CN115477633A - Preparation method of fluoroethylene carbonate - Google Patents

Preparation method of fluoroethylene carbonate Download PDF

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CN115477633A
CN115477633A CN202211256236.2A CN202211256236A CN115477633A CN 115477633 A CN115477633 A CN 115477633A CN 202211256236 A CN202211256236 A CN 202211256236A CN 115477633 A CN115477633 A CN 115477633A
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carbonate
reaction
fluoroethylene carbonate
chloroethylene
preparing
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曾德荣
叶翠花
杨秋转
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Zhuhai Baichuan Petrochemical Engineering Design Co ltd
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Zhuhai Baichuan Petrochemical Engineering Design Co ltd
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0025—Organic electrolyte
    • 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 preparation method of fluoroethylene carbonate, and relates to the technical field of chemical material preparation. The method comprises the steps of 1, preparing an intermediate product of chloroethylene carbonate, 2, generating fluoroethylene carbonate under the action of polyethylene glycol, and 3, obtaining fluoroethylene carbonate crystals through centrifugal drying, reduced pressure rectification and crystallization. According to the invention, when the water content in the chlorination reaction is more than 800ppm, initiators of azodiisobutyronitrile and thionyl chloride are added in time, so that the conversion rate of the reaction is improved, and the reaction is subjected to acid removal after the reaction, so that the influence of an acid value on the reaction is further reduced, and the conversion rate of the subsequent fluorination reaction is improved.

Description

Preparation method of fluoroethylene carbonate
Technical Field
The invention relates to the technical field of chemical material preparation, and particularly relates to a preparation method of fluoroethylene carbonate.
Background
With the rapid development of lithium ion battery technology at home and abroad, lithium ion batteries have become an indispensable important product in daily life, but the performance requirements of people on battery performance are continuously improved, electrolyte is used as one of important materials of the lithium ion batteries, and fluoroethylene carbonate is an important lithium battery electrolyte additive, namely fluoroethylene carbonate with higher purity is required in the lithium ion battery industry.
The domestic synthetic methods of fluoroethylene carbonate mainly comprise two methods: (1) direct fluorination method and (2) halogen exchange method. The direct fluorination method adopts fluorine gas to directly react, fluorine has high toxicity and high activity, the reaction process is difficult to control, a plurality of byproducts are generated, the requirement on equipment is high, the process condition is harsh, and the reaction yield is low. The halogen exchange method is characterized in that a chlorination reagent and ethylene carbonate firstly carry out chlorination reaction to produce chlorinated ethylene carbonate and a fluorination reagent carries out fluorination reaction to synthesize fluoroethylene carbonate, the method needs to strictly control the moisture content, and if no catalyst is used, the reaction time is too long, and the product is easy to decompose.
In the prior art patent: the fluorination reaction has more side reactions, the purity of the product is difficult to reach the standard, subsequent treatment is needed, the production cost is increased, an initiator and a catalyst are also needed to be added in the reaction process to improve the reaction efficiency, and the difficulty in improving the purity for subsequent rectification is also increased, so that the fluoroethylene carbonate preparation method is needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of fluoroethylene carbonate, which comprises the following steps,
step 1: adding ethylene carbonate into a chlorination kettle, introducing liquid chlorine, and irradiating under the action of ultraviolet lamp light and an initiator to prepare chlorinated ethylene carbonate;
step 2: deacidifying the chloroethylene carbonate prepared in the step 1, dropwise adding the treated chloroethylene carbonate solution into a fluorination kettle, mixing the solution with potassium fluoride and acetonitrile solution, and generating fluoroethylene carbonate under the action of polyethylene glycol;
and step 3: and (3) carrying out centrifugal drying, reduced pressure rectification and crystallization on the fluoroethylene carbonate prepared by the reaction in the step (2) to obtain fluoroethylene carbonate crystals.
Furthermore, in the step 1, the purity of the ethylene carbonate is more than 99.5 percent, and the water content is less than or equal to 80ppm.
Further, in the step 1, the purity of the liquid chlorine is more than 99.6 percent, and the water content is less than or equal to 400ppm.
Further, in the step 1, the mass ratio of the ethylene carbonate to the chlorine gas is 1:1.1 to 1.3, the reaction temperature of the substitution reaction is 80 ℃, and the reaction time is 12 to 14 hours.
Further, in the step 1, the initiator comprises azobisisobutyronitrile and thionyl chloride, wherein the azobisisobutyronitrile solute and the thionyl chloride are used as solvents, and the mass ratio of the azodiisobutyronitrile to the thionyl chloride is 1;
and (2) dropwise adding azodiisobutyronitrile and thionyl chloride when the water content in the chlorination kettle in the step (1) is more than 800 ppm.
Further, in the step 2, the deacidification treatment is nitrogen purging deacidification, and the pH value of the chlorinated ethylene carbonate solution after deacidification is more than or equal to 5.
Further, in the step 2, the mass ratio of the chloroethylene carbonate to the potassium fluoride is 1.7-0.9, the mass ratio of the chloroethylene carbonate to the acetonitrile is 1.1-1.3, the mass ratio of the chloroethylene carbonate to the polyethylene glycol is 1.03-0.05, the reaction temperature of the substitution reaction is 50 ℃, and the reaction time is 12 hours.
Further, in the step 3, the rectification under reduced pressure comprises FEC coarse purification and FEC purification, wherein the FEC coarse purification sequentially separates out acetonitrile, a byproduct vinylene carbonate and unreacted vinylene carbonate; the FEC refining sequentially separates unreacted ethylene carbonate and vinylene carbonate as a byproduct.
Furthermore, quartz tubes are arranged in the chlorination kettles, and high-pressure mercury lamps are arranged in the quartz tubes.
The invention has the following beneficial effects:
1. according to the invention, the water content in the chlorination reaction is more than 800ppm, and the initiators of azodiisobutyronitrile and thionyl chloride are added in time, so that the conversion rate of the reaction is improved. And the acid is removed after the reaction, so that the influence of the fluoroethylene carbonate acid value on the reaction is further reduced, and the conversion rate of the subsequent fluorination reaction is improved.
2. The invention strictly controls the reaction temperature of the fluorination reaction to be about 50 ℃, reduces the generation of side reactions, improves the conversion rate of the reaction and ensures the yield of products.
3. According to the invention, solid-liquid separation is carried out in time after the fluorination reaction, and byproducts generated by the reaction are removed outside the system, so that the complication of the intermediate process is avoided, and the purity and yield of the product are improved.
4. According to the invention, after acetonitrile is separated by primary rectification, deacidification is carried out to reduce the acid value of the system and improve the product purity.
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 schematic view of the preparation process of the present invention.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description. The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to practitioners skilled in this art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
The invention relates to a preparation method of fluoroethylene carbonate.A chlorination kettle is internally provided with quartz tubes which are internally provided with a high-pressure mercury lamp.
Example 1
Step 1: adding ethylene carbonate with the purity of more than 99.5 percent and the water content of less than or equal to 80ppm into a chlorination kettle, and introducing liquid chlorine with the purity of more than 99.6 percent and the water content of less than or equal to 400ppm, wherein the mass ratio of the ethylene carbonate to the chlorine is 1:1.1, under the irradiation of ultraviolet lamp light and the action of an initiator, the initiator comprises azobisisobutyronitrile and thionyl chloride, wherein azodiisobutyronitrile solute and the thionyl chloride are used as solvents, the mass ratio of the azodiisobutyronitrile to the thionyl chloride is 1/10, the water content in a chlorination kettle is more than 800ppm, the azodiisobutyronitrile and the thionyl chloride are dripped, a substitution reaction is carried out to prepare chloroethylene carbonate, the reaction temperature of the substitution reaction is 80 ℃, and the reaction time is 12 hours;
and 2, step: deacidifying the chloroethylene carbonate prepared in the step 1, wherein the deacidification treatment is nitrogen purging deacidification, the pH of the deacidified chloroethylene carbonate solution is more than or equal to 5, the treated chloroethylene carbonate solution is dripped into a fluorination kettle and is mixed with anhydrous acetonitrile solution with the purity of more than or equal to 99.0%, the water content of less than or equal to 0.2% and the water content of less than or equal to 0.05%;
wherein the mass ratio of the chloroethylene carbonate to the potassium fluoride is 1.7, the mass ratio of the chloroethylene carbonate to the acetonitrile is 1.1, the mass ratio of the chloroethylene carbonate to the polyethylene glycol is 1;
generating fluoroethylene carbonate under the action of polyethylene glycol;
and 3, step 3: carrying out centrifugal drying, reduced pressure rectification and crystallization on the fluoroethylene carbonate prepared by the reaction in the step 2 to obtain fluoroethylene carbonate crystals;
the rectification under reduced pressure comprises FEC coarse refining and FEC refining, wherein the FEC coarse refining sequentially separates acetonitrile, a byproduct vinylene carbonate and unreacted vinylene carbonate; FEC refining sequentially separates unreacted ethylene carbonate and vinylene carbonate as a byproduct;
after separating acetonitrile by FEC coarse refining, feeding the coarse fluoroethylene carbonate solution into an acid remover, and adding sodium bicarbonate to remove acid;
after FEC coarse refining, carrying out crystallization operation, adding MTBE into a crystallization kettle, mixing with coarse fluoroethylene carbonate, cooling to separate out fluoroethylene carbonate, carrying out heating melting to carry out secondary crystallization after primary crystallization is finished, and carrying out FEC refining after secondary crystallization is finished;
the purity of the fluoroethylene carbonate prepared in the embodiment is 98.99 percent through detection.
Example 2
Step 1: adding ethylene carbonate with the purity of more than 99.5 percent and the water content of less than or equal to 80ppm into a chlorination kettle, and introducing liquid chlorine with the purity of more than 99.6 percent and the water content of less than or equal to 400ppm, wherein the mass ratio of the ethylene carbonate to the chlorine is 1:1.2, under the irradiation of ultraviolet light and the action of an initiator, the initiator comprises azobisisobutyronitrile and thionyl chloride, wherein azodiisobutyronitrile solute and the thionyl chloride are used as solvents, the mass ratio of the azodiisobutyronitrile to the thionyl chloride is 1/10, the water content in a chlorination kettle is more than 800ppm, the azodiisobutyronitrile and the thionyl chloride are dripped, a substitution reaction is carried out to prepare chloroethylene carbonate, the reaction temperature of the substitution reaction is 80 ℃, and the reaction time is 12 hours;
and 2, step: deacidifying the chloroethylene carbonate prepared in the step 1, wherein the deacidifying treatment is nitrogen purging deacidification, the PH of a chloroethylene carbonate solution after deacidification is more than or equal to 5, and the treated chloroethylene carbonate solution is dropwise added into a fluorination kettle and mixed with an anhydrous acetonitrile solution with the purity of more than or equal to 99.0%, the water content of less than or equal to 0.2% and the water content of less than or equal to 0.05%;
wherein the mass ratio of the chloroethylene carbonate to the potassium fluoride is 1.8, the mass ratio of the chloroethylene carbonate to the acetonitrile is 1.2, the mass ratio of the chloroethylene carbonate to the polyethylene glycol is 1;
generating fluoroethylene carbonate under the action of polyethylene glycol;
and step 3: carrying out centrifugal drying, reduced pressure rectification and crystallization on the fluoroethylene carbonate prepared by the reaction in the step 2 to obtain fluoroethylene carbonate crystals;
the rectification under reduced pressure comprises FEC coarse refining and FEC refining, wherein the FEC coarse refining sequentially separates acetonitrile, a byproduct vinylene carbonate and unreacted vinylene carbonate; FEC refining sequentially separates unreacted ethylene carbonate and vinylene carbonate as a byproduct;
after separating acetonitrile by FEC coarse refining, feeding the coarse fluoroethylene carbonate solution into an acid remover, and adding sodium bicarbonate to remove acid;
after FEC coarse refining, carrying out crystallization operation, adding MTBE into a crystallization kettle, mixing with coarse fluoroethylene carbonate, cooling to separate out fluoroethylene carbonate, carrying out heating melting to carry out secondary crystallization after primary crystallization is finished, and carrying out FEC refining after secondary crystallization is finished;
the purity of the fluoroethylene carbonate prepared in the example is 99.99 percent through detection.
Example 3
Step 1: adding ethylene carbonate with the purity of more than 99.5 percent and the water content of less than or equal to 80ppm into a chlorination kettle, and introducing liquid chlorine with the purity of more than 99.6 percent and the water content of less than or equal to 400ppm, wherein the mass ratio of the ethylene carbonate to the chlorine is 1:1.3, under the irradiation of ultraviolet light and the action of an initiator, the initiator comprises azobisisobutyronitrile and thionyl chloride, wherein azobisisobutyronitrile solute and thionyl chloride are used as solvents, the mass ratio of the azobisisobutyronitrile to the thionyl chloride is 1, the water content in a chlorination kettle is more than 800ppm, the azobisisobutyronitrile and the thionyl chloride are dripped, the substitution reaction is carried out to prepare chloroethylene carbonate, the reaction temperature of the substitution reaction is 80 ℃, and the reaction time is 12 hours;
step 2: deacidifying the chloroethylene carbonate prepared in the step 1, wherein the deacidification treatment is nitrogen purging deacidification, the pH of the deacidified chloroethylene carbonate solution is more than or equal to 5, the treated chloroethylene carbonate solution is dripped into a fluorination kettle and is mixed with anhydrous acetonitrile solution with the purity of more than or equal to 99.0%, the water content of less than or equal to 0.2% and the water content of less than or equal to 0.05%;
wherein the mass ratio of the chloroethylene carbonate to the potassium fluoride is 1.9, the mass ratio of the chloroethylene carbonate to the acetonitrile is 1.3, the mass ratio of the chloroethylene carbonate to the polyethylene glycol is 1;
generating fluoroethylene carbonate under the action of polyethylene glycol;
and 3, step 3: carrying out centrifugal drying, reduced pressure rectification and crystallization on the fluoroethylene carbonate prepared by the reaction in the step 2 to obtain fluoroethylene carbonate crystals;
the rectification under reduced pressure comprises FEC coarse refining and FEC refining, wherein the FEC coarse refining sequentially separates acetonitrile, a byproduct vinylene carbonate and unreacted vinylene carbonate; FEC refining sequentially separates unreacted ethylene carbonate and vinylene carbonate as a byproduct;
after separating acetonitrile by FEC coarse refining, feeding the coarse fluoroethylene carbonate solution into a deacidification device, and adding sodium bicarbonate to remove acid;
after FEC coarse refining, carrying out crystallization operation, adding MTBE into a crystallization kettle, mixing with coarse fluoroethylene carbonate, cooling to separate out fluoroethylene carbonate, carrying out heating melting to carry out secondary crystallization after primary crystallization is finished, and carrying out FEC refining after secondary crystallization is finished;
the fluoroethylene carbonate prepared in the embodiment has the purity of 99.06 percent through detection.
In conclusion, it can be seen from the data of comparative examples 1 to 3 that the mass ratio of ethylene carbonate to chlorine gas is 1:1.2, the mass ratio of the chloroethylene carbonate to the potassium fluoride is 1.
The water content in the chlorination reaction is more than 800ppm, and initiators of azodiisobutyronitrile and thionyl chloride are added in time, so that the conversion rate of the reaction is improved. The acid is removed after the reaction, so that the influence of the fluoroethylene carbonate acid value on the reaction is further reduced, and the conversion rate of the subsequent fluorination reaction is improved;
the reaction temperature of the fluorination reaction is strictly controlled to be about 50 ℃, so that the generation of side reactions is reduced, the conversion rate of the reaction is improved, and the yield of the product is ensured;
after the fluorination reaction, the solid-liquid separation is carried out in time, and by-products generated by the reaction are removed from the system, so that the complication of the intermediate process is avoided, and the purity and the yield of the product are improved;
the high-purity fluoroethylene carbonate is generated, can be used as a lithium battery additive to form a compact Solid Electrolyte Interface (SEI) film, so that the possibility of decomposition of the electrolyte is reduced, the charge and discharge performance of the lithium battery is improved, and the high and low temperature performance of the lithium battery electrolyte is improved.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by one of ordinary skill in the art and related arts based on the embodiments of the present invention without any creative effort, shall fall within the protection scope of the present invention. Structures, devices, and methods of operation not specifically described or illustrated herein are generally practiced in the art without specific recitation or limitation.

Claims (9)

1. The preparation method of fluoroethylene carbonate is characterized by comprising the following steps:
step 1: adding ethylene carbonate into a chlorination kettle, introducing liquid chlorine, and preparing chlorinated ethylene carbonate under the irradiation of ultraviolet lamp light and the action of an initiator;
step 2: deacidifying the chloroethylene carbonate prepared in the step 1, dropwise adding the treated chloroethylene carbonate solution into a fluorination kettle, mixing the solution with potassium fluoride and acetonitrile solution, and generating fluoroethylene carbonate under the action of polyethylene glycol;
and step 3: and (3) carrying out centrifugal drying, reduced pressure rectification and crystallization on the fluoroethylene carbonate prepared by the reaction in the step (2) to obtain the fluoroethylene carbonate.
2. The method for preparing fluoroethylene carbonate according to claim 1, wherein in step 1, the purity of ethylene carbonate is more than 99.5%, and the water content is less than or equal to 80ppm.
3. The method for preparing fluoroethylene carbonate according to claim 1, wherein in step 1, the purity of liquid chlorine is greater than 99.6%, and the water content is less than or equal to 400ppm.
4. The method for preparing fluoroethylene carbonate according to claim 1, wherein in the step 1, the mass ratio of ethylene carbonate to chlorine gas is 1:1.1 to 1.3, the reaction temperature of the substitution reaction is 80 ℃, and the reaction time is 12 to 14 hours.
5. The method for preparing fluoroethylene carbonate according to claim 1, wherein in step 1, the initiator comprises azobisisobutyronitrile and thionyl chloride, wherein the azobisisobutyronitrile solute and the thionyl chloride are used as solvents, and the mass ratio of the azobisisobutyronitrile to the thionyl chloride is 1;
and (3) beginning to dropwise add azodiisobutyronitrile and thionyl chloride when the water content in the chlorination kettle in the step (1) is more than 800 ppm.
6. The method for preparing fluoroethylene carbonate according to claim 1, wherein in the step 2, the deacidification treatment is nitrogen purging to remove acid, and the pH of the chloroethylene carbonate solution after the deacidification treatment is more than or equal to 5.
7. The method for preparing fluoroethylene carbonate according to claim 1, wherein in the step 2, the mass ratio of chloroethylene carbonate to potassium fluoride is 1.7-0.9, the mass ratio of chloroethylene carbonate to acetonitrile is 1.1-1.3, the mass ratio of chloroethylene carbonate to polyethylene glycol is 1.
8. The method for preparing fluoroethylene carbonate according to claim 1, wherein in the step 3, the vacuum rectification comprises an FEC coarse purification and an FEC purification, and the FEC coarse purification sequentially separates out acetonitrile, vinylene carbonate as a byproduct and unreacted vinylene carbonate; the FEC refining sequentially separates unreacted ethylene carbonate and vinylene carbonate as a byproduct.
9. The method for preparing fluoroethylene carbonate according to claim 1, wherein the chlorination reactor is provided with a quartz tube, and the quartz tube is provided with a high-pressure mercury lamp.
CN202211256236.2A 2022-10-14 2022-10-14 Preparation method of fluoroethylene carbonate Pending CN115477633A (en)

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