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Method for continuously preparing vinylene carbonate by tubular reactor

A technology of vinylene carbonate and tubular reactor, which is applied in the field of continuous production of vinylene carbonate by using tubular reactor, which can solve the problems of inability to carry out continuous production, high production environment requirements, and unsuitability for continuous production. , to reduce equipment and production environment requirements, meet continuous production, and prevent polymerization

Active Publication Date: 2015-08-19
RONGCHENG QINGMU CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has a low yield of only 40%, and requires the use of highly toxic chlorine gas and flammable ether with a low boiling point as solvents, which requires high equipment and production environments.
[0006] U.S. Patent No. 3,457,279 discloses a method for preparing vinylene carbonate by direct dehydrogenation of ethylene carbonate under the action of a catalyst, but the reaction temperature of this method needs to be reacted at a high temperature of 300 ° C or above, the yield is low, and the requirements for equipment are high. Not conducive to industrial production
[0007] Chinese patent CN20081223674 discloses a method for synthesizing chloroethylene carbonate at a lower temperature with ethylene carbonate and sulfuryl chloride as raw materials and with azobisisobutyronitrile as an initiator, but the batch operation is adopted and the yield is not high. Too ideal and cumbersome to operate, not suitable for continuous production
[0008] Chinese patent CN201210440209 discloses a method for preparing vinylene carbonate by the direct reaction of chloroethylene carbonate and triethylamine. Although this method avoids the use of solvents and reduces costs, this method requires inert gas protection, and The product is easy to polymerize and cannot be used for continuous production

Method used

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  • Method for continuously preparing vinylene carbonate by tubular reactor
  • Method for continuously preparing vinylene carbonate by tubular reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) After preheating 88.06kg (1000mol) ethylene carbonate to 30~40°C, fully dissolve and mix with 202kg (1500mol) sulfuryl chloride and 880g azobisisobutyronitrile in a mixer, then use a flow rate of 0.05m / s Inject into a horizontal tubular reactor and react at 40-45°C for 100-200 minutes to replace the SO produced by the reaction 2 and HCl are absorbed using a four-stage falling film absorption tower, and the chlorinated products enter the 1.5m 3 The intermediate tank is equipped with an emptying pipe, and the volatilized sulfuryl chloride in the tank is discharged into the main emptying pipe through the emptying pipe, and then pumped into the 6.5m by a vacuum pump. 3 Carry out rectification in the rectification kettle, collect 80 ℃ / 2.66×10 respectively 3 Pa and 106-107℃ / 1.33×10 3 The cut of Pa obtains 100.9 kg of chloroethylene carbonate, the content of chloroethylene carbonate is 96.5%, and the yield is 82%.

[0030] 2) After fully dissolving and mixing 61.3kg (500...

Embodiment 2

[0032] 1) After preheating 88.06kg (1000mol) ethylene carbonate to 30~40℃, fully dissolve and mix with 202kg (1500mol) sulfuryl chloride and 220g benzoyl peroxide in the mixer, inject at a flow rate of 0.05m / s In a horizontal tubular reactor, react at 40~45°C for 200~300 minutes to replace the SO produced by the reaction 2 and HCl are absorbed using a four-stage falling film absorption tower, and the chlorinated products enter the 1.5m 3 The intermediate tank is equipped with an emptying pipe, and the volatilized sulfuryl chloride in the tank is discharged into the main emptying pipe through the emptying pipe, and then pumped into the 6.5m by a vacuum pump. 3 Carry out rectification in the rectification kettle, collect 80 ℃ / 2.66×10 respectively 3 Pa and 106-107℃ / 1.33×103 The cut of Pa obtains 88kg of chloroethylene carbonate, the content of chloroethylene carbonate is 94.5%, and the yield is 71.5%.

[0033] 2) After fully dissolving and mixing 61.3kg (500mol) chloroethylene ...

Embodiment 3

[0035] 1) After preheating 88.06kg (1000mol) ethylene carbonate to 30~40°C, fully dissolve and mix with 202kg (2500mol) sulfuryl chloride and 440g benzoyl peroxide in the mixer, inject at a flow rate of 0.1m / s In a horizontal tubular reactor, react at 50~55°C for 200~300 minutes to replace the SO produced by the reaction 2 and HCl are absorbed using a four-stage falling film absorption tower, and the chlorinated products enter the 1.5m 3 The intermediate tank is equipped with an emptying pipe, and the volatilized sulfuryl chloride in the tank is discharged into the main emptying pipe through the emptying pipe, and then pumped into the 6.5m by a vacuum pump. 3 Carry out rectification in the rectification kettle, collect 80 ℃ / 2.66×10 respectively 3 Pa and 106-107℃ / 1.33×10 3 The cut of Pa obtains 107kg of chloroethylene carbonate, the content of chloroethylene carbonate is 97.5%, and the yield is 87.3%.

[0036] 2) After fully dissolving and mixing 61.3kg (500mol) chloroethyle...

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Abstract

The invention provides a method for continuously preparing vinylene carbonate by a tubular reactor. The method includes using chlorosulfuric acid and ethylene carbonate as raw materials to be synthesized into chloroethylene carbonate in the tubular reactor under the action of initiator, rectifying the chloroethylene carbonate and subjecting the rectified chloroethylene carbonate to elimination reaction with trimethylamine in the tubular reactor with existence of organic solvent and generating the vinylene carbonate. By the method for continuously preparing vinylene carbonate by the tubular reactor, existing intermittent production methods are changed, reaction speed is greatly increased, reaction period is reduced, yield is increased and productivity can be effectively improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a method for continuously preparing vinylene carbonate using a tubular reactor. Background technique [0002] Vinylene carbonate (VC) is a colorless liquid with a melting point of 19~22°C and is a very important additive for lithium battery electrolyte. After vinylene carbonate is added to the electrolyte, it can undergo free radical polymerization reaction with the surface material of carbon negative electrode, and then generate polyalkyl carbonate compounds, thereby effectively inhibiting the co-intercalation reaction of solvent molecules, and can effectively increase the lithium ion density. The charge and discharge efficiency and cycle characteristics of the secondary battery can be improved, and various performances such as the storage resistance of the battery can be improved. [0003] The method for preparing vinylene carbonate mainly contains ...

Claims

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Application Information

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IPC IPC(8): C07D317/40
CPCC07D317/40
Inventor 刘晓波李维平孙朋波刘学松宋丽丽孙燕超李晓明
Owner RONGCHENG QINGMU CHEM MATERIALS
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