CN114907307A - Continuous production process of chlorinated ethylene carbonate - Google Patents
Continuous production process of chlorinated ethylene carbonate Download PDFInfo
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- CN114907307A CN114907307A CN202210534540.2A CN202210534540A CN114907307A CN 114907307 A CN114907307 A CN 114907307A CN 202210534540 A CN202210534540 A CN 202210534540A CN 114907307 A CN114907307 A CN 114907307A
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- Prior art keywords
- ethylene carbonate
- chlorine
- continuous production
- production process
- gas
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a continuous production process of chlorinated ethylene carbonate, which comprises a distillation tower and a heat exchanger, wherein a liquid distributor is fixedly arranged near the middle position in the distillation tower, a nitrogen interface is fixedly arranged near the middle position on one side of the distillation tower, a feeding pipe is fixedly arranged near the middle position on the other side of the distillation tower, a vacuum interface is fixedly arranged at the top of the distillation tower, a centrifugal pump is arranged at the bottom of the distillation tower, an inlet of the centrifugal pump is communicated with an outlet at the bottom of the distillation tower, an outlet of the centrifugal pump is communicated with an inlet of the heat exchanger, and an outlet of the heat exchanger is communicated with the feeding pipe. The continuous production process of the chloroethylene carbonate reduces the distillation temperature of the tris (trimethylsilyl) phosphate, can distill the tris (trimethylsilyl) phosphate at a lower temperature, can obtain an electronic-grade product through one-time simple distillation, is simple and efficient, improves the product quality, and is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of lithium ion battery electrolyte additives, in particular to a continuous production process of chlorinated ethylene carbonate.
Background
The functional additive of the lithium ion battery electrolyte can improve the performance of an SEI film, the high and low temperature performance of the electrolyte, the conductivity of the electrolyte, the safety of the battery and the cycling stability of the battery. The vinylene carbonate is a novel organic film forming additive and an overcharge protection additive for the lithium ion battery, has good high and low temperature performance and an anti-gas expansion function, and can improve the capacity and the cycle life of the battery. The fluoroethylene carbonate can be reduced at a lower reduction potential, so that an SEI film with a compact structure and low resistance is formed on the surface of the negative electrode, and the capacity, low-temperature stability and cycling stability of the lithium ion battery are improved.
Chlorinated ethylene carbonate is a common intermediate raw material for preparing vinylene carbonate and fluoroethylene carbonate, chlorine and ethylene carbonate are commonly subjected to substitution reaction under the action of an initiator in industry to prepare chlorinated ethylene carbonate, but the existing process mostly adopts kettle type intermittent reaction, has long reaction time, more decomposition products and multi-substitution products, and has low yield, more byproducts, large waste treatment capacity and high cost.
Disclosure of Invention
The invention aims to provide a continuous production process of chlorinated ethylene carbonate, which aims to solve the problems of low yield, more byproducts, large waste treatment capacity and high cost caused by the fact that the prior art mostly adopts kettle type intermittent reaction, the reaction time is long, and more decomposition products and multi-substitution products are provided in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a continuous production process of chlorinated ethylene carbonate comprises a chlorine storage tank, a middle tank, a chlorine heat exchanger, a delivery pump, a gas-liquid mixer, a reaction kettle, a sprayer, an LED light source and a product storage tank, and comprises the following steps:
s1, heating chlorine from the chlorine storage tank through a chlorine heat exchanger;
s2, heating ethylene carbonate in a middle tank;
s3, fully mixing chlorine and ethylene carbonate in a gas-liquid mixer, fully atomizing the ethylene carbonate by high-pressure chlorine, spraying the ethylene carbonate into a reaction kettle through a spray head, introducing tail gas into a tail gas absorption system by an LED light source, and introducing a liquid product into a product storage tank.
And the heating temperature of the chlorine in the step S1 is 80-120 ℃.
The heating temperature of the vinyl carbonate in the step S2 is 70-100 ℃.
The flow rate of the chlorine gas in the step S3 is 200-400kg/h, and the mass ratio of the chlorine gas to the ethylene carbonate is 1: 0.7-0.9.
In the step S3, the LED light source is used with a wavelength of 300-500 nm.
And the output end at the top of the reaction kettle in the step S3 is connected with an exhaust system.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, chlorine is adopted to atomize the ethylene carbonate raw material to improve the gas-liquid mixing effect, and chlorination reaction is carried out under the initiation of the LED light source, so that the gas-liquid mixing effect is good, the gas-liquid contact time is short, the decomposed products and the multi-substituted products are few, and the byproducts and the energy consumption are greatly reduced; and the continuous production of the chlorinated ethylene carbonate is realized, the manual operation is reduced, the production efficiency is improved, and the method is suitable for large-scale production.
Drawings
FIG. 1 is a schematic view of the present invention.
In the figure: 1. a chlorine storage tank; 2. an intermediate tank; 3. a chlorine gas heat exchanger; 4. a delivery pump; 5. a gas-liquid mixer; 6. a reaction kettle; 7. a spray head; 8. an LED light source.
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.
Referring to fig. 1, the present invention provides the following technical solutions:
example 1
The chlorine gas is heated to 100 ℃ by a chlorine gas heat exchanger, the ethylene carbonate is heated to 80 ℃ in an intermediate tank, the chlorine gas flow is 300kg/h, the ethylene carbonate flow is 250kg/h, the wavelength of an LED light source is 350-450nm, the liquid product after the reaction is 337.2kg/h, the content of chloroethylene carbonate in the liquid product is 94.36 percent, the content of ethylene carbonate is 3.51 percent, the content of dichloroethylene carbonate is 0.48 percent, and the yield is 91.38 percent in a GC test.
Example 2
Chlorine gas is heated to 95 ℃ by a chlorine gas heat exchanger, ethylene carbonate is heated to 90 ℃ in an intermediate tank, the chlorine gas flow is 350kg/h, the ethylene carbonate flow is 250kg/h, the wavelength of an LED light source is 350-450nm, the liquid product after reaction is 341.1kg/h, the content of chlorinated ethylene carbonate in the liquid product is 95.28 percent, the content of ethylene carbonate is 2.16 percent, the content of dichloroethylene carbonate is 0.73 percent, and the yield is 93.36 percent in a GC test.
Example 3
Chlorine gas is heated to 100 ℃ by a chlorine gas heat exchanger, ethylene carbonate is heated to 90 ℃ in an intermediate tank, the chlorine gas flow is 320kg/h, the ethylene carbonate flow is 250kg/h, the wavelength of an LED light source is 350-450nm, the liquid product after reaction is 339.6kg/h, the content of chlorinated ethylene carbonate in the liquid product is 94.81 percent, the content of ethylene carbonate is 3.07 percent, the content of dichloroethylene carbonate is 0.66 percent, and the yield is 92.52 percent in a GC test.
The key equipment of the invention comprises a chlorine heat exchanger 3, a gas-liquid mixer 5, a reaction kettle 6 and an LED light source 8. Chlorine is heated from a chlorine storage tank 1 through a chlorine heat exchanger 3, ethylene carbonate is heated from an intermediate tank 2, the chlorine and the ethylene carbonate are fully mixed in a gas-liquid mixer 5, the ethylene carbonate is fully atomized by high-pressure chlorine and is sprayed into a reaction kettle 6 through a spray head 7, the chlorine is initiated by an LED light source 8, tail gas enters a tail gas absorption system, and a liquid product enters a product storage tank 9.
In summary, the following steps: according to the invention, chlorine is adopted to atomize the ethylene carbonate raw material to improve the gas-liquid mixing effect, and chlorination reaction is carried out under the initiation of the LED light source, so that the gas-liquid mixing effect is good, the gas-liquid contact time is short, the decomposed products and the multi-substituted products are few, and the byproducts and the energy consumption are greatly reduced; and the continuous production of the chlorinated ethylene carbonate is realized, the manual operation is reduced, the production efficiency is improved, and the method is suitable for large-scale production.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The utility model provides a serialization production technology of chlorinated ethylene carbonate, includes chlorine storage tank (1), pans (2), chlorine heat exchanger (3), delivery pump (4), gas-liquid mixer (5), reation kettle (6), shower nozzle (7), LED light source (8) and product storage tank (9), its characterized in that: the process comprises the following steps:
s1, heating chlorine from the chlorine storage tank (1) through the chlorine heat exchanger (3);
s2, heating ethylene carbonate in an intermediate tank (2);
s3, fully mixing chlorine and ethylene carbonate in a gas-liquid mixer (5), fully atomizing the ethylene carbonate by high-pressure chlorine, spraying the ethylene carbonate into a reaction kettle (6) through a spray head (7), initiating by an LED light source (8), introducing tail gas into a tail gas absorption system, and introducing a liquid product into a product storage tank (9).
2. The continuous production process of chlorinated ethylene carbonate according to claim 1, characterized in that: and the heating temperature of the chlorine in the step S1 is 80-120 ℃.
3. The continuous production process of chlorinated ethylene carbonate according to claim 1, characterized in that: the heating temperature of the ethylene carbonate in the step S2 is 70-100 ℃, and the ethylene carbonate is conveyed by the conveying pump (4).
4. The continuous production process of chlorinated ethylene carbonate according to claim 1, characterized in that: the flow rate of the chlorine gas in the step S3 is 200-400kg/h, and the mass ratio of the chlorine gas to the ethylene carbonate is 1: 0.7-0.9.
5. The continuous production process of chlorinated ethylene carbonate according to claim 1, characterized in that: in the step S3, the LED light source is used with a wavelength of 300-500 nm.
6. The continuous production process of chlorinated ethylene carbonate according to claim 1, characterized in that: and the output end at the top of the reaction kettle (6) in the step S3 is connected with an exhaust system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210534540.2A CN114907307A (en) | 2022-05-17 | 2022-05-17 | Continuous production process of chlorinated ethylene carbonate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210534540.2A CN114907307A (en) | 2022-05-17 | 2022-05-17 | Continuous production process of chlorinated ethylene carbonate |
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| CN114907307A true CN114907307A (en) | 2022-08-16 |
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| CN202210534540.2A Pending CN114907307A (en) | 2022-05-17 | 2022-05-17 | Continuous production process of chlorinated ethylene carbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115572279A (en) * | 2022-11-22 | 2023-01-06 | 山东孚日新能源材料有限公司 | Method for preparing chloroethylene carbonate by forced external circulation |
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2022
- 2022-05-17 CN CN202210534540.2A patent/CN114907307A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115572279A (en) * | 2022-11-22 | 2023-01-06 | 山东孚日新能源材料有限公司 | Method for preparing chloroethylene carbonate by forced external circulation |
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