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Dehydration crystallization method of vinylene carbonate

A vinylene carbonate and water agent technology, applied in the direction of organic chemistry, etc., can solve the problems of unfavorable enterprises in energy saving and emission reduction, easy polymerization and coking, and high water residue, and achieves the advantages of avoiding polymerization and coking, good repeatability and easy operation. Effect

Active Publication Date: 2021-11-12
ZHUHAI LEE & MAN MATERIALS SCI CO LTD
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method has the following disadvantages: the first is that vinylene carbonate is easy to polymerize and coke under heating, the loss of raw materials is large, and the efficiency is not high
The second is that vinylene carbonate itself has a high boiling point, which leads to a corresponding large energy consumption in the distillation method, which is not conducive to the energy saving and emission reduction of enterprises.
The third is that the residual moisture in the product is still relatively high

Method used

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  • Dehydration crystallization method of vinylene carbonate

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Experimental program
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Effect test

Embodiment 1

[0022] In a 200L reactor, add 180kg of crude vinylene carbonate with a purity of 95%, and then add activated Molecular sieve 36kg was soaked to remove water, and the Karl Fischer water measurement method was used for online monitoring and water content measurement. When the water content is less than or equal to 50ppm, the vinylene carbonate is sent to a centrifuge for centrifugation, and the obtained centrifuged liquid is sent to a filter for filtration. The obtained clear liquid is sent to the temperature-controllable crystallization tank. Start the stirring system, the stirring rate is 250rpm, the temperature control system is set to drop from the initial 30°C to the end point 12°C, and the temperature drop time is set to 4 hours. After the crystallization process is completed, the crystals are transported to a three-in-one filter (filtering, washing, air blowing) for filtration treatment at 15°C, and the filtration accuracy is 300 mesh. The obtained crystals are blown...

Embodiment 2

[0024] The operation of this embodiment is basically the same as that of Embodiment 1, the difference is that the solid dewatering agent of this embodiment is Molecular sieve. Present embodiment obtains product and finally weighs 154kg. Yield: 85.6%. The liquid was taken for analysis, and the GC-MS purity was 99.73%. Trace detection results: ICP-OES (ppm): Na + =7.363ppm, Fe 2+ = 0.189ppm, Ca 2+ = 2.629ppm; Mg 2+ = 0.018ppm; IC: Cl － =14.91ppm, NO 3 － =3.28ppm, SO 4 2- =6.19ppm, PO 4 3- = 0.87ppm. KF: H 2 O=5.92ppm.

Embodiment 3

[0026] In a 200L reactor, add 150kg of vinylene carbonate crude product, then add 15kg of calcium hydride to carry out stirring reaction to remove water, and the stirring speed of the stirring blade is set to 350rpm. The Karl Fischer water measurement method is used for online monitoring and water content measurement. When the water content is less than or equal to 50ppm, stop stirring, let stand for 2 hours and wait for the solid-liquid layering, then transport the supernatant vinylene carbonate to a centrifuge for centrifugation, and then transport the obtained centrifuged liquid to a filter for filtration. The obtained clear liquid is sent to the temperature-controllable crystallization tank. Start the stirring system, the stirring rate is 250rpm, the temperature control system is set to drop from the initial 30°C to the end point 10°C, and the temperature drop time is set to 6 hours. After the crystallization process is completed, the crystals are transported to a three-i...

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Abstract

The invention discloses a dehydration crystallization method of vinylene carbonate. The method comprises the following steps: removing water by using a solid water removal agent before crystallization until the water content is less than or equal to 50ppm, then gradually conducting cooling and dynamical crystallizing while stirring, so as to achieve the effects of stable crystallization rate and more uniform dispersed crystallized crystals, and then conducting filtering at a low temperature to obtain vinylene carbonate crystals. The operation is simple and convenient, the repeatability is good, the crystal diameter is uniform, the product quality is improved, and the method is suitable for industrial production, heating in the whole process of water removal and crystallization is not adopted, polymerization of vinylene carbonate due to heating is avoided, and the problems of large energy consumption, low efficiency and high moisture content in a traditional heating distillation method are solved.

Description

Technical field: [0001] The invention relates to the technical field of crystallization, in particular to a dehydration crystallization method of vinylene carbonate. Background technique: [0002] Vinylene carbonate (VC for short), as a lithium battery electrolyte additive, has good high and low temperature performance and anti-flat function, it can increase the stability of the electrolyte, effectively inhibit the decomposition of the electrolyte, and at the same time It can promote the formation of SEI film and improve the cycle performance of the battery. Vinylene carbonate can also be used in the polymer industry and can be polymerized to obtain polyvinylene carbonate. Vinylene carbonate can also be used as a chemical raw material to react with most diene compounds, and it also has a good application prospect in the field of organic synthesis. In order to obtain higher purity vinylene carbonate, the industry usually adopts rectification method for purification. But th...

Claims

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Application Information

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IPC IPC(8): C07D317/40
CPCC07D317/40Y02E60/10
Inventor 谢文健梁海波辛伟贤陈新滋
Owner ZHUHAI LEE & MAN MATERIALS SCI CO LTD
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