the production of LIFSI.
In the prior art, HFSI is prepared by exchanging fluorine and chlorine with fluorine-containing raw materials such as dichlorosulfinic acid and a fluorinating agent, for example hydrofluoric acid, metal fluoride and the like under the action of a catalyst to generate the difluoro sulfimide. The process is complex, the yield is low, and the equipment corrosion is serious.
The microchannel continuous flow reactor has the advantages of high chemical reaction efficiency, small laboratory trial and production amplification gap and the like, and the reactor is designed into corrosion-resistant, high-temperature-resistant and high-pressure-resistant materials, such as silicon-carbon alloy and the like, and the materials are fluorine-resistant, corrosion-resistant, high-temperature-resistant and high-pressure-resistant, and high in safety, and are particularly suitable for fluorine-containing and high-temperature reactions.
The Chinese patent application with the application publication number of CN113880057A discloses a clean production process of difluoro sulfimide, which uses an intermittent reaction kettle as a pre-reaction device, a micro-channel reactor as a main reaction device, wherein the micro-channel reactor comprises a first temperature zone and a second temperature zone which are connected in series, and the two temperature zones comprise a plurality of reaction modules connected in series; firstly adding sulfamic acid, sulfur trioxide and thionyl chloride into an intermittent reaction kettle for reaction to obtain a pre-reaction liquid, then pumping the pre-reaction liquid into a first temperature zone for reaction to obtain a dichloro reaction liquid, simultaneously pumping the dichloro reaction liquid and hydrogen fluoride liquid into a second temperature zone for reaction to obtain a difluoro reaction liquid, and carrying out reduced pressure rectification to obtain a high-purity difluoro sulfimide product. The method is based on a microchannel reactor, and the high-purity bis-fluorosulfonyl imide product is obtained through high-efficiency fluorogenic reaction of hydrogen fluoride and rectification purification from the synthesis of the bis-chlorosulfonyl imide.
In the method, the first temperature zone is subjected to microchannel reaction to obtain the dichloro-sulfonyl-imide (dichloro reaction feed liquid), and the second temperature zone is subjected to reaction between the dichloro-sulfonyl-imide and hydrogen fluoride to generate HFSI, wherein the temperature reaches about 90-120 ℃, and the hydrogen fluoride is in a gas state, so that the prior art describes that: the micro-channel reactor can obviously improve the gas-liquid two-phase mass transfer efficiency, not only reduces the use amount of hydrogen fluoride, but also greatly shortens the fluorination reaction time. The indexes of the method such as reaction yield, raw material utilization rate and the like are still to be further improved so as to be better suitable for industrial large-scale production.
Disclosure of Invention
The invention aims to provide a preparation method of difluoro sulfimide, which solves the problems of low reaction efficiency of hydrofluoric acid and dichloro sulfimide and low utilization rate of raw materials in the prior art.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing bis-fluorosulfonyl imide, comprising the following steps: mixing anhydrous hydrofluoric acid, difluoro-sulfonyl imide and dichloro-sulfonyl imide to obtain a homogeneous mixture; the homogeneous mixture is reacted in a reactor to produce the difluoro-sulfonyl imide.
The anhydrous hydrofluoric acid and the dichlorsulfimide are not mutually soluble, and the hydrofluoric acid and the dichlorsulfimide can be in a homogeneous state after the dichlorsulfimide is added, so that the hydrofluoric acid and the dichlorsulfimide are better contacted, and the reaction efficiency is improved. Compared with the gas-liquid two-phase reaction, the homogeneous phase reaction can further improve the reaction efficiency, has good stability and controllability in the reaction process, and is more suitable for industrialized amplified production.
On the premise of ensuring the solubility of anhydrous hydrofluoric acid and considering the reaction efficiency, the molar ratio of the anhydrous hydrofluoric acid to the bisfluorosulfonyl imide is preferably (1-2): (0.5-1).
Preferably, the molar ratio of hydrofluoric acid to dichlorosulfimide is (1-2): 1. by adopting the reaction strategy, the raw materials can be controlled in the proportion to obtain good effects, and the method is excellent in the aspects of improving the reaction yield, the product purity, simplifying post-treatment and the like.
In order to ensure efficient progress of the HFSI formation reaction, it is preferred that the reaction temperature be in the range of 70 to 150 ℃. In order to further increase the economy of the reaction and to avoid corrosion of the equipment that may be caused by high temperatures, it is preferred that the temperature of the reaction is between 75 and 100 ℃.
Preferably, the reactor is a microchannel reactor. The homogeneous phase mixture formed by the three materials is subjected to homogeneous reaction in the microchannel reactor, so that the reaction efficiency is high, the use mode that hydrogen fluoride is excessively introduced in the prior art and the excessive hydrogen fluoride is recycled in the later stage can be changed, the utilization rate of raw material hydrogen fluoride is improved, and the post-treatment difficulty is reduced.
In order to further simplify the separation and purification operation of the product and ensure the yield and purity of the product, preferably, the liquid product obtained by the reaction is distilled and separated to obtain the difluoro sulfimide.
Detailed Description
The invention provides a method for preparing difluoro sulfimide by adopting a microchannel continuous flow reactor, which has high reaction efficiency, simple operation and no corrosion to equipment, and concretely comprises the following steps:
1) Mixing dichlorsulfimide, difluosulfimide and anhydrous hydrofluoric acid according to a certain proportion to obtain a homogeneous mixture;
2) The homogeneous mixture is added to a reactor and reacted at elevated temperature to form the bis-fluorosulfonyl imide.
The reaction equation is as follows:
HN(SO2Cl)2+2HF→HN(SO2F)2+2HCl
For the case where the reactor is a microchannel reactor, the specific operating steps are as follows:
1) Anhydrous hydrofluoric acid, difluoro sulfonyl imide and dichloro sulfonyl imide are mixed evenly according to the proportion of (1-2) to (0.5-1) to 1, and a homogeneous phase mixture is obtained.
2) The temperature of the microchannel continuous reaction flow reaction module is adjusted to 70-150 ℃.
3) Pumping the mixture into the microchannel reaction stream by a peristaltic pump connected with the microchannel continuous reaction stream at a pump speed of 3-20 mL/min; the peristaltic pump outlet pipe uses the refrigerating bath to cool down, in order to cool down the reaction product, facilitate collecting. The reaction is carried out in a microchannel reactor for 7-20min, thus achieving good reaction effect.
4) Collecting reaction products, wherein the gas products are a mixture of hydrogen fluoride and hydrogen chloride, absorbing the hydrogen fluoride in the mixture by using sodium fluoride particles to generate sodium bifluoride, and absorbing the residual hydrogen chloride gas by using alkali liquor. And (3) distilling the liquid product under reduced pressure to obtain the difluoro sulfimide product. The reduced pressure distillation temperature may be set to 90 to 100℃and the vacuum degree may be set to-0.09 MPa or more.
The following describes the practice of the invention in detail with reference to specific examples.
1. Specific examples of the preparation method of the bisfluorosulfonyl imide of the present invention are as follows:
example 1
The preparation method of the difluoro sulfonyl imide comprises the following steps:
1) Cleaning the micro-channel reaction pipeline, and connecting the constant-temperature bath with the micro-channel continuous flow reactor and each pipeline; the oil bath was opened and the temperature was raised to 100℃until the temperature of the 6 microchannel continuous reaction streams was raised to 100 ℃.
2) Anhydrous hydrofluoric acid, difluoro sulfonyl imide and dichloro sulfonyl imide are added into a mixer in sequence according to the mol ratio of 1.5:1:1, and are uniformly mixed.
3) Firstly, opening a peristaltic pump, and adjusting the pump speed of the peristaltic pump to 10mL/min; and (3) pumping mixed liquid into the micro-channel, wherein the total reaction time is 7min, and collecting the reaction liquid, wherein the reaction liquid is the primary product.
4) Distilling the primary product at 100 ℃ and vacuum degree of-0.09 MPa to obtain light component which is monofluoro-monochloro-sulfonyl imide which is not fluorinated completely, and obtaining the residual heavy component which is difluoro-sulfonyl imide.
Example 2
The preparation method of the difluoro sulfonyl imide comprises the following steps:
1) Cleaning the micro-channel reaction pipeline, and connecting the constant-temperature bath with the micro-channel continuous flow reactor and each pipeline; and opening an oil bath, heating to 80 ℃, closing the first two micro-channel reaction blocks, and heating the rest 4 micro-channel continuous reaction streams to 80+/-5 ℃.
2) Anhydrous hydrofluoric acid, difluoro sulfonyl imide and dichloro sulfonyl imide are added into a mixer in sequence according to the mol ratio of 1.2:0.5:1, and are uniformly mixed.
3) Firstly, opening a peristaltic pump, and adjusting the pump speed of the peristaltic pump to 3mL/min; and (3) pumping mixed liquid into the micro-channel, wherein the total reaction time is 20min, and collecting the reaction liquid, wherein the reaction liquid is the primary product.
4) Distilling the primary product at 100 ℃ and vacuum degree of-0.09 MPa to obtain light component which is monofluoro-monochloro-sulfonyl imide which is not fluorinated completely, and obtaining the residual heavy component which is difluoro-sulfonyl imide.
Example 3
The preparation method of the difluoro sulfonyl imide comprises the following steps:
1) Cleaning the micro-channel reaction pipeline, and connecting the constant-temperature bath with the micro-channel continuous flow reactor and each pipeline; the oil bath was opened and the temperature was raised to 80℃until the temperature of the 6 microchannel continuous reaction streams was raised to 80 ℃.
2) Anhydrous hydrofluoric acid, difluoro sulfonyl imide and dichloro sulfonyl imide are added into a mixer in sequence according to the mol ratio of 2:1:1, and are uniformly mixed.
3) Firstly, opening the peristaltic pump, and adjusting the pump speed of the peristaltic pump to 5mL/min; and (3) pumping mixed liquid into the micro-channel, wherein the total reaction time is 13min, and collecting the reaction liquid, wherein the reaction liquid is the primary product.
4) Distilling the primary product at 100 ℃ and vacuum degree of-0.09 MPa to obtain light component which is monofluoro-monochloro-sulfonyl imide which is not fluorinated completely, and obtaining the residual heavy component which is difluoro-sulfonyl imide.
Example 4
The preparation method of the difluoro sulfonyl imide comprises the following steps:
1) Cleaning the micro-channel reaction pipeline, and connecting the constant-temperature bath with the micro-channel continuous flow reactor and each pipeline; the oil bath was opened and the temperature was raised to 75℃and the temperature of the microchannel continuous reaction stream was maintained at 75.+ -. 5 ℃.
2) Anhydrous hydrofluoric acid, difluoro sulfonyl imide and dichloro sulfonyl imide are added into a mixer in sequence according to the mol ratio of 1.2:0.8:1, and are uniformly mixed.
3) Firstly, opening a peristaltic pump, and adjusting the pump speed of the peristaltic pump to 3mL/min; and (3) pumping mixed liquid into the micro-channel, wherein the total reaction time is 20min, and collecting the reaction liquid, wherein the reaction liquid is the primary product.
4) Distilling the primary product at 100 ℃ and vacuum degree of-0.09 MPa to obtain light component which is monofluoro-monochloro-sulfonyl imide which is not fluorinated completely, and obtaining the residual heavy component which is difluoro-sulfonyl imide.
Based on the above reaction principle, the reaction raw materials of the above embodiments are adopted to react in a conventional reactor, and corresponding improvement effects can be obtained.
2. Comparative example
Comparative example 1
The process for the preparation of the bis-fluorosulfonyl imide of the present comparative example differs from that of example 1 in that in step 2), bis-fluorosulfonyl imide is not added and two peristaltic pumps are used for feeding separately.
Comparative example 2
The process for the preparation of the bis-fluorosulfonyl imide of the present comparative example differs from that of example 2 in that in step 2), bis-fluorosulfonyl imide is not added and two peristaltic pumps are used for feeding separately.
Comparative example 3
The process for the preparation of the bis-fluorosulfonyl imide of the present comparative example differs from that of example 1 in that in step 2) the solvent acetonitrile is used instead of bis-fluorosulfonyl imide. In step 4), the separation of the product is completed by two-step distillation, wherein the first-step distillation is carried out at the temperature of 100 ℃ and the vacuum degree of-0.09 MPa, and the heavy component is bis-fluorosulfonyl imide, so that the time is longer because more distillate needs to be distilled off; the second step is to distill the object to be the first step and distill the fraction, this fraction needs to separate acetonitrile and monofluoro monochlorosulfimide and unreacted dichloro sulfimide, adopt the following gradient distillation scheme, distill at 85 deg.C normal pressure first, distill light component acetonitrile, then carry on the vacuum distillation of 90 deg.C, the fraction is the monofluoro monochlorosulfimide not fluorinated completely, the kettle is the dichloro sulfimide.
3. Experimental example
The index of purity, yield, chlorine content and the like of the bisfluorosulfonyl imide product obtained in each example were tested in this experimental example, and the results are shown in table 1. The yield was calculated from the mass ratio of the difluorosulfimide to be produced and the actual difluorosulfimide to be produced according to the theory of the input of perchloric acid.
TABLE 1 Performance index of bis-fluorosulfonyl imide products
| Example numbering | Yield% | Purity of% | Chlorine content, ppm |
| Example 1 | 98.2％ | 98.9％ | 199 |
| Example 2 | 98.0％ | 99.0％ | 151 |
| Example 3 | 98.0％ | 99.2％ | 139 |
| Example 4 | 97.2％ | 98.7％ | 143 |
| Comparative example 1 | 16.6％ | 44.5％ | 15349 |
| Comparative example 2 | 22.5％ | 48.2％ | 7988 |
| Comparative example 3 | 92.7％ | 95.5％ | 642 |
As is clear from the results in Table 1, comparative examples 1 and 2 were fed separately by two peristaltic pumps without HFSI, the reaction yield was less than 25%, the distillation time was long, and the purity after distillation was less than 50%. The method provided by the embodiment of the invention has the characteristics of homogeneous reaction, and the two reaction raw materials are better in contact and more sufficient in reaction, so that the method is high in yield, better in distillation effect and capable of conveniently obtaining higher purity. Meanwhile, the chlorine content is as low as 200ppm or less, and the HFSI has excellent overall quality. Comparative example 3 the method using acetonitrile solvent decreased yield and product purity, increased chlorine content, and increased post-treatment difficulty.
In a comprehensive view, the method provided by the invention has the characteristics of high raw material utilization rate, low post-treatment difficulty, high reaction efficiency and the like, and is very suitable for industrial production.
Claims (5)
1. The preparation method of the difluoro sulfimide is characterized by comprising the following steps of: mixing anhydrous hydrofluoric acid, difluoro-sulfonyl imide and dichloro-sulfonyl imide to obtain a homogeneous mixture; reacting the homogeneous mixture in a reactor to obtain difluoro-sulfonyl imide; the molar ratio of anhydrous hydrofluoric acid to bisfluorosulfonyl imide to bischlorosulfonyl imide is (1-2) (0.5-1) 1.
2. The method for producing a bisfluorosulfonyl imide according to claim 1, wherein the reaction temperature is 70 to 150 ℃.
3. The method for producing a bisfluorosulfonyl imide according to claim 1, wherein said reactor is a microchannel reactor.
4. The method for producing a bisfluorosulfonyl imide according to claim 2, wherein the reaction temperature is 75 to 100 ℃.
5. The method for producing a bisfluorosulfonyl imide according to claim 1, wherein the reaction products obtained by the reaction are a gaseous product and a liquid product, and the liquid product obtained by the reaction is distilled and separated to obtain a bisfluorosulfonyl imide.
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| Title |
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| 张学铭.化学小辞典.科学技术文献出版社,1984,第124页. * |
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