CN117586221A - Method for preparing ultra-high purity fluoroethylene carbonate by coupling melt crystallization - Google Patents
Method for preparing ultra-high purity fluoroethylene carbonate by coupling melt crystallization Download PDFInfo
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- CN117586221A CN117586221A CN202311568415.4A CN202311568415A CN117586221A CN 117586221 A CN117586221 A CN 117586221A CN 202311568415 A CN202311568415 A CN 202311568415A CN 117586221 A CN117586221 A CN 117586221A
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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 77
- 238000002425 crystallisation Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 55
- 230000008025 crystallization Effects 0.000 title claims abstract description 53
- 238000010168 coupling process Methods 0.000 title claims abstract description 13
- 230000008878 coupling Effects 0.000 title claims abstract description 12
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims description 47
- 230000008018 melting Effects 0.000 claims description 47
- 238000001816 cooling Methods 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 32
- 239000000725 suspension Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 18
- 239000007790 solid phase Substances 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 8
- 230000000630 rising effect Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- 230000035900 sweating Effects 0.000 claims description 2
- 210000004243 sweat Anatomy 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000007086 side reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 38
- 239000012452 mother liquor Substances 0.000 description 5
- 239000012043 crude product Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000011552 falling film Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000001640 fractional crystallisation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 241000183024 Populus tremula Species 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of purification of electronic chemicals, and particularly relates to a method for preparing ultra-high purity fluoroethylene carbonate by coupling melt crystallization. Is suitable for purifying fluoroethylene carbonate (the mass percentage content is more than or equal to 60 percent, preferably more than or equal to 90 percent), and the purity of the obtained product is more than or equal to 99.99 percent. The method has the advantages of low operation temperature, no additional solvent, simple operation, low energy consumption, high purity, high yield, no three-waste discharge, no side reaction and the like, and belongs to a green separation and purification process.
Description
Technical Field
The invention belongs to the field of chemical purification, and relates to a preparation method of fluoroethylene carbonate, in particular to a method for preparing ultra-high-purity fluoroethylene carbonate by coupling melt crystallization.
Background
The melting point of fluoroethylene carbonate is 20-23 ℃ and the boiling point is 212 ℃. Can be used as an additive in the electrolyte of the lithium ion battery, can form an SEI film at the electrode/electrolyte interface, has compact structure but does not increase impedance, and can prevent the electrolyte from further decomposition. The additive amount is small, but the cycle life of the battery is prolonged, the safety of the battery is improved, and the low-temperature performance of the battery is improved. Thus, fluoroethylene carbonate plays an important role in the battery industry. At present, fluoroethylene carbonate is purified by rectification or rectification and crystallization phase combination modes, and the method comprises the following steps:
the patent CN105801554A 'purification method of high-purity fluoroethylene carbonate' and the patent CN103113344A 'purification method of high-purity fluoroethylene carbonate' are both that the crude fluoroethylene carbonate is subjected to reduced pressure distillation, solution crystallization and drying to obtain the product with the purity of more than 99.95 percent. However, the purity of the product prepared by the process is low, and new organic solvents (the crystallization solvents are selected from toluene, ethylbenzene, n-hexane, dimethyl carbonate and cyclohexane) are introduced in the crystallization process, so that the environment is seriously polluted, and the problems of three waste discharge, solvent recovery and cost are caused.
Patent CN112266374a discloses a purification method of fluoroethylene carbonate, which performs physical property calculation by Aspen Plus software, and removes impurities in raw materials by a light component removal column reaction, a falling film evaporator reaction and a heavy component removal column reaction. The process does not mention the purity and yield of the finished product produced.
Patent CN101870652A discloses a refining method of high-purity fluoroethylene carbonate, which adopts a distillation process to improve the purity of a crude fluoroethylene carbonate product to more than 98 percent, then carries out solution crystallization and rectification again to obtain a high-purity product. The method has higher purity requirement on the fluoroethylene carbonate product after distillation, does not mention the purity of the final product, introduces new organic solvent in the solution crystallization process, and has serious environmental pollution.
Patent CN113563300a discloses a "purification method of fluoroethylene carbonate and its obtained product", which is to perform pressure crystallization on a crude fluoroethylene carbonate, mix the crystallized de-heavy component with the de-light component of the non-crystallized mother liquor, and purify the mixed liquor by adopting a falling film crystallization mode, thus obtaining a high-purity product. However, the method does not refer to specific yield, and the process needs pressure crystallization, falling film crystallization, heavy removal and light removal, and has the advantages of large operating temperature difference, low safety, complex process and high cost. The purity of the fluoroethylene carbonate obtained by the method can reach more than 99.97%, and the purity of the fluoroethylene carbonate prepared by the novel coupling melt crystallization can reach more than 99.99%.
Patent CN102887883a discloses a "continuous purification method of crude fluoroethylene carbonate", which is to subject the crude fluoroethylene carbonate to decolorization and vacuum rectification, and remove impurities through a light and heavy removal rectifying tower to obtain refined fluoroethylene carbonate with purity of over 99.95%. However, the finished product prepared by the method has low purity, and the energy consumption in the rectification process is high, so that the cost is increased.
Patent CN110878078A discloses a "method for preparing electronic grade fluoroethylene carbonate by fractional crystallization", rectifying a crude fluoroethylene carbonate product to obtain fractions with different purities; fractional crystallization of fractions with different purities, and then distillation and material melting are carried out; finally, the fluoroethylene carbonate with high purity is obtained through decoloration and dehydration. However, the method requires the steps of rectification, low-temperature distillation, decoloration and dehydration, and has the advantages of high process crystallization level, complex process and high energy consumption. The vaporization latent heat of fluoroethylene carbonate is 58.93kJ/moL, the melting enthalpy is 18.87kJ/moL, the energy required by rectification is high, and the practical application cost of the patent is far higher than that of the patent.
Foreign patent US20120157695 discloses a process wherein crude fluoroethylene carbonate is obtained by fluorination of ethylene carbonate and less than 5% hf in elemental fluorine; HF is removed through multistage rectification purification (adsorption step can be added), and finally refined fluoroethylene carbonate with the HF content not more than 30ppm can be obtained.
Most of the methods adopt a mode of combining rectification and solution crystallization phase to purify fluoroethylene carbonate, but fluoroethylene carbonate has higher boiling point, even if a vacuum rectification process is adopted, the operation temperature is still higher, and residual thermosensitive substances are easily decomposed and polymerized, so that quality indexes such as chromaticity, purity and the like of products are influenced. And the material is evaporated-condensed for multiple times in the rectification process, so that the energy consumption is higher. In some methods, new organic solvents are introduced, which has serious environmental pollution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a novel method for preparing ultra-high purity fluoroethylene carbonate by coupling melt crystallization. The ultra-high purity fluoroethylene carbonate product with the purity of more than 99.99 percent is prepared through coupling melting crystallization. If the purity of the raw materials is more than 99.3%, the theoretical yield can reach 99%, which is superior to most of the purifying processes of fluoroethylene carbonate; the method has the advantages of simple process, low cost, environmental protection and no generation of three wastes, and accords with the development direction of green chemical industry.
The invention adopts the following technical scheme to realize the aim:
a method for preparing ultra-high purity fluoroethylene carbonate by coupling melt crystallization, which comprises the following steps:
1) Suspension melting crystallization: continuously feeding fluoroethylene carbonate (the mass percentage content is more than or equal to 60%) into a suspension melting crystallization device at a certain rate, and continuously cooling, suspending and crystallizing at the crystallization temperature of-15-10 ℃ for 2-8 h.
2) And (3) filtering: and (3) carrying out solid-liquid separation, taking a solid phase as a raw material in the step (3), recrystallizing a liquid phase until the mass percentage of fluoroethylene carbonate is less than 50%, and discharging residual liquid.
3) Layer-type melt crystallization: melting the solid phase obtained in the step 2), and then adding the melted solid phase into a layered melting crystallizer for cooling; the cooling rate is 0.1-20K/h, and the final cooling temperature is-20-10 ℃; keeping the temperature for 0.5-1 h; discharging residual liquid; heating up and sweating the crystals in the crystallizer, wherein the heating up rate of the cold source is 1-30K/h; heating to 22-24 ℃; keeping the temperature for 0.5-1 h; discharging perspiration; and heating the crystals in the crystallizer to above 25 ℃ until the materials are completely melted, and discharging the crystals out of the crystallizer in a liquid form to obtain a high-purity product.
Further preferably, the mass percentage of the fluoroethylene carbonate raw material in the step 1) is more than or equal to 60%.
It is further preferred that the crystallization temperature in step 1) is-10 to 10℃and the residence time is 2 to 6 hours.
It is further preferred that the temperature difference between the cold source for cooling and the material in step 1) is < 2 ℃.
Further preferably, the cooling rate of the cold source in the step 3) is 0.2-10K/h, the final cooling temperature is-10 ℃, and the constant temperature is 0.5-1 h.
Further preferably, the residual liquid which is not crystallized after the temperature reduction in the step 3) is returned to the step 1) as a raw material.
Further preferably, the temperature rising rate of the cold source in the step 3) is 1-20K/h, the final temperature of the temperature rising is 22-24 ℃, and the temperature is kept for 0.5-1 h.
It is further preferred that step 3) the perspiration from the crystals in the crystallizer during the heating up to the final temperature is returned to step 3) as raw material.
The coupling process of suspension melting crystallization and layered melting crystallization is preferably selected in the steps 1), 2) and 3), and when the treatment capacity exceeds 3000 tons/year, the suspension crystallization process is preferably operated continuously.
The invention has the advantages and beneficial effects that:
1. the invention provides a method for separating pure fluoroethylene carbonate from crude products containing fluoroethylene carbonate, which adopts a melting crystallization process. The invention has the advantages that the suspension melting crystallization method is adopted to initially purify the materials, reduce the purity of the mother liquor and improve the total yield; secondly, purifying the materials to a purity of more than 99.99% by adopting a layered melting crystallization method. The invention creatively couples suspension and layered melt crystallization processes, improves the purity of fluoroethylene carbonate to more than 99.99 percent, and solves the industrial problems that the yield is difficult to improve and the cost is reduced while the purity of fluoroethylene carbonate is improved by a person skilled in the art.
2. The invention is suitable for the crude product of fluoroethylene carbonate (the mass percentage content is more than or equal to 60%). After the process raw materials enter a separation process, materials with the mass percent of fluoroethylene carbonate more than or equal to 50% obtained in each step can be reused. The fluoroethylene carbonate of the whole system can be recovered and purified again, and if the purity of the raw material is more than 99.3%, the theoretical recovery rate can reach 99%.
3. The process of the invention has the advantages of no additional solvent, reduced operation cost, simplified operation, environmental protection, no generation of three wastes, and capability of preparing the ultra-high purity fluoroethylene carbonate with the purity of more than 99.99 percent. The invention has flexible process and can be adjusted according to actual needs.
Detailed Description
The present invention will be described in further detail with reference to the preferred embodiments, so that those skilled in the art can better understand the technical solutions of the present invention.
Example 1
515.63g of crude fluoroethylene carbonate with the content of 90.2% is put into a 500ml suspension melting crystallizer, and the temperature is reduced according to the cooling rate of 8K/h, the final temperature is minus 15 ℃, and the temperature is kept for 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product.
And heating the fluoroethylene carbonate product prepared by suspension melting crystallization to 25 ℃ to enable the materials to be completely melted into a liquid state, and then putting the liquid state into a 500ml layered melting crystallizer. Cooling according to the cooling rate of 7K/h, wherein the final cooling temperature is 5 ℃, and the temperature is kept constant for 1h; mother liquor is discharged. Heating the material to 23 ℃ at a heating rate of 15K/h, and keeping the temperature for 0.5h; discharging perspiration; and heating and melting to obtain the product. The product purity of fluoroethylene carbonate was 99.99% and the total yield was 85.5%.
Comparative example 1
515.63g of crude fluoroethylene carbonate with the content of 90.2% is put into a 500ml suspension melting crystallizer, and the temperature is reduced according to the cooling rate of 8K/h, the final temperature is minus 15 ℃, and the temperature is kept for 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product.
And heating the fluoroethylene carbonate product prepared by primary suspension melting crystallization to 25 ℃ to enable the materials to be completely melted into a liquid state, and then putting the liquid state into a 300ml suspension melting crystallizer. And cooling according to the cooling rate of 7K/h, wherein the final cooling temperature is 5 ℃, and the constant temperature is 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product. The product purity of fluoroethylene carbonate was 95.02% and the total yield was 92.37%.
Example 2
355.83g of 75.1% fluoroethylene carbonate crude product is put into a 300ml suspension melting crystallizer, and is cooled according to the cooling rate of 5K/h, the final cooling temperature is minus 15 ℃, and the temperature is kept for 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product.
And heating the fluoroethylene carbonate product prepared by suspension melting crystallization to 25 ℃ to enable the materials to be completely melted into a liquid state, and then putting the liquid state into a 300ml layered melting crystallizer. Cooling according to the cooling rate of 8K/h, wherein the final cooling temperature is 4 ℃, and the temperature is kept for 1h; mother liquor is discharged. Heating the material to 23 ℃ at a heating rate of 14K/h, and keeping the temperature for 0.5h; discharging perspiration; and heating and melting to obtain the product. The product purity of fluoroethylene carbonate was 99.99% and the total yield was 60.47%.
Comparative example 2
355.83g of 75.1% fluoroethylene carbonate crude product is put into a 300ml suspension melting crystallizer, and is cooled according to the cooling rate of 5K/h, the final cooling temperature is minus 15 ℃, and the temperature is kept for 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product.
And heating the fluoroethylene carbonate product prepared by primary suspension melting crystallization to 25 ℃ to enable the materials to be completely melted into a liquid state, and then putting the liquid state into a 300ml suspension melting crystallizer. And cooling according to the cooling rate of 8K/h, wherein the final cooling temperature is 4 ℃, and the constant temperature is 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product. The product purity of fluoroethylene carbonate was 88.12% and the total yield was 62.25%.
Example 3
In a 500ml suspension melting crystallizer, 485.83g of crude fluoroethylene carbonate with 85.4 percent of content is put into the suspension melting crystallizer, the temperature is reduced according to the temperature reduction rate of 6K/h, the final temperature of the temperature reduction is minus 10 ℃, and the temperature is kept for 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product.
And heating the fluoroethylene carbonate product prepared by suspension melting crystallization to 25 ℃ to enable the materials to be completely melted into a liquid state, and then putting the liquid state into a 500ml layered melting crystallizer. Cooling according to a cooling rate of 5K/h, wherein the final cooling temperature is 6 ℃, and keeping the temperature for 1h; mother liquor is discharged. Heating the material to 23 ℃ at a heating rate of 15K/h, and keeping the temperature for 0.5h; discharging perspiration; and heating and melting to obtain the product. The product purity of fluoroethylene carbonate was 99.99% and the total yield was 82.5%.
Comparative example 3
In a 500ml suspension melting crystallizer, 485.83g of crude fluoroethylene carbonate with 85.4 percent of content is put into the suspension melting crystallizer, the temperature is reduced according to the temperature reduction rate of 6K/h, the final temperature of the temperature reduction is minus 10 ℃, and the temperature is kept for 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product.
And heating the fluoroethylene carbonate product prepared by primary suspension melting crystallization to 25 ℃ to enable the materials to be completely melted into a liquid state, and then putting the liquid state into a 500ml suspension melting crystallizer. And cooling according to the cooling rate of 5K/h, wherein the final cooling temperature is 6 ℃, and the constant temperature is 0.5h. And then carrying out solid-liquid separation to obtain a solid-phase fluoroethylene carbonate product. The product purity of fluoroethylene carbonate was 95.12% and the total yield was 91.25%.
As can be seen from comparison of two-stage suspension melting crystallization and coupling melting crystallization processes, the two-stage suspension melting crystallization cannot achieve the purity of the coupling melting crystallization, and if the two-stage suspension melting crystallization is required to achieve the same purity, the problems of low single pass yield and high investment and operation cost can be caused. The layered melting crystallization is beneficial to improving the purity, but the yield of the layered melting crystallization is low, and if the yield which is equal to that of the coupled crystallization is required to be achieved, the investment cost and the operation cost are also obviously improved. The coupling melt crystallization has the advantages of less investment of suspension melt crystallization, automatic continuous production and production cost of 1/3-1/5 of that of layered melt crystallization, and can improve the purity of the product, thus being a preferable process.
The foregoing is merely illustrative of the present invention and variations in terms of specific embodiments and application scope will occur to those skilled in the art upon consideration of the teachings of the present invention, and this disclosure is not to be construed as limiting the invention.
Claims (8)
1. A method for preparing ultra-high purity fluoroethylene carbonate by coupling melt crystallization is characterized in that: the method comprises the following steps:
1) Suspension melting crystallization: continuously feeding fluoroethylene carbonate with the mass percent of more than or equal to 60 percent into a suspension melting crystallization device at a certain speed, and continuously cooling, suspending and crystallizing at the crystallization temperature of-15-10 ℃ for 2-8 h.
2) And (3) filtering: and (3) carrying out solid-liquid separation, taking a solid phase as a raw material in the step (3), recrystallizing a liquid phase until the mass percentage of fluoroethylene carbonate is less than 50%, and discharging residual liquid.
3) Layer-type melt crystallization: melting the solid phase obtained in the step 2), and then adding the melted solid phase into a layered melting crystallizer for cooling; the cooling rate is 0.1-20K/h, and the final cooling temperature is-20-10 ℃; keeping the temperature for 0.5-1 h; discharging residual liquid; heating up and sweating the crystals in the crystallizer, wherein the heating up rate of the cold source is 1-30K/h; heating to 22-24 ℃; keeping the temperature for 0.5-1 h; discharging perspiration; and heating the crystals in the crystallizer to above 25 ℃ until the materials are completely melted, and discharging the crystals out of the crystallizer in a liquid form to obtain a high-purity product.
2. The method according to claim 1, characterized in that: the mass percentage of the fluoroethylene carbonate raw material in the step 1) is more than or equal to 60 percent.
3. The method according to claim 1, characterized in that: the crystallization temperature in the step 1) is-10 to 10 ℃ and the residence time is 2 to 6 hours.
4. The method according to claim 1, characterized in that: the temperature difference between the cold source for cooling and the materials in the step 1 is less than 2 ℃.
5. The method according to claim 1, characterized in that: and 3) cooling the cold source at a cooling rate of 0.2-10K/h, keeping the final cooling temperature at-10 ℃ and keeping the temperature for 0.5-1 h.
6. The method according to claim 1, characterized in that: and 3) returning the residual liquid which is not crystallized after the temperature reduction in the step 3) to the step 1) as a raw material.
7. The method according to claim 1, characterized in that: step 3) the temperature rising rate of the cold source is 1-20K/h, the final temperature of the temperature rising is 22-24 ℃, and the constant temperature is 0.5-1 h.
8. The method according to claim 1, characterized in that: step 3) the perspiration liquid during the period when the crystal in the crystallizer sweats and rises to the final temperature returns to step 3) as the raw material.
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