CN110878078B - Method for preparing electronic-grade fluoroethylene carbonate through fractional crystallization - Google Patents
Method for preparing electronic-grade fluoroethylene carbonate through fractional crystallization Download PDFInfo
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- CN110878078B CN110878078B CN201910968421.6A CN201910968421A CN110878078B CN 110878078 B CN110878078 B CN 110878078B CN 201910968421 A CN201910968421 A CN 201910968421A CN 110878078 B CN110878078 B CN 110878078B
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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 37
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001640 fractional crystallisation Methods 0.000 title claims abstract description 14
- 238000002425 crystallisation Methods 0.000 claims abstract description 51
- 230000008025 crystallization Effects 0.000 claims abstract description 51
- 239000000047 product Substances 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 238000004821 distillation Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 abstract description 7
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract 1
- 125000004122 cyclic group Chemical group 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- XWRPBQMMTJWUSL-UHFFFAOYSA-N 1,3-dioxolan-2-one fluoroethene Chemical compound FC=C.O=C1OCCO1 XWRPBQMMTJWUSL-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-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
- 238000004042 decolorization Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000002000 Electrolyte additive Substances 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
-
- 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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization, which comprises the following steps: rectifying the fluoroethylene carbonate crude product, and collecting fluoroethylene carbonate with different purities in stages; aiming at the difference of the purity of the fluoroethylene carbonate, fractional crystallization is carried out under different crystallization conditions, so that the utilization rate is improved, the impurity content is reduced, and the product purity is improved; then distilling and melting; and finally, decoloring and dehydrating to obtain the electronic-grade fluoroethylene carbonate. The method has the advantages of simple process, economy, environmental protection, easy industrialization and the like, and the purification effect is good, the obtained product has high purity, the chromatographic purity is not less than 99.99 percent, and the product can be directly used as an additive of battery electrolyte.
Description
Technical Field
The invention relates to a method for purifying fluoroethylene carbonate ethylene ester, in particular to a method for purifying electronic-grade fluoroethylene carbonate ethylene ester, and belongs to the technical field of lithium ion battery electrolyte additives.
Background
Fluoroethylene carbonate is a special ethylene carbonate, is an important fine chemical material and is mainly used as a film forming additive and an explosion-proof solvent of lithium battery electrolyte. The electrolyte can form a compact structure layer without increasing impedance, inhibits the decomposition of partial electrolyte, forms an SEI film with excellent performance on the surface of a negative electrode to reduce the impedance of the battery, can obviously improve the specific capacity and the cycle life of the battery, and improves the cycle stability of the battery. Therefore, fluoroethylene carbonate is widely used in the lithium battery industry.
Meanwhile, fluoroethylene carbonate applied to the electrolyte has high purity requirement, and a crude fluoroethylene carbonate product is generally purified and then applied to the electrolyte of the lithium ion battery. CN101870652A discloses a method for refining high-purity fluoroethylene carbonate, which comprises the steps of improving the purity of a fluoroethylene carbonate crude product to more than 98% by adopting a distillation process, crystallizing, and rectifying to obtain a high-purity product, wherein the method has higher requirement on the purity of the fluoroethylene carbonate product after distillation and distillation. CN103113344A discloses a method for purifying high-purity fluoroethylene carbonate, which is characterized in that a high-purity product is obtained by carrying out reduced pressure distillation, crystallization and drying on crude fluoroethylene carbonate, and a new organic solvent is introduced into a crystallization process, so that the environmental pollution is serious.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization comprises the following steps:
s1, rectifying a fluoroethylene carbonate crude product, and collecting fluoroethylene carbonate in stages according to different purity of fractions;
s2, carrying out fractional crystallization on the products with different purities obtained in the S1 in different crystallization kettles;
s3, distilling the crystallized product in the S2 at low temperature, and melting;
and S4, decoloring and dehydrating the product in the S3 through a decoloring adsorption column and a dehydrating adsorption column to obtain the electronic-grade fluoroethylene carbonate.
The technical scheme is preferably as follows: in the S1, the vacuum pressure is not higher than-0.09 MPa, and the temperature is 90-110 ℃.
The technical scheme is preferably as follows: in the S1, the fraction collected after the rectification is started is used as the front fraction; when the purity of the fluoroethylene carbonate is not less than 99.5 percent, switching the middle distillate collecting tank; when the purity is less than 99.5%, the back distillation collecting tank is switched.
The technical scheme is preferably as follows: and in the S2, the crystallization kettle is filled with nitrogen to keep the pressure at 0.005-0.015 Mpa.
The technical scheme is preferably as follows: the middle distillation part is cleaned for the first grade, the crystallization temperature is 6-15 ℃, and the crystallization time is 3-7 h; the front distillation part is subjected to secondary crystallization, the primary crystallization temperature is-7 to 5 ℃, and the crystallization time is 3 to 5 hours; the secondary crystallization temperature is 6-15 ℃, and the crystallization time is 3-7 h; the back distillation part is subjected to three-stage crystallization, the first-stage crystallization temperature is between 14 ℃ below zero and 8 ℃ below zero, and the crystallization time is 2 to 7 hours; the second-stage crystallization temperature is-7-5 ℃, the crystallization time is 3-5 h, the third-stage crystallization temperature is 6-15 ℃, and the crystallization time is 3-7 h.
The technical scheme is preferably as follows: in the S3, the distillation temperature is 18-23 ℃, the purity of the distillate is less than 65% and returns to the rectification section for utilization, the purity of the distillate is not less than 65% and returns to the crystallization section for utilization, and the distillate is recycled for 4 times and then discarded.
The technical scheme is preferably as follows: in the S3, the material melting temperature is 25-35 ℃ and the time is 4-8 h.
The technical scheme is preferably as follows: and in the S4, the decolorized adsorption column filling material is carbon fiber, and the dehydrated adsorption column filling material is a molecular sieve.
The technical scheme is preferably as follows: in the S4, the decoloring and dehydrating temperature is 23-27 ℃, and the time is 13-18 h.
The invention has the technical effects and advantages that: for overcoming the defects of the prior art, the invention provides a method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization, and the chromatographic purity of the product reaches more than 99.99 percent. The method has the advantages of simple process, economy, environmental protection, easy industrialization and the like, improves the utilization rate of the fluoroethylene carbonate crude product, namely respectively collects fluoroethylene carbonate with different purities in the rectification stage, and finally can meet the requirements of electronic-grade products after crystallization, decoloration and dehydration, thereby reducing the waste of raw materials. No new organic solvent is introduced in the crystallization process, so that the influence of the new organic solvent on the environment is avoided; further removal of impurities in the distillation stage; the obtained product has high purity and can be directly used as an additive of battery electrolyte.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to these examples.
Example 1
The embodiment provides a method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization, which comprises the following steps:
(1) And (3) rectification: 450kg of fluoroethylene carbonate crude product with the purity of 85.93 percent is rectified under the vacuum degree of-0.09 Mpa and the temperature of 100 ℃, and the purity of fluoroethylene carbonate in the distillate is checked at any time. 150kg of front distillation with purity of 91.23 percent, 180kg of middle distillation with purity of 99.93 percent and 50kg of rear distillation with purity of 82.56 percent are obtained.
(2) Crystallization, distillation and material melting:
(1) performing primary crystallization on the middle distillate at the pressure of 0.01MPa and the temperature of 12 ℃ for 4h. And after the crystallization is finished, discharging materials, and returning the mother liquor to the rectification section for cyclic utilization. Then heating to 20 ℃ for distillation, collecting distillate, detecting to obtain the product with the purity of 90.53%, and returning the distillate to the crystallization section for use. Heating the rest crystal part to 25 deg.C, and maintaining under 0.01MPa for 6 hr.
(2) The middle distillate is firstly subjected to first-stage crystallization: the pressure is 0.01MPa, the temperature is-5 ℃, and the time is 3h. And after the completion, discharging, and returning the mother liquor to the rectification section for cyclic utilization. And secondary crystallization is carried out: the pressure is 0.01Mpa, the temperature is 6 ℃, and the time is 4h. And discharging after the completion, and returning the mother liquor to the rectification section for cyclic utilization. Then heating to 22 ℃ for distillation, collecting distillate, detecting to obtain the purity of 83.44%, and returning to the crystallization section for utilization. Heating the rest crystal part to 30 deg.C, and maintaining at 0.01MPa for 4 hr.
(3) The post-distillation is firstly subjected to primary crystallization: the pressure is 0.01MPa, the temperature is-12 ℃, and the time is 3h. And after the completion, discharging, and returning the mother liquor to the rectification section for cyclic utilization. And then secondary crystallization is carried out: the pressure is 0.01Mpa, the temperature is-3 ℃, and the time is 4h. And after the completion, discharging, and returning the mother liquor to the rectification section for cyclic utilization. And finally, carrying out three-stage crystallization: the pressure is 0.01Mpa, the temperature is 10 ℃, and the time is 3h. And after the completion, discharging, and returning the mother liquor to the rectification section for cyclic utilization. And (3) heating to 23 ℃, distilling, collecting distillate, detecting to obtain 62.35% purity, and returning to the rectification working section for utilization. Heating the rest crystal part to 30 deg.C, and maintaining at 0.01MPa for 4 hr.
(3) Decoloring and dehydrating: decolorizing the materials at 25 deg.C for 15 hr, and dehydrating at 25 deg.C for 16 hr. Sampling analysis shows that the product has the chromatographic purity of 99.999 percent, the chroma of 9 and the water content of 9ppm, and the yield is 96.4 percent.
Example 2
Example 2 corresponds to the procedure of example 1, except for the specific parameters of rectification, crystallization, distillation, material melting, dehydration and decolorization. Example 2 the specific parameters and results are given in table 1.
TABLE 1
Example 3
Example 3 corresponds to the procedure of example 1, except for the specific parameters of rectification, crystallization, distillation, material melting, dehydration and decolorization. Example 3 specific parameters and results are shown in table 2.
TABLE 2
The embodiment shows that the yield of the method for preparing the electronic-grade fluoroethylene carbonate is over 95 percent, the yield is high, and the product purity can reach 99.999 percent.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still make modifications to the technical solutions described in the foregoing embodiments, or make equivalent substitutions and improvements to part of the technical features of the foregoing embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization comprises the following steps:
s1, rectifying a fluoroethylene carbonate crude product, and collecting fluoroethylene carbonate in stages according to different purity of fractions;
in the S1, the pressure is not higher than-0.09 MPa during rectification, and the temperature is 90-110 ℃;
in the S1, the fraction collected after the rectification is started is used as the front fraction; when the purity of the fluoroethylene carbonate is not less than 99.5 percent, switching the middle distillate collecting tank; when the purity is less than 99.5%, the post-distillation collection tank is switched again;
s2, carrying out fractional crystallization on the products with different purities obtained in the S1 in different crystallization kettles;
in the S2, the pressure in the crystallization kettle is kept between 0.005 and 0.015MPa;
the middle distillation part is subjected to primary crystallization at the crystallization temperature of 6-15 ℃ for 3-7 h; the front distillation part is subjected to secondary crystallization, the primary crystallization temperature is-7 to 5 ℃, and the crystallization time is 3 to 5 hours; the secondary crystallization temperature is 6-15 ℃, and the crystallization time is 3-7 h; the back distillation part is subjected to three-stage crystallization, the first-stage crystallization temperature is-14 to-8 ℃, and the crystallization time is 2 to 7 hours; the second-stage crystallization temperature is-7-5 ℃, the crystallization time is 3-5 h, the third-stage crystallization temperature is 6-15 ℃, and the crystallization time is 3-7 h; the fluoroethylene carbonate with different purities is subjected to fractional crystallization under different conditions, so that the utilization rate of the distillate can be improved, the impurity content in the product can be reduced, and the product purity can be improved;
s3, distilling and melting the product crystallized in the S2 at 18-23 ℃;
and S4, decoloring and dehydrating the product in the S3 through a decoloring adsorption column and a dehydrating adsorption column to obtain the electronic-grade fluoroethylene carbonate.
2. The method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization according to claim 1, wherein: the distillate in the S3 with the purity of less than 65 percent returns to a rectification section, the distillate with the purity of not less than 65 percent returns to a crystallization section, and the distillate is recycled for 4 times and then discarded; the material melting temperature is 25-35 ℃ and the time is 4-8 h.
3. The method for preparing electronic-grade fluoroethylene carbonate by fractional crystallization according to claim 1, wherein: in S4, the filling material of the decoloring adsorption column is carbon fiber, the filling material of the dehydration adsorption column is a molecular sieve, the decoloring and dehydration temperature is 23-27 ℃, and the time is 13-18 h.
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| CN113636999B (en) * | 2021-07-26 | 2022-10-18 | 珠海理文新材料有限公司 | Water removal and crystallization method of vinylene carbonate |
| CN113563300B (en) * | 2021-07-26 | 2022-05-06 | 山东海科创新研究院有限公司 | Method for purifying fluoroethylene carbonate and product obtained by same |
| CN113845507A (en) * | 2021-08-26 | 2021-12-28 | 珠海理文新材料有限公司 | Method for removing water and chloride ions in fluoroethylene carbonate |
| CN113845506B (en) * | 2021-10-18 | 2022-09-23 | 惠州市宙邦化工有限公司 | Dynamic crystallization purification method of ethylene carbonate |
| CN115215831A (en) * | 2022-07-28 | 2022-10-21 | 珠海正杏新材料科技有限公司 | Method for preparing fluoroethylene carbonate fine product |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4552575A (en) * | 1982-02-04 | 1985-11-12 | Ruetgerswerke Aktiengesellschaft | Method for the mass separation of a liquid mixture through fractional crystallization |
| US5556972A (en) * | 1989-05-23 | 1996-09-17 | Van Den Bergh Foods Co., Division Of Conopco, Inc. | Counter current dry fractional crystallization |
| CN101870652A (en) * | 2009-04-24 | 2010-10-27 | 中国科学院福建物质结构研究所 | A kind of refining method of high-purity fluoroethylene carbonate |
| CN103113344A (en) * | 2012-09-26 | 2013-05-22 | 中国海洋石油总公司 | Purification method of high-purity fluoroethylene carbonate |
| CN106854195A (en) * | 2016-12-08 | 2017-06-16 | 江苏理文化工有限公司 | A kind of preparation method of fluoro ethylene carbonate with high purity |
| WO2018184379A1 (en) * | 2017-04-06 | 2018-10-11 | 多氟多化工股份有限公司 | Preparation method for high purity fluoroethylene carbonate |
-
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- 2019-10-12 CN CN201910968421.6A patent/CN110878078B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4552575A (en) * | 1982-02-04 | 1985-11-12 | Ruetgerswerke Aktiengesellschaft | Method for the mass separation of a liquid mixture through fractional crystallization |
| US5556972A (en) * | 1989-05-23 | 1996-09-17 | Van Den Bergh Foods Co., Division Of Conopco, Inc. | Counter current dry fractional crystallization |
| CN101870652A (en) * | 2009-04-24 | 2010-10-27 | 中国科学院福建物质结构研究所 | A kind of refining method of high-purity fluoroethylene carbonate |
| CN103113344A (en) * | 2012-09-26 | 2013-05-22 | 中国海洋石油总公司 | Purification method of high-purity fluoroethylene carbonate |
| CN106854195A (en) * | 2016-12-08 | 2017-06-16 | 江苏理文化工有限公司 | A kind of preparation method of fluoro ethylene carbonate with high purity |
| WO2018184379A1 (en) * | 2017-04-06 | 2018-10-11 | 多氟多化工股份有限公司 | Preparation method for high purity fluoroethylene carbonate |
Non-Patent Citations (1)
| Title |
|---|
| 分级结晶工艺生产精萘过程的研究;李超群等;《石油炼制与化工》;20070312(第03期);10-13 * |
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