CN115353504A - Ultrapure fluoroethylene carbonate and preparation method thereof - Google Patents
Ultrapure fluoroethylene carbonate and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of chemical synthesis, in particular to ultrapure fluoroethylene carbonate and a preparation method thereof, which comprises the following steps: chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate; and (3) fluorination reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate; solid-liquid separation and purification: the fluoro reaction product is subjected to solid-liquid separation to obtain solid mixed salt and liquid, and the liquid is purified to obtain the fluoroethylene carbonate; the invention synthesizes fluoroethylene carbonate under the conditions of no solvent and no catalyst, fluorinates chloroethylene carbonate liquid by using a liquid fluorinating agent, has high local concentration of the fluorinating agent, is easy to react, and is easy to separate products.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, in particular to ultrapure fluoroethylene carbonate and a preparation method thereof.
Background
In recent years, with the high importance of various countries on environmental protection, the scale of the downstream industries such as the lithium battery industry and new energy automobiles is continuously enlarged, the requirements of the lithium battery on safety, cycle life and energy density are improved, and the demand of the electrolyte additive is increased year by year. The most used electrolyte is the conventional additives such as Vinylene Carbonate (VC), fluoroethylene carbonate (FEC) and Phenylsulfone (PS). The synthesis process of fluoroethylene carbonate (FEC) mainly uses Ethylene Carbonate (EC) as a raw material, and the current FEC synthesis route has the following methods, namely: the direct fluorine reaction method is to synthesize fluoroethylene carbonate by reacting Ethylene Carbonate (EC) with a mixed gas of fluorine and nitrogen. The synthetic route is shown as follows: the raw material used in the method is fluorine gas, the fluorine gas has high toxicity, high reaction activity and violent reaction heat release, the pressure in a reaction container is easily high, danger occurs, and the fluorine gas has strong corrosivity, so the method has high requirements on reaction equipment, high industrial danger and high implementation difficulty; the second method comprises the following steps: the halogen exchange reaction method uses Ethylene Carbonate (EC) as a raw material, chloridizes the EC with chlorine or other chlorinating reagents to generate monochlorethylene carbonate (CEC), and reacts with a fluorinating reagent after CEC purification to obtain a target product, namely fluoroethylene carbonate (FEC). The synthetic route is as follows: the method does not relate to toxic fluorine gas, the safety cost is greatly reduced, and the production process is easier to control. But because of two-step reaction, the total yield is lower, and the raw material investment is large; the third method comprises the following steps: the electrochemical fluorination method obtains fluoroethylene carbonate by anode fluorination of 4-substituted arylthio ethylene carbonate. The synthetic route is shown as follows: the method can be reacted under safe and relatively simple equipment conditions, but is still in the laboratory theoretical research stage. For example, the Chinese patent application with the application publication number CN102060839A uses an organic base catalyst to catalyze CEC and hydrogen fluoride to carry out a fluorination reaction at the temperature of between 20 ℃ below zero and 250 ℃. The technology adds the fluorinating agent step by step, and compared with chloroethylene carbonate, the fluorinating agent has low local concentration, slow fluorination speed and incomplete fluorination. The organic base catalyst adopted in the prior art also has the problem of difficult removal, and the post-treatment process is complex and is not beneficial to the purification of fluoroethylene carbonate.
Disclosure of Invention
The invention aims to overcome the technical defects in the prior art and provide a preparation method of ultrapure fluoroethylene carbonate.
In order to achieve the above object, the present invention provides a method for preparing ultrapure fluoroethylene carbonate, comprising the steps of:
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluoro reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
Preferably, the complex fluorinating agent is HF-KF complex and/or HF-KHF2 complex.
Preferably, the proportion of potassium fluoride and hydrogen fluoride in the HF-KF complex is 1:2 to 4; the ratio of potassium bifluoride to hydrogen fluoride in the HF-KHF2 complex is 1:4 to 5.
Preferably, the molar ratio of the chlorinating agent to ethylene carbonate is 1:3 to 7.
Preferably, the complex fluorinating agent is prepared by a process comprising the steps of: introducing hydrogen fluoride into potassium fluoride and/or potassium bifluoride at the temperature of 10-20 ℃, continuing introducing hydrogen fluoride when the molar ratio of the hydrogen fluoride to the potassium fluoride and/or the potassium bifluoride reaches 1-3, then heating to 70-80 ℃ under stirring the system for complex reaction, and stopping introducing the hydrogen fluoride when the ratio of the potassium fluoride and/or the potassium bifluoride to the hydrogen fluoride in the reaction product reaches a set value.
Preferably, the complex fluorinating agent is HF-KF complex and HF-KHF2 complex; the synthetic method of the fluoroethylene carbonate further comprises the following steps: and carrying out a complex reaction on the solid obtained by the solid-liquid separation and hydrogen fluoride to prepare the complex fluorinating agent.
Preferably, the purification method in step (3) comprises the following steps: removing a solvent ethylene carbonate ester in the liquid, and then carrying out falling film crystallization, wherein the falling film crystallization process comprises a plurality of times of circulating melt crystallization, and the melt crystallization sequentially comprises the steps of crystallization, sweating and melting.
Preferably, the temperature of the reaction vessel is controlled between 120 and 180 ℃ during the addition of ethylene carbonate in the chlorination reaction.
Preferably, the temperature of a reaction vessel is controlled to be 60-70 ℃ in the process of adding the complex fluorinating agent in the fluorination reaction, and the reaction time is 6-8 h.
Ultrapure fluoroethylene carbonate is prepared by the above process.
The preparation method of the ultrapure fluoroethylene carbonate provided by the invention has the beneficial effects that:
1. the method for preparing the ethylene carbonate has the advantages of simple equipment, simple operation and mild reaction conditions;
2. the invention synthesizes fluoroethylene carbonate under the conditions of no solvent and no catalyst, fluorinates chloroethylene carbonate liquid by using a liquid fluorinating agent, has high local concentration of the fluorinating agent, is easy to react, and is easy to separate products.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of ultrapure fluoroethylene carbonate, which comprises the following steps:
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluoro reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
Preferably, the complex fluorinating agent is HF-KF complex and/or HF-KHF2 complex.
Preferably, the ratio of potassium fluoride to hydrogen fluoride in the HF-KF complex is 1:2 to 4; the ratio of potassium bifluoride to hydrogen fluoride in the HF-KHF2 complex is 1:4 to 5.
Preferably, the molar ratio of the chlorinating agent to ethylene carbonate is 1:3 to 7.
Preferably, the complex fluorinating agent is prepared by a process comprising the steps of: introducing hydrogen fluoride into potassium fluoride and/or potassium bifluoride at the temperature of 10-20 ℃, continuing to introduce hydrogen fluoride when the molar ratio of the hydrogen fluoride to the potassium fluoride and/or potassium bifluoride reaches 1-3, then heating to 70-80 ℃ under stirring the system for complex reaction, and stopping introducing the hydrogen fluoride when the ratio of the potassium fluoride and/or potassium bifluoride to the hydrogen fluoride in the reaction product reaches a set value.
Preferably, the complex fluorinating agent is HF-KF complex and HF-KHF2 complex; the synthetic method of the fluoroethylene carbonate further comprises the following steps: and carrying out a complex reaction on the solid obtained by the solid-liquid separation and hydrogen fluoride to prepare the complex fluorinating agent.
Preferably, the purification method in step (3) comprises the following steps: and (2) removing the solvent ethylene carbonate in the liquid, and then carrying out falling film crystallization, wherein the falling film crystallization process comprises a plurality of circulating melt crystallization steps, and the melt crystallization steps comprise crystallization, sweating and melting in sequence.
Preferably, the temperature of the reaction vessel is controlled between 120 and 180 ℃ during the addition of the ethylene carbonate in the chlorination reaction.
Preferably, the temperature of a reaction vessel is controlled to be 60-70 ℃ in the process of adding the complex fluorinating agent in the fluorination reaction, and the reaction time is 6-8 h.
Ultrapure fluoroethylene carbonate is prepared by the above process.
The present invention will be described in detail below by way of examples.
Example 1
This example illustrates the preparation of ultrapure fluoroethylene carbonate according to the present invention.
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochloroethylene carbonate, wherein chlorinated reaction products comprise monochloroethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluoro reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
The method comprises the following conditions: the complex fluorinating agent is HF-KF complex and HF-KHF2 complex; wherein the ratio of potassium fluoride to hydrogen fluoride in the HF-KF complex is 1:2; wherein the proportion of potassium bifluoride and hydrogen fluoride in the HF-KHF2 complex is 1:4; the mol ratio of the chlorinated reagent to the ethylene carbonate is 1:3.
example 2
This example illustrates a process for the preparation of ultrapure fluoroethylene carbonate in accordance with the present invention.
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluoro reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
The method comprises the following conditions: the complex fluorinating agent is HF-KF complex and HF-KHF2 complex; wherein the ratio of potassium fluoride to hydrogen fluoride in the HF-KF complex is 1:4; wherein the ratio of potassium bifluoride to hydrogen fluoride in the HF-KHF2 complex is 1:5; the mol ratio of the chlorinated reagent to the ethylene carbonate is 1:7.
example 3
This example illustrates the preparation of ultrapure fluoroethylene carbonate according to the present invention.
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluorination reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
The method comprises the following conditions: the complex fluorinating agent is an HF-KF complex; wherein the ratio of potassium fluoride to hydrogen fluoride in the HF-KF complex is 1:2; the mol ratio of the chlorinated reagent to the ethylene carbonate is 1:3.
example 4
This example illustrates a process for the preparation of ultrapure fluoroethylene carbonate in accordance with the present invention.
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluorination reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
The method comprises the following conditions: the complex fluorinating agent is an HF-KF complex; wherein the ratio of potassium fluoride to hydrogen fluoride in the HF-KF complex is 1:4; the mol ratio of the chlorinated reagent to the ethylene carbonate is 1:7.
example 5
This example illustrates the preparation of ultrapure fluoroethylene carbonate according to the present invention.
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochloroethylene carbonate, wherein chlorinated reaction products comprise monochloroethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluoro reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
The method comprises the following conditions: the complex fluorinating agent is an HF-KHF2 complex; wherein the proportion of potassium bifluoride and hydrogen fluoride in the HF-KHF2 complex is 1:4; the mol ratio of the chlorinated reagent to the ethylene carbonate is 1:3.
example 6
This example illustrates a process for the preparation of ultrapure fluoroethylene carbonate in accordance with the present invention.
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluorination reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
The method comprises the following conditions: the complex fluorinating agent is an HF-KHF2 complex; wherein the proportion of potassium bifluoride and hydrogen fluoride in the HF-KHF2 complex is 1:5; the mol ratio of the chlorinated reagent to the ethylene carbonate is 1:7.
the preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A preparation method of ultrapure fluoroethylene carbonate is characterized by comprising the following steps: the method comprises the following steps:
(1) Chlorination reaction: chlorinating the chlorinated reagent and excessive ethylene carbonate under the action of light to generate monochlorethylene carbonate, wherein the chlorinated reaction products comprise monochlorethylene carbonate and unreacted ethylene carbonate;
(2) And (3) fluoro reaction: adding a complex fluorinating agent into the blending liquid of monochloroethylene carbonate and ethylene carbonate, and reacting by taking ethylene carbonate as a solvent to generate fluoroethylene carbonate;
(3) Solid-liquid separation and purification: and (3) carrying out solid-liquid separation on the fluoro reaction product to obtain solid mixed salt and liquid, and purifying the liquid to obtain the fluoroethylene carbonate.
2. The method for preparing ultrapure fluoroethylene carbonate according to claim 1, wherein the complex fluorinating agent is HF-KF complex and/or HF-KHF2 complex.
3. The method for preparing the ultrapure fluoroethylene carbonate according to claim 2, wherein the ratio of potassium fluoride to hydrogen fluoride in the HF-KF complex is 1:2 to 4; the ratio of potassium bifluoride to hydrogen fluoride in the HF-KHF2 complex is 1:4 to 5.
4. The method for preparing ultrapure fluoroethylene carbonate according to claim 1, wherein the molar ratio of the chlorinating agent to the ethylene carbonate is 1:3 to 7.
5. The method of claim 1, wherein the complexing fluorinating agent is prepared by a method comprising: introducing hydrogen fluoride into potassium fluoride and/or potassium bifluoride at the temperature of 10-20 ℃, continuing introducing hydrogen fluoride when the molar ratio of the hydrogen fluoride to the potassium fluoride and/or the potassium bifluoride reaches 1-3, then heating to 70-80 ℃ under stirring the system for complex reaction, and stopping introducing the hydrogen fluoride when the ratio of the potassium fluoride and/or the potassium bifluoride to the hydrogen fluoride in the reaction product reaches a set value.
6. The method for preparing ultrapure fluoroethylene carbonate according to claim 1, wherein the complex fluorinating agent is HF-KF complex or HF-KHF2 complex; the synthetic method of the fluoroethylene carbonate further comprises the following steps: and carrying out a complex reaction on the solid obtained by the solid-liquid separation and hydrogen fluoride to prepare the complex fluorinating agent.
7. The method for preparing ultrapure fluoroethylene carbonate according to claim 1, wherein the purification method in the step (3) comprises the steps of: removing a solvent ethylene carbonate ester in the liquid, and then carrying out falling film crystallization, wherein the falling film crystallization process comprises a plurality of times of circulating melt crystallization, and the melt crystallization sequentially comprises the steps of crystallization, sweating and melting.
8. The method for preparing ultrapure fluoroethylene carbonate according to claim 1, wherein the temperature of the reaction vessel is controlled to be 120-180 ℃ during the addition of the chloroethylene carbonate in the chlorination reaction.
9. The method for preparing the ultrapure fluoroethylene carbonate according to claim 1, wherein the temperature of the reaction vessel is controlled to be 60-70 ℃ during the addition of the complex fluorinating agent in the fluorination reaction, and the reaction time is 6-8 h.
10. The ultrapure fluoroethylene carbonate prepared by the preparation method of any one of claims 1 to 9.
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2023201999A1 (en) * | 2022-04-21 | 2023-10-26 | 上海东庚化工技术有限公司 | Production method and system for electrolyte additive |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20080114198A (en) * | 2007-06-27 | 2008-12-31 | 리켐주식회사 | A method for preparation of mono-halogenated ethylene carbonate |
WO2018113628A1 (en) * | 2016-12-19 | 2018-06-28 | 上海惠和化德生物科技有限公司 | Rapid continuous-flow synthesis process for fluoroethylene carbonate. |
CN108329293A (en) * | 2018-04-20 | 2018-07-27 | 北京宇极科技发展有限公司 | The method that gas phase continuously prepares fluorinated ethylene carbonate or/and vinylene carbonate |
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 |
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 |
CN114736185A (en) * | 2022-04-21 | 2022-07-12 | 上海东庚化工技术有限公司 | Energy-saving production process and system for ultrapure fluoroethylene carbonate |
-
2022
- 2022-08-30 CN CN202211045682.9A patent/CN115353504A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20080114198A (en) * | 2007-06-27 | 2008-12-31 | 리켐주식회사 | A method for preparation of mono-halogenated ethylene carbonate |
WO2018113628A1 (en) * | 2016-12-19 | 2018-06-28 | 上海惠和化德生物科技有限公司 | Rapid continuous-flow synthesis process for fluoroethylene carbonate. |
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 |
CN108329293A (en) * | 2018-04-20 | 2018-07-27 | 北京宇极科技发展有限公司 | The method that gas phase continuously prepares fluorinated ethylene carbonate or/and vinylene carbonate |
CN114736185A (en) * | 2022-04-21 | 2022-07-12 | 上海东庚化工技术有限公司 | Energy-saving production process and system for ultrapure 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 |
Non-Patent Citations (2)
Title |
---|
MASAFUMI KOBAYASHI,等: "Development of direct fluorination technology for application to materials for lithium batteries", 《JOURNAL OF FLUORINE CHEMISTRY》, pages 105 - 110 * |
任章顺,等: "氟代碳酸乙烯酯的合成与精制进展", 《化学推进剂与高分子材料》, pages 39 - 44 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2023201999A1 (en) * | 2022-04-21 | 2023-10-26 | 上海东庚化工技术有限公司 | Production method and system for electrolyte additive |
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