CN113336737A - Method for preparing high-purity chloroethylene carbonate by continuous two-stage liquid phase reaction - Google Patents
Method for preparing high-purity chloroethylene carbonate by continuous two-stage liquid phase reaction Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity chloroethylene carbonate by continuous two-stage liquid phase reaction, which comprises the steps of carrying out two-stage liquid phase reaction on liquid chlorine, ethylene carbonate and a catalyst at high temperature and high pressure to produce chloroethylene carbonate, and separating chloroethylene carbonate, dichloroethylene carbonate and unreacted ethylene carbonate from reaction products by high vacuum rectification to obtain high-purity chloroethylene carbonate.
Description
Technical Field
The invention belongs to the field of chemical engineering, and particularly relates to a method for preparing high-purity chlorinated ethylene carbonate through continuous two-stage liquid phase reaction.
Background
With the development of lithium ion batteries, the amount of electrolyte additives fluoroethylene carbonate (FEC) and Vinylene Carbonate (VC) is rapidly increasing. FEC may improve the cycle life of a battery, increase the safety of a battery, and may improve the low temperature life of a three-cell battery. The chloroethylene carbonate (CEC) is mainly used for preparing fluoroethylene carbonate and vinylene carbonate of lithium battery electrolyte, the fluoroethylene carbonate can be produced by reacting with potassium fluoride, and the vinylene carbonate can be produced under the action of a catalyst. The high-purity chloroethylene carbonate can also be directly used as a flame retardant additive of the lithium battery electrolyte, so that the cycle performance of the lithium battery electrolyte is improved, and the service life is prolonged. Both lithium ion battery electrolyte additives with larger dosage are produced by taking CEC as a raw material, so the demand of CEC is obviously increased along with the increase of the demand of FEC and VC.
The prior technical routes for preparing the chlorinated ethylene carbonate comprise a chlorination reagent substitution method, a direct chlorine substitution method, a solvent chlorine substitution method, a phosgene method and the like, but most of the methods are in a kettle type reactor, the process is complex, and the disadvantages of high content of byproducts, low reaction efficiency and yield, low product purity and the like caused by uneven chlorine dispersion exist. In addition, ethylene dichlorocarbonate produced in the reaction is not easily separated.
CN108003131A discloses a green production method of chloroethylene carbonate, which adopts the reaction of chlorine and ethylene carbonate under the catalysis of ultraviolet light to generate chloroethylene carbonate, and also adds vinylene carbonate but does not describe the function of vinylene carbonate in the method. The chlorinated ethylene carbonate product is obtained in a tubular falling film crystallizer, but the method does not show a solution for removing the byproduct of the chlorinated ethylene carbonate, the content of the chlorinated ethylene carbonate is only 90-95%, the purity of the product cannot be guaranteed, and the requirement of a lithium battery user cannot be met.
CN108586423A discloses a production process of a novel chloroethylene carbonate, which adopts the reaction of chlorine and ethylene carbonate under the catalysis of ultraviolet light to generate chloroethylene carbonate. However, in the patent, vinylene carbonate is added in the step 1), and the reaction of chlorine gas with the vinylene carbonate occurs in the step 3), so that the reaction mechanism has errors according to the conventional theory. And the subsequent chloroethylene carbonate product is subjected to rectification in a rectifying tower to obtain the chloroethylene carbonate product. The inventor verifies that the simple rectifying still is difficult to obtain products with the purity of 99-99.5%. Further, this method does not describe a solution for removing ethylene dichlorocarbonate as a by-product after chlorination.
CN109942536A discloses a method for preparing high-purity chloroethylene carbonate by reactive distillation, which adopts a reactive distillation device to combine a reaction kettle and a distillation tower to produce chloroethylene carbonate. The equipment used by the method is complex and only suitable for intermittent production, the reaction time of one kettle needs 8-10 hours, and the rectification needs to be carried out in the equipment, the production time of a batch of products exceeds 12 hours, and the production efficiency is low. The mass fraction of the rectified chloroethylene carbonate is about 95%, and the requirement of lithium battery users cannot be met.
CN110003164A discloses a method for preparing chlorinated ethylene carbonate by adopting a two-stage reaction, which comprises the following steps: the method comprises the following steps: adding a certain amount of ethylene carbonate into a first-stage chlorination reaction kettle and a second-stage chlorination reaction kettle; step two: preparing an initiator solution from the initiator and ethylene carbonate and transferring the initiator solution into a chlorination high-position dropping kettle; step three: respectively introducing chlorine gas into a first-stage chlorination reaction kettle and a second-stage chlorination reaction kettle, simultaneously heating the first-stage chlorination reaction kettle and the second-stage chlorination reaction kettle, and slowly dropwise adding an initiator solution into the first-stage chlorination reaction kettle and the second-stage chlorination reaction kettle; step four: after reacting for a period of time, finishing the reaction to obtain the chloroethylene carbonate. The process greatly improves the use efficiency of chlorine and reduces the load of a tail gas treatment device through two-stage chlorination reaction. The initiator is one or a mixture of a plurality of azodiisobutyronitrile, azodiisoheptonitrile, azodiisobutyronitrile dimethyl ester, benzoyl peroxide and diisopropyl peroxydicarbonate. The second-order reaction disclosed in this patent is carried out with chlorine gas and does not disclose a method for removing ethylene dichlorocarbonate as a by-product, and it is difficult to obtain ethylene chlorocarbonate of high purity.
Through comparative analysis and actual production experience, the following problems are found in the prior art:
1. the reaction kettle is basically used for the reaction of chlorine and ethylene carbonate, the intermittent production is realized, and the production efficiency is low;
2. the ethylene dichlorocarbonate which is a byproduct generated by the reaction of chlorine and ethylene carbonate is not easy to separate, and most patents do not provide a separation process.
Disclosure of Invention
The invention aims to provide a method for preparing high-purity chloroethylene carbonate by continuous two-stage liquid phase reaction, which can continuously produce high-purity chloroethylene carbonate and simultaneously remove byproduct dichloroethylene carbonate. The purity of the chloroethylene carbonate product is guaranteed.
The invention relates to a method for preparing high-purity chloroethylene carbonate, which comprises the steps of carrying out two-stage liquid phase reaction on liquid chlorine, ethylene carbonate and a catalyst at high temperature and high pressure, and separating chloroethylene carbonate from dichloroethylene carbonate by high vacuum rectification of reactant products to obtain high-purity chloroethylene carbonate. The invention uses liquid chlorine to react with ethylene carbonate, which can greatly shorten the chlorination reaction time, greatly improve the reaction rate, and has stronger reaction selectivity, reduced side reaction by-products and greatly improved main product yield.
In one embodiment, the method for preparing high-purity chlorinated ethylene carbonate comprises the following steps,
1) carrying out liquid phase reaction on liquid chlorine, ethylene carbonate and a catalyst in a high-temperature high-pressure first-stage reactor, wherein the high temperature is 70-100 ℃, and the high pressure is 2.0-3.5 Mpa;
2) carrying out liquid phase reaction on the reaction liquid obtained in the step 1) in a high-temperature high-pressure secondary reactor, wherein the high temperature is 80-110 ℃, and the high pressure is 2.0-3.5 Mpa;
3) and (3) carrying out high vacuum rectification on the reaction product obtained in the step (2) to obtain high-purity chloroethylene carbonate, wherein the high vacuum pressure is 300-600 Pa, and the temperature is 70-100 ℃.
In the above embodiment, in the method of the present invention, in the first-stage reactor, the evaporated light component is condensed and returned to the first-stage reactor for continuous reaction; in the secondary reactor, the evaporated light component is condensed and returned to the secondary reactor for continuous reaction,
in the above embodiments, the process of the invention, the primary reactor, starts with ethylene carbonate: the mass ratio of the catalyst is 8-12: 1, ethylene carbonate: the mol ratio of liquid chlorine is 2-3: 1.
in the above embodiment, the rectification in step 3) of the process of the present invention separates ethylene chlorocarbonate from ethylene dichlorocarbonate, and removes ethylene dichlorocarbonate.
In the above embodiments, the reactor of the process of the present invention is preferably a reaction column, preferably a chlorination reaction column.
In the above method of the present invention, the catalyst is azobisisobutyronitrile, benzoyl peroxide or a mixture of the two.
In a specific embodiment, the invention relates to a method for preparing high-purity chloroethylene carbonate by a continuous two-stage liquid phase reaction, which comprises the following steps:
1) adding the ethylene carbonate after pre-melting, the ethylene carbonate recycled in the working section, a catalyst and liquid chlorine into a primary chlorination reaction tower T1, wherein the liquid chlorine and the ethylene carbonate react under the action of the catalyst at high temperature and high pressure, and a heat source of the primary chlorination reaction tower is provided by a steam heating heat exchanger E1. The gas phase of the light components at the top of the tower is discharged from the top of the tower, condensed by a condenser E2 and then enters a reflux tank V1, the non-condensable gas is discharged from the top of V1, and the condensed liquid is totally refluxed to a chlorination reaction tower T1 by a reflux pump P2;
2) pressurizing the kettle liquid of the first-stage chlorination reaction tower T1 in the step 1) through a feed pump P1, then sending the kettle liquid into a second-stage chlorination reaction tower T2, continuously reacting unreacted liquid chlorine and ethylene carbonate under the action of a catalyst at high temperature and high pressure, and providing a heat source of the second-stage chlorination reaction tower by a steam heating heat exchanger E3. The gas phase of the light components at the top of the tower is discharged from the top of the tower, condensed by a condenser E4 and then enters a reflux tank V2, the non-condensable gas is discharged from the top of V2, and the condensed liquid is totally refluxed to a chlorination reaction tower T2 by a reflux pump P4;
3) pressurizing the kettle liquid of the secondary chlorination reaction tower T2 in the step 2) by a feed pump P3, and then sending the kettle liquid to a high vacuum rectification tower T3, wherein the heat source of the rectification tower T3 is provided by a steam heating heat exchanger E5. Byproducts of dichloroethylene carbonate and residual hydrogen chloride gas are extracted from the tower top, qualified product chloroethylene carbonate is extracted from the side line, and the chloroethylene carbonate extracted from the tower bottom is sent to a feeding pipeline of a first-stage chlorination reaction tower T1 through a discharge pump P5.
In the above embodiment, the method of the present invention, the ethylene carbonate added to the primary chlorination reaction column in step 1): the mass ratio of the catalyst is 8-12: 1, ethylene carbonate: the mol ratio of liquid chlorine is 2-3: 1, the catalyst is azobisisobutyronitrile, benzoyl peroxide or a mixture of the azobisisobutyronitrile and the benzoyl peroxide; the temperature of the primary chlorination reaction tower in the step 1) is 70-100 ℃, and the pressure is 2.0-3.5 MPa; the temperature of the secondary chlorination reaction tower in the step 2) is 80-110 ℃, and the pressure is 2.0-3.5 MPa; and 3) 300-600 Pa of the high-vacuum rectifying tower, wherein the temperature of the top of the tower is 70-100 ℃.
The method has the beneficial effects that:
the invention adopts continuous two-stage liquid phase reaction and combines with rectification technology, and can continuously produce high-purity chloroethylene carbonate. The invention has the advantages that:
1. the high-purity chlorinated ethylene carbonate with the purity of 99.9-99.99 percent can be obtained by the process route, and the requirements of lithium battery users can be met;
2. the process adopts a two-stage liquid phase reaction combined rectification process, is continuous operation, and further improves the productivity of the device while ensuring stable product quality;
3. the process uses liquid chlorine to react with ethylene carbonate, so that the reaction time can be greatly shortened, the reaction selectivity is stronger, byproducts are lower, and a high-purity main product is easier to obtain.
Drawings
FIG. 1 is a schematic diagram of a reaction process flow.
Detailed Description
The invention is further described below with reference to examples: but are representative. To aid in understanding the spirit of the invention and not to limit the scope of the invention in any way.
The reaction process flow in the following examples is shown in FIG. 1.
Example 1
Step 1): adding 1000Kg of ethylene carbonate (containing ethylene carbonate recycled in workshop section) after pre-melting, azodiisobutyronitrile and liquid chlorine serving as catalysts into a primary chlorination reaction tower T1, wherein the ethylene carbonate: the mass ratio of the azodiisobutyronitrile is 10: 1, ethylene carbonate: the molar ratio of liquid chlorine is 2; 1, controlling the pressure of a first-stage chlorination reaction tower to be 3.0MPa and the temperature to be 90 ℃. Discharging gas phase of light components (hydrogen chloride and a small amount of ethylene carbonate and the like carried by the hydrogen chloride) at the top of the tower from the top of the tower, condensing the gas phase by a condenser E2, and then entering a reflux tank V1, discharging non-condensable gas hydrogen chloride from the top of V1, fully refluxing condensate (containing ethylene carbonate) to a chlorination reaction tower T1 by a reflux pump P2, wherein the retention time of the added ethylene carbonate, catalyst, liquid chlorine and the like in a primary chlorination reaction tower is 3 hours;
step 2): pressurizing the kettle liquid of the first-stage chlorination reaction tower T1 in the step 1) through a feed pump P1, then sending the kettle liquid into a second-stage chlorination reaction tower T2, continuously reacting unreacted liquid chlorine and ethylene carbonate under the action of a catalyst at high temperature and high pressure, and controlling the pressure of the second-stage chlorination reaction tower T2 to be 3.0MPa and the temperature to be 100 ℃. And a light component gas phase at the top of the tower is discharged from the top of the tower, condensed by a condenser E4 and then enters a reflux tank V2, non-condensable gas hydrogen chloride is discharged from the top of V2 and recycled, and the condensed liquid is totally refluxed to a chlorination reaction tower T2 by a reflux pump P4. The retention time of the mixed liquid from the first-stage chlorination reaction tower in the second-stage chlorination reaction tower T2 is 3 hours;
step 3): pressurizing the kettle liquid of the secondary chlorination reaction tower T2 in the step 2) by a feed pump P3, and then sending the kettle liquid to a high vacuum rectification tower T3, wherein the pressure of the rectification tower T3 is controlled to be 500Pa, and the temperature is controlled to be 90.5 ℃. Byproducts dichloroethylene carbonate and residual hydrogen chloride gas are extracted from the tower top, 1353.89Kg of qualified chloroethylene carbonate is extracted from the lateral line, the yield is 97.32 percent, and the purity is 99.96 percent. Unreacted ethylene carbonate extracted from the tower bottom is sent to a feed line of a first-stage chlorination reaction tower T1 through a discharge pump P5.
Example 2
Example 2 the ethylene carbonate feed rate was the same as that of example 1, except that the parameters were different, and in example 2, in step 1), the ethylene carbonate: the mass ratio of the azodiisobutyronitrile is 8: 1, ethylene carbonate: the molar ratio of liquid chlorine is 3: 1, the pressure of a first-stage chlorination reaction tower is 2.0MPa, and the temperature is 100 ℃. The retention time of each component in a first-stage chlorination reaction tower T1 is 2 hours;
the pressure of the secondary chlorination reaction tower in the step 2) is 2.0MPa, and the temperature is 110 ℃. The retention time of each component in a first-stage chlorination reaction tower T1 is 2 hours;
in the step 3), the pressure of the rectifying tower is 300pa, and the temperature is 70 ℃. 1334.00Kg of chlorinated ethylene carbonate which is a qualified product is obtained, the yield is 95.89%, and the purity is 99.91%.
Example 3
Example 3 the ethylene carbonate feed rate was the same as that of example 1, except that the parameters were different, and in example 3, in step 1), the ethylene carbonate: the mass ratio of the azodiisobutyronitrile is 12: 1, ethylene carbonate: the molar ratio of liquid chlorine is 3: 1, the pressure of a first-stage chlorination reaction tower is 3.5MPa, and the temperature is 70 ℃. The retention time of each component in a first-stage chlorination reaction tower T1 is 2 hours;
the pressure of the secondary chlorination reaction tower in the step 2) is 3.5MPa, and the temperature is 80 ℃. The retention time of each component in a first-stage chlorination reaction tower T1 is 2 hours;
in the step 3), the pressure of the rectifying tower is 600pa, and the temperature is 100 ℃. 1343.61Kg of qualified chloroethylene carbonate is obtained, the yield is 96.65 percent, and the purity is 99.92 percent.
Comparative example 1
Comparative example 1 the same batch as in example 1, except for the different parameters, in comparative example 1, step 1), ethylene carbonate: the mass ratio of the azodiisobutyronitrile is 7: 1, ethylene carbonate: the molar ratio of liquid chlorine is 1: 1, the pressure of a first-stage chlorination reaction tower is 1.8MPa, and the temperature is 70 ℃. The retention time of each component in a first-stage chlorination reaction tower T1 is 2 hours;
the pressure of the secondary chlorination reaction tower in the step 2) is 1.9MPa, and the temperature is 80 ℃. The retention time of each component in a first-stage chlorination reaction tower T1 is 1 hour;
in the step 3), the pressure of the rectifying tower is 700pa, and the temperature is 100 ℃.
1238.43Kg of chlorinated ethylene carbonate which is a qualified product is obtained, the yield is 89.02 percent, and the purity is 99.76 percent.
The experimental data are as follows by integrating the product yield and product concentration of each example and comparative example:
| yield of chlorinated ethylene carbonate/% | Mass fraction/% of chlorinated ethylene carbonate | |
| Example 1 | 97.32 | 99.96 |
| Example 2 | 95.89 | 99.91 |
| Example 3 | 96.65 | 99.92 |
| Comparative example 1 | 89.02 | 99.76 |
The above examples are merely representative, and any simple modification or variation made within the spirit of the present invention is within the scope of the present invention.
Claims (9)
1. A method for preparing high-purity chloroethylene carbonate comprises the steps of carrying out two-stage liquid phase reaction on liquid chlorine, ethylene carbonate and a catalyst at high temperature and high pressure, and separating chloroethylene carbonate from dichloroethylene carbonate through high-altitude rectification of a reactant product to obtain the high-purity chloroethylene carbonate.
2. The method of claim 1, comprising the steps of,
1) carrying out liquid phase reaction on liquid chlorine, ethylene carbonate and a catalyst in a primary reactor at high temperature and high pressure, wherein the high temperature is 70-100 ℃, and the high pressure is 2.0-3.5 Mpa;
2) carrying out liquid phase reaction on the reaction liquid obtained in the step 1) in a secondary reactor at high temperature and high pressure, wherein the high temperature is 80-110 ℃, and the high pressure is 2.0-3.5 Mpa;
3) and (3) carrying out high vacuum rectification on the reaction product obtained in the step (2) to obtain high-purity chloroethylene carbonate, wherein the high vacuum pressure is 300-600 Pa, and the temperature of a rectification tower is 70-100 ℃.
3. The process of claim 2 wherein the distilled light components are condensed in the first reactor and returned to the first reactor for further reaction.
4. The process of claim 2, wherein the light components distilled off in the secondary reactor are condensed and returned to the secondary reactor for further reaction.
5. The process of claim 2, in the primary reactor, the starting materials ethylene carbonate: the mass ratio of the catalyst is 8-12: 1, ethylene carbonate: the mol ratio of liquid chlorine is 2-3: 1.
6. the process of claim 2 or 5, wherein the catalyst is azobisisobutyronitrile, benzoyl peroxide, or a mixture of the two.
7. The method according to claim 2, wherein the rectification in step 3) separates ethylene chlorocarbonate from ethylene dichlorocarbonate, and removes ethylene dichlorocarbonate.
8. The process according to claim 5, wherein the mass ratio of ethylene carbonate to azobisisobutyronitrile is 10: 1, ethylene carbonate: the molar ratio of liquid chlorine is 2: 1.
9. the method according to claim 2, wherein the pressure of the first reaction tower is 3.0MPa and the temperature is 90 ℃ in the step 1), and the pressure of the second reaction tower is 3.0MPa and the temperature is 100 ℃ in the step 2).
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| CN202110606063.1A CN113336737A (en) | 2021-05-31 | 2021-05-31 | Method for preparing high-purity chloroethylene carbonate by continuous two-stage liquid phase reaction |
| CN202210019365.3A CN114163413B (en) | 2021-05-31 | 2022-01-10 | Method for preparing high-purity chloroethylene carbonate by continuous double-stage liquid phase reaction |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912581A (en) * | 2021-09-28 | 2022-01-11 | 四平市精细化学品有限公司 | Preparation method of high-purity chlorinated ethylene carbonate |
| CN114011107A (en) * | 2021-11-18 | 2022-02-08 | 中建安装集团有限公司 | Novel device and method for continuously producing high-purity vinylene carbonate |
| CN116462655A (en) * | 2022-03-02 | 2023-07-21 | 上海惠和化德生物科技有限公司 | Process for preparing chloroethylene carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102596930A (en) * | 2009-10-21 | 2012-07-18 | 苏威氟有限公司 | Method for the manufacture of fluorinated ethylene carbonates |
| CN106810528A (en) * | 2017-01-06 | 2017-06-09 | 淮安瀚康新材料有限公司 | A kind of method that microchannel plate should prepare chlorocarbonic acid vinyl acetate |
| CN109942536A (en) * | 2019-04-16 | 2019-06-28 | 张家港瀚康化工有限公司 | A kind of reactive distillation prepares high-purity chloro for the method for ethylene carbonate |
| CN110003164A (en) * | 2019-05-23 | 2019-07-12 | 泰兴华盛精细化工有限公司 | A kind of synthesis technology of chlorocarbonic acid vinyl acetate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912581A (en) * | 2021-09-28 | 2022-01-11 | 四平市精细化学品有限公司 | Preparation method of high-purity chlorinated ethylene carbonate |
| CN113912581B (en) * | 2021-09-28 | 2023-08-29 | 四平市精细化学品有限公司 | Preparation method of high-purity chloroethylene carbonate |
| CN114011107A (en) * | 2021-11-18 | 2022-02-08 | 中建安装集团有限公司 | Novel device and method for continuously producing high-purity vinylene carbonate |
| CN114011107B (en) * | 2021-11-18 | 2022-06-24 | 中建安装集团有限公司 | Novel device and method for continuously producing high-purity vinylene carbonate |
| CN116462655A (en) * | 2022-03-02 | 2023-07-21 | 上海惠和化德生物科技有限公司 | Process for preparing chloroethylene carbonate |
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