Method for preparing high-purity chloro-cyclic carbonates

A cyclic carbonate and chlorinated technology, applied in the field of compound preparation, can solve the problems of lack of high-purity neutral chlorinated cyclic carbonate preparation method, low purity, etc.

Active Publication Date: 2008-06-18
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Abstract
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Problems solved by technology

[0004] But the weak point of above-mentioned method is, all can generate acidic chlorinated cyclic carbonate and other by-products, cause purity to be lower than 90%
[0005] In summary, this area lacks a kind of preparation method that can prepare high-purity neutral chlorinated cyclic carbonate, to avoid the inconvenience that follow-up processing brings

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  • Method for preparing high-purity chloro-cyclic carbonates
  • Method for preparing high-purity chloro-cyclic carbonates
  • Method for preparing high-purity chloro-cyclic carbonates

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preparation example Construction

[0051] The method for preparing high-purity chlorinated cyclic carbonate of the present invention, the method comprises the following steps:

[0052] (a) Provide cyclic carbonate and chlorination reagent raw materials;

[0053] (b) performing a photocatalytic chlorination reaction on the raw materials in step (a) in the presence of specific ultraviolet light to generate chlorinated cyclic carbonates. The specific ultraviolet light refers to the light emitted by the ultraviolet light source with an intensity of 300-2000w and a light wavelength of 300-360nm.

[0054] Further, the above preparation method may optionally include step (c): neutralizing the chlorinated cyclic carbonate obtained in step (b) to obtain a neutral chlorinated cyclic carbonate.

[0055] Each processing condition or parameter of above-mentioned method is described in detail below:

[0056] Cyclic Carbonate Raw Materials

[0057] Cyclic carbonate of the present invention can be ethylene carbonate, propy...

Embodiment 1

[0117] In the quartz bottle that is filled with ethylene carbonate 352g (4mol), maintain the negative pressure in the bottle as -0.02kPa, feed chlorine 4mol bubbling at 50 DEG C and start the ultraviolet light source as shown in Figure 1 (light intensity, 300W; wavelength, 300nm) for 24 hours. Cool and replace by blowing nitrogen gas for 1 hour to obtain 480 g of reaction liquid. Analysis of the components of the reaction liquid by gas chromatography (GC-2014, Shimadzu) revealed that the reaction liquid was 93.18% by weight of 4-chloro-1,3-dioxolan-2-one.

[0118] To the filtrate obtained as above, 240 g of 10% by weight sodium bicarbonate aqueous solution was added dropwise, stirred for 0.5 hour, static, layered, the lower floor neutral filtrate obtained had a pH value of 7, dried over anhydrous magnesium sulfate, and the filtrate obtained by filtration was reduced Pressure rectification, collect 80-120 ℃ / (2-5kPa) fraction 430g, analyze by GC / MS mass spectrometry, m / z: 122, ...

Embodiment 2

[0128] In the quartz bottle filled with ethylene carbonate 352g (4.00mol), maintain the negative pressure in the bottle to be-0.08kPa, feed 16mol chlorine bubbles at 70°C and start the ultraviolet light source as shown in Figure 1 (light intensity, 500w; wavelength, 360nm, water layer thickness 2mm) keep warm for 24 hours. Cool and replace by blowing nitrogen gas for 1 hour to obtain 480 g of reaction liquid. Analysis of the components of the reaction liquid by gas chromatography (GC-2014, Shimadzu) revealed that the reaction liquid was 92.68% by weight of 4-chloro-1,3-dioxolan-2-one.

[0129] To the filtrate obtained above, 960 g of 10% by weight of sodium bicarbonate aqueous solution was added dropwise, stirred for 0.5 hour, static, layered, the obtained lower floor neutral filtrate, the pH value was 7, dried over anhydrous magnesium sulfate, and the filtrate obtained by filtration was carried out Vacuum rectification, 423g of fractions at 80-120°C / 2-5kPa were collected, an...

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Abstract

The invention provides a preparation method of high-purity chloro cyclic carbonate. The method comprises the following procedures, firstly, the cyclic carbonate and the chlorination agent of the raw material is provided, secondly the raw material in the first steps carries out the photocatalysis chlorination reaction at the existence of the certain ultraviolet light with the intensity of 300 to 2000w and the light wave length of 300 to 360nm, and finally the chloro cyclic carbonate is obtained. The preparation method of the invention has the advantages of simple synthesis process, low price and availability of the raw material and high yield, and obtaining the high-purity chloro cyclic carbonate.

Description

technical field [0001] The present invention relates to a preparation method of a compound, more specifically to a method for preparing high-purity neutral chlorinated cyclic carbonate. Background technique [0002] Chlorinated cyclic carbonates are mainly used in the synthesis of vinylene carbonate for lithium battery electrolytes. The high-purity neutral chlorinated cyclic carbonate can be used in the lithium-ion electrolyte of high-power lithium batteries, which can effectively improve its cycle performance and increase its service life. In addition, in practical applications, in some cases, a mixture of chlorinated cyclic carbonate and vinylene carbonate can be used directly. For example, in the case of improving the high-temperature cycle performance of the lithium battery electrolyte, a mixture containing 1-10% by weight of chlorinated cyclic carbonate and 90-99% by weight of vinylene carbonate can be used. [0003] In the existing research on the synthesis of chlori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/34B01J19/12
Inventor 张先林杨志勇刘东汪许诚曹晓东
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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