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Method of preparing chloroethylene carbonate by adopting novel initiator

A technology for chlorinated ethylene carbonate and ethylene carbonate, which is applied in the field of preparation of chlorinated ethylene carbonate, can solve problems such as unfavorable enterprises in large-scale production, easy introduction of moisture, long reaction time, etc. Intake, no waste, high molar yield

Inactive Publication Date: 2020-01-17
江苏瀚康新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Chloroethylene carbonate is widely used in the field of raw materials for the production of lithium battery additives. At present, chlorinated ethylene carbonate is prone to moisture in the production process, the reaction time is long, and the recovery rate is not high, which is not conducive to large-scale production of enterprises.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a custom-made glass reaction kettle with circulation pump, thermometer, glove box, vacuum gauge, jet pump, spray head, and condenser, add 2200g of ethylene carbonate to raise the temperature to 75°C, and then add a new type of initiator at this temperature The agent contains 2.25 g of a mixture of 50% benzoyl peroxide and 50% dicyclohexyl phthalate, and feeds chlorine gas at a flow rate of 40 ml / h for 1 hour to cultivate free radicals. After 1 hour, change the chlorine flow rate to 120ml / h, keep the kettle temperature at 85°C, keep it for 5 hours, add 18g of initiator every 20 minutes; change the chlorine flow rate to 60ml / h after 5 hours, and keep the kettle temperature at 85 ℃, maintained for 4 hours, adding 9g of initiator every 20 minutes, hydrogen chloride and chlorine tail gas produced in the reaction process were absorbed with water and lye respectively to generate by-product concentrated hydrochloric acid with a content greater than 30% and sodium hypochlorite...

Embodiment 2

[0018] In a custom-made glass reaction kettle with circulation pump, thermometer, glove box, vacuum gauge, jet pump, spray head, and condenser, add 2205g of ethylene carbonate to raise the temperature to 75°C, and then add a new type of initiator at this temperature The agent contains 2.25 g of a mixture of 50% benzoyl peroxide and 50% dicyclohexyl phthalate, and feeds chlorine gas at a flow rate of 40 ml / h for 1 hour to cultivate free radicals. After 1 hour, change the chlorine flow rate to 120ml / h, keep the kettle temperature at 85°C, keep it for 5 hours, add 18g of initiator every 20 minutes; change the chlorine flow rate to 60ml / h after 5 hours, and keep the kettle temperature at 85 ℃, maintain for 4 hours, add 9g of initiator every 20 minutes; after 4 hours, change the flow rate of chlorine to 50ml / h, control the temperature of the kettle at 85℃, add 7.5g of initiator every 20 minutes, maintain for 2 hours, Hydrogen chloride and chlorine tail gas produced in the reaction ...

Embodiment 3

[0020] In a custom-made glass reaction kettle with circulation pump, thermometer, glove box, vacuum gauge, jet pump, spray head, and condenser, add 2210g of ethylene carbonate to raise the temperature to 75°C, and then add a new type of initiator at this temperature The agent contains 2.25 g of a mixture of 50% benzoyl peroxide and 50% dicyclohexyl phthalate, and feeds chlorine gas at a flow rate of 40 ml / h for 1 hour to cultivate free radicals. After 1 hour, change the chlorine flow rate to 120ml / h, keep the kettle temperature at 85°C, keep it for 5 hours, add 18g of initiator every 20 minutes; change the chlorine flow rate to 60ml / h after 5 hours, and keep the kettle temperature at 85 ℃, maintain for 4 hours, add 9g of initiator every 20 minutes; after 4 hours, change the flow rate of chlorine to 50ml / h, control the temperature of the kettle at 85℃, add 7.5g of initiator every 20 minutes, maintain for 2 hours, Hydrogen chloride and chlorine tail gas produced in the reaction ...

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Abstract

The invention discloses a method of preparing chloroethylene carbonate by adopting a novel initiator. The method comprises the following steps: 1) with ethylene carbonate and chlorine as reaction rawmaterials, controlling the temperature of a kettle to be 80-90 DEG C, taking a mixture of benzoyl peroxide and dicyclohexyl phthalate as a novel initiator, and carrying out a reaction under the actionof the novel initiator to generate chloroethylene carbonate; 2) absorbing hydrogen chloride and chlorine tail gas generated by a chlorination reaction with clear water and alkali liquor respectivelyto generate byproducts including concentrated hydrochloric acid with a content of greater than 30% and sodium hypochlorite with a content of greater than 10%; and 3) transferring a chloroethylene carbonate mixed solution into a deacidification kettle for deacidification treatment by using a transfer pump, controlling the temperature of the deacidification kettle to be 90-105 DEG C, performing vacuumizing while stirring, and carrying out deacidifying for 5 h to obtain chloroethylene carbonate with relatively low moisture and acidity. The preparation method provided by the invention can reduce water introduction, shorten reaction time and improve recovery efficiency, and is suitable for large-scale production in enterprises.

Description

technical field [0001] The invention relates to the field of raw materials for electrolyte additives of lithium ion batteries, in particular to a preparation method of chloroethylene carbonate which can be used as raw materials for electrolyte additives of lithium ion batteries. Background technique [0002] Chloroethylene carbonate is widely used in the field of raw materials for the production of lithium battery additives. At present, chlorinated ethylene carbonate is prone to moisture in the production process, the reaction time is long, and the recovery rate is not high, which is not conducive to large-scale production of enterprises. Contents of the invention [0003] The object of the present invention is to provide a kind of preparation method of the chloroethylene carbonate that adopts novel initiator, to solve the technical problem that proposes in the above-mentioned background technology. [0004] For solving the problems of the technologies described above, the...

Claims

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Application Information

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IPC IPC(8): C07D317/40C01B7/01C01B11/06
CPCC01B7/01C01B11/062C07D317/40
Inventor 朱会文林涛孙西船
Owner 江苏瀚康新材料有限公司
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