CN114230549A - A kind of synthetic method of fluorinated vinylene carbonate - Google Patents
A kind of synthetic method of fluorinated vinylene carbonate Download PDFInfo
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Abstract
本申请公开了一种氟代碳酸亚乙烯酯的合成方法。该氟代碳酸亚乙烯酯的合成方法包括步骤：将碳酸二甲酯和1‑氟‑2‑氯代碳酸乙烯酯混合后，在合成反应温度、常压条件下滴加碱，进行合成反应第一时间后分析氟代碳酸乙烯酯转化率，当合格后转入中转釜待用；过滤脱除反应生成的盐酸盐形成母液，将母液转入母液中间罐，加入稳定剂后进行粗馏以脱除碳酸二甲酯，粗馏合格后，转入精馏中间罐进行精馏，得到合格的氟代碳酸亚乙烯酯成品。本申请的氟代碳酸亚乙烯酯的合成方法反应条件简单、操作简单、生产产率高、产品纯度较高。The present application discloses a method for synthesizing fluorinated vinylene carbonate. The method for synthesizing fluoroethylene carbonate comprises the steps of: after mixing dimethyl carbonate and 1-fluoro-2-chloroethylene carbonate, adding alkali dropwise at the synthesis reaction temperature and normal pressure, and carrying out the synthesis reaction step After a period of time, the conversion rate of fluoroethylene carbonate was analyzed, and when it was qualified, it was transferred to the transfer kettle for use; the hydrochloride generated by the reaction was filtered and removed to form a mother liquor, and the mother liquor was transferred to the mother liquor intermediate tank, and after adding a stabilizer, crude distillation was carried out to After removing the dimethyl carbonate, after the crude distillation is qualified, it is transferred to the rectification intermediate tank for rectification to obtain the qualified fluoroethylene carbonate finished product. The method for synthesizing fluoroethylene carbonate of the present application has simple reaction conditions, simple operation, high production yield and high product purity.
Description
Technical Field
The invention relates to the technical field of a production method of fluoroethylene carbonate, in particular to a synthetic method of fluoroethylene carbonate.
Background
The 1-fluoro-2-chloroethylene carbonate is a tower bottom high boiling point component in the vinylene carbonate VC production process, and if deep processing and utilization cannot be carried out, hazardous waste is formed. Fluoroethylene carbonate is an important additive material of lithium battery electrolyte, and the material can form a compact and stable organic film on the surface of a battery. The organic film generates polyalkyl lithium carbonate compound under the conditions of not losing conductivity and not increasing internal resistance of the battery, the compound can effectively inhibit solvent molecules and solvated lithium ions from being inserted into graphite, decomposition of electrolyte is reduced, stability of a graphite cathode is improved, and further charge and discharge performance of the lithium battery is improved, and high-purity fluoroethylene carbonate is required in the lithium battery industry.
The conventional production process of fluoroethylene carbonate has various processes: one is that fluorine gas reacts with ethylene carbonate directly, because the preparation difficulty of fluorine gas is great, the reaction activity is higher, the reaction is violent, the control difficulty is greater, the resulting product is more complicated (there are monofluoro thing, many fluoro things, etc., even ethylene carbonate decomposes into carbon tetrafluoride directly), the yield of reaction is lower, must achieve the fluoro ethylene carbonate of stable high purity, the cost is higher and the pollution is greater; in addition, the reaction of chloroethylene carbonate and potassium fluoride needs to strictly control the moisture content, the potassium fluoride needs to be correspondingly spray-dried, and meanwhile, the potassium fluoride needs to be dissolved in anhydrous polar solvents such as acetonitrile, sulfolane and the like, so that the problems of high control requirement, low yield and the like are solved. For example, patent CN101676282A discloses a method for producing fluoroethylene carbonate, which uses chlorine gas to directly substitute or uses other chlorinating agents such as sulfuryl chloride to perform chlorination to produce chloroethylene carbonate, the chloroethylene carbonate is refined and purified, and then undergoes halogen exchange reaction with fluorinating agents in proper solvents to produce fluoroethylene carbonate, the yield of fluoroethylene carbonate is less than 70%, and the purity is low.
Disclosure of Invention
The invention aims to provide a synthetic method of fluoroethylene carbonate, which is used for solving the technical problems of complex process, low production yield and low purity of the conventional synthetic method of fluoroethylene carbonate.
In order to achieve the above object, an embodiment of the present invention provides a method for synthesizing fluoroethylene carbonate, which comprises the steps of: mixing dimethyl carbonate and 1-fluoro-2-chloroethylene carbonate, dripping alkali at the synthesis reaction temperature under normal pressure, analyzing the conversion rate of fluoroethylene carbonate after the first time of synthesis reaction, and transferring to a transfer kettle for later use after the conversion rate is qualified; filtering to remove hydrochloride generated by the reaction to form mother liquor, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank for rectification after the rough distillation is qualified, and obtaining a qualified fluoroethylene carbonate finished product.
Further, in the mixture of the dimethyl carbonate and the 1-fluoro-2-chloroethylene carbonate, the molar ratio of the dimethyl carbonate to the 1-fluoro-2-chloroethylene carbonate is 1.2-2.5.
Further, the synthesis reaction temperature is 50-100 ℃.
Further, in the synthesis reaction process, the dropwise added alkali is one of ethylenediamine, triethylamine, dipropylamine, tripropylamine, diisopropylamine, butylamine, dibutylamine, tributylamine, isobutylamine and sec-butylamine.
Further, in the synthesis reaction process, the molar ratio of the dropwise added alkali to the 1-fluoro-2-chloroethylene carbonate is 1.05-1.2.
Further, the first time for carrying out the synthesis reaction is 2-12 h.
Further, the added stabilizer is one or more of hydroquinone, p-hydroxyanisole, 2, 6-di-tert-butyl-p-cresol, 2, 5-di-tert-butyl-hydroquinone, 2-tert-butyl-hydroquinone, p-benzoquinone, methyl hydroquinone, 2,6, 6-tetramethyl-4-hydroxypiperidine nitroxide free radical (TMHP0), copper N-di-N-butyl-dithiocarbamate, phenothiazine and p-hydroxyanisole.
Further, the mass of the added stabilizer is 0.001-0.1% of the total mass of the materials.
Further, tower separation is adopted for both rough distillation and rectification, a rough distillation tower is used in the rough distillation process, and a rectification tower is used in the rectification process; the crude distillation tower and the rectifying tower adopt a plate tower or a packed tower.
Furthermore, the crude distillation tower and the rectification tower are controlled by adopting a batch operation mode.
The invention has the beneficial effects that after 1-fluoro-2-chloroethylene carbonate is separated from heavy components at the bottoms of the vinylene carbonate VC rough distillation tower and the rectification tower, the high-boiling-point hazardous waste resource utilization in the vinylene carbonate process can be realized, the amount of hazardous waste is reduced, the comprehensive competitiveness of the vinylene carbonate process is improved, and the formed fluoroethylene carbonate product can also be used as an additive of a lithium battery electrolyte. The synthesis method of the fluoroethylene carbonate has the advantages of simple reaction conditions, simple operation, high production yield and high product purity.
Detailed Description
The technical solutions in the embodiments of the present application are clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present application and not all 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 application.
The following disclosure provides many different embodiments or examples for implementing different features of the application. In order to simplify the disclosure of the present application, specific example components and arrangements are described below. Of course, they are merely examples and are not intended to limit the present application. In addition, examples of various specific processes and materials are provided herein, but one of ordinary skill in the art may recognize applications of other processes and/or use of other materials.
Specifically, the embodiment of the present application provides a method for synthesizing fluoroethylene carbonate, which comprises the steps of: mixing dimethyl carbonate and 1-fluoro-2-chloroethylene carbonate, dripping alkali at the synthesis reaction temperature under normal pressure, analyzing the conversion rate of fluoroethylene carbonate after the first time of synthesis reaction, and transferring to a transfer kettle for later use after the conversion rate is qualified; filtering to remove hydrochloride generated by the reaction to form mother liquor, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank for rectification after the rough distillation is qualified, and obtaining a qualified fluoroethylene carbonate finished product.
In the embodiment of the application, in the mixture of the dimethyl carbonate and the 1-fluoro-2-chloroethylene carbonate, the molar ratio of the dimethyl carbonate to the 1-fluoro-2-chloroethylene carbonate is 1.2-2.5.
In the examples of the present application, the synthesis reaction temperature is 50 to 100 ℃. Wherein the synthesis reaction temperature is optimized to be 60-80 ℃, so that the reaction temperature is not high and controllable.
In the embodiment of the application, in the synthesis reaction process, the dropwise added alkali is one of ethylenediamine, triethylamine, dipropylamine, tripropylamine, diisopropylamine, butylamine, dibutylamine, tributylamine, isobutylamine and sec-butylamine.
In the embodiment of the application, the molar ratio of the dropwise added alkali to the 1-fluoro-2-chloroethylene carbonate in the synthesis reaction process is 1.05-1.2.
In the examples of the present application, the first time for carrying out the synthesis reaction is 2 to 12 hours.
In the embodiment of the application, the added stabilizer is one or more of hydroquinone, p-hydroxyanisole, 2, 6-di-tert-butyl-p-cresol, 2, 5-di-tert-butyl-hydroquinone, 2-tert-butyl-hydroquinone, p-benzoquinone, methyl hydroquinone, 2,6, 6-tetramethyl-4-hydroxypiperidine nitroxide free radical (TMHP0), copper N-di-N-butyl-dithiocarbamate, phenothiazine and p-hydroxyanisole.
In the embodiment of the application, the mass of the added stabilizer is 0.001-0.1% of the total mass of the materials.
In the embodiment of the application, tower separation is adopted for both rough distillation and rectification, a rough distillation tower is used in the rough distillation process, and a rectification tower is used in the rectification process; the crude distillation tower and the rectifying tower adopt a plate tower or a packed tower. The rectification column and the crude distillation column are preferably structured packing.
In this application embodiment, the rough distillation tower and the rectifying column adopt intermittent operation mode to control, can promote energy utilization, avoid the not enough problem of the fractional distillation inefficiency that leads to of intermediate product to promote production efficiency.
Specifically, the method for synthesizing vinylene fluorocarbonate will be specifically described below with reference to the following examples.
Example 1
200g of dimethyl carbonate and 52g of 1-fluoro-2-chloroethylene carbonate are weighed and put into a reactor, nitrogen is replaced until the oxygen content is less than 0.3%, stirring is started, 25g of ethylenediamine is dripped when the temperature is raised to 70 ℃, circulating water is started to keep the reaction temperature at 70 ℃, dripping is carried out for 3 hours, the conversion rate of the fluoroethylene carbonate is analyzed, and the fluoroethylene carbonate is transferred into a transfer kettle with stirring after being qualified. Filtering and removing hydrochloride generated in the reaction by using a vacuum filtration bottle, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank after the rough distillation is qualified, performing rectification, and obtaining a qualified fluoroethylene carbonate finished product at the tower top.
Example 2
200g of dimethyl carbonate and 52g of 1-fluoro-2-chloroethylene carbonate are weighed and put into a reactor, nitrogen is replaced until the oxygen content is less than 0.3%, stirring is started, 42g of triethylamine is dripped when the temperature is raised to 70 ℃, circulating water is started to keep the reaction temperature at 70 ℃, dripping is carried out for 4 hours, the conversion rate of the fluoroethylene carbonate is analyzed, and the fluoroethylene carbonate is transferred into a transfer kettle with stirring after being qualified. Filtering and removing hydrochloride generated in the reaction by using a vacuum filtration bottle, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank after the rough distillation is qualified, performing rectification, and obtaining a qualified fluoroethylene carbonate finished product at the tower top.
Example 3
200g of dimethyl carbonate and 52g of 1-fluoro-2-chloroethylene carbonate are weighed and put into a reactor, nitrogen is replaced until the oxygen content is less than 0.3%, stirring is started, 42g of dipropylamine is dripped when the temperature is raised to 70 ℃, circulating water is started to keep the reaction temperature at 70 ℃, dripping is carried out for 3 hours, the conversion rate of the fluoroethylene carbonate is analyzed, and the fluoroethylene carbonate is transferred into a transfer kettle with stirring after being qualified. Filtering and removing hydrochloride generated in the reaction by using a vacuum filtration bottle, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank after the rough distillation is qualified, performing rectification, and obtaining a qualified fluoroethylene carbonate finished product at the tower top.
Example 4
200g of dimethyl carbonate and 52g of 1-fluoro-2-chloroethylene carbonate are weighed and put into a reactor, nitrogen is replaced until the oxygen content is less than 0.3%, stirring is started, 58g of tripropylamine is dripped when the temperature is raised to 70 ℃, circulating water is started to keep the reaction temperature at 70 ℃, dripping is carried out for 3 hours, the conversion rate of the fluoroethylene carbonate is analyzed, and the fluoroethylene carbonate is transferred into a transfer kettle with stirring after being qualified. Filtering and removing hydrochloride generated in the reaction by using a vacuum filtration bottle, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank after the rough distillation is qualified, performing rectification, and obtaining a qualified fluoroethylene carbonate finished product at the tower top.
Example 5
200g of dimethyl carbonate and 52g of 1-fluoro-2-chloroethylene carbonate are weighed and put into a reactor, nitrogen is replaced until the oxygen content is less than 0.3%, stirring is started, 42g of diisopropylamine is dripped when the temperature is raised to 70 ℃, circulating water is started to keep the reaction temperature at 70 ℃, dripping is carried out for 4 hours, the conversion rate of the fluoroethylene carbonate is analyzed, and the fluoroethylene carbonate is transferred into a transfer kettle with stirring after being qualified. Filtering and removing hydrochloride generated in the reaction by using a vacuum filtration bottle, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank after the rough distillation is qualified, performing rectification, and obtaining a qualified fluoroethylene carbonate finished product at the tower top.
Example 6
200g of dimethyl carbonate and 52g of 1-fluoro-2-chloroethylene carbonate are weighed and put into a reactor, nitrogen is replaced until the oxygen content is less than 0.3%, stirring is started, 42g of triethylamine is dripped when the temperature is raised to 80 ℃, circulating water is started to keep the reaction temperature at 80 ℃, dripping is carried out for 4 hours, the conversion rate of the fluoroethylene carbonate is analyzed, and the fluoroethylene carbonate is transferred into a transfer kettle with stirring after being qualified. Filtering and removing hydrochloride generated in the reaction by using a vacuum filtration bottle, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank after the rough distillation is qualified, performing rectification, and obtaining a qualified fluoroethylene carbonate finished product at the tower top.
The invention has the beneficial effects that after 1-fluoro-2-chloroethylene carbonate is separated from heavy components at the bottoms of the vinylene carbonate VC rough distillation tower and the rectification tower, the high-boiling-point hazardous waste resource utilization in the vinylene carbonate process can be realized, the amount of hazardous waste is reduced, the comprehensive competitiveness of the vinylene carbonate process is improved, and the formed fluoroethylene carbonate product can also be used as an additive of a lithium battery electrolyte. The synthesis method of the fluoroethylene carbonate has the advantages of simple reaction conditions, simple operation, high production yield and high product purity.
The above embodiments of the present application are described in detail, and specific examples are applied in the present application to explain the principles and implementations of the present application, and the description of the above embodiments is only used to help understand the technical solutions and core ideas of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present disclosure as defined by the appended claims.
Claims (10)
1. A method for synthesizing fluoroethylene carbonate is characterized by comprising the following steps: mixing dimethyl carbonate and 1-fluoro-2-chloroethylene carbonate, dripping alkali at the synthesis reaction temperature under normal pressure, analyzing the conversion rate of fluoroethylene carbonate after the first time of synthesis reaction, and transferring to a transfer kettle for later use after the conversion rate is qualified; filtering to remove hydrochloride generated by the reaction to form mother liquor, transferring the mother liquor into a mother liquor intermediate tank, adding a stabilizing agent, performing rough distillation to remove dimethyl carbonate, transferring the mother liquor into a rectification intermediate tank for rectification after the rough distillation is qualified, and obtaining a qualified fluoroethylene carbonate finished product.
2. The method of synthesizing fluoroethylene carbonate according to claim 1, wherein the molar ratio of dimethyl carbonate to 1-fluoro-2-chloroethylene carbonate in the mixture of dimethyl carbonate and 1-fluoro-2-chloroethylene carbonate is 1.2 to 2.5.
3. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein the synthesis reaction temperature is 50-100 ℃.
4. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein the dropwise addition of the base during the synthesis reaction is one of ethylenediamine, triethylamine, dipropylamine, tripropylamine, diisopropylamine, butylamine, dibutylamine, tributylamine, isobutylamine and sec-butylamine.
5. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein the molar ratio of the dropwise added alkali to the 1-fluoro-2-chloroethylene carbonate is 1.05 to 1.2 during the synthesis reaction.
6. The method of claim 1, wherein the first time period for the synthesis reaction is 2-12 hours.
7. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein the stabilizer is one or more selected from hydroquinone, p-hydroxyanisole, 2, 6-di-tert-butyl-p-cresol, 2, 5-di-tert-butyl-hydroquinone, 2-tert-butyl-hydroquinone, p-benzoquinone, methyl hydroquinone, 2,6, 6-tetramethyl-4-hydroxypiperidine nitroxide free radical, copper N-di-N-butyl-dithiocarbamate, phenothiazine and p-hydroxyanisole.
8. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein the mass of the stabilizer added is 0.001 to 0.1% of the total mass of the materials.
9. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein the rough distillation and the rectification both adopt tower separation, the rough distillation process adopts a rough distillation tower, and the rectification process adopts a rectification tower; the crude distillation tower and the rectifying tower adopt a plate tower or a packed tower.
10. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein the crude distillation column and the rectification column are controlled in a batch operation.
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