CN114835671A - Production process of high-purity fluoroethylene carbonate - Google Patents
Production process of high-purity fluoroethylene carbonate Download PDFInfo
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- CN114835671A CN114835671A CN202210624243.7A CN202210624243A CN114835671A CN 114835671 A CN114835671 A CN 114835671A CN 202210624243 A CN202210624243 A CN 202210624243A CN 114835671 A CN114835671 A CN 114835671A
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- fluoroethylene carbonate
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- carbonate
- fluoride
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- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 60
- 239000002253 acid Substances 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004821 distillation Methods 0.000 claims abstract description 21
- OYOKPDLAMOMTEE-UHFFFAOYSA-N 4-chloro-1,3-dioxolan-2-one Chemical compound ClC1COC(=O)O1 OYOKPDLAMOMTEE-UHFFFAOYSA-N 0.000 claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 17
- 239000002516 radical scavenger Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 9
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000002912 waste gas Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 3
- 239000002910 solid waste Substances 0.000 abstract description 2
- PQLFROTZSIMBKR-UHFFFAOYSA-N ethenyl carbonochloridate Chemical compound ClC(=O)OC=C PQLFROTZSIMBKR-UHFFFAOYSA-N 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 4
- GRLXVBPHGMHJQW-UHFFFAOYSA-N ethenyl carbonofluoridate Chemical compound FC(=O)OC=C GRLXVBPHGMHJQW-UHFFFAOYSA-N 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000011775 sodium fluoride Substances 0.000 description 2
- 235000013024 sodium fluoride Nutrition 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003444 phase transfer catalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/42—Halogen atoms or nitro radicals
-
- 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
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The application provides a production process of high-purity fluoroethylene carbonate, belonging to the technical field of fluoroethylene carbonate production. The production process of the high-purity fluoroethylene carbonate comprises the following steps: adding fluoride and a catalyst to a reaction vessel; then adding chloroethylene carbonate, reacting the reactants in a reaction container, and controlling the reaction temperature to be 50-120 ℃ under the protection of nitrogen to finally obtain a mixture containing fluoroethylene carbonate; adding an acid scavenger which is insoluble in fluoroethylene carbonate and can react with free acid in fluoroethylene carbonate to generate precipitate or volatile matter into fluoroethylene carbonate, so as to obtain fluoroethylene carbonate with certain purity; and then carrying out distillation purification to obtain the required high-purity fluoroethylene carbonate. The fluoroethylene carbonate can be effectively dehydrated and purified, the product yield is over 95 percent, and no solid waste is generated.
Description
Technical Field
The application relates to the field of fluoroethylene carbonate production, in particular to a production process of high-purity fluoroethylene carbonate.
Background
The fluoroethylene carbonate is mainly applied to the lithium ion electrolyte of the lithium battery, the fluoroethylene carbonate can effectively improve the high and low temperature resistance of the lithium ion electrolyte and improve the flame resistance of the lithium ion electrolyte, if the fluoroethylene carbonate is used as an electrolyte solvent, the charging and discharging cycle characteristics and the current efficiency of chemical devices such as a secondary battery, a capacitor and the like can be improved,
at present, when fluoroethylene carbonate is produced, a mixed gas of fluorine gas and nitrogen gas is adopted to react with ethylene carbonate, so that the method is a common method for preparing fluoroethylene carbonate, however, because the raw material used in the method is fluorine gas, and the fluorine gas has the characteristics of high toxicity and high reaction activity, the reaction result is not easy to control, phenomena of severe heating and high pressure in a reaction container occur, and the potential safety hazard during the production of fluoroethylene carbonate is increased.
Disclosure of Invention
In order to make up for the defects, the application provides a production process of high-purity fluoroethylene carbonate, aiming at solving the problems that the reaction result is not easy to control, the potential safety hazard in the production of fluoroethylene carbonate is increased, the purity of the prepared fluoroethylene carbonate is low, the production quality of fluoroethylene carbonate is reduced, and the use requirement of high-quality batteries cannot be met.
The embodiment of the application provides a production process of high-purity fluoroethylene carbonate, which comprises the following steps:
adding fluoride and a catalyst to a reaction vessel;
then adding chloroethylene carbonate, reacting the reactants in a reaction container, and controlling the reaction temperature to be 50-120 ℃ under the protection of nitrogen to finally obtain a mixture containing fluoroethylene carbonate;
adding an acid scavenger which is insoluble in fluoroethylene carbonate and can react with free acid in fluoroethylene carbonate to generate precipitate or volatile matter into fluoroethylene carbonate, so as to obtain fluoroethylene carbonate with certain purity;
and then carrying out distillation purification to obtain the required high-purity fluoroethylene carbonate.
In the implementation process, the mol ratio of the chloroethylene carbonate to the fluoride is as follows: 1.0: 1.0-1.0: 1.2, wherein the mass of the catalyst is 0.01-0.5 times of the total mass of the chloroethylene carbonate and the fluoride.
In the implementation process, the temperature of the reaction container is controlled to be between 10 and 200 ℃ in the process of dropwise adding the chlorinated ethylene carbonate, and the temperature is controlled to be between 90 and 110 ℃ after the dropwise adding is finished.
In the implementation process, the acid scavenger is at least one of oxides of magnesium, calcium, silicon and aluminum, and the addition amount of the acid scavenger is 0.01-10% of the weight of the fluoroethylene carbonate.
In the implementation process, the reaction temperature of the acid scavenger is 20-35 ℃, and the reaction time is 0.5-5 hours.
In the implementation process, the fluoride is introduced into the reaction container at a speed of 0.1-0.3L/min, and the nitrogen is introduced into the reaction container at a speed of 0.5-1.5L/min.
In the implementation process, the reaction container is provided with alkaline liquid so as to absorb waste gas generated in the reaction process.
In the above implementation, the exhaust gas includes hydrogen chloride gas and hydrogen fluoride gas.
In the implementation process, the distillation purification process comprises the following steps: carrying out reduced pressure distillation under the pressure of 10mmHg, and collecting 90-110 ℃ fractions, namely fluoroethylene carbonate.
In the implementation process, the reaction temperature of the distillation purification is 60-90 ℃, and the reaction time of the distillation purification is 4-24 hours.
Compared with the prior art, the invention has the beneficial effects that: by using the catalyst and under the protection of nitrogen, the reaction condition is mild, the content of free acid in the fluoroethylene carbonate can be effectively reduced, the fluoroethylene carbonate can be effectively dehydrated and purified, the product yield is over 95 percent, no solid waste is generated, the produced waste gas, namely hydrogen fluoride and hydrogen chloride gas, is absorbed by alkali liquor, and no environmental pollution is caused basically.
Detailed Description
The technical solutions in the embodiments of the present application will be described below with reference to the embodiments of the present application.
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments obtained by a person of ordinary skill in the art without any inventive work based on the embodiments in the present application are within the scope of protection of the present application.
Example 1
The application provides a production process of high-purity fluoroethylene carbonate, which comprises the following steps:
adding fluoride and a catalyst to a reaction vessel;
then adding chloroethylene carbonate, reacting the reactants in a reaction container, and controlling the reaction temperature to be 50-120 ℃ under the protection of nitrogen to finally obtain a mixture containing fluoroethylene carbonate;
adding an acid scavenger which is insoluble in fluoroethylene carbonate and can react with free acid in fluoroethylene carbonate to generate precipitate or volatile matter into fluoroethylene carbonate, so as to obtain fluoroethylene carbonate with certain purity;
and then carrying out distillation purification to obtain the required high-purity fluoroethylene carbonate.
In a particular embodiment, the molar ratio of vinyl chlorocarbonate to fluoride is: 1.0: 1.0-1.0: 1.2, and the mass of the added catalyst is 0.01-0.5 times of the total mass of the chloroethylene carbonate and the fluoride.
In a specific embodiment, the temperature of the reaction vessel is controlled between 10 ℃ and 200 ℃ during the dropping of the chloroethylene carbonate, and the temperature is controlled between 90 ℃ and 110 ℃ after the dropping is finished.
More specifically, 44g of sodium fluoride is added into a reaction container and stirred, 3.4g of polyethylene glycol phase transfer catalyst is added, 122.5g of chloroethylene carbonate is dripped, the dripping temperature is controlled to be 50-70 ℃, the color of the mixture turns into dark brown along with the dripping, the mixture automatically releases heat and heats up, after the dripping is finished, the mixture is very viscous, after the mixture is kept at 100 ℃ for 3 hours, the mixture is cooled to 30 ℃, then centrifugal suction filtration is used, black filtrate is obtained, wherein 0.5% of unreacted chloroethylene carbonate, 92% of fluoroethylene carbonate and other impurities brought by raw materials are contained, the black filtrate is subjected to reduced pressure rectification, and finally 59g of a product with the purity of 99.9% is obtained, and the reaction can be rapidly and completely carried out by using the catalyst.
In a specific embodiment, the acid scavenger is at least one of oxides of magnesium, calcium, silicon and aluminum, and is added in an amount of 0.01-10% by weight of fluoroethylene carbonate.
In a specific embodiment, the reaction temperature of the acid scavenger is 20-35 ℃ and the reaction time is 0.5-5 hours.
More specifically, fluoroethylene carbonate having a purity of 99.5%, water content of 100ppm and free acid of 120ppm was prepared by adding 3% magnesium oxide to 100g of fluoroethylene carbonate and subjecting the mixture to a deacidification treatment at 20 ℃ for 2 hours to give 21ppm free acid.
In a specific embodiment, the fluoride is introduced into the reaction vessel at a rate of 0.1 to 0.3L/min, and the nitrogen is introduced into the reaction vessel at a rate of 0.5 to 1.5L/min.
In a particular embodiment, the reaction vessel is provided with an alkaline liquid to absorb the off-gases generated during the reaction.
In a particular embodiment, the off-gas comprises hydrogen chloride gas and hydrogen fluoride gas.
More specifically, hydrogen fluoride gas was continuously fed into the reaction vessel at a rate of 0.1L/min, and nitrogen gas was continuously fed at a rate of 0.5L/min, hydrogen fluoride and hydrogen chloride gas as off-gases generated during the reaction were absorbed by an alkali solution, and after 4 hours of the heat-insulating reaction, sampling analysis showed that vinyl chlorocarbonate was 15.5% and vinyl fluorocarbonate was 58.2%, and after 8 hours of the heat-insulating reaction, sampling analysis showed that vinyl chlorocarbonate was 1.1% and vinyl fluorocarbonate was 72.3%.
In a specific embodiment, the distillation purification process is: carrying out reduced pressure distillation under the pressure of 10mmHg, and collecting 90-110 ℃ fractions, namely fluoroethylene carbonate.
In a specific embodiment, the reaction temperature of the distillation purification is 60-90 ℃, and the reaction time of the distillation purification is 4-24 hours.
More specifically, a fraction of 90-110 ℃/10mmHg was collected, wherein 105g (content: 96.2%) of fluoroethylene carbonate was obtained, and the yield was 95.2%.
Example 2
The application provides a production process of high-purity fluoroethylene carbonate, which comprises the following steps:
adding fluoride and a catalyst to a reaction vessel;
then adding chloroethylene carbonate, reacting the reactants in a reaction container, and controlling the reaction temperature to be 50-120 ℃ under the protection of nitrogen to finally obtain a mixture containing fluoroethylene carbonate;
adding an acid scavenger which is insoluble in fluoroethylene carbonate and can react with free acid in fluoroethylene carbonate to generate precipitate or volatile matter into fluoroethylene carbonate, so as to obtain fluoroethylene carbonate with certain purity;
and then carrying out distillation purification to obtain the required high-purity fluoroethylene carbonate.
In a particular embodiment, the molar ratio of vinyl chlorocarbonate to fluoride is: 1.0: 1.0-1.0: 1.2, and the mass of the added catalyst is 0.01-0.5 times of the total mass of the chloroethylene carbonate and the fluoride.
In a specific embodiment, the temperature of the reaction vessel is controlled between 10 ℃ and 200 ℃ during the dropping of the chloroethylene carbonate, and the temperature is controlled between 90 ℃ and 110 ℃ after the dropping is finished.
More specifically, 2.8g of polyethylene glycol catalyst and 122.5g of chloroethylene carbonate are added and mixed, 42g of sodium fluoride powder is gradually added into the mixed solution at 40 ℃, the adding speed is slow, the reaction temperature is controlled to be 50-70 ℃, the material becomes extremely viscous after the heat preservation is carried out for 3 hours, the material is cooled to 30 ℃, and then centrifugal suction filtration is carried out to obtain black filtrate, wherein the black filtrate contains 4% of unreacted chloroethylene carbonate, 89% of fluoroethylene carbonate and impurities brought by other raw materials.
In a specific embodiment, the acid scavenger is at least one of oxides of magnesium, calcium, silicon and aluminum, and is added in an amount of 0.01-10% by weight of fluoroethylene carbonate.
In a specific embodiment, the reaction temperature of the acid scavenger is 20-35 ℃ and the reaction time is 0.5-5 hours.
More specifically, fluoroethylene carbonate had a purity of 99.8%, a water content of 80ppm and a free acid of 95 ppm. 100g of fluoroethylene carbonate was taken, 0.1% of a mixture of calcium oxide and silicon oxide was added, and the acid-removing treatment was carried out at 35 ℃ for 5 hours, whereby 28ppm of the free acid was obtained after the treatment.
In a specific embodiment, the fluoride is introduced into the reaction vessel at a rate of 0.1 to 0.3L/min, and the nitrogen is introduced into the reaction vessel at a rate of 0.5 to 1.5L/min.
In a particular embodiment, the reaction vessel is provided with an alkaline liquid to absorb the off-gases generated during the reaction.
In a particular embodiment, the off-gas comprises hydrogen chloride gas and hydrogen fluoride gas.
More specifically, hydrogen fluoride gas was continuously fed into the reaction vessel at a rate of 0.2L/min, while nitrogen gas was continuously fed at a rate of 1L/min, hydrogen fluoride and hydrogen chloride gas, which were off-gases generated during the reaction, were absorbed by an alkaline solution, and after 4 hours of the heat-insulating reaction, the samples were analyzed to find that vinyl chlorocarbonate was 7.2% and vinyl fluorocarbonate was 78.3%, and after 6 hours of the heat-insulating reaction, the samples were analyzed to find that vinyl chlorocarbonate was 0.5% and vinyl fluorocarbonate was 87.4%, and the reaction was terminated.
In a specific embodiment, the distillation purification process is: carrying out reduced pressure distillation under the pressure of 10mmHg, and collecting 90-110 ℃ fractions, namely fluoroethylene carbonate.
In a specific embodiment, the reaction temperature of the distillation purification is 60-90 ℃, and the reaction time of the distillation purification is 4-24 hours.
More specifically, a fraction of 90-110 ℃/10mmHg was collected, wherein 104g (97.7% content) of fluoroethylene carbonate was obtained, and the yield was 95.9%.
The above description is only an example of the present application and is not intended to limit the scope of the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
The above description is only for the specific embodiments of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present application, and shall be covered by the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (10)
1. The production process of the high-purity fluoroethylene carbonate is characterized by comprising the following steps of:
adding fluoride and a catalyst to a reaction vessel;
then adding chloroethylene carbonate, reacting the reactants in a reaction container, and controlling the reaction temperature to be 50-120 ℃ under the protection of nitrogen to finally obtain a mixture containing fluoroethylene carbonate;
adding an acid scavenger which is insoluble in fluoroethylene carbonate and can react with free acid in fluoroethylene carbonate to generate precipitate or volatile matter into fluoroethylene carbonate, so as to obtain fluoroethylene carbonate with certain purity;
and then carrying out distillation purification to obtain the required high-purity fluoroethylene carbonate.
2. The process for producing high-purity fluoroethylene carbonate according to claim 1, wherein the molar ratio of chloroethylene carbonate to fluoride is as follows: 1.0: 1.0-1.0: 1.2, wherein the mass of the catalyst is 0.01-0.5 times of the total mass of the chloroethylene carbonate and the fluoride.
3. The process for producing high-purity fluoroethylene carbonate according to claim 1, wherein the temperature of the reaction vessel is controlled to be between 10 ℃ and 200 ℃ during the dropwise addition of the chloroethylene carbonate, and is controlled to be between 90 ℃ and 110 ℃ after the dropwise addition.
4. The process for producing high-purity fluoroethylene carbonate according to claim 1, wherein the acid scavenger is at least one of oxides of magnesium, calcium, silicon and aluminum, and is added in an amount of 0.01-10% by weight based on fluoroethylene carbonate.
5. The process for producing high-purity fluoroethylene carbonate according to claim 1, wherein the reaction temperature of the acid scavenger is 20-35 ℃ and the reaction time is 0.5-5 hours.
6. The process for producing high-purity fluoroethylene carbonate according to claim 1, wherein the fluoride is introduced into the reaction vessel at a rate of 0.1 to 0.3L/min, and the nitrogen is introduced into the reaction vessel at a rate of 0.5 to 1.5L/min.
7. The process for preparing high-purity fluoroethylene carbonate according to claim 1, wherein an alkaline liquid is provided in the reaction vessel to absorb the waste gas generated during the reaction.
8. The process of claim 7, wherein the waste gas comprises hydrogen chloride gas and hydrogen fluoride gas.
9. The process for producing high-purity fluoroethylene carbonate according to claim 1, wherein the distillation purification comprises the following steps: carrying out reduced pressure distillation under the pressure of 10mmHg, and collecting 90-110 ℃ fractions, namely fluoroethylene carbonate.
10. The process for producing high-purity fluoroethylene carbonate according to claim 9, wherein the reaction temperature for the distillation purification is 60 to 90 ℃, and the reaction time for the distillation purification is 4 to 24 hours.
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| CN101210005A (en) * | 2006-12-30 | 2008-07-02 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing fluoroethylene carbonate |
| CN101717389A (en) * | 2009-10-29 | 2010-06-02 | 张家港市华盛化学有限公司 | Disacidifying and dewatering method of fluoroethylene carbonate |
| CN103113345A (en) * | 2013-01-21 | 2013-05-22 | 张家港瀚康化工有限公司 | Preparation method of fluoroethylene carbonate |
| CN106916137A (en) * | 2017-03-01 | 2017-07-04 | 山东瀛寰化工有限公司 | A kind of industrial process of electron level fluorinated ethylene carbonate |
| CN107033119A (en) * | 2017-04-06 | 2017-08-11 | 多氟多化工股份有限公司 | A kind of preparation method of high-purity fluorinated ethylene carbonate |
| CN111285838A (en) * | 2018-12-10 | 2020-06-16 | 浙江蓝天环保高科技股份有限公司 | Continuous preparation method of fluoroethylene carbonate |
| CN110684007A (en) * | 2019-10-27 | 2020-01-14 | 淮安瀚康新材料有限公司 | Preparation method of fluoroethylene carbonate |
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