CN115433155A - Synthetic method of fluoroethylene carbonate - Google Patents
Synthetic method of fluoroethylene carbonate Download PDFInfo
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- CN115433155A CN115433155A CN202211168878.7A CN202211168878A CN115433155A CN 115433155 A CN115433155 A CN 115433155A CN 202211168878 A CN202211168878 A CN 202211168878A CN 115433155 A CN115433155 A CN 115433155A
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- hydrogen fluoride
- carbonate
- solid base
- base catalyst
- reaction
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- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000010189 synthetic method Methods 0.000 title claims abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 46
- 239000007787 solid Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- OYOKPDLAMOMTEE-UHFFFAOYSA-N 4-chloro-1,3-dioxolan-2-one Chemical compound ClC1COC(=O)O1 OYOKPDLAMOMTEE-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000002585 base Substances 0.000 claims description 34
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 22
- 239000000945 filler Substances 0.000 claims description 18
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 16
- 239000000460 chlorine Substances 0.000 claims description 16
- 229910052801 chlorine Inorganic materials 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 239000012458 free base Substances 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 9
- 239000011737 fluorine Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 9
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 239000011780 sodium chloride Substances 0.000 abstract description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 12
- 239000000047 product Substances 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 7
- 239000010935 stainless steel Substances 0.000 description 7
- 235000003270 potassium fluoride Nutrition 0.000 description 6
- 239000011698 potassium fluoride Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 238000003682 fluorination reaction Methods 0.000 description 4
- 239000002000 Electrolyte additive Substances 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000006266 etherification reaction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- PQLFROTZSIMBKR-UHFFFAOYSA-N ethenyl carbonochloridate Chemical compound ClC(=O)OC=C PQLFROTZSIMBKR-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a synthetic method of fluoroethylene carbonate, which relates to the technical field of organic chemical synthesis, and takes chloroethylene carbonate and hydrogen fluoride loaded by a resin solid base catalyst as raw materials, adopts hydrogen fluoride liquid as a reaction raw material, and has the highest molar ratio of 1:1.1, the waste of the fluorine source is greatly reduced; the solid base catalyst loaded with hydrogen fluoride avoids the problem of large equipment investment caused by hydrogen fluoride, and greatly reduces equipment investment; no waste salt is generated in the reaction process, and the activated solid base catalyst only generates sodium chloride; the method has high yield, the reaction is carried out in a pure liquid phase, the requirements on equipment except a packed column are low, and the reaction solution does not have the problem of low reaction yield caused by solid-liquid two phases; the solid base catalyst can be recycled after being activated and dried, only consumes anhydrous hydrogen fluoride, greatly reduces the cost of raw materials, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of organic chemical synthesis, in particular to a synthetic method of fluoroethylene carbonate.
Background
As the requirements of batteries on high energy density, high safety performance, long cycle life, high rate performance, wide temperature range use and the like are continuously increased, the market of electrolyte additives is receiving more and more attention. Fluoroethylene carbonate (FEC) is a mainstream additive in the current market, and FEC can be used as an organic solvent, an organic synthesis intermediate, a medical intermediate, an electronic chemical and an electrolyte additive, wherein the electrolyte additive of the lithium ion battery is mainly applied to the market, the performance of an SEI film formed by FEC is good, a compact structure layer can be formed, the impedance is not increased, and the low-temperature performance of the electrolyte is improved. The additive is a mainstream additive in the current lithium battery electrolyte market, and the market share is close to about 21%.
The prior method for preparing fluoroethylene carbonate has two main routes, namely fluorination before etherification and etherification before fluorination. Since fluoroethylene carbonate has good development prospect in the field of lithium batteries, the synthesis process route has many reports, and Hideki Ishii and the like adopt an electrochemical method to synthesize FEC by taking vinylene carbonate as a raw material through two steps, but the cost is extremely high, and the fluoroethylene carbonate is not suitable for industrial production. The current fluoroethylene carbonate synthesis process has a plurality of processes: fluorine gas direct fluorination. The fluorine gas is directly reacted with the ethylene carbonate, the fluorine gas has strong activity, the reaction control is difficult in the production process, polyfluorinated byproducts are easily generated, the method has high requirements on equipment and process, and the equipment cost is high. In order to solve the safety problem caused by fluorine gas, CN108250176A proposes a method for synthesizing fluoroethylene carbonate by using an integrated continuous reactor, but the activity of fluorine gas is too high, resulting in generation of multi-fluorine generation products. Therefore, the yield can only reach about 85% although the conversion rate is high.
The method commonly used in industry at present is the exchange fluorination method of potassium fluoride and chloroethylene carbonate. The reaction has extremely high requirements on the quality of water and potassium fluoride, and the reaction control also needs higher standards, so the reaction yield is lower, and because the reaction is a solid-liquid reaction, the using amount of the potassium fluoride is usually 1.5 to 3 times of the total chlorine, and the potassium fluoride and the potassium chloride are difficult to separate, so a large amount of waste salt is generated. In order to solve the problem of low reaction yield caused by potassium fluoride, CN106916137A proposes to use high-purity potassium fluoride with small size for reaction, and the yield is between 78% and 82%. CN105968083B and CN103113345B respectively adopt liquid anhydrous hydrogen fluoride and gaseous anhydrous hydrogen fluoride to directly react with chlorinated ethylene carbonate, and the reaction is difficult to carry out because fluorine has a strong hydrogen bonding effect on hydrogen, so the molar ratio of the liquid and gaseous hydrogen fluoride to the chlorinated ethylene carbonate reaches 1-10, and great waste and safety risk exist. The preparation method of fluoroethylene carbonate generally has the problems of low yield, difficult post-treatment, rigorous condition control and higher raw material requirement, and is not suitable for large-scale continuous production.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a method for synthesizing fluoroethylene carbonate, which has the advantages of high reaction yield, short reaction time, safety, no toxicity and less raw material loss.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a synthetic method of fluoroethylene carbonate comprises the following specific synthetic steps:
(1) Filling solid base catalyst into a filler column, introducing liquid anhydrous hydrogen fluoride at-10 deg.C, and maintaining
The temperature of the packed column is 0-20 ℃, and the solid base catalyst packed column rich in fluorinion is obtained;
the solid base catalyst is Tulsimer A-8X MP, wherein the content of free base is 18 percent calculated by chlorine;
the anhydrous hydrogen fluoride has a water content of <50ppm;
the molar ratio of the free base of the solid base catalyst to the anhydrous hydrogen fluoride is 1.0-1.1;
(2) Dissolving chloroethylene carbonate in dimethyl carbonate to obtain dimethyl carbonate solution of chloroethylene carbonate, introducing the solution into the solid base catalyst filled column rich in fluorinion prepared in the step (1) at the temperature of 60-90 ℃, and circulating for 1-3h after introduction is finished to obtain reaction liquid;
wherein the mass concentration of the chloroethylene carbonate is 76 percent, and the total chlorine content is 30.26 percent;
the mass ratio of the chloroethylene carbonate to the dimethyl carbonate is 1:3-8;
the molar ratio of the anhydrous hydrogen fluoride to the total chlorine content in the chloroethylene carbonate is 1.0-1.1;
(3) And (3) after the reaction is finished, cooling the reaction liquid obtained in the step (2) to 25-30 ℃, distilling under reduced pressure to remove dimethyl carbonate, and rectifying to obtain fluoroethylene carbonate with the content of more than 99%.
Preferably, the molar ratio of the solid base catalyst free base to the anhydrous hydrogen fluoride in step (1) is 1.04-1.07.
Preferably, the molar ratio of the anhydrous hydrogen fluoride to the total chlorine content in the vinyl chlorocarbonate in the step (2) is 1.03-1.09.
Preferably, the cycle time in step (2) is 2h.
In the step (3), the absolute distillation pressure is 3 mbar, and fractions with the temperature of 64-95 ℃ are collected.
The invention has the following beneficial effects:
the synthesis method of fluoroethylene carbonate takes chloroethylene carbonate and hydrogen fluoride loaded by a resin solid base catalyst as raw materials, adopts hydrogen fluoride liquid as a reaction raw material, and has the highest molar ratio of 1:1.1, the waste of the fluorine source is greatly reduced; the solid base catalyst loaded with hydrogen fluoride avoids the problem of large equipment investment caused by hydrogen fluoride, and greatly reduces the equipment investment; no waste salt is produced in the reaction process, and only sodium chloride is produced by activating the solid base catalyst.
The synthetic method of fluoroethylene carbonate has high yield, the reaction is carried out in a pure liquid phase, the requirements on equipment except a filler column are low, and the reaction solution does not have the problem of low reaction yield caused by solid-liquid two phases. The solid base catalyst can be recycled after being activated and dried, only consumes anhydrous hydrogen fluoride, greatly reduces the cost of raw materials, and is suitable for industrial production.
Detailed Description
The invention will be further described with reference to specific examples, but the invention is not limited thereto, and the specific protection scope is as set forth in the claims.
Example 1
Filling 1.85kg of Tulsimer A-8X MP solid base catalyst of a Tulsimer, namely a Dusheng into a stainless steel filler column, introducing 0.17kg of anhydrous hydrogen fluoride at the temperature of-10 ℃, keeping the temperature of the filler column at 20 ℃ to obtain a solid base filler column rich in hydrogen fluoride, dissolving 0.9kg of chloroethylene carbonate (76 percent of content and 30.26 percent of total chlorine content) into 7.2kg of dimethyl carbonate, pumping the solution through the solid base filler column rich in hydrogen fluoride at the temperature of 90 ℃, circulating for 3 hours, cooling to 30 ℃ after the reaction is finished, removing the dimethyl carbonate by reduced pressure distillation, and finally obtaining 0.527kg of fluoroethylene carbonate product by rectification, wherein the reaction yield is 89%.
Example 2
Filling 1.77kg of Tulsimer A-8X MP solid base catalyst of the Dusheng into a stainless steel packed column, introducing 0.172kg of anhydrous hydrogen fluoride at the temperature of-10 ℃, and keeping the temperature of the packed column at 15 ℃ to obtain a solid base packed column rich in hydrogen fluoride; 1kg of chloroethylene carbonate (76% content, 30.26% total chlorine content) was dissolved in 4kg of dimethyl carbonate, passed through a column of solid basic material rich in hydrogen fluoride at 70 ℃ by means of a pump and circulated for 3h; after the reaction is finished, cooling to 28 ℃, then removing dimethyl carbonate by reduced pressure distillation, and finally obtaining 0.599kg of fluoroethylene carbonate product by rectification, wherein the reaction yield is 91%.
Example 3
Filling 1.77kg of Tulsimer A-8X MP solid base catalyst of the Dusheng into a stainless steel packed column, introducing 0.18kg of anhydrous hydrogen fluoride at the temperature of-10 ℃, and keeping the temperature of the packed column at 0 ℃ to obtain a solid base packed column rich in hydrogen fluoride; 1.054kg of chloroethylene carbonate (76% content, 30.26% total chlorine content) were dissolved in 3.162kg of dimethyl carbonate, passed through a column of solid alkali-filled hydrogen fluoride-rich material at 60 ℃ by means of a pump and circulated for 1h; after the reaction is finished, cooling to 25 ℃, then removing dimethyl carbonate by reduced pressure distillation, and finally obtaining 0.610kg of fluoroethylene carbonate product by rectification, wherein the reaction yield is 88%.
Example 4
Filling 1.77kg of Tulsimer A-8X MP solid base catalyst of the Dusheng into a stainless steel packed column, introducing 0.176kg of anhydrous hydrogen fluoride at the temperature of-10 ℃, and keeping the temperature of the packed column at 15 ℃ to obtain a solid base packed column rich in hydrogen fluoride; 1kg of chloroethylene carbonate (76% content, 30.26% total chlorine content) was dissolved in 3kg of dimethyl carbonate, passed through a column of solid alkali-filled hydrogen fluoride by means of a pump at 80 ℃ and circulated for 1h; after the reaction is finished, the temperature is reduced to 28 ℃, then dimethyl carbonate is removed by reduced pressure distillation, and finally 0.592kg of fluoroethylene carbonate product is obtained by rectification, with the reaction yield of 90%.
Example 5
Filling 1.85kg of Tulsimer A-8X MP solid base catalyst of the Dusheng into a stainless steel filler column, introducing 0.188kg of anhydrous hydrogen fluoride at the temperature of-10 ℃, and keeping the temperature of the filler column at 10 ℃ to obtain a solid base filler column rich in hydrogen fluoride; 1kg of chloroethylene carbonate (76% content, 30.26% total chlorine content) was dissolved in 5kg of dimethyl carbonate, passed through a column of solid base-filled with hydrogen fluoride by means of a pump at 70 ℃ and circulated for 1h. After the reaction is finished, the temperature is reduced to 26 ℃, then dimethyl carbonate is removed by reduced pressure distillation, and finally 0.592kg of fluoroethylene carbonate product is obtained by rectification, with the reaction yield of 90%.
Example 6
Filling 1.85kg of Tulsimer A-8X MP solid base catalyst of a Dusheng into a stainless steel filler column, introducing 0.179kg of anhydrous hydrogen fluoride at the temperature of minus 10 ℃, keeping the temperature of the filler column at 10 ℃ to obtain a solid base filler column rich in hydrogen fluoride, dissolving 1kg of chloroethylene carbonate (76 percent of content and 30.26 percent of total chlorine content) into 6kg of dimethyl carbonate, flowing the chloroethylene carbonate through the solid base filler column rich in hydrogen fluoride by a pump at the temperature of 70 ℃, circulating for 2 hours, cooling to 26 ℃ after the reaction is finished, then removing the dimethyl carbonate by reduced pressure distillation, finally obtaining 0.612kg of fluoroethylene carbonate product by rectification, wherein the reaction yield is 93 percent.
Example 7
Filling 1.77g Tulsimer A-8X MP solid base catalyst of Dusheng into a stainless steel filler column, introducing 0.179kg of anhydrous hydrogen fluoride at-10 ℃, keeping the temperature of the filler column at 5 ℃ to obtain a solid base filler column rich in hydrogen fluoride, dissolving 1kg of chloroethylene carbonate (76 percent of content and 30.26 percent of total chlorine content) in 4kg of dimethyl carbonate, flowing the chloroethylene carbonate through the solid base filler column rich in hydrogen fluoride by a pump at 70 ℃, circulating for 1h, cooling to 27 ℃ after the reaction is finished, then removing the dimethyl carbonate by reduced pressure distillation, finally obtaining 0.599kg of fluoroethylene carbonate product by rectification, wherein the reaction yield is 91%.
Claims (5)
1. A synthetic method of fluoroethylene carbonate is characterized in that: the specific synthetic steps are as follows:
filling solid base catalyst into a filler column, introducing liquid anhydrous hydrogen fluoride at-10 deg.C, and maintaining
The temperature of the packed column is 0-20 ℃, and a solid base catalyst packed column rich in fluorinion is obtained;
the solid base catalyst is Tulsimer A-8X MP, wherein the Tulsimer A-8X MP contains 18 percent of free base calculated by chlorine;
the anhydrous hydrogen fluoride has a water content of <50ppm;
the molar ratio of free base to anhydrous hydrogen fluoride in the solid base catalyst is 1.0-1.1;
(2) Dissolving chloroethylene carbonate in dimethyl carbonate to obtain dimethyl carbonate solution of chloroethylene carbonate, introducing the solution into the solid base catalyst filled column rich in fluorinion prepared in the step (1) at the temperature of 60-90 ℃, and circulating for 1-3h after introduction is finished to obtain reaction liquid;
wherein the mass concentration of the chloroethylene carbonate is 76 percent, and the total chlorine content is 30.26 percent;
the mass ratio of the chloroethylene carbonate to the dimethyl carbonate is 1:3-8;
the molar ratio of the anhydrous hydrogen fluoride to the total chlorine content in the chloroethylene carbonate is 1.0-1.1;
(3) And (3) after the reaction is finished, cooling the reaction liquid obtained in the step (2) to 25-30 ℃, removing dimethyl carbonate by reduced pressure distillation, and rectifying to obtain fluoroethylene carbonate with the content of more than 99%.
2. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein: the molar ratio of the free base in the solid base catalyst in the step (1) to the anhydrous hydrogen fluoride is 1.04-1.09.
3. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein: the mol ratio of the anhydrous hydrogen fluoride to the total chlorine content in the chloroethylene carbonate in the step (2) is 1.03-1.09:1.0.
4. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein: the cycle time in the step (2) is 2h.
5. The method for synthesizing fluoroethylene carbonate according to claim 1, wherein: in the step (3), the absolute pressure of the rectification is 3 mbar, and the fraction with the temperature of 64-95 ℃ is collected.
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| CN202211168878.7A CN115433155A (en) | 2022-09-25 | 2022-09-25 | Synthetic method of fluoroethylene carbonate |
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