CN117362265A - Method for improving atom utilization rate of ethylene carbonate - Google Patents
Method for improving atom utilization rate of ethylene carbonate Download PDFInfo
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- CN117362265A CN117362265A CN202311418988.9A CN202311418988A CN117362265A CN 117362265 A CN117362265 A CN 117362265A CN 202311418988 A CN202311418988 A CN 202311418988A CN 117362265 A CN117362265 A CN 117362265A
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- ethylene carbonate
- carbonate
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- photoreaction
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- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- OYOKPDLAMOMTEE-UHFFFAOYSA-N 4-chloro-1,3-dioxolan-2-one Chemical compound ClC1COC(=O)O1 OYOKPDLAMOMTEE-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000243 solution Substances 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 22
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 claims abstract description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000460 chlorine Substances 0.000 claims abstract description 10
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 10
- 239000012452 mother liquor Substances 0.000 claims abstract description 8
- 239000010413 mother solution Substances 0.000 claims abstract description 3
- 238000002425 crystallisation Methods 0.000 claims description 22
- 230000008025 crystallization Effects 0.000 claims description 21
- 208000012839 conversion disease Diseases 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 abstract description 18
- 239000011698 potassium fluoride Substances 0.000 abstract description 14
- 235000003270 potassium fluoride Nutrition 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 39
- 230000008569 process Effects 0.000 description 16
- 239000000706 filtrate Substances 0.000 description 14
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 11
- 238000004821 distillation Methods 0.000 description 11
- 238000005660 chlorination reaction Methods 0.000 description 10
- 238000010907 mechanical stirring Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 239000012467 final product Substances 0.000 description 7
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 125000003963 dichloro group Chemical group Cl* 0.000 description 3
- 238000003682 fluorination reaction Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- DSMUTQTWFHVVGQ-UHFFFAOYSA-N 4,5-difluoro-1,3-dioxolan-2-one Chemical compound FC1OC(=O)OC1F DSMUTQTWFHVVGQ-UHFFFAOYSA-N 0.000 description 1
- 239000002000 Electrolyte additive Substances 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- -1 ethylene carbonate compound Chemical class 0.000 description 1
- 238000004334 fluoridation Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of organic synthesis, and discloses a method for improving the atomic utilization rate of ethylene carbonate, which comprises the steps of reacting ethylene carbonate with chlorine to obtain a reaction solution; crystallizing the reaction solution at low temperature to obtain ethylene carbonate crystals and mother solution containing chlorinated ethylene carbonate; reacting mother liquor containing chlorinated ethylene carbonate with KF to prepare the fluorinated ethylene carbonate. The vinyl carbonate crystal is melted and chlorinated to generate chloroethylene carbonate, so that the chloroethylene carbonate can be recycled, and the atom utilization rate of the vinyl carbonate is improved. The impurity content of the synthesized FEC by using the CEC with high purity is low, the use amount of potassium fluoride is reduced, and complex post-treatment is avoided, so that the production cost is reduced.
Description
Technical Field
The invention relates to the technical field of organic synthesis, in particular to a method for improving the atomic utilization rate of ethylene carbonate.
Background
The ethylene carbonate compound has larger dielectric constant and high ionic conductivity, can form a stable SEI film on the surface of the negative electrode, and is a common solvent in electrolyte.
The additive is a substance with specific functions in the electrolyte, has lower content, and can obviously improve the electrochemical performance of the battery. The electrolyte generally contains various additives, namely Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC), which are the most commonly used electrolyte additives at present, and an SEI/CEI film can be formed on the surface of an electrode, so that lithium ions can freely enter and exit, and solvent molecules are difficult to pass through, thereby realizing the effects of maintaining the stable performance of electrode materials and improving the capacity and cycle performance of the battery. The raw materials of Vinylene Carbonate (VC) and fluoroethylene carbonate (FEC) are both Ethylene Carbonate (EC). It is seen that from the viewpoint of the market and production of electrolyte, it is important to improve the atomic utilization of ethylene carbonate.
The current common process for producing fluoroethylene carbonate in industry is that Ethylene Carbonate (EC) is chlorinated to generate chloroethylene carbonate (CEC), and the chloroethylene carbonate is fluorinated to generate fluoroethylene carbonate (FEC). In the first process, the vinyl carbonate is chlorinated to form chloroethylene carbonate, and by-products dichloro and polychlorinated ethylene carbonate are inevitably easily formed. Before the second step process, the byproducts are required to be removed, the process flow is complicated, the atom utilization rate is low, and even the byproducts are not completely removed, the byproducts are brought into the second step process and fluorinated together with the chloroethylene carbonate to generate difluoro-ethylene carbonate and poly-fluoro-ethylene carbonate. In industrial production, rectification is needed to obtain a refined FEC pure product, which clearly increases the production cost of FEC and reduces the atomic utilization rate of ethylene carbonate.
How to optimize the process route and improve the atom utilization rate of the ethylene carbonate is a problem to be solved urgently.
Disclosure of Invention
In order to solve the technical problems, the invention researches the process optimization of the process for synthesizing chloroethylene carbonate and fluoroethylene carbonate by using ethylene carbonate, thereby improving the atom utilization rate of ethylene carbonate.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
a method for improving the atomic utilization of ethylene carbonate comprising the steps of:
s1, reacting ethylene carbonate with chlorine to obtain a reaction solution;
s2, crystallizing the reaction solution at low temperature to obtain ethylene carbonate crystals and mother solution containing chlorinated ethylene carbonate; reacting mother liquor containing chlorinated ethylene carbonate with KF to prepare the fluorinated ethylene carbonate.
Preferably, in the step S1, the reaction conversion rate of the ethylene carbonate and the chlorine gas to generate chloroethylene carbonate is controlled to be 5-50%. Further, the reaction conversion rate of the ethylene carbonate and chlorine to generate chloroethylene carbonate is controlled to be 25-35%.
Preferably, in the step S1, the ethylene carbonate is ethylene carbonate crystals; the ethylene carbonate crystal is put into a reaction vessel and heated to be liquid, and chlorine is introduced under the stirring state.
Preferably, in the step S1, the introducing rate of the chlorine is 600mL/min.
Preferably, in the step S1, the reaction temperature is 65 to 70 ℃; the reaction time is 2-8 h.
Specifically, crystals of Ethylene Carbonate (EC) were added to a photoreaction flask, the flask was heated at 65 ℃ and the ethylene carbonate was gradually melted to a liquid state, and finally maintained at 65 ℃ and mechanical stirring was turned on. Then, dry chlorine gas is introduced into the photoreaction bottle at a rate of 600mL/min, the reaction is gentle and exothermic, and the temperature in the photoreaction bottle is controlled to be constant at 65 ℃. Samples were taken after a period of reaction and yield was tested by GC. Controlling the reaction progress by reducing the conversion rate of EC to synthesize CEC in the process; in the specific CEC synthesis process, the reaction is controlled to be about 25-35% in conversion rate. The reduction in reaction conversion results in reduced by-product production.
The control of the reaction conversion rate can be selected by those skilled in the art with more practical reaction conditions, and can be specifically realized by adopting a mode of controlling the reaction time and the like.
Preferably, in the step S2, the temperature of the low-temperature crystallization is-20 to 10 ℃;
preferably, the vinyl carbonate crystals are heated to melt and then chlorinated again to obtain chloroethylene carbonate.
Specifically, the reaction solution is placed at a low temperature of between 20 ℃ below zero and 10 ℃ for crystallization, so that EC crystals are separated out, mother liquor containing CEC is obtained, the mother liquor containing CEC reacts with a certain amount of KF to prepare FEC, and after the EC crystals are heated and melted, chlorination is carried out again to obtain chloroethylene carbonate. The KF is used in an amount of 1.05eq (hereinafter abbreviated as 1.05 eq), and the reaction time of the CEC-containing mother liquor with KF may be 2 to 5 hours.
Compared with the prior art, the invention has the beneficial effects that:
the invention aims to solve the problem of improving the atom utilization rate of the ethylene carbonate through optimizing a process route. The method comprises the steps of chloridizing ethylene carbonate to generate chloroethylene carbonate, crystallizing the system directly at a certain temperature, separating out ethylene carbonate, filtering, and taking filtrate (mother liquor containing chloroethylene carbonate) for fluoridation to generate fluoroethylene carbonate. The vinyl carbonate crystal is melted and then chlorinated to generate chloroethylene carbonate, so that the cycle is realized, the atom utilization rate of the vinyl carbonate is improved, the complex post-treatment is avoided, the impurity content of the FEC synthesized by using high-purity CEC is low, the use amount of potassium fluoride is reduced, and meanwhile, the byproducts are less, the post-treatment is simpler, so that the production cost is also reduced.
Detailed Description
The invention is further described in terms of specific examples, illustrative examples and illustrations of which are provided herein to illustrate the invention, but are not to be construed as limiting the invention. In the following examples, unless otherwise specified, all the raw materials used were commercial industrial grade products.
Example 1
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 3h to obtain a reaction solution A (EC conversion rate 33.01%); the reaction solution from the above step was subjected to crystallization at-10℃to precipitate EC crystals, which were filtered to give a solid weight of 629.71g (for the next chlorination reaction) and 500.21g of CEC-containing filtrate (CEC content: 457.11 g).
The fluorination process comprises the following steps: 300g of the filtrate containing CEC is taken, 227.64g of potassium fluoride (1.05 eq.) and 300g of dimethyl carbonate are added for reaction at 80 ℃, 517.15g of filtrate is obtained by filtration after the reaction is completed, 291.63g of solvent is recovered at 70 ℃ under-96 KPa, 225.45g of crude FEC is obtained by distillation at 100 ℃ under-99 KPa. The crude FEC product is melted and crystallized to obtain 216.44g of FEC finished product, the yield is 83.34 percent, and the purity is 99.97 percent.
Example 2
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 2h to obtain a reaction solution A (EC conversion rate is 24.40%); the reaction solution from the above step was subjected to crystallization at-10℃to precipitate EC crystals, which were filtered to give a solid weight of 711.55g (for the next chlorination reaction) and 384.52g of CEC-containing filtrate (CEC content: 337.76 g).
300g of filtrate containing CEC is taken, 168.20g of potassium fluoride (1.05 eq.) and 300g of dimethyl carbonate are added for reaction at 80 ℃, and the 208.04g of FEC finished product is obtained through filtration, desolventizing (solvent is recovered at 70 ℃ below 96 KPa), distillation (crude FEC product is obtained through distillation at 100 ℃), crystallization (the crude FEC product is obtained through melt crystallization), and the yield is 80.11%, and the purity is 99.96%.
Example 3
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 4 hours to obtain a reaction solution A (EC conversion rate 48.79%); the reaction solution from the above step was subjected to crystallization at-10℃to precipitate EC crystals, which were filtered to give a solid weight of 434.16g (for the next chlorination reaction) and 763.14g of CEC-containing filtrate (CEC content: 656.88 g).
300g of filtrate containing CEC is taken, 327.12g of potassium fluoride (1.05 eq.) and 300g of dimethyl carbonate are added for reaction at 80 ℃, and the final product of FEC 203.86g is obtained by filtration, desolventizing (solvent is recovered at 70 ℃ below 96 KPa), distillation (crude FEC is obtained by distillation at 100 ℃), crystallization (the crude FEC is obtained by melting and crystallization), and the yield 78.50% and the purity of the final product of FEC are 99.91%.
Example 4
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 3h to obtain a reaction solution A (EC conversion rate 32.57%); the reaction solution from the above step was subjected to crystallization at-20℃to precipitate EC crystals, which were filtered to give a solid weight of 636.13g (for the next chlorination reaction) and 492.02g of CEC-containing filtrate (CEC content: 451.10 g).
300g of filtrate containing CEC is taken, 224.65g of potassium fluoride (1.05 eq.) and 300g of dimethyl carbonate are added for reaction at 80 ℃, and the final product of FEC 217.14g is obtained by filtration, desolventizing (solvent is recovered at 70 ℃ below 96 KPa), distillation (crude FEC is obtained by distillation at 100 ℃), crystallization (the crude FEC is obtained by melting and crystallization), and the yield 83.62% and the purity of the final product of FEC are 99.96%.
Example 5
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 3h to obtain a reaction solution A (EC conversion rate is 32.88%); the reaction solution of the above step was subjected to crystallization at 0℃to precipitate EC crystals, which were filtered to give a solid weight of 529.51g (for the next batch of chlorination), and 599.81g of CEC-containing filtrate (CEC content: 455.61 g) was obtained.
300g of filtrate containing CEC is taken, 226.90g of potassium fluoride (1.05 eq.) and 300g of dimethyl carbonate are added for reaction at 80 ℃, and the final product of FEC 179.90g is obtained by filtration, desolventizing (solvent is recovered at 70 ℃ below 96 KPa), distillation (crude FEC is obtained by distillation at 100 ℃), crystallization (the crude FEC is obtained by melting and crystallization), and the yield 69.28% and the purity of the final product of FEC are 99.87%.
Example 6
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 3h to obtain a reaction solution A (EC conversion rate is 33.14%); the reaction solution of the above step was subjected to crystallization at 10℃to precipitate EC crystals, which were filtered to give a solid weight of 117.14g (for the next batch of chlorination), and 1013.23g of CEC-containing filtrate (CEC content: 459.12 g) was obtained.
300g of filtrate containing CEC is taken, 228.64g of potassium fluoride (1.05 eq.) and 300g of dimethyl carbonate are added for reaction at 80 ℃, and the final product of FEC 107.32g is obtained by filtration, desolventizing (solvent is recovered at 70 ℃ under minus 96 KPa), distillation (crude FEC is obtained by distillation at 100 ℃), crystallization (the crude FEC is obtained by melting and crystallization), and the yield is 41.32% and the purity is 99.81%.
Comparative example 1
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 6h to obtain a reaction solution A (EC conversion rate 73.19%); and (3) placing the reaction solution in the previous step at the temperature of minus 10 ℃ for crystallization, wherein crystals are not precipitated.
Comparative example 2
1Kg of Ethylene Carbonate (EC) was added to a photoreaction flask of a photoreaction generator, the photoreaction flask was heated to 65℃and mechanical stirring was turned on. Then introducing dry chlorine gas into the photoreaction bottle at the rate of 600mL/min, reacting gently and exothermically, controlling the temperature in the photoreaction bottle to be constant at 65-70 ℃ and reacting for 8 hours to obtain a reaction solution A (EC conversion rate 97.58%); and (3) placing the reaction solution in the previous step at the temperature of minus 10 ℃ for crystallization, wherein crystals are not precipitated.
The data of the yield test of the reaction solution A obtained in the above process by GC, the data of the reaction process and the data of the reaction product are shown in Table 1.
TABLE 1
By comparing the above examples, it is evident that the cost of fluoroethylene carbonate is indirectly controlled by controlling the chlorination reaction process. In the first chlorination step, the conversion of EC increases with increasing reaction time, with a corresponding increase in dichloro and polychlorinated impurities. According to the method, when the reaction conversion rate of ethylene carbonate and chlorine gas to generate chloroethylene carbonate is controlled to be 25-35%, the amounts of dichloro and polychlorinated impurities in the chlorination process can be controlled to be below 0.15% (i.e. impurity amount is less than 0.15%), unreacted EC is directly separated out and removed at the temperature of minus 10 ℃, mother liquor is directly used for fluorination reaction, the amount of polychlorinated impurities in the system is reduced, the consumption of potassium fluoride can be obviously reduced, byproducts in the fluorination process are further reduced, FEC can be separated out by a crystallization method, rectification and purification operation is avoided, and the post-treatment cost is reduced. In addition, the product loss caused by the heat stability of the FEC in the post-treatment process of industrial production is serious, and the production cost of the FEC is obviously increased. In summary, the method of the invention has significant advantages.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.
Claims (8)
1. A method for improving the atomic utilization rate of ethylene carbonate, which is characterized by comprising the following steps: the method comprises the following steps:
s1, reacting ethylene carbonate with chlorine to obtain a reaction solution;
s2, crystallizing the reaction solution at low temperature to obtain ethylene carbonate crystals and mother solution containing chlorinated ethylene carbonate; reacting mother liquor containing chlorinated ethylene carbonate with KF to prepare the fluorinated ethylene carbonate.
2. A method for improving the atomic utilization of ethylene carbonate according to claim 1, wherein: in the step S1, the reaction conversion rate of the ethylene carbonate and chlorine to generate chloroethylene carbonate is controlled to be 5-50%.
3. A method for improving the atomic utilization of ethylene carbonate according to claim 1, wherein: the conversion rate of the reaction of the ethylene carbonate and the chlorine to generate chloroethylene carbonate is controlled between 25 and 35 percent.
4. A method for improving the atomic utilization of ethylene carbonate according to claim 1, wherein: in the step S1, ethylene carbonate is ethylene carbonate crystal; the ethylene carbonate crystal is put into a reaction vessel and heated to be liquid, and chlorine is introduced under the stirring state.
5. The method for improving the atomic utilization of ethylene carbonate according to claim 4, wherein: in the step S1, the introducing rate of the chlorine is 600mL/min.
6. A method for increasing the atom utilization of ethylene carbonate according to any one of claims 2 or 3, wherein: in the step S1, the reaction temperature is 65-70 ℃; the reaction time is 2-8 h.
7. A method for improving the atomic utilization of ethylene carbonate according to claim 1, wherein: in the step S2, the temperature of the low-temperature crystallization is-20-10 ℃.
8. A method for improving the atomic utilization of ethylene carbonate according to claim 1, wherein: in the step S2, the vinyl carbonate crystal is heated and melted and then chloridized again to obtain chloroethylene carbonate.
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