CN115536630A - Preparation method of ethylene sulfate based on lithium ion battery electrolyte additive - Google Patents
Preparation method of ethylene sulfate based on lithium ion battery electrolyte additive Download PDFInfo
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- CN115536630A CN115536630A CN202211364685.9A CN202211364685A CN115536630A CN 115536630 A CN115536630 A CN 115536630A CN 202211364685 A CN202211364685 A CN 202211364685A CN 115536630 A CN115536630 A CN 115536630A
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- C07D327/00—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms
- C07D327/10—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms two oxygen atoms and one sulfur atom, e.g. cyclic sulfates
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Abstract
The invention discloses a preparation method of a lithium ion battery electrolyte additive-based vinyl sulfate, and relates to the technical field of lithium ion batteries. The invention comprises the following steps: cyclization reaction: adding chloroalkane and ethylene glycol into a reaction kettle R1, then gradually dropwise adding thionyl chloride, reacting for 0.75 to 1.5 hours at the system temperature of 25 to 30 ℃, adjusting the pH value of the system to be neutral, and standing, separating and extracting to obtain an ethylene sulfite solution; and (3) oxidation reaction: adding an ethylene sulfite solution into a reaction kettle R2 filled with chloroalkane, adding a catalyst, adjusting the pH to 4~7, adding solid sodium hypochlorite in batches, controlling the temperature to be between minus 5 and 10 ℃, keeping the temperature for reaction for 10 to 30 min, standing, separating liquid, filtering to obtain a vinyl sulfate solution, drying, primarily filtering, concentrating, cooling, crystallizing, filtering and drying to obtain a vinyl sulfate product. The whole preparation process has the advantages of small amount of wastewater, high equipment volume efficiency, low energy consumption, short reaction time and high product purity meeting the electronic grade requirement.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a lithium ion battery electrolyte additive-based vinyl sulfate.
Background
The lithium ion battery is composed of an electrode material, electrolyte, a diaphragm and a packaging material. The development of new energy vehicles and electric vehicles is supported by multiple national policy measures; under the continuous development of computer, communication and consumer electronic products, the demand for lithium ion batteries is continuously increased, the electrolyte is called as blood of the lithium ion battery and plays a central role in the lithium ion battery, and the electrolyte additive is added into a small amount of the electrolyte, so that the performance of the electrolyte can be greatly improved, and the working performance of the lithium ion battery is improved.
In recent years, with the continuous development of the lithium ion battery industry, the electrolyte additive also receives great attention, and the vinyl sulfate serving as the lithium ion battery electrolyte additive can improve the SEI film-forming property of an electrode, enhance the moving efficiency of lithium ions between a positive electrode and a negative electrode, improve the performance of a lithium ion battery to a great extent, effectively prolong the cycle service life of the battery, greatly reduce the reduction speed of the initial capacity of the battery, effectively improve the charge and discharge performance of the battery, enhance the low-temperature heavy charge and discharge performance of the lithium ion battery, and is an indispensable lithium ion battery electrolyte additive.
However, the current preparation method of the vinyl sulfate has the problems of large water consumption, low volumetric efficiency of equipment, high energy consumption, large acidity value, high water content and the like. In view of the above, the invention provides a preparation method of vinyl sulfate with less wastewater, high volumetric efficiency of equipment, low energy consumption, short reaction time and high product purity aiming at the defects of the prior art.
Disclosure of Invention
The invention aims to provide a preparation method of a vinyl sulfate ester based on a lithium ion battery electrolyte additive, which solves the problems of large wastewater amount, low equipment volumetric efficiency, high energy consumption, large acidity value and high moisture content of the conventional preparation method of the vinyl sulfate ester.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a preparation method of a lithium ion battery electrolyte additive-based vinyl sulfate, which comprises the following steps:
(1) Cyclization reaction: adding chloroalkane and ethylene glycol into a reaction kettle R1, stirring to form a uniform reaction system, gradually dropwise adding thionyl chloride into the uniform reaction system, keeping the temperature of the system at 25 to 30 ℃ for reaction for 0.75 to 1.5 h, adjusting the pH of the reaction system to be neutral, and standing, separating liquid and extracting to obtain an ethylene sulfite solution;
(2) And (3) oxidation reaction: adding an ethylene sulfite solution prepared by a cyclization reaction into a reaction kettle R2 filled with chloroalkane, adding a catalyst, adjusting the pH of a reaction system to 4~7, adding solid sodium hypochlorite in batches, controlling the temperature of the system to be between-5 and 10 ℃ after the addition, carrying out heat preservation reaction for 10 to 30 min, standing, carrying out liquid separation and filtering to obtain a vinyl sulfate solution;
(3) And sequentially drying, primary filtering, concentrating, cooling and crystallizing, filtering again and drying the prepared vinyl sulfate solution to obtain the vinyl sulfate.
Preferably, the mass ratio of the chloroalkane to the ethylene glycol during the cyclization reaction is 1.
Preferably, the chloroalkane is one or more of dichloromethane, 1,2-dichloroethane, 1,1-dichloroethane, chloroform, carbon tetrachloride.
Preferably, the pH adjusting reagent of the reaction system in the cyclization reaction process is one or more of a sodium bicarbonate solution, a sodium carbonate solution, a potassium carbonate solution and a potassium bicarbonate solution, and the pH adjusting reagent of the reaction system in the oxidation reaction process is one or more of an ammonia bisulfate solution, a potassium dihydrogen phosphate-sodium hydroxide buffer solution and a potassium dihydrogen phosphate-potassium hydrogen phosphate buffer solution.
Preferably, the hydrogen chloride tail gas generated in the cyclization reaction process is absorbed in a reduced pressure mode, and the pressure in the tail gas absorption process is controlled to be within-0.075 to-0.01 MPa.
Preferably, one or two of ruthenium trichloride and ruthenium trichloride hydrate are selected as the catalyst in the oxidation reaction process, and one or more of anhydrous sodium hypochlorite solid and sodium hypochlorite pentahydrate are selected as the solid sodium hypochlorite.
Preferably, during the oxidation reaction, the mass ratio of the catalyst to the ethylene sulfite is 1: 0.001 to 1: 0.1, and the molar ratio of the solid sodium hypochlorite to the ethylene sulfite is 1.
Preferably, the temperature for cooling and crystallization is controlled to be 0 to 15 ℃, and the crystallization time is 0.5 to 2 hours; controlling the temperature of vacuum drying to be 50-65 ℃, and the drying time to be 2-4 h; the drying agent used in the drying process is one or more of anhydrous magnesium sulfate, anhydrous sodium sulfate, anhydrous calcium chloride and molecular sieve.
In the above process for producing vinyl sulfate, the solvent obtained by distillation under reduced pressure can be recycled after drying.
The invention has the following beneficial effects:
the preparation method of the vinyl sulfate has high volume efficiency, and compared with a sodium hypochlorite aqueous solution, the adopted solid sodium hypochlorite has high effective chlorine content, low sodium chloride content and less free sodium hydroxide; the product is simple to refine, the purity of the obtained product is high, the moisture and the acidity are low, and the method is suitable for industrial production.
Compared with the preparation process of the vinyl sulfate by using the sodium hypochlorite aqueous solution, the whole preparation process has the advantages of small waste water amount, high equipment volume efficiency, low energy consumption, short reaction time and product purity meeting the requirement of electronic grade.
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 diagram of a preparation process of a vinyl sulfate based battery electrolyte additive.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The sodium hypochlorite aqueous solution is generally prepared by introducing chlorine gas into a strong alkali aqueous solution, and the prepared sodium hypochlorite aqueous solution often contains a large amount of chlorine salt and has a high pH value. The concentration of sodium hypochlorite is usually about 10%, the reaction volume ratio is low, and a large amount of salt-containing wastewater is brought in the reaction process. The alkali content and the salt content of the solid sodium hypochlorite are both lower, the effective chlorine content is far higher than that of a sodium hypochlorite aqueous solution, and the generation amount of salt-containing wastewater can be effectively reduced. Taking sodium hypochlorite pentahydrate as an example, the active chlorine content of the sodium hypochlorite pentahydrate is basically kept unchanged after being stored for 1 year at low temperature (7 ℃), the influence of short-time storage at 30 ℃ on the active chlorine content is small, the active chlorine content is higher than that of a 10% sodium hypochlorite solution after being stored for more than 20 days at 30 ℃, the sodium chloride content is only 0.1 to 0.5Wt%, the sodium hydroxide content is only 0.04 to 0.08Wt%, the pH of the sodium hypochlorite solution dissolved in water is only 11 to 12, and the pH of the 10% sodium hypochlorite aqueous solution is more than 13, so that the solid sodium hypochlorite aqueous solution adopted in the preparation method of the vinyl sulfate is obviously better than the 10% sodium hypochlorite aqueous solution.
Example 1
(1) Cyclization reaction: adding 1,2 dichloroethane 100g and ethylene glycol 100g into a reaction kettle R1, stirring to form a uniform reaction system, gradually dropwise adding thionyl chloride 201.3 g into the uniform reaction system, controlling the temperature of the reaction system to be 25-30 ℃ after dropwise adding, preserving heat to react at 1h, absorbing generated hydrogen chloride by a tail gas absorption device in the reaction process, adding a saturated sodium bicarbonate solution to adjust the pH of the solution to be neutral, stirring for 15 min, standing for 15 min, adding 1,2 dichloroethane 20 g into a water phase after liquid separation for extraction, combining organic phases obtained by two extractions after two extractions to obtain an ethylene sulfite solution 285.5 g with the molar yield of 95.1%.
(2) And (3) oxidation reaction: adding an ethylene sulfite solution prepared by cyclization reaction into a reaction kettle R2 filled with chloroalkane, adding 1,2 dichloroethane 707.5 g,1 mol/L ammonium bisulfate 100 mL, ruthenium trichloride 331 mg into the reaction kettle R2, starting stirring, reducing the temperature to-5 ℃, controlling the temperature to be not higher than 10 ℃, adding a catalyst, adjusting the pH of the reaction system to 4~7, adding pentahydrate 271.5 g in batches, after 20 min is finished, carrying out heat preservation reaction for 20 min, standing for 20 min after heat preservation reaction, adding 1,2 dichloroethane 50 g to extract after liquid separation, combining the organic phases obtained after two extractions, adding anhydrous magnesium sulfate 25 zft g, stirring 1h, carrying out filtration, concentrating a primary filtrate until solid is separated out precipitation, then cooling for 1h after extraction, placing in a vacuum crystallization, filtering a filtered cake 3530 zxft 3530, and drying the product with the water yield of 3579.79% of 356 ppm of sulfuric acid, wherein the yield is 3579 ppm, and the yield is 3530 ppm of the product.
Example 2
(1) Cyclization reaction: adding 1,2 dichloroethane 100g and ethylene glycol 100g into a reaction kettle R1, stirring to form a uniform reaction system, gradually dropwise adding thionyl chloride 191.7 g into the uniform reaction system, controlling the temperature of the reaction system to be 25-30 ℃ after dropwise adding, keeping the temperature to react for 1h, absorbing generated hydrogen chloride by a tail gas absorption device in the reaction process, adding a saturated sodium bicarbonate solution to adjust the pH of the solution to be neutral, stirring for 15 min, standing for 15 min, adding 1,2 dichloroethane 20 g into a water phase after liquid separation for extraction, combining organic phases obtained by the two extractions after the two extractions to obtain an ethylene sulfite solution 274.3 g, wherein the molar yield is 88.6%.
(2) And (3) oxidation reaction: adding an ethylene sulfite solution prepared by cyclization reaction into a reaction kettle R2 filled with chloroalkane, adding 1,2 dichloroethane 651.5 g,1 mol/L potassium dihydrogen phosphate 100 mL, ruthenium trichloride 331 mg into the reaction kettle R2, starting stirring, cooling to-5 ℃, controlling the temperature to be not higher than 10 ℃, adding a catalyst, adjusting the pH of the reaction system to 4~7, adding pentahydrate 271.5 g in batches, after the completion of adding 25 min, carrying out heat preservation reaction for 20 min, standing for 20 min after heat preservation reaction, after liquid separation, adding 1,2 dichloroethane 50 g into a water phase for extraction, combining the organic phases obtained after twice extraction, adding anhydrous magnesium sulfate 25 g, stirring for 1h, carrying out primary filtration, concentrating the primary filtrate until solid is separated out precipitation, then cooling to 10 ℃, standing for precipitation of vinyl ester 1 3265 zxft, then placing into 357 ppm of filtered acetic ester, obtaining a filtered cake with 357 ppm acidity, and drying the product with 357 ppm of sulfuric acid, wherein the yield is 357 ppm of sulfuric acid, and the yield is 3555 ppm of the product.
Example 3
(1) Cyclization reaction: adding 1,2 dichloroethane 100g and ethylene glycol 100g into a reaction kettle R1, stirring to form a uniform reaction system, gradually dropwise adding thionyl chloride 249.2 g into the uniform reaction system, controlling the temperature of the reaction system to be 25-30 ℃ after dropwise adding, carrying out heat preservation reaction on the reaction system to obtain 1h, absorbing generated hydrogen chloride by a tail gas absorption device in the reaction process, adding a saturated sodium bicarbonate solution to adjust the pH of the solution to be neutral, stirring for 15 min, standing for 15 min, adding 1,2 dichloroethane 20 g into a water phase after liquid separation, extracting twice, and combining organic phases obtained by two times of extraction to obtain an ethylene sulfite solution 258.4 g, wherein the molar yield is 79.5%.
(2) And (3) oxidation reaction: adding an ethylene sulfite solution prepared by cyclization reaction into a reaction kettle R2 filled with chloroalkane, adding 1,2 dichloroethane 572.3 g,1 mol/L ammonium bisulfate 100 mL, ruthenium trichloride 1.655 g into the reaction kettle R2, starting stirring and cooling to-5 ℃, controlling the temperature to be not higher than 10 ℃, adding a catalyst, adjusting the pH of the reaction system to 4~7, adding sodium hypochlorite 271.5 g in batches, after 30 min is finished, carrying out heat preservation reaction for 20 min, standing for 20 min after heat preservation reaction, after liquid separation, adding 1,2 dichloroethane 50 g into an aqueous phase for extraction, after twice extraction, combining organic phases obtained by twice extraction, adding anhydrous magnesium sulfate 25 zxft 3525, stirring h, filtering, concentrating a primary filter liquid until a solid vinyl ester is precipitated, then cooling to 10 ℃, standing for crystallization, adding anhydrous magnesium sulfate 25 zxft 3525, filtering a filtrate h, and drying a filter cake 5329.83% of sulfuric acid product to obtain a purity of 5229.8, wherein the filtrate is 5291 ppm, and the yield of the filtrate is 5283.23 ppm.
Experiments and analysis show that in the existing preparation method of the vinyl sulfate serving as the lithium battery electrolyte additive (a Chinese invention patent application with the application number of 201811489064.7 discloses a preparation method of the vinyl sulfate), the synthesis of 100g vinyl sulfate by using a sodium hypochlorite aqueous solution needs to consume 10% of sodium hypochlorite aqueous solution 903.6 g, and the dropwise addition needs to take 40 min to 60 min, so that salt-containing wastewater 1932.2 g is generated. The synthesis of 100g vinyl sulfate ester by using sodium hypochlorite pentahydrate (solid) only needs to consume sodium hypochlorite pentahydrate 205.3 g, the addition process only needs 20 min to 30 min, the produced salt-containing wastewater only needs 930.6 g and is less than one half of 10% sodium hypochlorite solution, the crude product only needs to be dissolved and recrystallized in the purification process, and the purification process is simple.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A preparation method of a lithium ion battery electrolyte additive-based vinyl sulfate is characterized by comprising the following steps: the method comprises the following steps:
cyclization reaction: adding chloroalkane and ethylene glycol into a reaction kettle R1, stirring to form a uniform reaction system, gradually dropwise adding thionyl chloride into the uniform reaction system, keeping the temperature of the system at 25 to 30 ℃ for reaction for 0.75 to 1.5 h, adjusting the pH of the reaction system to be neutral, and standing, separating liquid and extracting to obtain an ethylene sulfite solution;
and (3) oxidation reaction: adding an ethylene sulfite solution prepared by cyclization reaction into a reaction kettle R2 filled with chloroalkane, adding a catalyst, adjusting the pH of a reaction system to 4~7, adding solid sodium hypochlorite in batches, controlling the temperature of the reaction system to be minus 5 to 10 ℃ after the addition, keeping the temperature for reaction for 10 to 30 min, standing, separating liquid and filtering to obtain a vinyl sulfate solution;
and sequentially drying, primary filtering, concentrating, cooling and crystallizing, filtering again and drying the prepared vinyl sulfate solution to obtain the vinyl sulfate.
2. The preparation method of the vinyl sulfate based on the lithium ion battery electrolyte additive is characterized in that in the cyclization reaction process, the mass ratio of the chlorinated alkane to the ethylene glycol is 1 to 0.5-1, and the molar ratio of the ethylene glycol to the thionyl chloride is 1.
3. The method for preparing the vinyl sulfate based on the lithium ion battery electrolyte additive according to claim 1, wherein the chlorinated alkane is one or more of dichloromethane, 1,2-dichloroethane, 1,1-dichloroethane, chloroform and carbon tetrachloride.
4. The method for preparing ethylene sulfate based on the lithium ion battery electrolyte additive according to claim 1, wherein the pH adjusting reagent of the reaction system in the cyclization reaction process is one or more of sodium bicarbonate solution, sodium carbonate solution, potassium carbonate solution and potassium bicarbonate solution, and the pH adjusting reagent of the reaction system in the oxidation reaction process is one or more of ammonium bisulfate solution, potassium dihydrogen phosphate-sodium hydroxide buffer solution and potassium dihydrogen phosphate-potassium hydrogen phosphate buffer solution.
5. The preparation method of the vinyl sulfate based on the lithium ion battery electrolyte additive according to claim 1, wherein hydrogen chloride tail gas generated in the cyclization reaction process is absorbed in a decompression mode, and the pressure in the tail gas absorption process is controlled to be-0.075 to-0.01 MPa.
6. The method for preparing the vinyl sulfate based on the lithium ion battery electrolyte additive according to claim 1, wherein one or two of ruthenium trichloride and ruthenium trichloride hydrate are selected as a catalyst in the oxidation reaction process, and one or more of anhydrous sodium hypochlorite solid and sodium hypochlorite pentahydrate are selected as solid sodium hypochlorite.
7. The preparation method of the vinyl sulfate based on the lithium ion battery electrolyte additive is characterized in that in the oxidation reaction process, the mass ratio of the catalyst to the ethylene sulfite is 1: 0.001 to 1: 0.1, and the molar ratio of the solid sodium hypochlorite to the ethylene sulfite is 1.
8. The preparation method of the vinyl sulfate based on the lithium ion battery electrolyte additive as claimed in claim 1, wherein the temperature for cooling and crystallization in the step (3) is controlled to be 0 to 15 ℃, and the crystallization time is 0.5 to 2 hours; the temperature of vacuum drying is controlled to be 50 to 65 ℃, and the drying time is 2 to 4 hours.
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| CN102241662A (en) * | 2011-05-06 | 2011-11-16 | 凯莱英医药化学（天津）有限公司 | Synthetic method of thiophene-3-ethanol |
| CN109369609A (en) * | 2018-11-02 | 2019-02-22 | 珠海市赛纬电子材料股份有限公司 | A kind of preparation method of sulfuric acid vinyl ester |
| CN109776361A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The synthetic method of sulfuric acid vinyl ester |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241662A (en) * | 2011-05-06 | 2011-11-16 | 凯莱英医药化学（天津）有限公司 | Synthetic method of thiophene-3-ethanol |
| CN109776361A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The synthetic method of sulfuric acid vinyl ester |
| CN109369609A (en) * | 2018-11-02 | 2019-02-22 | 珠海市赛纬电子材料股份有限公司 | A kind of preparation method of sulfuric acid vinyl ester |
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