CN113979985A - Method for improving yield stability of fluoroethylene carbonate - Google Patents
Method for improving yield stability of fluoroethylene carbonate Download PDFInfo
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- CN113979985A CN113979985A CN202111363136.5A CN202111363136A CN113979985A CN 113979985 A CN113979985 A CN 113979985A CN 202111363136 A CN202111363136 A CN 202111363136A CN 113979985 A CN113979985 A CN 113979985A
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- 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
- C07D317/34—Oxygen atoms
- C07D317/36—Alkylene carbonates; Substituted alkylene carbonates
Abstract
The invention discloses a method for improving the stability of the yield of fluoroethylene carbonate, which relates to the technical field of fluoroethylene carbonate synthesis, and comprises the following steps: step S1: adding high-activity potassium fluoride and an aprotic solvent into a three-neck flask together, and performing ultrasonic treatment for 30-60 minutes by using ultrasonic waves to uniformly disperse the high-activity potassium fluoride; step S2: heating the potassium fluoride solution uniformly dispersed by ultrasonic to 100-110 ℃, and evaporating and dehydrating under the stirring condition until no fraction is extracted from a condensation column; step S3: after dehydration is finished, cooling to room temperature, adding chloroethylene carbonate with the molar weight of 0.9-0.98 times of that of potassium fluoride, heating to 50-60 ℃, reacting for 3-5 hours under the stirring condition, then sampling and detecting the content of chloroethylene carbonate, and finishing the reaction when the content of chloroethylene carbonate is less than 1%; the invention reduces the synthesis yield reduction of the fluoroethylene carbonate caused by moisture absorption and caking of the high-activity potassium fluoride, and reduces the synthesis cost.
Description
Technical Field
The invention relates to the technical field of fluoroethylene carbonate synthesis, in particular to a method for improving the stability of yield of fluoroethylene carbonate.
Background
Fluoroethylene carbonate (FEC) is a fluorine-containing lithium battery additive, has good SEI film property, can form a compact structure layer without increasing the overall impedance, can inhibit the further decomposition of the electrolyte, improves the low-temperature cycle performance of the electrolyte, and is an excellent electrolyte additive.
In the prior art, the published "review on the synthesis of fluoroethylene carbonate" analyzes the synthesis method of fluoroethylene carbonate, and there are two main methods for its preparation: the direct fluorination method is a one-step synthesis method under the conditions of high temperature and high pressure by taking fluorine gas, nitrogen and vinyl carbonate as raw materials, but after fluoroethylene carbonate is generated, the fluorine gas further reacts with the fluoroethylene carbonate to generate polyfluorinated vinyl carbonate, so that a large number of byproducts are generated, the reaction is difficult to control, the requirement on equipment is high, the process conditions are harsh, and the industrial large-scale application is difficult; secondly, a halogen exchange method, namely, performing chlorination reaction on ethylene carbonate to generate chlorinated ethylene carbonate, and then performing halogen substitution reaction on the chlorinated ethylene carbonate and a fluorinating reagent in the presence of an aprotic solvent to synthesize fluoroethylene carbonate. Among them, KF is used as a fluorinating agent, and substitution reaction is carried out in the presence of an aprotic solvent such as acetone, dimethyl carbonate, diethyl carbonate, etc. as a method most commonly used in the industry at present.
Normally, a fluorinating reagent needs to select high-activity potassium fluoride, but the high-activity potassium fluoride is very easy to absorb moisture, once the moisture is high and KF is caked, the product yield is reduced by 20-50%, and in severe cases, no product exists and only shutdown is needed, so that the solution of potassium fluoride dispersibility is very important for the yield of fluoroethylene carbonate.
Therefore, the improvement is made by those skilled in the relevant technical field, for example, chinese patent application No. CN102977070, proposes "a method for preparing a potassium fluoride solid dispersion by using a solid dispersion technology", in order to solve the problem of potassium fluoride moisture absorption and agglomeration, potassium fluoride and its tiny crystal grains are present on the surface of the silica gel micropowder to improve the activity of potassium fluoride. However, potassium chloride is generated on the surface of the micro-powder silica gel after the reaction is finished, and simultaneously, part of unreacted potassium fluoride exists and exists in a solid waste form, so that the potassium fluoride is difficult to treat, and the silica gel loaded potassium fluoride increases the raw material cost.
Therefore, a method for improving the yield stability of fluoroethylene carbonate is provided.
Disclosure of Invention
The invention aims to overcome the problems in the prior art, provides a method for improving the stability of the yield of fluoroethylene carbonate, optimizes the synthesis process of fluoroethylene carbonate, solves the problem of reduced yield of fluoroethylene carbonate caused by moisture absorption and caking of high-activity potassium fluoride in the process of synthesizing fluoroethylene carbonate by adopting high-activity potassium fluoride, solves the problem that potassium chloride cannot be treated in the prior art, improves the synthesis yield of fluoroethylene carbonate, and reduces the synthesis cost.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a method for improving the yield stability of fluoroethylene carbonate comprises the following steps:
step S1: adding high-activity potassium fluoride and an aprotic solvent into a three-neck flask together, and performing ultrasonic treatment for 30-60 minutes by using ultrasonic waves to uniformly disperse the high-activity potassium fluoride;
step S2: heating the potassium fluoride solution uniformly dispersed by ultrasonic to 100-110 ℃, and evaporating and dehydrating under the stirring condition until no fraction is extracted from a condensation column;
step S3: after dehydration is finished, cooling to room temperature, adding chloroethylene carbonate with the molar weight of 0.9-0.98 times of that of potassium fluoride, heating to 50-60 ℃, reacting for 3-5 hours under the stirring condition, then sampling and detecting the content of chloroethylene carbonate, and finishing the reaction when the content of chloroethylene carbonate is less than 1%;
step S4: filtering the reaction liquid after the reaction is finished, putting filter residues which mainly comprise potassium fluoride, potassium chloride and partial organic matters into a muffle furnace for sintering, adding water until salt is completely dissolved after the organic matters are removed, wherein the solubility of the potassium fluoride in water is 0.923g/ml at the temperature of 18 ℃, the solubility of the potassium chloride in water is 0.35g/ml at the temperature of 18 ℃, recrystallizing to obtain qualified potassium chloride salt by utilizing the different solubilities of the potassium fluoride and the potassium chloride in water, and drying the mixture of the residual potassium fluoride and the potassium chloride to be used as a raw material for synthesizing fluoroethylene carbonate again;
step S5: the filtrate mainly comprises an aprotic solvent, fluoroethylene carbonate, a side reaction product and part of impurities, and the method comprises the steps of firstly carrying out reduced pressure distillation, controlling the distillation temperature, and steaming out the aprotic solvent to obtain fluoroethylene carbonate with the purity of more than 90%;
step S6: the fluoroethylene carbonate with the purity of more than 90 percent enters a rectifying column for rectification, and a fluoroethylene carbonate product with the purity of more than 98 percent is collected from the top of the tower in an intermittent rectification mode;
step S7: the fluoroethylene carbonate product with the purity of more than 98 percent enters a melt crystallizer to be crystallized, and the electronic grade fluoroethylene carbonate product with the purity of more than 99.99 percent can be obtained.
Preferably, in step S1, the aprotic solvent is one or more of carbon tetrachloride, acetone, N-N dimethylformamide, dimethyl carbonate, and diethyl carbonate.
Preferably, in step S1, the high-activity potassium fluoride is commercially available high-activity potassium fluoride, and the effect of potassium fluoride on the reaction under different water contents is simulated, and the result shows that the high-activity potassium fluoride used has a water content of 0.1% to 10% and the reaction maintains a good yield, and the yield fluctuation is less than 1%.
Preferably, in step S2, the evaporation dehydration is performed by using a common distillation apparatus, the heating is performed by using an oil bath, and the temperature of the heat transfer oil is controlled between 120 ℃ and 150 ℃.
Preferably, in step S3, the chlorinated ethylene carbonate has a purity of > 80%, preferably a purity of > 90%.
Preferably, in step S4, the chloroethylene carbonate conversion rate is > 99%, the fluoroethylene carbonate selectivity in the product is > 90%, and the overall product yield is > 75%.
Compared with the prior art, the invention has the following beneficial effects:
the invention has reasonable structural design, optimizes the synthesis process of fluoroethylene carbonate, and ensures that potassium fluoride is more uniformly dispersed in a solvent by adopting an ultrasonic dispersion mode in the process of synthesizing fluoroethylene carbonate by adopting high-activity potassium fluoride, thereby reaching the molecular level, increasing the specific surface area of potassium fluoride in the reaction process and improving the yield of the whole reaction; meanwhile, a dehydration process is added before the reaction, so that the problem of potassium fluoride water absorption and agglomeration is further avoided, the requirement on the water content of the raw material potassium fluoride is lowered, and the stability of the reaction yield can be ensured under different water content conditions; and a post-treatment mode is added, and a mixture of potassium fluoride and potassium chloride as byproducts is recycled, so that the reaction cost is reduced.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a block diagram of the electronic level FEC synthesis process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a method for improving the stability of fluoroethylene carbonate yield comprises the following steps:
step S1: adding high-activity potassium fluoride and an aprotic solvent into a three-neck flask together, and performing ultrasonic treatment for 30-60 minutes by using ultrasonic waves to uniformly disperse the high-activity potassium fluoride;
the high-activity potassium fluoride is high-activity potassium fluoride sold in the market, and the influence of the potassium fluoride on the reaction under different water contents is simulated, and the result shows that the adopted high-activity potassium fluoride has the water content of 0.1-10 percent, the reaction keeps good yield, and the yield fluctuation is less than 1 percent;
the aprotic solvent is one or more of carbon tetrachloride, acetone, N-N dimethylformamide, dimethyl carbonate and diethyl carbonate;
step S2: heating the potassium fluoride solution uniformly dispersed by ultrasonic to 100-110 ℃, and evaporating and dehydrating under the stirring condition until no fraction is extracted from a condensation column;
the evaporation and dehydration adopt a common distillation device, the heating adopts oil bath heating, and the temperature of heat conducting oil is controlled between 120 ℃ and 150 ℃;
step S3: after dehydration, cooling to room temperature, adding chloroethylene carbonate with the molar weight of potassium fluoride being 0.9-0.98 times, wherein the purity of the chloroethylene carbonate is more than 80%, preferably more than 90%, heating to 50-60 ℃, reacting for 3-5 hours under the stirring condition, sampling and detecting the content of the chloroethylene carbonate, and finishing the reaction when the content of the chloroethylene carbonate is less than 1%;
step S4: filtering the reaction liquid after the reaction is finished, putting filter residues which mainly comprise potassium fluoride, potassium chloride and partial organic matters into a muffle furnace for sintering, adding water until salt is completely dissolved after the organic matters are removed, wherein the solubility of the potassium fluoride in water is 0.923g/ml at the temperature of 18 ℃, the solubility of the potassium chloride in water is 0.35g/ml at the temperature of 18 ℃, recrystallizing to obtain qualified potassium chloride salt by utilizing the different solubilities of the potassium fluoride and the potassium chloride in water, and drying the mixture of the residual potassium fluoride and the potassium chloride to be used as a raw material for synthesizing fluoroethylene carbonate again;
the conversion rate of the chlorinated ethylene carbonate is more than 99 percent, the selectivity of the fluorinated ethylene carbonate in the product is more than 90 percent, and the overall product yield is more than 75 percent;
step S5: the filtrate mainly comprises an aprotic solvent, fluoroethylene carbonate, a side reaction product and part of impurities, and the method comprises the steps of firstly carrying out reduced pressure distillation, controlling the distillation temperature, and steaming out the aprotic solvent to obtain fluoroethylene carbonate with the purity of more than 90%;
step S6: the fluoroethylene carbonate with the purity of more than 90 percent enters a rectifying column for rectification, and a fluoroethylene carbonate product with the purity of more than 98 percent is collected from the top of the tower in an intermittent rectification mode;
step S7: the fluoroethylene carbonate product with the purity of more than 98 percent enters a melt crystallizer to be crystallized, and the electronic grade fluoroethylene carbonate product with the purity of more than 99.99 percent can be obtained.
The chemical reaction equation of the invention is as follows:
example 1
Step S1: adding 145g of high-activity potassium fluoride (containing 10 percent of water) and 900g of dimethyl carbonate into a three-neck flask together, and uniformly dispersing the high-activity potassium fluoride by adopting ultrasonic waves for 60 minutes;
step S2: a distillation device is set up, the temperature of the heat-conducting oil is controlled to be 130-150 ℃, and evaporation dehydration is carried out under the condition of stirring rotation speed of 200r/s until no fraction is extracted from a condensation column;
step S3: after dehydration, cooling to room temperature, adding 280g of chloroethylene carbonate (with the content of 95%), controlling the reaction temperature to be 50-60 ℃, after reacting for 4 hours under the stirring condition, sampling and detecting the content of chloroethylene carbonate, detecting that the content of chloroethylene carbonate is 0.6%, and stopping reaction;
step S4: carrying out suction filtration on the reaction liquid, placing filter residues into a muffle furnace for sintering to obtain 170g of mixed salt, adding 1kg of deionized water to heat and dissolve the mixed salt, then carrying out recrystallization by utilizing the different solubility of potassium fluoride and potassium chloride in water to obtain qualified potassium chloride salt, and drying the remaining mixture of potassium fluoride and potassium chloride to obtain a mixture of 50% potassium chloride and 50% potassium fluoride;
step S5: carrying out reduced pressure distillation on the filtrate, controlling the vacuum degree to be 5kPa and the temperature of heat conducting oil to be 60-80 ℃, evaporating a dimethyl carbonate solvent, and detecting that the purity of the dimethyl carbonate solvent is 99.7 percent and the purity of kettle residual liquid is 94 percent and the mass is 227 g;
step S6: adding the residual liquid in a tower kettle of a rectifying device, wherein the rectifying device adopts negative pressure rectification, the vacuum degree is 2kPa, the tower kettle adopts heat conducting oil for heating, the temperature of the tower kettle is controlled to be 80-110 ℃, the rectifying device adopts a rectifying column with the specification of phi 25 x 5 x 2700mm, the reflux ratio of the tower top is controlled to be 5:1, and 198g of fluoroethylene carbonate products with the purity of more than 98 percent are collected from the tower top in an accumulated manner;
step S7: the fluoroethylene carbonate product with the purity of more than 98 percent enters a melting crystallizer for crystallization to obtain 186g of electronic-grade fluoroethylene carbonate, the mother liquor returns to a rectifying device for recycling, and the overall yield is 81 percent.
Example 2
Step S1: adding 150g of high-activity potassium fluoride (containing 5 percent of water) and 910g of dimethyl carbonate into a three-neck flask together, and uniformly dispersing the high-activity potassium fluoride by adopting ultrasonic waves for 60 minutes;
step S2: a distillation device is set up, the temperature of the heat-conducting oil is controlled to be 130-150 ℃, and evaporation dehydration is carried out under the condition of stirring rotation speed of 200r/s until no fraction is extracted from a condensation column;
step S3: after dehydration, cooling to room temperature, adding 300g of chloroethylene carbonate (with the content of 95%), controlling the reaction temperature to be 50-60 ℃, after reacting for 4 hours under the stirring condition, sampling and detecting the content of chloroethylene carbonate, detecting the content of chloroethylene carbonate to be 0.4%, and stopping reaction;
step S4: carrying out suction filtration on the reaction liquid, putting filter residues into a muffle furnace for sintering to obtain 182g of mixed salt, adding 210kg of deionized water into the mixed salt to heat and dissolve the mixed salt, then carrying out recrystallization by utilizing the different solubility of potassium fluoride and potassium chloride in water to obtain qualified potassium chloride salt, and drying the remaining potassium fluoride and potassium chloride mixture to obtain a potassium chloride and potassium fluoride mixture;
step S5: carrying out reduced pressure distillation on the filtrate, controlling the vacuum degree to be 5kPa and the temperature of heat transfer oil to be 60-80 ℃, evaporating a dimethyl carbonate solvent, and detecting that the purity of the dimethyl carbonate solvent is 99.7 percent and the purity of kettle residual liquid is 93 percent and the mass is 231 g;
step S6: adding the residual liquid in a tower kettle of a rectifying device, wherein the rectifying device adopts negative pressure rectification, the vacuum degree is 2kPa, the tower kettle adopts heat conducting oil for heating, the temperature of the tower kettle is controlled to be 80-110 ℃, the rectifying device adopts a rectifying column with the specification of phi 25 x 5 x 2700mm, the reflux ratio of the tower top is controlled to be 5:1, and 201g of fluoroethylene carbonate products with the purity of more than 98 percent are collected from the tower top in an accumulated manner;
step S7: the fluoroethylene carbonate product with the purity of more than 98 percent enters a melting crystallizer for crystallization to obtain 193g of electronic-grade fluoroethylene carbonate, and the mother liquor returns to a rectifying device for recycling, so that the overall yield is 81.4 percent.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. A method for improving the yield stability of fluoroethylene carbonate is characterized in that: the method comprises the following steps:
step S1: adding high-activity potassium fluoride and an aprotic solvent into a three-neck flask together, and performing ultrasonic treatment for 30-60 minutes by using ultrasonic waves to uniformly disperse the high-activity potassium fluoride;
step S2: heating the potassium fluoride solution uniformly dispersed by ultrasonic to 100-110 ℃, and evaporating and dehydrating under the stirring condition until no fraction is extracted from a condensation column;
step S3: after dehydration is finished, cooling to room temperature, adding chloroethylene carbonate with the molar weight of 0.9-0.98 times of that of potassium fluoride, heating to 50-60 ℃, reacting for 3-5 hours under the stirring condition, then sampling and detecting the content of chloroethylene carbonate, and finishing the reaction when the content of chloroethylene carbonate is less than 1%;
step S4: filtering the reaction liquid after the reaction is finished, putting filter residues which mainly comprise potassium fluoride, potassium chloride and partial organic matters into a muffle furnace for sintering, adding water until salt is completely dissolved after the organic matters are removed, wherein the solubility of the potassium fluoride in water is 0.923g/ml at the temperature of 18 ℃, the solubility of the potassium chloride in water is 0.35g/ml at the temperature of 18 ℃, recrystallizing to obtain qualified potassium chloride salt by utilizing the different solubilities of the potassium fluoride and the potassium chloride in water, and drying the mixture of the residual potassium fluoride and the potassium chloride to be used as a raw material for synthesizing fluoroethylene carbonate again;
step S5: the filtrate mainly comprises an aprotic solvent, fluoroethylene carbonate, a side reaction product and part of impurities, and the method comprises the steps of firstly carrying out reduced pressure distillation, controlling the distillation temperature, and steaming out the aprotic solvent to obtain fluoroethylene carbonate with the purity of more than 90%;
step S6: the fluoroethylene carbonate with the purity of more than 90 percent enters a rectifying column for rectification, and a fluoroethylene carbonate product with the purity of more than 98 percent is collected from the top of the tower in an intermittent rectification mode;
step S7: the fluoroethylene carbonate product with the purity of more than 98 percent enters a melt crystallizer to be crystallized, and the electronic grade fluoroethylene carbonate product with the purity of more than 99.99 percent can be obtained.
2. The method for improving the yield stability of fluoroethylene carbonate according to claim 1, wherein: in step S1, the aprotic solvent is one or more of carbon tetrachloride, acetone, N-N dimethylformamide, dimethyl carbonate, and diethyl carbonate.
3. The method for improving the yield stability of fluoroethylene carbonate according to claim 1, wherein: in step S1, the high-activity potassium fluoride is commercially available and simulates the effect of potassium fluoride on the reaction under different water contents, and the result shows that the reaction with 0.1% to 10% of water content of the high-activity potassium fluoride has a good yield, and the yield fluctuation is less than 1%.
4. The method for improving the yield stability of fluoroethylene carbonate according to claim 1, wherein: in step S2, the evaporation dehydration is performed by using a common distillation device, the heating is performed by using an oil bath, and the temperature of the heat conducting oil is controlled between 120 ℃ and 150 ℃.
5. The method for improving the yield stability of fluoroethylene carbonate according to claim 1, wherein: in step S3, the chlorinated ethylene carbonate has a purity of > 80%, preferably > 90%.
6. The method for improving the yield stability of fluoroethylene carbonate according to claim 1, wherein: in step S4, the conversion rate of the chlorinated ethylene carbonate is more than 99%, the selectivity of the fluorinated ethylene carbonate in the product is more than 90%, and the overall product yield is more than 75%.
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| CN114621178A (en) * | 2022-03-23 | 2022-06-14 | 内蒙古源宏精细化工有限公司 | Preparation process of fluoroethylene carbonate |
| CN114716403A (en) * | 2022-05-11 | 2022-07-08 | 多氟多新材料股份有限公司 | Synthetic method of fluoroethylene carbonate |
| CN114957195A (en) * | 2022-06-23 | 2022-08-30 | 中国五环工程有限公司 | Preparation method of fluoroethylene carbonate with high yield |
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| CN114957195B (en) * | 2022-06-23 | 2023-12-01 | 中国五环工程有限公司 | Preparation method of high-yield fluoroethylene carbonate |
| CN115353123A (en) * | 2022-08-16 | 2022-11-18 | 珠海正杏新材料科技有限公司 | Method for recovering potassium fluoride |
| CN115353123B (en) * | 2022-08-16 | 2023-12-05 | 珠海正杏新材料科技有限公司 | Recovery method of potassium fluoride |
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