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Method for photochemically synthesizing monochloroethylene carbonate and photochemical reactor

A chloroethylene carbonate, photochemical reactor technology, applied in chemical instruments and methods, chemical/physical/physical-chemical processes, chemical/physical/physical-chemical processes of applied energy, etc. problem, to achieve the effect of easy separation and purification, fast reaction speed and high safety factor

Active Publication Date: 2015-11-04
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, experiments have shown that chlorine reacts before ethylene carbonate and tetrachloroethylene under light conditions, and its main product is solid hexachloroethane, so tetrachloroethylene is not suitable as a solvent for photochlorination reactions

Method used

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  • Method for photochemically synthesizing monochloroethylene carbonate and photochemical reactor
  • Method for photochemically synthesizing monochloroethylene carbonate and photochemical reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] See figure 1 In the shown internal immersion upward bubbling photochemical reactor, a clamp made of glass that can filter out light with a wavelength shorter than 300nm is arranged in an internal immersion photoreactor 1 made of high borosilicate glass. A jacketed sinker 2, a high-pressure mercury lamp 3 of 500 watts or 1 kilowatt is installed in the jacketed sinker, and the jacket is provided with an inlet and outlet for cooling water; The bottom of the type photoreactor communicates with a pipeline with a gas-liquid mixing valve 4, a gas inlet 5 is arranged on the pipeline above the gas-liquid mixing valve, and the gas inlet 5 is arranged below the gas-liquid mixing valve. The inlet 6 of the reaction solution is arranged on the pipeline; the outlet 7 of the reaction solution is arranged above the said in-immersion photoreactor.

[0027] The photochemical synthesis of monochloroethylene carbonate is carried out by using the above-mentioned internal immersion upward bu...

Embodiment 2

[0039] The photochemical synthesis of monochloroethylene carbonate was carried out using the internal immersion upward bubbling photochemical reactor of Example 1.

[0040] The solid ethylene carbonate of 176g is directly heated and melted, and the liquid ethylene carbonate is pumped into the described inner immersion upward bubbling photochemical reactor from the inlet of the reaction solution of the inner immersion upward bubbling photochemical reactor In the in-immersion photoreactor, feed nitrogen into the described liquid ethylene carbonate in the in-in-immersion photoreactor from the gas inlet, then open the chlorine valve, with the flow rate of 3g / min, by The gas inlet feeds chlorine gas into the liquid ethylene carbonate in the immersion photoreactor, adjusts the flow of nitrogen to make the bubbling uniform; The 500-watt high-pressure mercury lamp in the jacketed sinker in the liquid ethylene carbonate carries out photochemical chlorination reaction, and the temperatu...

Embodiment 3

[0044] The photochemical synthesis of monochloroethylene carbonate was carried out using the internal immersion upward bubbling photochemical reactor of Example 1.

[0045] The solid ethylene carbonate of 176g is directly heated and melted, and the liquid ethylene carbonate is pumped into the described inner immersion upward bubbling photochemical reactor from the inlet of the reaction solution of the inner immersion upward bubbling photochemical reactor In the in-immersion photoreactor, feed nitrogen into the described liquid ethylene carbonate in the in-in-immersion photoreactor from the gas inlet, then open the chlorine valve, with the flow rate of 4g / min, by The gas inlet feeds chlorine gas into the liquid ethylene carbonate in the immersion photoreactor, adjusts the flow of nitrogen to make the bubbling uniform; The 500-watt high-pressure mercury lamp in the jacketed sinker in the liquid ethylene carbonate carries out photochemical chlorination reaction, and the temperatu...

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Abstract

The invention relates to a method for photochemical synthesis of monochloroethylene carbonate and a photochemical reactor. The invention employs an inner immersion type reactor, which is provided with a chuck type sinking trap, and an inner immersion ascending bubbling type photochemical reactor with high pressure mercury lamp is installed in the chuck type sinking trap for photochemical synthesis of monochloroethylene carbonate; the reaction is under the protection of inert gas, especially traditional reaction solvents with hypertoxicity are removed, and thereby the raw materials ethylene carbonate and chlorine are directly contacted for reaction, and the reaction does not need reaction solvent. The reaction adopts an inner immersion type illumination mode, and ascending and bubbling methods are used for completing the reaction. Monochloroethylene carbonate prepared by the method has high yield which reaches to 90%, and the product is easy to be separated and purified, and the purity reaches more than 98.5%. The method of the present invention does not relate to traditionally used solvents with hypertoxicity, and has the advantages of fast reaction speed, high safety coefficient and low equipment requirement, and the method is good for industrial production of large scale.

Description

technical field [0001] The invention belongs to the technical field of organic photochemical synthesis, and in particular relates to a method for photochemically synthesizing monochloroethylene carbonate by using light energy to initiate free radical reaction, and a photochemical reactor suitable for the method. Background technique [0002] Lithium-ion battery is a green new energy developed in the 1990s. This type of battery has occupied a dominant position in the current battery market due to its high energy density and high cycle performance. High-purity monochloroethylene carbonate is used in the electrolyte of high-power lithium-ion batteries, which can effectively improve the cycle performance of the battery and greatly extend the life of the battery. In addition, vinylene carbonate prepared from monochloroethylene carbonate is currently the most effective organic film-forming additive for lithium-ion batteries. [0003] The synthetic method of monochloroethylene car...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/42B01J19/12
CPCB01J19/127C07D317/42
Inventor 李超王雪松程学新张宝文
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI